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

ERIC Educational Resources Information Center

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

2004-01-01

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

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.

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.

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.

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.

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.

Flow injection analysis-flame atomic absorption spectrometry system for indirect determination of sulfite after on-line reduction of solid-phase manganese (IV) dioxide reactor.

PubMed

Zare-Dorabei, Rouholah; Boroun, Shokoufeh; Noroozifar, Meissam

2018-02-01

A new and simple flow injection method followed by atomic absorption spectrometry was developed for indirect determination of sulfite. The proposed method is based on the oxidation of sulfite to sulphate ion using solid-phase manganese dioxide (30% W/W suspended on silica gel beads) reactor. MnO 2 will be reduced to Mn(II) by sample injection in to the column under acidic carrier stream of HNO 3 (pH 2) with flow rate of 3.5mLmin -1 at room temperature. Absorption measurement of Mn(II) which is proportional to the concentration of sulfite in the sample was carried out by atomic absorption spectrometry. The calibration curve was linear up to 25mgL -1 with a detection limit (DL) of 0.08mgL -1 for 400µL injection sample volume. The presented method is efficient toward sulfite determination in sugar and water samples with a relative standard deviation (RSD) less than 1.2% and a sampling rate of about 60h -1 . Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of palladium and platinum by atomic absorption

USGS Publications Warehouse

Schnepfe, M.M.; Grimaldi, F.S.

1969-01-01

Palladium and platinum are determined by atomic absorption after fire-assay concentration into a gold bead. The limit of determination is ~0??06 ppm in a 20-g sample. Serious depressive interelement interferences are removed by buffering the solutions with a mixture of cadmium and copper sulphates with cadmium and copper concentrations each at 0??5%. Substantial amounts of Ag, Al, Au, Bi, Ca, Co, Cr, Fe, Hg, K, La, Mg, Mn, Mo, Na, Ni, Pb, Te, Ti, V, Y, Zn, and the platinum metals do not interfere in the atomic-absorption determination. ?? 1969.

Anomalous small-angle scattering as a way to solve the Babinet principle problem

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

Boiko, M. E., E-mail: m.e.boiko@mail.ioffe.ru; Sharkov, M. D.; Boiko, A. M.

2013-12-15

X-ray absorption spectra (XAS) have been used to determine the absorption edges of atoms present in a sample under study. A series of small-angle X-ray scattering (SAXS) measurements using different monochromatic X-ray beams at different wavelengths near the absorption edges is performed to solve the Babinet principle problem. The sizes of clusters containing atoms determined by the method of XAS were defined in SAXS experiments. In contrast to differential X-ray porosimetry, anomalous SAXS makes it possible to determine sizes of clusters of different atomic compositions.

Anomalous small-angle scattering as a way to solve the Babinet principle problem

NASA Astrophysics Data System (ADS)

Boiko, M. E.; Sharkov, M. D.; Boiko, A. M.; Bobyl, A. V.

2013-12-01

X-ray absorption spectra (XAS) have been used to determine the absorption edges of atoms present in a sample under study. A series of small-angle X-ray scattering (SAXS) measurements using different monochromatic X-ray beams at different wavelengths near the absorption edges is performed to solve the Babinet principle problem. The sizes of clusters containing atoms determined by the method of XAS were defined in SAXS experiments. In contrast to differential X-ray porosimetry, anomalous SAXS makes it possible to determine sizes of clusters of different atomic compositions.

Determination of Cd in urine by cloud point extraction-tungsten coil atomic absorption spectrometry.

PubMed

Donati, George L; Pharr, Kathryn E; Calloway, Clifton P; Nóbrega, Joaquim A; Jones, Bradley T

2008-09-15

Cadmium concentrations in human urine are typically at or below the 1 microgL(-1) level, so only a handful of techniques may be appropriate for this application. These include sophisticated methods such as graphite furnace atomic absorption spectrometry and inductively coupled plasma mass spectrometry. While tungsten coil atomic absorption spectrometry is a simpler and less expensive technique, its practical detection limits often prohibit the detection of Cd in normal urine samples. In addition, the nature of the urine matrix often necessitates accurate background correction techniques, which would add expense and complexity to the tungsten coil instrument. This manuscript describes a cloud point extraction method that reduces matrix interference while preconcentrating Cd by a factor of 15. Ammonium pyrrolidinedithiocarbamate and Triton X-114 are used as complexing agent and surfactant, respectively, in the extraction procedure. Triton X-114 forms an extractant coacervate surfactant-rich phase that is denser than water, so the aqueous supernatant is easily removed leaving the metal-containing surfactant layer intact. A 25 microL aliquot of this preconcentrated sample is placed directly onto the tungsten coil for analysis. The cloud point extraction procedure allows for simple background correction based either on the measurement of absorption at a nearby wavelength, or measurement of absorption at a time in the atomization step immediately prior to the onset of the Cd signal. Seven human urine samples are analyzed by this technique and the results are compared to those found by the inductively coupled plasma mass spectrometry analysis of the same samples performed at a different institution. The limit of detection for Cd in urine is 5 ngL(-1) for cloud point extraction tungsten coil atomic absorption spectrometry. The accuracy of the method is determined with a standard reference material (toxic metals in freeze-dried urine) and the determined values agree with the reported levels at the 95% confidence level.

On-line ion-exchange preconcentration and determination of traces of platinum by electrothermal atomic absorption spectrometry.

PubMed

González García, M M; Sánchez Rojas, F; Bosch Ojeda, C; García de Torres, A; Cano Pavón, J M

2003-04-01

A method to determine trace amounts of platinum in different samples based on electrothermal atomic absorption spectrometry is described. The preconcentration step is performed on a chelating resin microcolumn [1,5-bis(2-pyridyl)-3-sulfophenyl methylene thiocarbonohydrazide (PSTH) immobilized on an anion-exchange resin (Dowex 1x8-200)] placed in the autosampler arm. The combination of a peristaltic pump for sample loading and the atomic absorption spectrometer pumps for elution through a selection valve simplifies the hardware. The peristaltic pump and the selection valve are easily controlled electronically with two switches placed in the autosampler, which are activated when the autosampler arm is down. Thus, the process is fully automated without any modification of the software of the atomic absorption spectrometer. Under the optimum conditions with a 60-s preconcentration time, a sample flow rate of 2.4 mL min(-1), and an injection volume of eluent of 40 microL, a linear calibration graph was obtained in the range 0-100 ng mL(-1). The enrichment factor was 14. The detection limit under these conditions is 1 ng mL(-1), and the relative standard deviation (RSD) is 1.6% for 10 ng mL(-1) of Pt. The method has been applied to the determination of platinum in catalyst, vegetation, soil, and natural water samples. The results showed good agreement with the certified value and the recoveries of Pt added to samples were 98-105%.

Procedure for rapid determination of nickel, cobalt, and chromium in airborne particulate samples

NASA Technical Reports Server (NTRS)

Davis, W. F.; Graab, J. W.

1972-01-01

A rapid, selective procedure for the determination of 1 to 20 micrograms of nickel, chromium, and cobalt in airborne particulates is described. The method utilizes the combined techniques of low temperature ashing and atomic absorption spectroscopy. The airborne particulates are collected on analytical filter paper. The filter papers are ashed, and the residues are dissolved in hydrochloric acid. Nickel, chromium, and cobalt are determined directly with good precision and accuracy by means of atomic absorption. The effects of flame type, burner height, slit width, and lamp current on the atomic absorption measurements are reported.

Major and trace element concentrations in samples from 72275 and 72255. [chemical composition of lunar rocks

NASA Technical Reports Server (NTRS)

Haskin, L. A.; Blanchard, D. P.; Korotev, R.; Jacobs, J. W.; Brannon, J. A.; Herrmann, A. G.

1974-01-01

Analytical data have been obtained for Co, Sc, Hf, Zn, Cr, Ga, Rb, Cs, Ni, major elements, and rare earth elements in eight samples from boulder 1. The data for trace elements were obtained by radiochemical neutron activation analysis. Major elements, except Na and Mn, were obtained by atomic absorption spectral photometry. Values for Na and Mn were obtained by neutron activation analysis of the same powder that was later dissolved to provide the atomic absorption analyses.

Determination of silver in irons and steels by atomic-absorption spectrometry with an induction furnace: Direct analysis of solid samples.

PubMed

Aziz-Alrahman, A M; Headridge, J B

1978-07-01

The silver contents of 17 irons and steels have been determined by dropping 0.5-20mg of millings or turnings of the metals into an induction furnace situated within an atomic-absorption spectrophotometer. The limit of detection was 0.005 mug/g and the relative standard deviations were 12% or better for silver contents of not less than 0.05 mug/g. Samples are added to the furnace at 4-5 min intervals.

Fluorescence detection of white-beam X-ray absorption anisotropy: towards element-sensitive projections of local atomic structure

PubMed Central

Korecki, P.; Tolkiehn, M.; Dąbrowski, K. M.; Novikov, D. V.

2011-01-01

Projections of the atomic structure around Nb atoms in a LiNbO3 single crystal were obtained from a white-beam X-ray absorption anisotropy (XAA) pattern detected using Nb K fluorescence. This kind of anisotropy results from the interference of X-rays inside a sample and, owing to the short coherence length of a white beam, is visible only at small angles around interatomic directions. Consequently, the main features of the recorded XAA corresponded to distorted real-space projections of dense-packed atomic planes and atomic rows. A quantitative analysis of XAA was carried out using a wavelet transform and allowed well resolved projections of Nb atoms to be obtained up to distances of 10 Å. The signal of nearest O atoms was detected indirectly by a comparison with model calculations. The measurement of white-beam XAA using characteristic radiation indicates the possibility of obtaining element-sensitive projections of the local atomic structure in more complex samples. PMID:21997909

Super-resolution atomic force photoactivated microscopy of biological samples (Conference Presentation)

NASA Astrophysics Data System (ADS)

Lee, Seunghyun; Kim, Hyemin; Shin, Seungjun; Doh, Junsang; Kim, Chulhong

2017-03-01

Optical microscopy (OM) and photoacoustic microscopy (PAM) have previously been used to image the optical absorption of intercellular features of biological cells. However, the optical diffraction limit ( 200 nm) makes it difficult for these modalities to image nanoscale inner cell structures and the distribution of internal cell components. Although super-resolution fluorescence microscopy, such as stimulated emission depletion microscopy (STED) and stochastic optical reconstruction microscopy (STORM), has successfully performed nanoscale biological imaging, these modalities require the use of exogenous fluorescence agents, which are unfavorable for biological samples. Our newly developed atomic force photoactivated microscopy (AFPM) can provide optical absorption images with nanoscale lateral resolution without any exogenous contrast agents. AFPM combines conventional atomic force microscopy (AFM) and an optical excitation system, and simultaneously provides multiple contrasts, such as the topography and magnitude of optical absorption. AFPM can detect the intrinsic optical absorption of samples with 8 nm lateral resolution, easily overcoming the diffraction limit. Using the label-free AFPM system, we have successfully imaged the optical absorption properties of a single melanoma cell (B16F10) and a rosette leaf epidermal cell of Arabidopsis (ecotype Columbia (Col-0)) with nanoscale lateral resolution. The remarkable images show the melanosome distribution of a melanoma cell and the biological structures of a plant cell. AFPM provides superior imaging of optical absorption with a nanoscale lateral resolution, and it promises to become widely used in biological and chemical research.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of chromium in water by graphite furnace atomic absorption spectrophotometry

USGS Publications Warehouse

McLain, B.J.

1993-01-01

Graphite furnace atomic absorption spectrophotometry is a sensitive, precise, and accurate method for the determination of chromium in natural water samples. The detection limit for this analytical method is 0.4 microg/L with a working linear limit of 25.0 microg/L. The precision at the detection limit ranges from 20 to 57 percent relative standard deviation (RSD) with an improvement to 4.6 percent RSD for concentrations more than 3 microg/L. Accuracy of this method was determined for a variety of reference standards that was representative of the analytical range. The results were within the established standard deviations. Samples were spiked with known concentrations of chromium with recoveries ranging from 84 to 122 percent. In addition, a comparison of data between graphite furnace atomic absorption spectrophotometry and direct-current plasma atomic emission spectrometry resulted in suitable agreement between the two methods, with an average deviation of +/- 2.0 microg/L throughout the analytical range.

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

PubMed

Issa, M M; Nejem, R M; El-Abadla, N S; Al-Kholy, M; Saleh, Akila A

2008-01-01

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

Novel Atomic Absorption Spectrometric and Rapid Spectrophotometric Methods for the Quantitation of Paracetamol in Saliva: Application to Pharmacokinetic Studies

PubMed Central

Issa, M. M.; Nejem, R. M.; El-Abadla, N. S.; Al-Kholy, M.; Saleh, Akila. A.

2008-01-01

A novel atomic absorption spectrometric method and two highly sensitive spectrophotometric methods were developed for the determination of paracetamol. These techniques based on the oxidation of paracetamol by iron (III) (method I); oxidation of p-aminophenol after the hydrolysis of paracetamol (method II). Iron (II) then reacts with potassium ferricyanide to form Prussian blue color with a maximum absorbance at 700 nm. The atomic absorption method was accomplished by extracting the excess iron (III) in method II and aspirates the aqueous layer into air-acetylene flame to measure the absorbance of iron (II) at 302.1 nm. The reactions have been spectrometrically evaluated to attain optimum experimental conditions. Linear responses were exhibited over the ranges 1.0-10, 0.2-2.0 and 0.1-1.0 μg/ml for method I, method II and atomic absorption spectrometric method, respectively. A high sensitivity is recorded for the proposed methods I and II and atomic absorption spectrometric method value indicate: 0.05, 0.022 and 0.012 μg/ml, respectively. The limit of quantitation of paracetamol by method II and atomic absorption spectrometric method were 0.20 and 0.10 μg/ml. Method II and the atomic absorption spectrometric method were applied to demonstrate a pharmacokinetic study by means of salivary samples in normal volunteers who received 1.0 g paracetamol. Intra and inter-day precision did not exceed 6.9%. PMID:20046743

Determination of cadmium in urine by extraction and flameless atomic-absorption spectrophotometry Comparison of urine from smokers and non-smokers of different sex and age.

PubMed

Jawaid, M; Lind, B; Elinder, C G

1983-07-01

A method is presented for determining cadmium in urine by nameless atomic-absorption spectrophotometry after extraction. The sample is dried, ashed in the presence of nitric acid, and then the residue is dissolved in hydrochloric acid. Cadmium is extracted as its tetrahexylammonium iodide complex into methyl isobutyl ketone. The organic phase is analysed for cadmium by atomic-absorption spectrophotometry with electrothermal atomization. The median urinary excretion of cadmium for smokers aged 50-64 has been found to be 0.7 and 0.75 mug l . for males and females respectively, the values for non-smokers being 0.25 and 0.4mug l .

Determination of ruthenium in pharmaceutical compounds by graphite furnace atomic absorption spectroscopy.

PubMed

Jia, Xiujuan; Wang, Tiebang; Bu, Xiaodong; Tu, Qiang; Spencer, Sandra

2006-04-11

A graphite furnace atomic absorption (GFAA) spectrometric method for the determination of ruthenium (Rh) in solid and liquid pharmaceutical compounds has been developed. Samples are dissolved or diluted in dimethyl sulfoxide (DMSO) without any other treatment before they were analyzed by GFAA with a carefully designed heating program to avoid pre-atomization signal loss and to achieve suitable sensitivity. Various inorganic and organic solvents were tested and compared and DMSO was found to be the most suitable. In addition, ruthenium was found to be stable in DMSO for at least 5 days. Spike recoveries ranged from 81 to 100% and the limit of quantitation (LOQ) was determined to be 0.5 microg g(-1) for solid samples or 0.005 microg ml(-1) for liquid samples based a 100-fold dilution. The same set of samples was also analyzed by ICP-MS with a different sample preparation method, and excellent agreement was achieved.

Atomic-absorption determination of rhodium in chromite concentrates

USGS Publications Warehouse

Schnepfe, M.M.; Grimaldi, F.S.

1969-01-01

Rhodium is determined in chromite concentrates by atomic absorption after concentration either by co-precipitation with tellurium formed by the reduction of tellurite with tin(II) chloride or by fire assay into a gold bead. Interelement interferences in the atomic-absorption determination are removed by buffering the solutions with lanthanum sulphate (lanthanum concentration 1%). Substantial amounts of Ag, Al, Au, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ho, Hg, K, La, Mg, Mn, Mo, Na, Ni, Pb, Te, Ti, V, Y, Zn and platinum metals can be tolerated. A lower limit of approximately 0.07 ppm Rh can be determined in a 3-g sample. ?? 1969.

Evaluation of Thermal Control Coatings and Polymeric Materials Exposed to Ground Simulated Atomic Oxygen and Vacuum Ultraviolet Radiation

NASA Technical Reports Server (NTRS)

Kamenetzky, R. R.; Vaughn, J. A.; Finckenor, M. M.; Linton, R. C.

1995-01-01

Numerous thermal control and polymeric samples with potential International Space Station applications were evaluated for atomic oxygen and vacuum ultraviolet radiation effects in the Princeton Plasma Physics Laboratory 5 eV Neutral Atomic Oxygen Facility and in the MSFC Atomic Oxygen Drift Tube System. Included in this study were samples of various anodized aluminum samples, ceramic paints, polymeric materials, and beta cloth, a Teflon-impregnated fiberglass cloth. Aluminum anodizations tested were black duranodic, chromic acid anodize, and sulfuric acid anodize. Paint samples consisted of an inorganic glassy black paint and Z-93 white paint made with the original PS7 binder and the new K2130 binder. Polymeric samples evaluated included bulk Halar, bulk PEEK, and silverized FEP Teflon. Aluminized and nonaluminized Chemfab 250 beta cloth were also exposed. Samples were evaluated for changes in mass, thickness, solar absorptance, and infrared emittance. In addition to material effects, an investigation was made comparing diffuse reflectance/solar absorptance measurements made using a Beckman DK2 spectroreflectometer and like measurements made using an AZ Technology-developed laboratory portable spectroreflectometer.

Infrared reduction, an efficient method to control the non-linear optical property of graphene oxide in femtosecond regime

NASA Astrophysics Data System (ADS)

Bhattacharya, S.; Maiti, R.; Saha, S.; Das, A. C.; Mondal, S.; Ray, S. K.; Bhaktha, S. B. N.; Datta, P. K.

2016-04-01

Graphene Oxide (GO) has been prepared by modified Hummers method and it has been reduced using an IR bulb (800-2000 nm). Both as grown GO and reduced graphene oxide (RGO) have been characterized using Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). Raman spectra shows well documented Dband and G-band for both the samples while blue shift of G-band confirms chemical functionalization of graphene with different oxygen functional group. The XPS result shows that the as-prepared GO contains 52% of sp2 hybridized carbon due to the C=C bonds and 33% of carbon atoms due to the C-O bonds. As for RGO, increment of the atomic % of the sp2 hybridized carbon atom to 83% and rapid decrease in atomic % of C=O bonds confirm an efficient reduction with infrared radiation. UV-Visible absorption spectrum also confirms increment of conjugation with increased reduction. Non-linear optical properties of both GO and RGO are measured using single beam open aperture Z-Scan technique in femtosecond regime. Intensity dependent nonlinear phenomena are observed. Depending upon the intensity, both saturable absorption and two photon absorption contribute to the non-linearity of both the samples. Saturation dominates at low intensity (~ 127 GW/cm2) while two photon absorption become prominent at higher intensities (from 217 GW/cm2 to 302 GW/cm2). We have calculated the two-photon absorption co-efficient and saturation intensity for both the samples. The value of two photon absorption co-efficient (for GO~ 0.0022-0.0037 cm/GW and for RGO~ 0.0128-0.0143 cm/GW) and the saturation intensity (for GO~57 GW/cm2 and for RGO~ 194GW/cm2) is increased with reduction. Increase in two photon absorption coefficient with increasing intensity can also suggest that there may be multi-photon absorption is taking place.

Measurements of sulfur compounds in CO 2 by diode laser atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Franzke, J.; Stancu, D. G.; Niemax, K.

2003-07-01

Two simple methods for the analysis of the total concentration of sulfur in CO 2 by diode laser atomic absorption spectrometry of excited, metastable sulfur atoms in a direct current discharge are presented. In the first method, the CO 2 sample gas is mixed with the plasma gas (Ar or He) while the second is based on reproducible measurements of the sulfur released from the walls in a helium discharge after being deposited as a result of operating the discharge in pure CO 2 sample gas. The detection limits obtained satisfy the requirements for the control of sulfur compounds in CO 2 used in the food and beverage industry.

Direct sampling graphite furnace atomic absorption spectrometry - feasibility of Na and K determination in desalted crude oil

NASA Astrophysics Data System (ADS)

Seeger, Tassia S.; Machado, Eduarda Q.; Flores, Erico M. M.; Mello, Paola A.; Duarte, Fabio A.

2018-03-01

In this study, Na and K were determined in desalted crude oil by direct sampling graphite furnace atomic absorption spectrometry (DS-GF AAS), with the use of a Zeeman-effect background correction system with variable magnetic field. The analysis was performed in low and high sensitivity conditions. Sodium determination was performed in two low-sensitivity conditions: 1) main absorption line (589.0 nm), gas stop flow during the atomization step and 3-field dynamic mode (0.6-0.8 T); and 2) secondary absorption line (330.3 nm), gas stop flow during the atomization and 2-field mode (0.8 T). In K determination, some parameters, such as high-sensitivity mode, main absorption line (766.5 nm), gas stop flow during the atomization and 2-field mode (0.8 T), were used. Suitability of chemical modifiers, such as Pd and W-Ir was also evaluated. The heating program for Na and K was based on the pyrolysis and atomization curves. Calibration was performed by aqueous standards. Accuracy was evaluated by the analysis of Green Petroleum Coke (SRM NIST 2718) and Trace Elements in Fuel Oil (SRM NIST 1634c). Recovery tests were also performed and results were compared with those obtained by GF AAS after crude oil digestion by microwave-assisted digestion. The characteristic mass of Na was 17.1 pg and 0.46 ng in conditions 1 and 2, respectively, while the one of K was 1.4 pg. Limits of detection and quantification by DS-GF AAS were 30 and 40 ng g-1 for Na and 3.2 and 4.2 ng g-1 for K, respectively. Sodium and K were determined in three crude oil samples with API density ranging from 20.9 to 28.0. Sodium and K concentration ranged from 1.5 to 73 μg g-1 and from 23 to 522 ng g-1, respectively.

Solid-phase extraction and separation procedure for trace aluminum in water samples and its determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS).

PubMed

Ciftci, Harun; Er, Cigdem

2013-03-01

In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L(-1) HNO(3) and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L(-1) and 3.91 μg L(-1), respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples.

Improved graphite furnace atomizer

DOEpatents

Siemer, D.D.

1983-05-18

A graphite furnace atomizer for use in graphite furnace atomic absorption spectroscopy is described wherein the heating elements are affixed near the optical path and away from the point of sample deposition, so that when the sample is volatilized the spectroscopic temperature at the optical path is at least that of the volatilization temperature, whereby analyteconcomitant complex formation is advantageously reduced. The atomizer may be elongated along its axis to increase the distance between the optical path and the sample deposition point. Also, the atomizer may be elongated along the axis of the optical path, whereby its analytical sensitivity is greatly increased.

An atomic-absorption method for the determination of gold in large samples of geologic materials

USGS Publications Warehouse

VanSickle, Gordon H.; Lakin, Hubert William

1968-01-01

A laboratory method for the determination of gold in large (100-gram) samples has been developed for use in the study of the gold content of placer deposits and of trace amounts of gold in other geologic materials. In this method the sample is digested with bromine and ethyl ether, the gold is extracted into methyl isobutyl ketone, and the determination is made by atomicabsorption spectrophotometry. The lower limit of detection is 0.005 part per million in the sample. The few data obtained so far by this method agree favorably with those obtained by assay and by other atomic-absorption methods. About 25 determinations can be made per man-day.

Correlation between Wavelength Dispersive X-ray Fluorescence (WDXRF) analysis of hardened concrete for chlorides vs. Atomic Absorption (AA) analysis in accordance with AASHTO T- 260; sampling and testing for chloride ion in concrete and concrete raw mater

DOT National Transportation Integrated Search

2014-04-01

A correlation between Wavelength Dispersive X-ray Fluorescence(WDXRF) analysis of Hardened : Concrete for Chlorides and Atomic Absorption (AA) analysis (current method AASHTO T-260, procedure B) has been : found and a new method of analysis has been ...

Determination of Fe Content of Some Food Items by Flame Atomic Absorption Spectroscopy (FAAS): A Guided-Inquiry Learning Experience in Instrumental Analysis Laboratory

ERIC Educational Resources Information Center

Fakayode, Sayo O.; King, Angela G.; Yakubu, Mamudu; Mohammed, Abdul K.; Pollard, David A.

2012-01-01

This article presents a guided-inquiry (GI) hands-on determination of Fe in food samples including plantains, spinach, lima beans, oatmeal, Frosted Flakes cereal (generic), tilapia fish, and chicken using flame atomic absorption spectroscopy (FAAS). The utility of the GI experiment, which is part of an instrumental analysis laboratory course,…

Micro determination of plasma and erythrocyte copper by atomic absorption spectrophotometry

PubMed Central

Blomfield, Jeanette; Macmahon, R. A.

1969-01-01

The free and total plasma copper and total erythrocyte copper levels have been determined by simple, yet sensitive and highly specific methods, using atomic absorption spectrophotometry. For total copper determination, the copper was split from its protein combination in plasma or red cells by the action of hydrochloric acid at room temperature. The liberated copper was chelated by ammonium pyrrolidine dithiocarbamate and extracted into n-butyl acetate by shaking and the organic extract was aspirated into the atomic absorption spectrophotometer flame. The entire procedure was carried out in polypropylene centrifuge tubes, capped during shaking. For the free plasma copper measurement the hydrochloric acid step was omitted. Removal of the plasma or erythrocyte proteins was found to be unnecessary, and, in addition, the presence of trichloracetic acid caused an appreciable lowering of absorption. Using a double-beam atomic absorption spectrophotometer and scale expansion × 10, micro methods have been derived for determining the total copper of plasma or erythrocytes with 0·1 ml of sample, and the free copper of plasma with 0·5 ml. The macro plasma copper method requires 2 ml of plasma and is suitable for use with single-beam atomic absorption spectrophotometers. With blood from 50 blood donors, normal ranges of plasma and erythrocyte copper have been determined. PMID:5776543

Formation of nanostructures in Eu3+ doped glass-ceramics: an XAS study.

PubMed

Pellicer-Porres, J; Segura, A; Martínez-Criado, G; Rodríguez-Mendoza, U R; Lavín, V

2013-01-16

We describe the results of x-ray absorption experiments carried out to deduce structural and chemical information in Eu(3+) doped, transparent, oxyfluoride glass and nanostructured glass-ceramic samples. The spectra were measured at the Pb and Eu-L(III) edges. The Eu environment in the glass samples is observed to be similar to that of EuF(3). Complementary x-ray diffraction experiments show that thermal annealing creates β-PbF(2) type nanocrystals. X-ray absorption indicates that Eu ions act as seeds in the nanocrystal formation. There is evidence of interstitial fluorine atoms around Eu ions as well as Eu dimers. X-ray absorption at the Pb-L(III) edge shows that after the thermal treatment most lead atoms form a PbO amorphous phase and that only 10% of the lead atoms remain available to form β-PbF(2) type nanocrystals. Both x-ray diffraction and absorption point to a high Eu content in the nanocrystals. Our study suggests new approaches to the oxyfluoride glass-ceramic synthesis in order to further improve their properties.

Determination of lead in flour samples directly by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Tinas, Hande; Ozbek, Nil; Akman, Suleyman

2018-02-01

In this study, lead concentrations in various flour samples were determined by high-resolution continuum source graphite furnace atomic absorption spectrometry with solid sampling. Since samples were analyzed directly, the risks and disadvantages of sample digestion were eliminated. Solid flour samples were dried, weighed on the platforms, Pd was added as a modifier and introduced directly into a graphite tube using a manual solid sampler. Platforms and tubes were coated with Zr. The optimized pyrolysis and atomization temperatures were 800 °C and 2200 °C, respectively. The sensitivities of lead in various flour certified reference materials (CRMs) and aqueous standards were not significantly different. Therefore, aqueous standards were safely used for calibration. The absolute limit of detection and characteristic mass were 7.2 pg and 9.0 pg of lead, respectively. The lead concentrations in different types of flour samples were found in the range of 25-52 μg kg- 1. Finally, homogeneity factors representing the heterogeneity of analyte distribution for lead in flour samples were determined.

The physical basis for absorption of light. [effects on wave functions of gas molecules and atoms

NASA Technical Reports Server (NTRS)

Pickett, H. M.

1979-01-01

The effects of light absorption on the wave functions of gas-phase molecules and atoms are investigated by high resolution spectral measurements of radiation emerging from a sample. A Stark-modulated sample of methyl fluoride was irradiated at the 102 GHz rotational transition and the emergent radiation was resolved by means of a spectrum analyzer. For signal oscillator frequencies below or above the molecular resonance by one modulation frequency, the amplitudes of the upper and lower modulation sidebands are found to be of nonuniform intensity, which is inconsistent with amplitude modulation. Emission due to polarization is, however, calculated to be consistent with the results observed, indicating that light absorption should be considered as a subtractive stimulated emission.

Liquid chromatography-hydride generation-atomic absorption spectrometry for the speciation of tin in seafoods.

PubMed

Viñas, Pilar; López-García, Ignacio; Merino-Meroño, Beatriz; Campillo, Natalia; Hernández-Cordóba, Manuel

2004-04-01

Liquid chromatography with hydride generation atomic absorption spectrometry as the detection system was applied to the separation and determination of inorganic tin, tributyltin, dibutyltin, monobutyltin, diphenyltin and monophenyltin. A reversed phase C18 column and a methanol/water/acetic acid (70:27:3, v/v/v) mixture containing 0.05%(v/v) triethylamine and 0.1%(w/v) tropolone as the mobile phase (isocratic elution) were used. Extraction of organotins from the samples was carried out using methanol containing 0.05%(w/v) tropolone, a process that was repeated twice. The supernatants were shaken with water and dichloromethane in a separating funnel and the organic phase was collected and evaporated to dryness. When the method was applied to the speciation of tin in fresh and canned mussels, no organotins above the detection limits were identified in any of the samples, inorganic tin being the only species detected. The reliability of the procedure was checked by analyzing the total tin content of the samples by electrothermal atomic absorption spectrometry and by speciation of tin in a certified reference material, mussel tissue (CRM 477). The method can be used for environmental monitoring of organotins contaminated samples.

Manganese dioxide causes spurious gold values in flame atomic-absorption readings from HBr-Br2 digestions

USGS Publications Warehouse

Campbell, W.L.

1981-01-01

False readings, apparently caused by the presence of high concentrations of manganese dioxide, have been observed in our current flame atomic-absorption procedure for the determination of gold. After a hydrobromic acid (HBr)-bromine (Br2) leach, simply heating the sample to boiling to remove excess Br2 prior to extraction with methyl-isobutyl-ketone (MIBK) eliminates these false readings. ?? 1981.

Rapid determination of nanogram amounts of tellurium in silicate rocks

USGS Publications Warehouse

Greenland, L.P.; Campbell, E.Y.

1976-01-01

A hydride-generation flameless atomic-absorption technique is used to determine as little as 5 ng g-1 tellurium in 0.25 g of silicate rock. After acid decomposition of the sample, tellurium hydride is generated with sodium borohydride and the vapor passed directly to a resistance-heated quartz cell mounted in an atomic-absorption spectrophotometer. Analyses of 11 U.S. Geological Survey standard rocks are presented. ?? 1976.

Simple method for determination of selenium in biological materials by flameless atomic-absorption spectrometry using a carbon-tube atomizer.

PubMed

Ishizaki, M

1978-03-01

A method for determination of selenium in biological materials by flameless atomic-absorption spectrometry using a carbon-tube atomizer is described. The sample is burned by an oxygen-flask combustion procedure, the resulting solution is treated with a cation-exchange resin to eliminate interfering cations, the selenium is extracted with dithizone in carbon tetrachloride and the resulting selenium dithizonate is combined with nickel nitrate in the carbon tube to enhance the sensitivity for selenium and avoid volatilization losses. The method measures selenium concentrations as low as 0.01 mug/g with a relative standard deviation of 8%.

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.

Determination of trace elements in automotive fuels by filter furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Anselmi, Anna; Tittarelli, Paolo; Katskov, Dmitri A.

2002-03-01

The determination of Cd, Cr, Cu, Pb and Ni was performed in gasoline and diesel fuel samples by electrothermal atomic absorption spectrometry using the Transverse Heated Filter Atomizer (THFA). Thermal conditions were experimentally defined for the investigated elements. The elements were analyzed without addition of chemical modifiers, using organometallic standards for the calibration. Forty-microliter samples were injected into the THFA. Gasoline samples were analyzed directly, while diesel fuel samples were diluted 1:4 with n-heptane. The following characteristic masses were obtained: 0.8 pg Cd, 6.4 pg Cr, 12 pg Cu, 17 pg Pb and 27 pg Ni. The limits of determination for gasoline samples were 0.13 μg/kg Cd, 0.4 μg/kg Cr, 0.9 μg/kg Cu, 1.5 μg/kg Pb and 2.5 μg/kg Ni. The corresponding limit of determination for diesel fuel samples was approximately four times higher for all elements. The element recovery was performed using the addition of organometallic compounds to gasoline and diesel fuel samples and was between 85 and 105% for all elements investigated.

Graphite furnace atomic absorption spectrometric determination of vanadium after cloud point extraction in the presence of graphene oxide

NASA Astrophysics Data System (ADS)

López-García, Ignacio; Marín-Hernández, Juan José; Hernández-Córdoba, Manuel

2018-05-01

Vanadium (V) and vanadium (IV) in the presence of a small concentration of graphene oxide (0.05 mg mL-1) are quantitatively transferred to the coacervate obtained with Triton X-114 in a cloud point microextraction process. The surfactant-rich phase is directly injected into the graphite atomizer of an atomic absorption spectrometer. Using a 10-mL aliquot sample and 150 μL of a 15% Triton X-114 solution, the enrichment factor for the analyte is 103, which results in a detection limit of 0.02 μg L-1 vanadium. The separation of V(V) and V(IV) using an ion-exchanger allows speciation of the element at low concentrations. Data for seven reference water samples with certified vanadium contents confirm the reliability of the procedure. Several beer samples are also analyzed, those supplied as canned drinks showing low levels of tetravalent vanadium.

Stoichiometric effects on the optical properties of LiInSe(2)

NASA Technical Reports Server (NTRS)

Smith, Cecily J.; Lowe, Calvin W.

1989-01-01

The diffuse reflectance of LiInSe(2) between 0.67 and 3.54 eV have been measured and the Kubelka-Munk theory was used to obtain the absorption coefficient from the data. The band gap in the samples is located at approximately 1.6 eV. The In and Se content of the samples was determined from atomic absorption measurements. Absorption peaks at 0.890 and 0.896 eV have been observed which are correlated, respectively, to the selenium and indium deficiencies in the samples.

Use of High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS) for Sequential Multi-Element Determination of Metals in Seawater and Wastewater Samples

NASA Astrophysics Data System (ADS)

Peña-Vázquez, E.; Barciela-Alonso, M. C.; Pita-Calvo, C.; Domínguez-González, R.; Bermejo-Barrera, P.

2015-09-01

The objective of this work is to develop a method for the determination of metals in saline matrices using high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Module SFS 6 for sample injection was used in the manual mode, and flame operating conditions were selected. The main absorption lines were used for all the elements, and the number of selected analytical pixels were 5 (CP±2) for Cd, Cu, Fe, Ni, Pb and Zn, and 3 pixels for Mn (CP±1). Samples were acidified (0.5% (v/v) nitric acid), and the standard addition method was used for the sequential determination of the analytes in diluted samples (1:2). The method showed good precision (RSD(%) < 4%, except for Pb (6.5%)) and good recoveries. Accuracy was checked after the analysis of an SPS-WW2 wastewater reference material diluted with synthetic seawater (dilution 1:2), showing a good agreement between certified and experimental results.

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.

Evaluation of methods for trace-element determination with emphasis on their usability in the clinical routine laboratory.

PubMed

Bolann, B J; Rahil-Khazen, R; Henriksen, H; Isrenn, R; Ulvik, R J

2007-01-01

Commonly used techniques for trace-element analysis in human biological material are flame atomic absorption spectrometry (FAAS), graphite furnace atomic absorption spectrometry (GFAAS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). Elements that form volatile hydrides, first of all mercury, are analysed by hydride generation techniques. In the absorption techniques the samples are vaporized into free, neutral atoms and illuminated by a light source that emits the atomic spectrum of the element under analysis. The absorbance gives a quantitative measure of the concentration of the element. ICP-AES and ICP-MS are multi-element techniques. In ICP-AES the atoms of the sample are excited by, for example, argon plasma at very high temperatures. The emitted light is directed to a detector, and the optical signals are processed to values for the concentrations of the elements. In ICP-MS a mass spectrometer separates and detects ions produced by the ICP, according to their mass-to-charge ratio. Dilution of biological fluids is commonly needed to reduce the effect of the matrix. Digestion using acids and microwave energy in closed vessels at elevated pressure is often used. Matrix and spectral interferences may cause problems. Precautions should be taken against trace-element contamination during collection, storage and processing of samples. For clinical problems requiring the analysis of only one or a few elements, the use of FAAS may be sufficient, unless the higher sensitivity of GFAAS is required. For screening of multiple elements, however, the ICP techniques are preferable.

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.

Scanning Auger Microprobe and atomic absorption studies of lunar volcanic volatiles

NASA Technical Reports Server (NTRS)

Cirlin, E. H.; Housley, R. M.

1979-01-01

Results on lunar volatile transport processes have been obtained by studying green and brown glass droplets, orange and black core tube samples and the surface sample 74241 with the Scanning Auger Microprobe (SAM) and by Flameless Atomic Absorption Analysis (FLAA). SAM analyses show that the most dominant volatiles in the top few atomic layers of droplets are Zn and S, confirming that the surface Zn and S are good indicators of pyroclastic origin, and they are not entirely present as ZnS. In addition, FLAA thermal release profiles show that almost all the Zn and Cd are on grain surfaces, indicating that Zn and Cd were completely outgassed from lava fountain products during the volcanic eruption, were recondensed during or after the eruptions, and are thus present as surface coating.

Direct determination of Pb in raw milk by graphite furnace atomic absorption spectrometry (GF AAS) with electrothermal atomization sampling from slurries.

PubMed

de Oliveira, Tatiane Milão; Augusto Peres, Jayme; Lurdes Felsner, Maria; Cristiane Justi, Karin

2017-08-15

Milk is an important food in the human diet due to its physico-chemical composition; therefore, it is necessary to monitor contamination by toxic metals such as Pb. Milk sample slurries were prepared using Triton X-100 and nitric acid for direct analysis of Pb using graphite furnace atomic absorption spectrometry - GF AAS. After dilution of the slurries, 10.00µl were directly introduced into the pyrolytic graphite tube without use of a chemical modifier, which acts as an advantage considering this type of matrix. The limits of detection and quantification were 0.64 and 2.14µgl -1 , respectively. The figures of merit studied showed that the proposed methodology without pretreatment of the raw milk sample and using external standard calibration is suitable. The methodology was applied in milk samples from the Guarapuava region, in Paraná State (Brazil) and Pb concentrations ranged from 2.12 to 37.36µgl -1 . Copyright © 2017 Elsevier Ltd. All rights reserved.

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.

Tunable Diode Laser Atomic Absorption Spectroscopy for Detection of Potassium under Optically Thick Conditions.

PubMed

Qu, Zhechao; Steinvall, Erik; Ghorbani, Ramin; Schmidt, Florian M

2016-04-05

Potassium (K) is an important element related to ash and fine-particle formation in biomass combustion processes. In situ measurements of gaseous atomic potassium, K(g), using robust optical absorption techniques can provide valuable insight into the K chemistry. However, for typical parts per billion K(g) concentrations in biomass flames and reactor gases, the product of atomic line strength and absorption path length can give rise to such high absorbance that the sample becomes opaque around the transition line center. We present a tunable diode laser atomic absorption spectroscopy (TDLAAS) methodology that enables accurate, calibration-free species quantification even under optically thick conditions, given that Beer-Lambert's law is valid. Analyte concentration and collisional line shape broadening are simultaneously determined by a least-squares fit of simulated to measured absorption profiles. Method validation measurements of K(g) concentrations in saturated potassium hydroxide vapor in the temperature range 950-1200 K showed excellent agreement with equilibrium calculations, and a dynamic range from 40 pptv cm to 40 ppmv cm. The applicability of the compact TDLAAS sensor is demonstrated by real-time detection of K(g) concentrations close to biomass pellets during atmospheric combustion in a laboratory reactor.

A new approach for the determination of sulphur in food samples by high-resolution continuum source flame atomic absorption spectrometer.

PubMed

Ozbek, N; Baysal, A

2015-02-01

The new approach for the determination of sulphur in foods was developed, and the sulphur concentrations of various fresh and dried food samples determined using a high-resolution continuum source flame atomic absorption spectrometer with an air/acetylene flame. The proposed method was optimised and the validated using standard reference materials, and certified values were found to be within the 95% confidence interval. The sulphur content of foods ranged from less than the LOD to 1.5mgg(-1). The method is accurate, fast, simple and sensitive. Copyright © 2014 Elsevier Ltd. All rights reserved.

Lead screening in DBS by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry: application to newborns and pregnant women.

PubMed

Rello, Luis; Aramendía, Maite; Belarra, Miguel A; Resano, Martín

2015-01-01

DBS have become a clinical specimen especially adequate for establishing home-based collection protocols. In this work, high-resolution continuum source graphite furnace atomic absorption spectrometry is evaluated for the direct monitoring of Pb in DBS, both as a quantitative tool and a screening method. The development of the screening model is based on the establishment of the unreliability region around the threshold limits, 100 or 50 μg l(-1). More than 500 samples were analyzed to validate the model. The screening method demonstrated high sensitivity (the rate of true positives detected was always higher than 95%), an excellent LOD (1 µg l(-1)) and high throughput (10 min per sample).

Simultaneous determination of Cd and Fe in beans and soil of different regions of Brazil using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling.

PubMed

dos Santos, Lisia M G; Welz, Bernhard; Araujo, Rennan G O; Jacob, Silvana do C; Vale, Maria Goreti R; Martens, Andreas; Gonzaga Martens, Irland B; Becker-Ross, Helmut

2009-11-11

A fast routine screening method for the simultaneous determination of cadmium and iron in bean and soil samples is proposed, using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling. The primary absorption line at 228.802 nm has been used for the determination of cadmium, and an adjacent secondary line, at 228.726 nm, for iron. Fourteen bean samples and 10 soil samples from nine states all over Brazil have been analyzed. The limits of detection (3 sigma, n = 10) were 2.0 microg kg(-1) for Cd and 4.5 mg kg(-1) for Fe. The relative standard deviation ranged from 4 to 7% for Cd and from 5 to 28% for Fe, which is usually acceptable for a screening method. The accuracy of the method has been confirmed by the analysis of two certified reference materials; the results were in agreement with the certified values at a 95% confidence interval.

Bismuth as a general internal standard for lead in atomic absorption spectrometry.

PubMed

Bechlin, Marcos A; Fortunato, Felipe M; Ferreira, Edilene C; Gomes Neto, José A; Nóbrega, Joaquim A; Donati, George L; Jones, Bradley T

2014-06-11

Bismuth was evaluated as internal standard for Pb determination by line source flame atomic absorption spectrometry (LS FAAS), high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) and line source graphite furnace atomic absorption spectrometry (LS GFAAS). Analysis of samples containing different matrices indicated close relationship between Pb and Bi absorbances. Correlation coefficients of calibration curves built up by plotting A(Pb)/A(Bi)versus Pb concentration were higher than 0.9953 (FAAS) and higher than 0.9993 (GFAAS). Recoveries of Pb improved from 52-118% (without IS) to 97-109% (IS, LS FAAS); 74-231% (without IS) to 96-109% (IS, HR-CS FAAS); and 36-125% (without IS) to 96-110% (IS, LS GFAAS). The relative standard deviations (n=12) were reduced from 0.6-9.2% (without IS) to 0.3-4.3% (IS, LS FAAS); 0.7-7.7% (without IS) to 0.1-4.0% (IS, HR-CS FAAS); and 2.1-13% (without IS) to 0.4-5.9% (IS, LS GFAAS). Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of total tin in geological materials by electrothermal atomic-absorption spectrophotometry using a tungsten-impregnated graphite furnace

USGS Publications Warehouse

Zhou, L.; Chao, T.T.; Meier, A.L.

1984-01-01

An electrothermal atomic-absorption spectrophotometric method is described for the determination of total tin in geological materials, with use of a tungsten-impregnated graphite furnace. The sample is decomposed by fusion with lithium metaborate and the melt is dissolved in 10% hydrochloric acid. Tin is then extracted into trioctylphosphine oxide-methyl isobutyl ketone prior to atomization. Impregnation of the furnace with a sodium tungstate solution increases the sensitivity of the determination and improves the precision of the results. The limits of determination are 0.5-20 ppm of tin in the sample. Higher tin values can be determined by dilution of the extract. Replicate analyses of eighteen geological reference samples with diverse matrices gave relative standard deviations ranging from 2.0 to 10.8% with an average of 4.6%. Average tin values for reference samples were in general agreement with, but more precise than, those reported by others. Apparent recoveries of tin added to various samples ranged from 95 to 111% with an average of 102%. ?? 1984.

[Determination of mercury in Boletus impolitus by flow injection-atomic absorption spectrometry].

PubMed

Li, Tao; Wang, Yuan-Zhong

2008-04-01

Various test conditions and effect factors for the determination of mercury by flow injection-atomic absorption spectrometry were discussed, and a method for the determination of mercury in Boletus impolitus has been developed. The linear range for mercury is 0-60 microg x L(-1). The relative standard deviation is less than 3.0%, and the recovery is 96%-107%. This method is simple, rapid and has been applied to the determination of mercury in Boletus impolitus samples with satisfactory results.

Determination of arsenic in geological materials by electrothermal atomic-absorption spectrometry after hydride generation

USGS Publications Warehouse

Sanzolone, R.F.; Chao, T.T.; Welsch, E.P.

1979-01-01

Rock and soil samples are decomposed with HClO4-HNO3; after further treatment, arsine is generated and absorbed in a dilute silver nitrate solution. Aliquots of this solution are injected into a carbon rod atomizer. Down to 1 ppm As in samples can be determined and there are no significant interferences, even from chromium in soils. Good results were obtained for geochemical reference samples. ?? 1979.

Analysis of Dithiocarbamate Fungicides in Vegetable Matrices Using HPLC-UV Followed by Atomic Absorption Spectrometry.

PubMed

Al-Alam, Josephine; Bom, Laura; Chbani, Asma; Fajloun, Ziad; Millet, Maurice

2017-04-01

A simple method combining ion-pair methylation, high-performance liquid chromatography (HPLC) analysis with detection at 272 nm and atomic absorption spectrometry was developed in order to determine 10 dithiocarbamate fungicides (Dazomet, Metam-sodium, Ferbam, Ziram, Zineb, Maneb, Mancozeb, Metiram, Nabam and Propineb) and distinguish ethylenbisdithiocarbamates (EBDTCs) Zineb, Maneb and Mancozeb in diverse matrices. This method associates reverse phase analysis by HPLC analysis with detection at 272 nm, with atomic absorption spectrometry in order to distinguish, with the same extraction protocol, Maneb, Mancozeb and Zineb. The limits of detection (0.4, 0.8, 0.5, 1.25 and 1.97) and quantification (1.18, 2.5, 1.52, 4.2 and 6.52) calculated in injected nanogram, respectively, for Dazomet, Metam-Na, dimethyldithiocarbamates (DMDTCs), EBDTCs and propylenebisdithiocarbamates (PBDTCs) justify the sensitivity of the method used. The coefficients of determination R2 were 0.9985, 0.9978, 0.9949, 0.988 and 0.9794, respectively, for Dazomet, Metam-Na, DMDTCs, EBDTCs and PBDTCs, and the recovery from fortified apple and leek samples was above 90%. Results obtained with the atomic absorption method in comparison with spectrophotometric analysis focus on the importance of the atomic absorption as a complementary specific method for the distinction between different EBDTCs fungicides. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

PubMed

Headridge, J B; Smith, D R

1972-07-01

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

Characterization of local atomic structure in Co/Zn based ZIFs by XAFS

NASA Astrophysics Data System (ADS)

Podkovyrina, Yulia; Butova, Vera; Bulanova, Elena; Budnyk, Andriy; Kremennaya, Maria; Soldatov, Alexander; Lamberti, Carlo

2018-03-01

The local atomic structure in bimetallic Co/Zn zeolitic imidazolate frameworks (ZIFs) was studied using X-ray Absorption Fine Structure (XAFS) spectroscopy and theoretical calculations. The experimental Co K-edge and Zn K-edge XANES (X-ray Absorption Near Edge Structure) spectra of Zn1-xCoxC8H10N4 samples (x = 0.05, 0.25, 0.75) synthesized by microwave synthesis were compared with the data for the ZIF-67 (x=1) and ZIF-8 (x=0). Theoretical XANES spectra for the bimetallic ZIFs were calculated. It was shown that in bimetallic ZIFs the Co and Zn atoms have the similar local environment.

Determination of mercury in fish tissue using a minianalyzer based on cold vapor atomic absorption spectrometry at the 184.9 nm line.

PubMed

Rizea, Maria-Cristina; Bratu, Maria-Cristina; Danet, Andrei Florin; Bratu, Adrian

2007-09-01

A sensitive method was proposed and optimized for the determination of total mercury in fish tissue by using wet digestion, followed by cold vapor atomic absorption spectrometry (CVAAS) at the main resonance line of mercury (184.9 nm). The measurements were made using a new type of a non-dispersive mercury minianalyzer. This instrument was initially designed and built for atmospheric mercury-vapor detection. For determining mercury in aqueous samples, the minianalyzer was linked with a mercury/hydride system, Perkin Elmer Model MHS-10. To check the method, the analyzed samples were spiked with a standard solution of mercury. The recoveries of mercury spiked to wet fish tissue were >90% for 0.5 - 0.8 g samples. The results showed a better sensitivity (about 2.5 times higher) when using the mercury absorption line at 184.9 nm compared with the sensitivity obtained by conventional CVAAS at 253.7 nm.

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.

A method for the routine determination of aluminium in serum and water by flameless atomic absorption spectrometry.

PubMed

Parkinson, I S; Ward, M K; Kerr, D N

1982-10-27

A simple but reliable method for the routine determination of aluminium in serum and water by flameless atomic absorption spectrometry is described. No preparatory procedures are required for water samples, although serum is mixed with a wetting agent (Triton X-100) to allow complete combustion of the samples and to improve analytical precision. Precautions to prevent contamination during sample handling are discussed and instrumental parameters are defined. The method has a sensitivity of 35.5 pg and detection limits of 2.3 micrograms Al/l for serum and 1.3 micrograms Al/l for water. The method was used to determine the aluminium concentration in serum of 46 normal subjects. The mean aluminium content was 7.3 micrograms/l (range 2--15 micrograms/l.

Determination of silver in soils, sediments, and rocks by organic-chelate extraction and atomic absorption spectrophotometry

USGS Publications Warehouse

Chao, T.T.; Ball, J.W.; Nakagawa, H.M.

1971-01-01

A useful method for the determination of silver in soil, sediment, and rock samples in geochemical exploration has been developed. The sample is digested with concentrated nitric acid, and the silver extracted with triisooctyl thiophosphate (TOTP) in methyl isobutyl ketone (MIBK) after dilution of the acid digest to approximately 6 M. The extraction of silver into the organic extractant is quantitative and not affected by the nitric acid concentration from 4 M to 8 M, or by different volumes of TOTP-MIBK. The extracted silver is stable and remains in the organic phase up to several days. The silver concentration is determined by atomic absorption spectrophotometry. ?? 1971.

EPA Method 245.2: Mercury (Automated Cold Vapor Technique)

EPA Pesticide Factsheets

Method 245.2 describes procedures for preparation and analysis of drinking water samples for analysis of mercury using acid digestion and cold vapor atomic absorption. Samples are prepared using an acid digestion technique.

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.

On the influence of crystal size and wavelength on native SAD phasing.

PubMed

Liebschner, Dorothee; Yamada, Yusuke; Matsugaki, Naohiro; Senda, Miki; Senda, Toshiya

2016-06-01

Native SAD is an emerging phasing technique that uses the anomalous signal of native heavy atoms to obtain crystallographic phases. The method does not require specific sample preparation to add anomalous scatterers, as the light atoms contained in the native sample are used as marker atoms. The most abundant anomalous scatterer used for native SAD, which is present in almost all proteins, is sulfur. However, the absorption edge of sulfur is at low energy (2.472 keV = 5.016 Å), which makes it challenging to carry out native SAD phasing experiments as most synchrotron beamlines are optimized for shorter wavelength ranges where the anomalous signal of sulfur is weak; for longer wavelengths, which produce larger anomalous differences, the absorption of X-rays by the sample, solvent, loop and surrounding medium (e.g. air) increases tremendously. Therefore, a compromise has to be found between measuring strong anomalous signal and minimizing absorption. It was thus hypothesized that shorter wavelengths should be used for large crystals and longer wavelengths for small crystals, but no thorough experimental analyses have been reported to date. To study the influence of crystal size and wavelength, native SAD experiments were carried out at different wavelengths (1.9 and 2.7 Å with a helium cone; 3.0 and 3.3 Å with a helium chamber) using lysozyme and ferredoxin reductase crystals of various sizes. For the tested crystals, the results suggest that larger sample sizes do not have a detrimental effect on native SAD data and that long wavelengths give a clear advantage with small samples compared with short wavelengths. The resolution dependency of substructure determination was analyzed and showed that high-symmetry crystals with small unit cells require higher resolution for the successful placement of heavy atoms.

Direct determination of total sulfur in wine using a continuum-source atomic-absorption spectrometer and an air-acetylene flame.

PubMed

Huang, Mao Dong; Becker-Ross, Helmut; Florek, Stefan; Heitmann, Uwe; Okruss, Michael

2005-08-01

Determination of sulfur in wine is an important analytical task, particularly with regard to food safety legislation, wine trade, and oenology. Hitherto existing methods for sulfur determination all have specific drawbacks, for example high cost and time consumption, poor precision or selectivity, or matrix effects. In this paper a new method, with low running costs, is introduced for direct, reliable, rapid, and accurate determination of the total sulfur content of wine samples. The method is based on measurement of the molecular absorption of carbon monosulfide (CS) in an ordinary air-acetylene flame by using a high-resolution continuum-source atomic-absorption spectrometer including a novel high-intensity short-arc xenon lamp. First results for total sulfur concentrations in different wine samples were compared with data from comparative ICP-MS measurements. Very good agreement within a few percent was obtained.

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%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A comparative study of gamma-ray interaction and absorption in some building materials using Zeff-toolkit

NASA Astrophysics Data System (ADS)

Mann, Kulwinder Singh; Heer, Manmohan Singh; Rani, Asha

2016-07-01

The gamma-ray shielding behaviour of a material can be investigated by determining its various interaction and energy-absorption parameters (such as mass attenuation coefficients, mass energy absorption coefficients, and corresponding effective atomic numbers and electron densities). Literature review indicates that the effective atomic number (Zeff) has been used as extensive parameters for evaluating the effects and defect in the chosen materials caused by ionising radiations (X-rays and gamma-rays). A computer program (Zeff-toolkit) has been designed for obtaining the mean value of effective atomic number calculated by three different methods. A good agreement between the results obtained with Zeff-toolkit, Auto_Zeff software and experimentally measured values of Zeff has been observed. Although the Zeff-toolkit is capable of computing effective atomic numbers for both photon interaction (Zeff,PI) and energy absorption (Zeff,En) using three methods in each. No similar computer program is available in the literature which simultaneously computes these parameters simultaneously. The computed parameters have been compared and correlated in the wide energy range (0.001-20 MeV) for 10 commonly used building materials. The prominent variations in these parameters with gamma-ray photon energy have been observed due to the dominance of various absorption and scattering phenomena. The mean values of two effective atomic numbers (Zeff,PI and Zeff,En) are equivalent at energies below 0.002 MeV and above 0.3 MeV, indicating the dominance of gamma-ray absorption (photoelectric and pair production) over scattering (Compton) at these energies. Conversely in the energy range 0.002-0.3 MeV, the Compton scattering of gamma-rays dominates the absorption. From the 10 chosen samples of building materials, 2 soils showed better shielding behaviour than did other 8 materials.

The determination of lead in sugar and sweets without digestion by electrothermal atomic absorption spectrometry (ETAAS) with a rhodium chemical modifier.

PubMed

Dias, V M C; Cardoso, A S B

2006-05-01

Reference methods for determining lead in food are usually time-consuming. This paper reports a straightforward procedure using electrothermal atomic absorption spectrometry (ETAAS), to determine lead (Pb) in fat-free sweets. Several chemical modifiers were examined and results showed that it is not necessary to digest the samples, when a rhodium (Rh) modifier was used. The samples were dissolved in nitric acid and the determination of Pb was performed by ETAAS, using Rh chemical modifier at a pyrolysis temperature of 900 degrees C and an atomization temperature of 1,500 degrees C. No ashing step was employed and aqueous standards were used, in the range 2-10 microg l(-1). The limit of quantification was 0.095 mg kg(-1), and the accuracy of the method was verified by analysing certified reference materials.

A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry.

PubMed

Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S; Korn, Maria G A; Bezerra, Marcos A

2009-03-15

A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L(-1) nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 microg L(-1), respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 microg L(-1). The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.

Method of trivalent chromium concentration determination by atomic spectrometry

DOEpatents

Reheulishvili, Aleksandre N [Tbilisi, 0183, GE; Tsibakhashvili, Neli Ya [Tbilisi, 0101, GE

2006-12-12

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

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

PubMed

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

2013-01-01

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

Gamma ray interaction studies of organic nonlinear optical materials in the energy range 122 keV-1330 keV

NASA Astrophysics Data System (ADS)

Awasarmol, V. V.; Gaikwad, D. K.; Raut, S. D.; Pawar, P. P.

The mass attenuation coefficients (μm) for organic nonlinear optical materials measured at 122-1330 keV photon energies were investigated on the basis of mixture rule and compared with obtained values of WinXCOM program. It is observed that there is a good agreement between theoretical and experimental values of the samples. All samples were irradiated with six radioactive sources such as 57Co, 133Ba, 22Na, 137Cs, 54Mn and 60Co using transmission arrangement. Effective atomic and electron numbers or electron densities (Zeff and Neff), molar extinction coefficient (ε), mass energy absorption coefficient (μen/ρ) and effective atomic energy absorption cross section (σa,en) were determined experimentally and theoretically using the obtained μm values for investigated samples and graphs have been plotted. The graph shows that the variation of all samples decreases with increasing photon energy.

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.

[Recent Development of Atomic Spectrometry in China].

PubMed

Xiao, Yuan-fang; Wang, Xiao-hua; Hang, Wei

2015-09-01

As an important part of modern analytical techniques, atomic spectrometry occupies a decisive status in the whole analytical field. The development of atomic spectrometry also reflects the continuous reform and innovation of analytical techniques. In the past fifteen years, atomic spectrometry has experienced rapid development and been applied widely in many fields in China. This review has witnessed its development and remarkable achievements. It contains several directions of atomic spectrometry, including atomic emission spectrometry (AES), atomic absorption spectrometry (AAS), atomic fluorescence spectrometry (AFS), X-ray fluorescence spectrometry (XRF), and atomic mass spectrometry (AMS). Emphasis is put on the innovation of the detection methods and their applications in related fields, including environmental samples, biological samples, food and beverage, and geological materials, etc. There is also a brief introduction to the hyphenated techniques utilized in atomic spectrometry. Finally, the prospects of atomic spectrometry in China have been forecasted.

NARROW Na AND K ABSORPTION LINES TOWARD T TAURI STARS: TRACING THE ATOMIC ENVELOPE OF MOLECULAR CLOUDS

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

Pascucci, I.; Simon, M. N.; Edwards, S.

2015-11-20

We present a detailed analysis of narrow Na i and K i absorption resonance lines toward nearly 40 T Tauri stars in Taurus with the goal of clarifying their origin. The Na i λ5889.95 line is detected toward all but one source, while the weaker K i λ7698.96 line is detected in about two-thirds of the sample. The similarity in their peak centroids and the significant positive correlation between their equivalent widths demonstrate that these transitions trace the same atomic gas. The absorption lines are present toward both disk and diskless young stellar objects, which excludes cold gas within themore » circumstellar disk as the absorbing material. A comparison of Na i and CO detections and peak centroids demonstrates that the atomic gas and molecular gas are not co-located, the atomic gas being more extended than the molecular gas. The width of the atomic lines corroborates this finding and points to atomic gas about an order of magnitude warmer than the molecular gas. The distribution of Na i radial velocities shows a clear spatial gradient along the length of the Taurus molecular cloud filaments. This suggests that absorption is associated with the Taurus molecular cloud. Assuming that the gradient is due to cloud rotation, the rotation of the atomic gas is consistent with differential galactic rotation, whereas the rotation of the molecular gas, although with the same rotation axis, is retrograde. Our analysis shows that narrow Na i and K i absorption resonance lines are useful tracers of the atomic envelope of molecular clouds. In line with recent findings from giant molecular clouds, our results demonstrate that the velocity fields of the atomic and molecular gas are misaligned. The angular momentum of a molecular cloud is not simply inherited from the rotating Galactic disk from which it formed but may be redistributed by cloud–cloud interactions.« less

Characterization of the physico-chemical properties of polymeric materials for aerospace flight. [differential thermal and atomic absorption spectroscopic analysis of nickel cadmium batteries

NASA Technical Reports Server (NTRS)

Rock, M.

1981-01-01

Electrodes and electrolytes of nickel cadmium sealed batteries were analyzed. Different thermal analysis of negative and positive battery electrodes was conducted and the temperature ranges of occurrence of endotherms indicating decomposition of cadmium hydroxide and nickel hydroxide are identified. Atomic absorption spectroscopy was used to analyze electrodes and electrolytes for traces of nickel, cadmium, cobalt, and potassium. Calibration curves and data are given for each sample analyzed. Instrumentation and analytical procedures used for each method are described.

Optical Diagnostics in the Gaseous Electronics Conference Reference Cell

PubMed Central

Hebner, G. A.; Greenberg, K. E.

1995-01-01

A number of laser-induced fluorescence and absorption spectroscopy studies have been conducted using Gaseous Electronics Conference Reference Cells. Laser-induced fluorescence has been used to measure hydrogen atom densities, to measure argon metastable spatial profiles, to determine the sheath electric field, and to infer the electron density and temperature. Absorption spectroscopy, using lamp sources and diode lasers, has been used to measure metastable atom densities in helium and argon discharges and fluorocarbon densities in silicon etching discharges. The experimental techniques and sample results of these investigations are reviewed. PMID:29151748

Identification of F impurities in F-doped ZnO by synchrotron X-ray absorption near edge structures

NASA Astrophysics Data System (ADS)

Na-Phattalung, Sutassana; Limpijumnong, Sukit; Min, Chul-Hee; Cho, Deok-Yong; Lee, Seung-Ran; Char, Kookrin; Yu, Jaejun

2018-04-01

Synchrotron X-ray absorption near edge structure (XANES) measurements of F K-edge in conjunction with first-principles calculations are used to identify the local structure of the fluorine (F) atom in F-doped ZnO. The ZnO film was grown by pulsed laser deposition with an Nd:YAG laser, and an oxyfluoridation method was used to introduce F ions into the ZnO films. The measured XANES spectrum of the sample was compared against the first-principles XANES calculations based on various models for local atomic structures surrounding F atoms. The observed spectral features are attributed to ZnF2 and FO defects in wurtzite bulk ZnO.

Statistical evaluation of an inductively coupled plasma atomic emission spectrometric method for routine water quality testing

USGS Publications Warehouse

Garbarino, J.R.; Jones, B.E.; Stein, G.P.

1985-01-01

In an interlaboratory test, inductively coupled plasma atomic emission spectrometry (ICP-AES) was compared with flame atomic absorption spectrometry and molecular absorption spectrophotometry for the determination of 17 major and trace elements in 100 filtered natural water samples. No unacceptable biases were detected. The analysis precision of ICP-AES was found to be equal to or better than alternative methods. Known-addition recovery experiments demonstrated that the ICP-AES determinations are accurate to between plus or minus 2 and plus or minus 10 percent; four-fifths of the tests yielded average recoveries of 95-105 percent, with an average relative standard deviation of about 5 percent.

[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.

A comparison of geochemical exploration techniques and sample media within accretionary continental margins: an example from the Pacific Border Ranges, Southern Alaska, U.S.A.

USGS Publications Warehouse

Sutley, S.J.; Goldfarb, R.J.; O'Leary, R. M.; Tripp, R.B.

1990-01-01

The Pacific Border Ranges of the southern Alaskan Cordillera are composed of a number of allochthonous tectonostratigraphic terranes. Within these terranes are widespread volcanogenic, massive sulfide deposits in and adjacent to portions of accreted ophiolite complexes, bands and disseminations of chromite in accreted island-arc ultramafic rocks, and epigenetic, gold-bearing quartz veins in metamorphosed turbidite sequences. A geochemical pilot study was undertaken to determine the most efficient exploration strategy for locating these types of mineral deposits within the Pacific Border Ranges and other typical convergent continental margin environments. High-density sediment sampling was carried out in first- and second-order stream channels surrounding typical gold, chromite and massive sulfide occurrences. At each site, a stream-sediment and a panned-concentrate sample were collected. In the laboratory, the stream sediments were sieved into coarse-sand, fine- to medium-sand, and silt- to clay-size fractions prior to analysis. One split of the panned concentrates was retained for analysis; a second split was further concentrated by gravity separation in heavy liquids and then divided into magnetic, weakly magnetic and nonmagnetic fractions for analysis. A number of different techniques including atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry and semi-quantitative emission spectrography were used to analyze the various sample media. Comparison of the various types of sample media shows that in this tectonic environment it is most efficient to include a silt- to clay-size sediment fraction and a panned-concentrate sample. Even with the relatively low detection limits for many elements by plasma spectrometry and atomic absorption spectrometry, anomalies reflecting the presence of gold veins could not be identified in any of the stream-sediment fractions. Unseparated panned-concentrate samples should be analyzed by emission spectroscopy and atomic absorption spectrometry for Ag and Au. If, however, magnetic and nonmagnetic concentrate fractions are used in a reconnaissance program, semiquantitative emission spectrography is adequate for all analytical work. ?? 1990.

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

PubMed

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

2018-03-01

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

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).

Evaluation of Optical Depths and Self-Absorption of Strontium and Aluminum Emission Lines in Laser-Induced Breakdown Spectroscopy (LIBS).

PubMed

Alfarraj, Bader A; Bhatt, Chet R; Yueh, Fang Yu; Singh, Jagdish P

2017-04-01

Laser-induced breakdown spectroscopy (LIBS) is a widely used laser spectroscopic technique in various fields, such as material science, forensic science, biological science, and the chemical and pharmaceutical industries. In most LIBS work, the analysis is performed using radiative transitions from atomic emissions. In this study, the plasma temperature and the product [Formula: see text] (the number density N and the absorption path length [Formula: see text]) were determined to evaluate the optical depths and the self-absorption of Sr and Al lines. A binary mixture of strontium nitrate and aluminum oxide was used as a sample, consisting of variety of different concentrations in powder form. Laser-induced breakdown spectroscopy spectra were collected by varying various parameters, such as laser energy, gate delay time, and gate width time to optimize the LIBS signals. Atomic emission from Sr and Al lines, as observed in the LIBS spectra of different sample compositions, was used to characterize the laser induced plasma and evaluate the optical depths and self-absorption of LIBS.

Validation of an analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals in soil

PubMed Central

2013-01-01

Background The aim of this paper was the validation of a new analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals (Ag, Cd, Co, Cr, Cu, Ni, Pb and Zn) in soil after microwave assisted digestion in aqua regia. Determinations were performed on the ContrAA 300 (Analytik Jena) air-acetylene flame spectrometer equipped with xenon short-arc lamp as a continuum radiation source for all elements, double monochromator consisting of a prism pre-monocromator and an echelle grating monochromator, and charge coupled device as detector. For validation a method-performance study was conducted involving the establishment of the analytical performance of the new method (limits of detection and quantification, precision and accuracy). Moreover, the Bland and Altman statistical method was used in analyzing the agreement between the proposed assay and inductively coupled plasma optical emission spectrometry as standardized method for the multielemental determination in soil. Results The limits of detection in soil sample (3σ criterion) in the high-resolution continuum source flame atomic absorption spectrometry method were (mg/kg): 0.18 (Ag), 0.14 (Cd), 0.36 (Co), 0.25 (Cr), 0.09 (Cu), 1.0 (Ni), 1.4 (Pb) and 0.18 (Zn), close to those in inductively coupled plasma optical emission spectrometry: 0.12 (Ag), 0.05 (Cd), 0.15 (Co), 1.4 (Cr), 0.15 (Cu), 2.5 (Ni), 2.5 (Pb) and 0.04 (Zn). Accuracy was checked by analyzing 4 certified reference materials and a good agreement for 95% confidence interval was found in both methods, with recoveries in the range of 94–106% in atomic absorption and 97–103% in optical emission. Repeatability found by analyzing real soil samples was in the range 1.6–5.2% in atomic absorption, similar with that of 1.9–6.1% in optical emission spectrometry. The Bland and Altman method showed no statistical significant difference between the two spectrometric methods for 95% confidence interval. Conclusions High-resolution continuum source flame atomic absorption spectrometry can be successfully used for the rapid, multielemental determination of hazardous/priority hazardous metals in soil with similar analytical performances to those in inductively coupled plasma optical emission spectrometry. PMID:23452327

Validation of an analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals in soil.

PubMed

Frentiu, Tiberiu; Ponta, Michaela; Hategan, Raluca

2013-03-01

The aim of this paper was the validation of a new analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals (Ag, Cd, Co, Cr, Cu, Ni, Pb and Zn) in soil after microwave assisted digestion in aqua regia. Determinations were performed on the ContrAA 300 (Analytik Jena) air-acetylene flame spectrometer equipped with xenon short-arc lamp as a continuum radiation source for all elements, double monochromator consisting of a prism pre-monocromator and an echelle grating monochromator, and charge coupled device as detector. For validation a method-performance study was conducted involving the establishment of the analytical performance of the new method (limits of detection and quantification, precision and accuracy). Moreover, the Bland and Altman statistical method was used in analyzing the agreement between the proposed assay and inductively coupled plasma optical emission spectrometry as standardized method for the multielemental determination in soil. The limits of detection in soil sample (3σ criterion) in the high-resolution continuum source flame atomic absorption spectrometry method were (mg/kg): 0.18 (Ag), 0.14 (Cd), 0.36 (Co), 0.25 (Cr), 0.09 (Cu), 1.0 (Ni), 1.4 (Pb) and 0.18 (Zn), close to those in inductively coupled plasma optical emission spectrometry: 0.12 (Ag), 0.05 (Cd), 0.15 (Co), 1.4 (Cr), 0.15 (Cu), 2.5 (Ni), 2.5 (Pb) and 0.04 (Zn). Accuracy was checked by analyzing 4 certified reference materials and a good agreement for 95% confidence interval was found in both methods, with recoveries in the range of 94-106% in atomic absorption and 97-103% in optical emission. Repeatability found by analyzing real soil samples was in the range 1.6-5.2% in atomic absorption, similar with that of 1.9-6.1% in optical emission spectrometry. The Bland and Altman method showed no statistical significant difference between the two spectrometric methods for 95% confidence interval. High-resolution continuum source flame atomic absorption spectrometry can be successfully used for the rapid, multielemental determination of hazardous/priority hazardous metals in soil with similar analytical performances to those in inductively coupled plasma optical emission spectrometry.

Application of Plackett-Burman and Doehlert designs for optimization of selenium analysis in plasma with electrothermal atomic absorption spectrometry.

PubMed

El Ati-Hellal, Myriam; Hellal, Fayçal; Hedhili, Abderrazek

2014-10-01

The aim of this study was the optimization of selenium determination in plasma samples with electrothermal atomic absorption spectrometry using experimental design methodology. 11 variables being able to influence selenium analysis in human blood plasma by electrothermal atomic absorption spectrometry (ETAAS) were evaluated with Plackett-Burman experimental design. These factors were selected from sample preparation, furnace program and chemical modification steps. Both absorbance and background signals were chosen as responses in the screening approach. Doehlert design was used for method optimization. Results showed that only ashing temperature has a statistically significant effect on the selected responses. Optimization with Doehlert design allowed the development of a reliable method for selenium analysis with ETAAS. Samples were diluted 1/10 with 0.05% (v/v) TritonX-100+2.5% (v/v) HNO3 solution. Optimized ashing and atomization temperatures for nickel modifier were 1070°C and 2270°C, respectively. A detection limit of 2.1μgL(-1) Se was obtained. Accuracy of the method was checked by the analysis of selenium in Seronorm™ Trace element quality control serum level 1. The developed procedure was applied for the analysis of total selenium in fifteen plasma samples with standard addition method. Concentrations ranged between 24.4 and 64.6μgL(-1), with a mean of 42.6±4.9μgL(-1). The use of experimental designs allowed the development of a cheap and accurate method for selenium analysis in plasma that could be applied routinely in clinical laboratories. Copyright © 2014 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF METALS FROM SOIL, DUST, AIR FILTER, AND SURFACE AND DERMAL SAMPLES FOR AA (GRAPHITE FURNACE OR FLAME) OR ICP-AES ANALYSIS (BCO-L-3.1)

EPA Science Inventory

The purpose of this SOP is to describe the acid digestion of soil, house dust, air filter, and surface or dermal wipe samples for analysis using inductively coupled plasma atomic emissions spectrometry (ICP-AES) and/or graphite furnace atomic absorption spectrometry (GFAAS) or fl...

Investigation of chemical modifiers for the direct determination of arsenic in fish oil using high-resolution continuum source graphite furnace atomic absorption spectrometry.

PubMed

Pereira, Éderson R; de Almeida, Tarcísio S; Borges, Daniel L G; Carasek, Eduardo; Welz, Bernhard; Feldmann, Jörg; Campo Menoyo, Javier Del

2016-04-01

High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) has been applied for the development of a method for the determination of total As in fish oil samples using direct analysis. The method does not use any sample pretreatment, besides dilution with 1-propanole, in order to decrease the oil viscosity. The stability and sensitivity of As were evaluated using ruthenium and iridium as permanent chemical modifiers and palladium added in solution over the sample. The best results were obtained with ruthenium as the permanent modifier and palladium in solution added to samples and standard solutions. Under these conditions, aqueous standard solutions could be used for calibration for the fish oil samples diluted with 1-propanole. The pyrolysis and atomization temperatures were 1400 °C and 2300 °C, respectively, and the limit of detection and characteristic mass were 30 pg and 43 pg, respectively. Accuracy and precision of the method have been evaluated using microwave-assisted acid digestion of the samples with subsequent determination by HR-CS GF AAS and ICP-MS; the results were in agreement (95% confidence level) with those of the proposed method. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of mercury in agroindustrial samples by flow-injection cold vapor atomic absorption spectrometry using ion exchange and reductive elution.

PubMed

Gomes Neto, J A; Zara, L F; Rocha, J C; Santos, A; Dakuzaku, C S; Nóbrega, J A

2000-03-06

A flow-injection system with a Chelite-S(R) cationic resin packed minicolumn is proposed for the determination of trace levels of mercury in agroindustrial samples by cold vapor atomic absorption spectrometry. Improved sensitivity and selectivity are attained since mercuric ions are on-line concentrated whereas other potential interferents are discarded. With on-line reductive elution procedure, concentrated hydrochloric acid could be replaced by 10% w/v SnCl(2), in 6 M HCl as eluent. The reversed-intermittent stream either carries the atomic mercury to the flow cell in the forward direction or removes the residue from reactor/gas-liquid separator to a discarding flask in the opposite direction. Concentration and volume of reagent, acidity, flow rates, commutation times and potential interfering species were investigated. For 120 s preconcentration time, the proposed system handles about 25 samples h(-1) (50.0-500 ng l(-1)), consuming about 10 ml sample and 5 mg SnCl(2) per determination. The detection limit is 0.8 ng l(-1) and the relative standard deviation (RSD) (n=12) of a 76.7 ng l(-1) sample is about 5%. Results are in agreement with certified value of standard materials at 95% confidence level and good recoveries (97-128%) of spiked samples were found.

Development of a simple method for the determination of lead in lipstick using alkaline solubilization and graphite furnace atomic absorption spectrometry.

PubMed

Soares, Aline Rodrigues; Nascentes, Clésia Cristina

2013-02-15

A simple method was developed for determining the total lead content in lipstick samples by graphite furnace atomic absorption spectrometry (GFAAS) after treatment with tetramethylammonium hydroxide (TMAH). Multivariate optimization was used to establish the optimal conditions of sample preparation. The graphite furnace heating program was optimized through pyrolysis and atomization curves. An aliquot containing approximately 50mg of the sample was mixed with TMAH and heated in a water bath at 60°C for 60 min. Using Nb as the permanent modifier and Pd as the chemical modifier, the optimal temperatures were 900°C and 1800°C for pyrolysis and atomization, respectively. Under optimum conditions, the working range was from 1.73 to 50.0 μg L(-1), with detection and quantification limits of 0.20 and 0.34 μg g(-1), respectively. The precision was evaluated under conditions of repeatability and intermediate precision and showed standard deviations of 2.37%-4.61% and 4.93%-9.75%, respectively. The % recovery ranged from 96.2% to 109%, and no significant differences were found between the results obtained using the proposed method and the microwave decomposition method for real samples. Lead was detected in 21 tested lipstick samples; the lead content in these samples ranged from 0.27 to 4.54 μg g(-1). Copyright © 2012 Elsevier B.V. All rights reserved.

Atomic-absorption spectrometric determination of cobalt, nickel, and copper in geological materials with matrix masking and chelation-extraction

USGS Publications Warehouse

Sanzolone, R.F.; Chao, T.T.; Crenshaw, G.L.

1979-01-01

An atomic-absorption spectrometric method is reported for the determination of cobalt, nickel, and copper in a variety of geological materials including iron- and manganese-rich, and calcareous samples. The sample is decomposed with HP-HNO3 and the residue is dissolved in hydrochloric acid. Ammonium fluoride is added to mask iron and 'aluminum. After adjustment to pH 6, cobalt, nickel, and copper are chelated with sodium diethyl-dithiocarbamate and extracted into methyl isobutyl ketone. The sample is set aside for 24 h before analysis to remove interferences from manganese. For a 0.200-g sample, the limits of determination are 5-1000 ppm for Co, Ni, and Cu. As much as 50% Fe, 25% Mn or Ca, 20% Al and 10% Na, K, or Mg in the sample either individually or in various combinations do not interfere. Results obtained on five U.S. Geological Survey rock standards are in general agreement with values reported in the literature. ?? 1979.

Photon interaction study of organic nonlinear optical materials in the energy range 122-1330 keV

NASA Astrophysics Data System (ADS)

Awasarmol, Vishal V.; Gaikwad, Dhammajyot K.; Raut, Siddheshwar D.; Pawar, Pravina P.

2017-01-01

In the present study, the mass attenuation coefficient (μm) of six organic nonlinear optical materials has been calculated in the energy range 122-1330 keV and compared with the obtained values from the WinXCOM program. It is found that there is a good agreement between theoretical and experimental values (<3%). The linear attenuation coefficients (μ) total atomic cross section (σt, a), and total electronic cross section (σt, el) have also been calculated from the obtained μm values and their variations with photon energy have been plotted. From the present work, it is observed that the variation of obtained values of μm, μ, σt, a, and σt, el strongly depends on the photon energy and decreases or increases due to chemical composition and density of the sample. All the samples have been studied extensively using transmission method with a view to utilize the material for radiation dosimetry. Investigated samples are good material for radiation dosimetry due their low effective atomic number. The mass attenuation coefficient (μm), linear attenuation coefficients (μ), total atomic cross section (σt, a), total electronic cross section (σt, el), effective atomic numbers (Zeff), molar extinction coefficient (ε), mass energy absorption coefficient (μen/ρ) and effective atomic energy absorption cross section (σa, en) of all sample materials have been carried out and transmission curves have been plotted. The transmission curve shows that the variation of all sample materials decreases with increasing photon energy.

Analytical characteristics of a continuum-source tungsten coil atomic absorption spectrometer.

PubMed

Rust, Jennifer A; Nóbrega, Joaquim A; Calloway, Clifton P; Jones, Bradley T

2005-08-01

A continuum-source tungsten coil electrothermal atomic absorption spectrometer has been assembled, evaluated, and employed in four different applications. The instrument consists of a xenon arc lamp light source, a tungsten coil atomizer, a Czerny-Turner high resolution monochromator, and a linear photodiode array detector. This instrument provides simultaneous multi-element analyses across a 4 nm spectral window with a resolution of 0.024 nm. Such a device might be useful in many different types of analyses. To demonstrate this broad appeal, four very different applications have been evaluated. First of all, the temperature of the gas phase was measured during the atomization cycle of the tungsten coil, using tin as a thermometric element. Secondly, a summation approach for two absorption lines for aluminum falling within the same spectral window (305.5-309.5 nm) was evaluated. This approach improves the sensitivity without requiring any additional preconcentration steps. The third application describes a background subtraction technique, as it is applied to the analysis of an oil emulsion sample. Finally, interference effects caused by Na on the atomization of Pb were studied. The simultaneous measurements of Pb and Na suggests that negative interference arises at least partially from competition between Pb and Na atoms for H2 in the gas phase.

21 CFR 862.2850 - Atomic absorption spectrophotometer for clinical use.

Code of Federal Regulations, 2012 CFR

2012-04-01

... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Atomic absorption spectrophotometer for clinical... Laboratory Instruments § 862.2850 Atomic absorption spectrophotometer for clinical use. (a) Identification. An atomic absorption spectrophotometer for clinical use is a device intended to identify and measure...

21 CFR 862.2850 - Atomic absorption spectrophotometer for clinical use.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Atomic absorption spectrophotometer for clinical... Laboratory Instruments § 862.2850 Atomic absorption spectrophotometer for clinical use. (a) Identification. An atomic absorption spectrophotometer for clinical use is a device intended to identify and measure...

21 CFR 862.2850 - Atomic absorption spectrophotometer for clinical use.

Code of Federal Regulations, 2013 CFR

2013-04-01

... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Atomic absorption spectrophotometer for clinical... Laboratory Instruments § 862.2850 Atomic absorption spectrophotometer for clinical use. (a) Identification. An atomic absorption spectrophotometer for clinical use is a device intended to identify and measure...

21 CFR 862.2850 - Atomic absorption spectrophotometer for clinical use.

Code of Federal Regulations, 2014 CFR

2014-04-01

... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Atomic absorption spectrophotometer for clinical... Laboratory Instruments § 862.2850 Atomic absorption spectrophotometer for clinical use. (a) Identification. An atomic absorption spectrophotometer for clinical use is a device intended to identify and measure...

Current role of ICP-MS in clinical toxicology and forensic toxicology: a metallic profile.

PubMed

Goullé, Jean-Pierre; Saussereau, Elodie; Mahieu, Loïc; Guerbet, Michel

2014-08-01

As metal/metalloid exposure is inevitable owing to its omnipresence, it may exert toxicity in humans. Recent advances in metal/metalloid analysis have been made moving from flame atomic absorption spectrometry and electrothermal atomic absorption spectrometry to the multi-elemental inductively coupled plasma (ICP) techniques as ICP atomic emission spectrometry and ICP-MS. ICP-MS has now emerged as a major technique in inorganic analytical chemistry owing to its flexibility, high sensitivity and good reproducibility. This in depth review explores the ICP-MS metallic profile in human toxicology. It is now routinely used and of great importance, in clinical toxicology and forensic toxicology to explore biological matrices, specifically whole blood, plasma, urine, hair, nail, biopsy samples and tissues.

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.

Method for the determination of cobalt from biological products with graphite furnace atomic absorption spectrometer

NASA Astrophysics Data System (ADS)

Zamfir, Oana-Liliana; Ionicǎ, Mihai; Caragea, Genica; Radu, Simona; Vlǎdescu, Marian

2016-12-01

Cobalt is a chemical element with symbol Co and atomic number 27 and atomic weight 58.93. 59 Co is the only stable cobalt isotope and the only isotope to exist naturally on Earth. Cobalt is the active center of coenzymes called cobalamin or cyanocobalamin the most common example of which is vitamin B12. Vitamin B12 deficiency can potentially cause severe and irreversible damage, especially to the brain and nervous system in the form of fatigue, depression and poor memory or even mania and psychosis. In order to study the degree of deficiency of the population with Co or the correctness of treatment with vitamin B12, a modern optoelectronic method for the determination of metals and metalloids from biological samples has been developed, Graphite Furnace - Atomic Absorption Spectrometer (GF- AAS) method is recommended. The technique is based on the fact that free atoms will absorb light at wavelengths characteristic of the element of interest. Free atoms of the chemical element can be produced from samples by the application of high temperatures. The system GF-AAS Varian used as biological samples, blood or urine that followed the digest of the organic matrix. For the investigations was used a high - performance GF-AAS with D2 - background correction system and a transversely heated graphite atomizer. As result of the use of the method are presented the concentration of Co in the blood or urine of a group of patient in Bucharest. The method is sensitive, reproducible relatively easy to apply, with a moderately costs.

Arsenic Speciation of Waters from the Aegean Region, Turkey by Hydride Generation: Atomic Absorption Spectrometry.

PubMed

Çiftçi, Tülin Deniz; Henden, Emur

2016-08-01

Arsenic in drinking water is a serious problem for human health. Since the toxicity of arsenic species As(III) and As(V) is different, it is important to determine the concentrations separately. Therefore, it is necessary to develop an accurate and sensitive method for the speciation of arsenic. It was intended with this work to determine the concentrations of arsenic species in water samples collected from Izmir, Manisa and nearby areas. A batch type hydride generation atomic absorption spectrometer was used. As(V) gave no signal under the optimal measurement conditions of As(III). A certified reference drinking water was analyzed by the method and the results showed excellent agreement with the reported values. The procedure was applied to 34 water samples. Eleven tap water, two spring water, 19 artesian well water and two thermal water samples were analyzed under the optimal conditions.

Determination of gold and cobalt dopants in advanced materials based on tin oxide by slurry sampling high-resolution continuum source graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Filatova, Daria G.; Eskina, Vasilina V.; Baranovskaya, Vasilisa B.; Vladimirova, Svetlana A.; Gaskov, Alexander M.; Rumyantseva, Marina N.; Karpov, Yuri A.

2018-02-01

A novel approach is developed for the determination of Co and Au dopants in advanced materials based on tin oxide using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS) with direct slurry sampling. Sodium carboxylmethylcellulose (Na-CMC) is an effective stabilizer for diluted suspensions. Use Na-CMC allows to transfer the analytes into graphite furnace completely and reproducibly. The relative standard deviation obtained by HR CS GFAAS was not higher than 4%. Accuracy was proven by means inductively coupled plasma mass spectrometry (ICP-MS) in solutions after decomposition as a comparative technique. To determine Au and Co in the volume of SnO2, the acid decomposition conditions (HCl, HF) of the samples were suggested by means of an autoclave in a microwave oven.

Cloud point extraction thermospray flame quartz furnace atomic absorption spectrometry for determination of ultratrace cadmium in water and urine

NASA Astrophysics Data System (ADS)

Wu, Peng; Zhang, Yunchang; Lv, Yi; Hou, Xiandeng

2006-12-01

A simple, low cost and highly sensitive method based on cloud point extraction (CPE) for separation/preconcentration and thermospray flame quartz furnace atomic absorption spectrometry was proposed for the determination of ultratrace cadmium in water and urine samples. The analytical procedure involved the formation of analyte-entrapped surfactant micelles by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution and a Triton X-114 solution. When the temperature of the system was higher than the cloud point of Triton X-114, the complex of cadmium-PDC entered the surfactant-rich phase and thus separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, the limit of detection was 0.04 μg/L for cadmium with a sample volume of 10 mL. The analytical results of cadmium in water and urine samples agreed well with those by ICP-MS.

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF METALS FROM SOIL, DUST, AIR FILTER, AND SURFACE AND DERMAL WIPE SAMPLES FOR AA (GRAPHITE FURNACE OR FLAME) OR ICP-AES ANALYSIS (BCO-L-3.1)

EPA Science Inventory

The purpose of this SOP is to describe the acid digestion of soil, house dust, air filter, and surface or dermal wipe samples for analysis using inductively coupled plasma atomic emissions spectrometry (ICP-AES) and/or graphite furnace atomic absorption spectrometry (GFAAS) or fl...

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.

Determination of Lead in Blood by Atomic Absorption Spectrophotometry1

PubMed Central

Selander, Stig; Cramér, Kim

1968-01-01

Lead in blood was determined by atomic absorption spectrophotometry, using a wet ashing procedure and a procedure in which the proteins were precipitated with trichloroacetic acid. In both methods the lead was extracted into isobutylmethylketone before measurement, using ammonium pyrrolidine dithiocarbamate as chelator. The simpler precipitation procedure was shown to give results identical with those obtained with the ashing technique. In addition, blood specimens were examined by the precipitation method and by spectral analysis, which method includes wet ashing of the samples, with good agreement. All analyses were done on blood samples from `normal' persons or from lead-exposed workers, and no additions of inorganic lead were made. The relatively simple protein precipitation technique gave accurate results and is suitable for the large-scale control of lead-exposed workers. PMID:5663425

Ultrasensitive determination of cadmium in seawater by hollow fiber supported liquid membrane extraction coupled with graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Peng, Jin-feng; Liu, Rui; Liu, Jing-fu; He, Bin; Hu, Xia-lin; Jiang, Gui-bin

2007-05-01

A new procedure, based on hollow fiber supported liquid membrane preconcentration coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection, was developed for the determination of trace Cd in seawater samples. With 1-octanol that contained a mixture of dithizone (carrier) and oleic acid immobilized in the pores of the polypropylene hollow fiber as a liquid membrane, Cd was selectively extracted from water samples into 0.05 M HNO 3 that filled the lumen of the hollow fiber as a stripping solution. The main extraction related parameters were optimized, and the effects of salinity and some coexisting interferants were also evaluated. Under the optimum extraction conditions, an enrichment factor of 387 was obtained for a 100-mL sample solution. In combination with graphite furnace atomic absorption spectrometry, a very low detection limit (0.8 ng L - 1 ) and a relative standard deviation (2.5% at 50 ng L - 1 level) were achieved. Five seawater samples were analyzed by the proposed method without dilution, with detected Cd concentration in the range of 56.4-264.8 ng L - 1 and the relative spiked recoveries over 89%. For comparison, these samples were also analyzed by the Inductively Coupled Plasma Mass Spectrometry (ICP-MS) method after a 10-fold dilution for matrix effect elimination. Statistical analysis with a one-way ANOVA shows no significant differences (at 0.05 level) between the results obtained by the proposed and ICP-MS methods. Additionally, analysis of certified reference materials (GBW (E) 080040) shows good agreement with the certified value. These results indicate that this present method is very sensitive and reliable, and can effectively eliminate complex matrix interferences in seawater samples.

Variable thickness double-refracting plate

DOEpatents

Hadeishi, Tetsuo

1976-01-01

This invention provides an A.C., cyclic, current-controlled, phase retardation plate that uses a magnetic clamp to produce stress birefringence. It was developed for an Isotope-Zeeman Atomic Absorption Spectrometer that uses polarization modulation to effect automatic background correction in atomic absorption trace-element measurements. To this end, the phase retardation plate of the invention is a variable thickness, photoelastic, double-refracting plate that is alternately stressed and released by the magnetic clamp selectively to modulate specific components selected from the group consisting of circularly and plane polarized Zeeman components that are produced in a dc magnetic field so that they correspond respectively to Zeeman reference and transmission-probe absorption components. The polarization modulation changes the phase of these polarized Zeeman components, designated as .sigma. reference and .pi. absorption components, so that every half cycle the components change from a transmission mode to a mode in which the .pi. component is blocked and the .sigma. components are transmitted. Thus, the Zeeman absorption component, which corresponds in amplitude to the amount of the trace element to be measured in a sample, is alternately transmitted and blocked by a linear polarizer, while the circularly polarized reference components are continuously transmitted thereby. The result is a sinusoidally varying output light amplitude whose average corresponds to the amount of the trace element present in the sample.

A comparison of simultaneous plasma, atomic absorption, and iron colorimetric determinations of major and trace constituents in acid mine waters

USGS Publications Warehouse

Ball, J.W.; Nordstrom, D. Kirk

1994-01-01

Sixty-three water samples collected during June to October 1982 from the Leviathan/Bryant Creek drainage basin were originally analyzed by simultaneous multielement direct-current plasma (DCP) atomic-emission spectrometry, flame atomic-absorption spectrometry, graphite-furnace atomic-absorption spectrometry (GFAAS) (thallium only), ultraviolet-visible spectrometry, and hydride-generation atomic-absorption spectrometry.Determinations were made for the following metallic and semi-metallic constituents: AI, As, B, Ba, Be, Bi, Cd, Ca, Cr, Co, Cu, Fe(11), Fe(total), Li, Pb, Mg, Mn, Mo, Ni, K, Sb, Se, Si, Na, Sr, TI, V, and Zn. These samples were re-analyzed later by simultaneous multielement inductively coupled plasma (ICP) atomic-emission spectrometry and Zeeman-corrected GFAAS to determine the concentrations of many of the same constituents with improved accuracy, precision, and sensitivity. The result of this analysis has been the generation of comparative concentration values for a significant subset of the solute constituents. Many of the more recently determined values replace less-than-detection values for the trace metals; others constitute duplicate analyses for the major constituents. The multiple determinations have yielded a more complete, accurate, and precise set of analytical data. They also have resulted in an opportunity to compare the performance of the plasma-emission instruments operated in their respective simultaneous multielement modes. Flame atomic-absorption spectrometry was judged best for Na and K and hydride-generation atomic-absorption spectrometry was judged best for As because of their lower detection limit and relative freedom from interelement spectral effects. Colorimetric determination using ferrozine as the color agent was judged most accurate, precise, and sensitive for Fe. Cadmium, lead, and vanadium concentrations were too low in this set of samples to enable a determination of whether ICP or DCP is a more suitable technique. Of the remaining elements, Ba, Be, Ca, Cr, Mg, Mn, Sr, and Zn have roughly equivalent accuracy, precision, and detection limit by ICP and DCP. Cobalt and Ni were determined to be better analyzed by ICP, because of lower detection limits; B, Cu, Mo, and Si were determined to be better analyzed by DCP, because of relative freedom from interferences. The determination oral by DCP was far more sensitive, owing to the use of a more sensitive wavelength, compared with the ICP. However, there is a very serious potential interference from a strong Ca emission line near the 396.15 nanometer DCP wavelength. Thus, there is no clear choice between the plasma techniques tested, for the determination oral. The ICP and DCP detection limits are typically between 0.001 and 0.5 milligrams per liter in acid mine waters. For those metals best analyzed by ICP and/or DCP, but below these limits, GFAAS is the method of choice because of its relatively greater sensitivity and specificity. Six of the elements were not determined by DCP, ICP or Zeeman-corrected GFAAS, and are not discussed in this report. These elements are: Bi, Fe(11), Li, Sb, Se, and TI.

Determination of nickel in water, food, and biological samples by electrothermal atomic absorption spectrometry after preconcentration on modified carbon nanotubes.

PubMed

Taher, Mohammad Ali; Mazaheri, Lida; Ashkenani, Hamid; Mohadesi, Alireza; Afzali, Daryoush

2014-01-01

A new and sensitive SPE method using modified carbon nanotubes for extraction and preconcentration, and electrothermal atomic absorption spectrometric determination of nickel (Ni) in real samples at ng/L levels was investigated. First, multiwalled carbon nanotubes were oxidized with concentrated HNO3, then modified with 2-(5-bormo-2-pyridylazo)-5-diethylaminophenol reagent. The adsorption was achieved quantitatively on a modified carbon nanotubes column in a pH range of 6.5 to 8.5; the adsorbed Ni(II) ions were then desorbed by passing 5.0 mL of 1 M HNO3. The effects of analytical parameters, including pH of the solution, eluent type and volume, sample volume, flow rate of the eluent, and matrix ions, were investigated for optimization of the presented procedure. The enrichment factor was 180, and the LOD for Ni was 4.9 ng/L. The method was applied to the determination of Ni in water, food, and biological samples, and reproducible results were obtained.

Atomic absorption spectrometric determination of copper, zinc, and lead in geological materials

USGS Publications Warehouse

Sanzolone, R.F.; Chao, T.T.

1976-01-01

An atomic absorption spectrometric method is described for the determination of copper, zinc, and lead in geological materials. The sample is digested with HF-HCl-H2O2; the final solution for analysis is in 10 % (v/v) HCl. Copper and zinc are determined directly by aspirating the solution into an air-acetylene flame. A separate aliquot of the solution is used for determination of lead; lead is extracted into TOPO-MIBK from the acidic solution in the presence of iodide and ascorbic acid. For a 0.50-g sample, the limits of determination are 10-2000 p.p.m. for Cu and Zn, and 5-5000 p.p.m. for Pb. As much as 40 % Fe or Ca. and 10 % Al, Mg, or Mn in the sample do not interfere. The proposed method can be applied to the determination of copper, zinc, and lead in a wide range of geological materials including iron- and manganese-rich, calcareous and carbonate samples. ?? 1976.

Automatic flow-batch system for cold vapor atomic absorption spectroscopy determination of mercury in honey from Argentina using online sample treatment.

PubMed

Domínguez, Marina A; Grünhut, Marcos; Pistonesi, Marcelo F; Di Nezio, María S; Centurión, María E

2012-05-16

An automatic flow-batch system that includes two borosilicate glass chambers to perform sample digestion and cold vapor atomic absorption spectroscopy determination of mercury in honey samples was designed. The sample digestion was performed by using a low-cost halogen lamp to obtain the optimum temperature. Optimization of the digestion procedure was done using a Box-Behnken experimental design. A linear response was observed from 2.30 to 11.20 μg Hg L(-1). The relative standard deviation was 3.20% (n = 11, 6.81 μg Hg L(-1)), the sample throughput was 4 sample h(-1), and the detection limit was 0.68 μg Hg L(-1). The obtained results with the flow-batch method are in good agreement with those obtained with the reference method. The flow-batch system is simple, allows the use of both chambers simultaneously, is seen as a promising methodology for achieving green chemistry goals, and is a good proposal to improving the quality control of honey.

Trace of heavy metals in maternal and umbilical cord blood samples in association with birth outcomes in Baghdad, Iraq

NASA Astrophysics Data System (ADS)

Hasan Rhaif Al-Sahlanee, Mayyadah; Maizan Ramli, Ramzun; Abdul Hassan Ali, Miami; Fadhil Tawfiq, Nada; Zahirah Noor Azman, Nurul; Abdul Rahman, Azhar; Shahrim Mustafa, Iskandar; Noor Ashikin Nik Abdul Razak, Nik; Zakiah Yahaya, Nor; Mohammed Al-Marri, Hana; Syuhada Ayob, Nur; Zakaria, Nabela

2017-10-01

Trace elements are essential nutritional components in humans and inconvenient tissue content that have a significant influence on infant size. The aim of this study is to evaluate the effects of concentration of elements (uranium (U), lead (Pb) and iron (Fe)) and absorption of Pb and Fe on maternal and umbilical cord blood samples. The concentration and absorption of Pb and Fe in blood samples were determined by using atomic absorption spectrophotometry device, while the uranium concentration was determined by using CR-39 detector. Fifty women of age 16-44 years are involved in this study. Results show that the maximum and minimum values of both concentration and absorption in the maternal samples were for Pb and Fe, respectively. In addition, for umbilical cord, the maximum values of concentration and absorption were for Fe and the minimum concentration and absorption were for U and Pb, respectively. A significant correlation between maternal and umbilical cord blood samples was found. This indicates that the Pb, U and Fe elements can easily transfer from maternal to the fetal body which impacts the growth of fetus.

Mid-Infrared Properties of OH Megamaser Host Galaxies. I. Spitzer IRS Low- and High-Resolution Spectroscopy

NASA Astrophysics Data System (ADS)

Willett, Kyle W.; Darling, Jeremy; Spoon, Henrik W. W.; Charmandaris, Vassilis; Armus, Lee

2011-03-01

We present mid-infrared spectra and photometry from the Infrared Spectrograph on the Spitzer Space Telescope for 51 OH megamasers (OHMs), along with 15 galaxies confirmed to have no megamaser emission above L OH = 102.3 L sun. The majority of galaxies display moderate-to-deep 9.7 μm amorphous silicate absorption, with OHM galaxies showing stronger average absorption and steeper 20-30 μm continuum emission than non-masing galaxies. Emission from multiple polycyclic aromatic hydrocarbons (PAHs), especially at 6.2, 7.7, and 11.3 μm, is detected in almost all systems. Fine-structure atomic emission (including [Ne II], [Ne III], [S III], and [S IV]) and multiple H2 rotational transitions are observed in more than 90% of the sample. A subset of galaxies show emission from rarer atomic lines, such as [Ne V], [O IV], and [Fe II]. Fifty percent of the OHMs show absorption from water ice and hydrogenated amorphous carbon grains, while absorption features from CO2, HCN, C2H2, and crystalline silicates are also seen in several OHMs. Column densities of OH derived from 34.6 μm OH absorption are similar to those derived from 1667 MHz OH absorption in non-masing galaxies, indicating that the abundance of masing molecules is similar for both samples. This data paper presents full mid-infrared spectra for each galaxy, along with measurements of line fluxes and equivalent widths, absorption feature depths, and spectral indices.

The determination of vanadium in brines by atomic absorption spectroscopy

USGS Publications Warehouse

Crump-Wiesner, Hans J.; Feltz, H.R.; Purdy, W.C.

1971-01-01

A standard addition method is described for the determination of vanadium in brines by atomic absorption spectroscopy with a nitrous oxide-acetylene flame. Sample pH is adjusted to 1.0 with concentrated hydrochloric acid and the vanadium is directly extracted with 5% cupferron in methyl isobutyl ketone (MIBK). The ketone layer is then aspirated into the flame and the recorded absorption values are plotted as a function of the concentration of the added metal. As little as 2.5 ??g l-1 of vanadium can be detected under the conditions of the procedure. Tungsten and tin interfere when present in excess of 5 and 10 ??g ml-1, respectively. The concentrations of the two interfering ions normally found in brines are well below interference levels. ?? 1971.

Temperature-controlled electrothermal atomization-atomic absorption spectrometry using a pyrometric feedback system in conjunction with a background monitoring device

NASA Astrophysics Data System (ADS)

Van Deijck, W.; Roelofsen, A. M.; Pieters, H. J.; Herber, R. F. M.

The construction of a temperature-controlled feedback system for electrothermal atomization-atomic absorption spectrometry (ETA-AAS) using an optical pyrometer applied to the atomization stage is described. The system was used in conjunction with a fast-response background monitoring device. The heating rate of the furnace amounted to 1400° s -1 with a reproducibility better than 1%. The precision of the temperature control at a steady state temperature of 2000°C was 0.1%. The analytical improvements offered by the present system have been demonstrated by the determination of cadmium and lead in blood and finally by the determination of lead in serum. Both the sensitivity and the precision of the method have been improved. The accuracy of the method was checked by determining the lead content for a number of scrum samples both by ETA-AAS and differential pulse anodic stripping voltametry (DPASV) and proved to be satisfactory.

QA/QC Guidance for Sampling and Analysis of Sediments, Water, and Tissues for Dredged Material Evaluations: Chemical Evaluations

DTIC Science & Technology

1995-04-01

J. Biochem. Physiol. 37:911-917. Bloom, N.S., E.A. Crecelius, and S . Berman . 1983. Determination of mercury in seawater at sub-nanogram per liter...procedure for determination of trace metal in seawater by atomic absorption spectrometry with electrothermal atomization. Anal. Chern. Acta 98:47-55...Nakashima, S ., R.E. Sturgeon, S.N. Willie, and S.S. Berman . 1988. Acid digestion of marine sample for trace element analysis using microwave heating

Determination of papaverine and cocaine by use of a precipitation system coupled on-line to an atomic absorption spectrometer.

PubMed

Eisman, M; Gallego, M; Varcárcel, M

1994-02-01

A continuous-precipitation flame-atomization atomic absorption spectrometric method for the determination of papaverine and cocaine hydrochlorides is proposed. The method is based on the precipitation of reineckates by injection of Reinecke's salt into a carrier containing the alkaloids and their subsequent retention on a stainless steel filter. In this way, papaverine and cocaine hydrochlorides can be determine over the ranges 5-85 and 50-850 micrograms ml-1 with a relative standard deviation of 1.3 and 3.2%, respectively, and a sampling frequency of 150 h-1. The proposed method is more sensitive and selective for papaverine than it is for cocaine and can be applied to the determination of papaverine HCl in pharmaceutical preparations.

Atomic-absorption determination of mercury in geological materials by flame and carbon-rod atomisation after solvent extraction and using co-extracted silver as a matrix modifier

USGS Publications Warehouse

Sanzolone, R.F.; Chao, T.T.

1983-01-01

Based on modifications and expansion of the original Tindall's solvent extraction flame atomic-absorption procedure, an atomic-absorption spectrophotometric method has been developed for the determination of mercury in geological materials. The sample is digested with nitric and hydrochloric acids in a boiling water-bath. The solution is made ammoniacal and potassium iodide and silver nitrate are added. The mercury is extracted into isobutyl methyl ketone as the tetraiodomercurate(ll). Added silver is co-extracted with mercury and serves as a matrix modifier in the carbon-rod atomiser. The mercury in the isobutyl methyl ketone extract may be determined by either the flame- or the carbon-rod atomisation method, depending on the concentration level. The limits of determination are 0.05-10 p.p.m. of mercury for the carbon-rod atomisation and 1 -200 p.p.m. of mercury for the flame atomisation. Mercury values for reference samples obtained by replicate analyses are in good agreement with those reported by other workers, with relative standard deviations ranging from 2.3 to 0.9%. Recoveries of mercury spiked at two levels were 93-106%. Major and trace elements commonly found in geological materials do not interfere.

Analysis of metal-laden water via portable X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Pearson, Delaina; Weindorf, David C.; Chakraborty, Somsubhra; Li, Bin; Koch, Jaco; Van Deventer, Piet; de Wet, Jandre; Kusi, Nana Yaw

2018-06-01

A rapid method for in-situ elemental composition analysis of metal-laden water would be indispensable for studying polluted water. Current analytical lab methods to determine water quality include flame atomic absorption spectrometry (FAAS), atomic absorption spectrophotometry (AAS), electrothermal atomic absorption spectrometry (EAAS), and inductively coupled plasma (ICP) spectroscopy. However only two field methods, colorimetry and absorptiometry, exist for elemental analysis of water. Portable X-ray fluorescence (PXRF) spectrometry is an effective method for elemental analysis of soil, sediment, and other matrices. However, the accuracy of PXRF is known to be affected while scanning moisture-laden soil samples. This study sought to statistically establish PXRF's predictive ability for various elements in water at different concentrations relative to inductively coupled plasma atomic emission spectroscopy (ICP-AES). A total of 390 metal-laden water samples collected from leaching columns of mine tailings in South Africa were analyzed via PXRF and ICP-AES. The PXRF showed differential effectiveness in elemental quantification. For the collected water samples, the best relationships between ICP and PXRF elemental data were obtained for K and Cu (R2 = 0.92). However, when scanning ICP calibration solutions with elements in isolation, PXRF results indicated near perfect agreement; Ca, K, Fe, Cu and Pb produced an R2 of 0.99 while Zn and Mn produced an R2 of 1.00. The utilization of multiple PXRF (stacked) beams produced stronger correlation to ICP relative to the use of a single beam in isolation. The results of this study demonstrated the PXRF's ability to satisfactorily predict the composition of metal-laden water as reported by ICP for several elements. Additionally this study indicated the need for a "Water Mode" calibration for the PXRF and demonstrates the potential of PXRF for future study of polluted or contaminated waters.

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.

Rapid separation on copper powder of total mercury in blood and determination of mercury by flameless atomic absorption spectrometry.

PubMed

Dogan, S; Haerdi, W

1979-01-01

The determination of mercury in blood by flameless atomic absorption spectrometry (FAAS) has been described. Prior to its analysis, the sample was decomposed by combustion and separated on a copper powder micro-column. A special type of cell has been used which gives a better sensitivity compared with the types of cells described in the literature and the method of FAAS analysis has been improved. The sensitivity of 0.1 ng for 1% absorbance was observed and the standard deviation for six determinations at this level was found to be +/- 0.05 ng, for 95% probability.

Automated atomic absorption spectrometric determination of total arsenic in water and streambed materials

USGS Publications Warehouse

Fishman, M.

1977-01-01

An automated method to determine both inorganic and organic forms of arsenic In water, water-suspended mixtures, and streambed materials Is described. Organic arsenic-containing compounds are decomposed by either ultraviolet radiation or by suHurlc acid-potassium persulfate digestion. The arsenic liberated, with Inorganic arsenic originally present, is reduced to arsine with sodium borohydrlde. The arable Is stripped from the solution with the aid of nitrogen and Is then decomposed In a tube furnace heated to 800 ??C which Is placed in the optical path of an atomic absorption spectrometer. Thirty samples per hour can be analyzed to levels of 1 ??g arsenic per liter.

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

PubMed

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

2007-12-01

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

40 CFR Appendix A to Subpart C of... - Alternative Testing Methods Approved for Analyses Under the Safe Drinking Water Act

Code of Federal Regulations, 2010 CFR

2010-07-01

... Absorption D 3697-07 Atomic Absorption; Furnace 3113 B Axially viewed inductively coupled plasma-atomic... C Hydride Atomic Absorption 3114 B D 2972-08 B Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES) 200.5, Revision 4.2. Barium Inductively Coupled Plasma 3120 B Atomic...

Comparison of Adsorbed Mercury Screening Method With Cold-Vapor Atomic Absorption Spectrophotometry for Determination of Mercury in Soil

NASA Technical Reports Server (NTRS)

Easterling, Donald F.; Hovanitz, Edward S.; Street, Kenneth W.

2000-01-01

A field screening method for the determination of elemental mercury in environmental soil samples involves the thermal desorption of the mercury from the sample onto gold and then the thermal desorption from the gold to a gold-film mercury vapor analyzer. This field screening method contains a large number of conditions that could be optimized for the various types of soils encountered. In this study, the conditions were optimized for the determination of mercury in silty clay materials, and the results were comparable to the cold-vapor atomic absorption spectrophotometric method of determination. This paper discusses the benefits and disadvantages of employing the field screening method and provides the sequence of conditions that must be optimized to employ this method of determination on other soil types.

Effect of Ram and Zenith Exposure on the Optical Properties of Polymers in Space

NASA Technical Reports Server (NTRS)

Li, Yuachun; de Groh, Kim K.; Banks, Bruce A.; Leneghan, Halle; Asmar, Olivia

2017-01-01

The temperature of spacecraft is influenced by the solar absorptance and thermal emittance of the external spacecraft materials. Optical and thermal properties can degrade over time in the harsh low Earth orbital (LEO) space environment where spacecraft external materials are exposed to various forms of radiation, thermal cycling, and atomic oxygen. Therefore, it is important to test the durability of spacecraft materials in the space environment. One objective of the Polymers and Zenith Polymers Experiments was to determine the effect of LEO space exposure on the optical properties of various spacecraft polymers. These experiments were flown as part of the Materials International Space Station Experiment 7 (MISSE 7) mission on the exterior of the International Space Station (ISS) for 1.5 years. Samples were flown in ram, wake or zenith directions, receiving varying amounts of atomic oxygen and solar radiation exposure. Total and diffuse reflectance and transmittance of flight and corresponding control samples were obtained post-flight using a Cary 5000 UV-Vis-NIR Spectrophotometer. Integrated air mass zero solar absorptance (s) of the flight and control samples were computed from the total transmittance and reflectance, and compared. The optical data are compared with similar polymers exposed to space for four years as part of MISSE 2, and with atomic oxygen erosion data, to help understand the degradation of these polymers in the space environment. Results show that prolonged space exposure increases the solar absorptance of some materials. Knowing which polymers remain stable will benefit future spacecraft design.

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. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of Cu, Cd, Pb and Cr in yogurt by slurry sampling electrothermal atomic absorption spectrometry: A case study for Brazilian yogurt.

PubMed

de Andrade, Camila Kulek; de Brito, Patrícia Micaella Klack; Dos Anjos, Vanessa Egéa; Quináia, Sueli Pércio

2018-02-01

A slurry sampling electrothermal atomic absorption spectrometric method is proposed for the determination of trace elements such as Cu, Cr, Cd and Pb in yogurt. The main factors affecting the slurry preparation were optimized: nature and concentration of acid solution and sonication time. The analytical method was validated in-house by calibration, linearity, limits of detection and quantification, precision and accuracy test obtaining satisfactory results in all cases. The proposed method was applied for the determination of Cd, Cr, Cu and Pb in some Brazilian yogurt samples. For these samples, the concentrations ranged from 2.5±0.2 to 12.4±0.2ngg -1 ; 34±3 to 899±7ngg -1 ; <8.3 to 12±1ngg -1 ; and <35.4 to 210±16ngg -1 for Cd, Cu, Cr and Pb, respectively. The daily intake of Cd, Cu, Cr and Pb via consumption of these samples was estimated. Copyright © 2017 Elsevier Ltd. All rights reserved.

Fast determination of phosphorus in honey, milk and infant formulas by electrothermal atomic absorption spectrometry using a slurry sampling procedure

NASA Astrophysics Data System (ADS)

López-García, I.; Viñas, P.; Romero-Romero, R.; Hernández-Córdoba, M.

2007-01-01

A procedure for the electrothermal atomic absorption spectrometric determination of phosphorus in honey, milk and infant formulas using slurried samples is described. Suspensions prepared in a medium containing 50% v/v concentrated hydrogen peroxide, 1% v/v concentrated nitric acid, 10% m/v glucose, 5% m/v sucrose and 100 mg l - 1 of potassium were introduced directly into the furnace. For the honey samples, multiple injection of the sample was necessary. The modifier selected was a mixture of 20 μg palladium and 5 μg magnesium nitrate, which was injected after the sample and before proceeding with the drying and calcination steps. Calibration was performed using aqueous standards prepared in the same suspension medium and the graph was linear between 5 and 80 mg l - 1 of phosphorus. The reliability of the procedure was checked by comparing the results obtained by the new developed method with those found when using a reference spectrophotometric method after a mineralization step, and by analyzing several certified reference materials.

EPA Method 3031 (SW-846): Acid Digestion of Oils for Metals Analysis by Atomic Absorption or ICP Spectrometry

EPA Pesticide Factsheets

Procedures are described for analysis of water samples and may be adapted for assessment of solid, particulate and liquid samples. The method uses real-time PCR assay for detecting Toxoplasma gondii DNA using gene-specific primers and probe.

New Active Optical Technique Developed for Measuring Low-Earth-Orbit Atomic Oxygen Erosion of Polymers

NASA Technical Reports Server (NTRS)

Banks, Bruce A.; deGroh, Kim K.; Demko, Rikako

2003-01-01

Polymers such as polyimide Kapton (DuPont) and Teflon FEP (DuPont, fluorinated ethylene propylene) are commonly used spacecraft materials because of desirable properties such as flexibility, low density, and in the case of FEP, a low solar absorptance and high thermal emittance. Polymers on the exterior of spacecraft in the low-Earth-orbit (LEO) environment are exposed to energetic atomic oxygen. Atomic oxygen reaction with polymers causes erosion, which is a threat to spacecraft performance and durability. It is, therefore, important to understand the atomic oxygen erosion yield E (the volume loss per incident oxygen atom) of polymers being considered in spacecraft design. The most common technique for determining E is a passive technique based on mass-loss measurements of samples exposed to LEO atomic oxygen during a space flight experiment. There are certain disadvantages to this technique. First, because it is passive, data are not obtained until after the flight is completed. Also, obtaining the preflight and postflight mass measurements is complicated by the fact that many polymers absorb water and, therefore, the mass change due to water absorption can affect the E data. This is particularly true for experiments that receive low atomic oxygen exposures or for samples that have a very low E. An active atomic oxygen erosion technique based on optical measurements has been developed that has certain advantages over the mass-loss technique. This in situ technique can simultaneously provide the erosion yield data on orbit and the atomic oxygen exposure fluence, which is needed for erosion yield determination. In the optical technique, either sunlight or artificial light can be used to measure the erosion of semitransparent or opaque polymers as a result of atomic oxygen attack. The technique is simple and adaptable to a rather wide range of polymers, providing that they have a sufficiently high optical absorption coefficient. If one covers a photodiode with a uniformly thick sheet of semitransparent polymer such as Kapton H polyimide, then as atomic oxygen erodes the polymer, the short-circuit current from the photodiode will increase in an exponential manner with fluence. This nonlinear response with fluence results in a lack of sensitivity for measuring low atomic oxygen fluences. However, if one uses a variable-thickness polymer or carbon sample, which is configured as shown in the preceding figure, then a linear response can be achieved for opaque materials using a parabolic well for a circular geometry detector or a V-shaped well for a rectangular-geometry detector. Variable-thickness samples can be fabricated using many thin polymer layers. For semitransparent polymers such as Kapton H polyimide, there is an initial short-circuit current that is greater than zero. This current has a slightly nonlinear dependence on atomic oxygen fluence in comparison to opaque materials such as black Kapton as shown in the graph. For this graph figure, the total thickness of Kapton H was assumed to be 0.03 cm. The photodiode short-circuit current shown in the graph was generated on the basis of preliminary measurements-a total reflectance rho of 0.0424 and an optical absorption coefficient a of 146.5 cm(sup -1). In addition to obtaining on-orbit data, the advantage of this active erosion and erosion yield measurement technique is its simplicity and reliance upon well-characterized fluence witness materials as well as a nearly linear photodiode short-circuit current dependence upon atomic oxygen fluence. The optical technique is useful for measuring either atomic oxygen fluence or erosion, depending on the information desired. To measure the atomic oxygen erosion yield of a test material, one would need to have two photodiode sensors, one for the test material and one that uses a known erosion yield material (such as Kapton) to measure the atomic oxygen fluence.

40 CFR Appendix A to Subpart C of... - Alternative Testing Methods Approved for Analyses Under the Safe Drinking Water Act

Code of Federal Regulations, 2012 CFR

2012-07-01

... coupled plasma-atomic emission spectrometry (AVICP-AES) 200.5, Revision 4.2. 2 Arsenic Atomic Absorption... inductively coupled plasma-atomic emission spectrometry (AVICP-AES) 200.5, Revision 4.2. 2 Barium Inductively Coupled Plasma 3120 B Atomic Absorption; Direct 3111 D Atomic Absorption; Furnace 3113 B 3113 B-04 Axially...

40 CFR Appendix A to Subpart C of... - Alternative Testing Methods Approved for Analyses Under the Safe Drinking Water Act

Code of Federal Regulations, 2011 CFR

2011-07-01

... coupled plasma-atomic emission spectrometry (AVICP-AES) 200.5, Revision 4.2. 2 Arsenic Atomic Absorption... inductively coupled plasma-atomic emission spectrometry (AVICP-AES) 200.5, Revision 4.2. 2 Barium Inductively Coupled Plasma 3120 B Atomic Absorption; Direct 3111 D Atomic Absorption; Furnace 3113 B 3113 B-04 Axially...

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of arsenic and selenium in water and sediment by graphite furnace atomic absorption spectrometry

USGS Publications Warehouse

Jones, Sandra R.; Garbarino, John R.

1999-01-01

Graphite furnace-atomic absorption spectrometry (GF-AAS) is a sensitive, precise, and accurate technique that can be used to determine arsenic and selenium in samples of water and sediment. The GF-AAS method has been developed to replace the hydride generation-atomic absorption spectrometry (HG-AAS) methods because the method detection limits are similar, bias and variability are comparable, and interferences are minimal. Advantages of the GF-AAS method include shorter sample preparation time, increased sample throughput from simultaneous multielement analysis, reduced amount of chemical waste, reduced sample volume requirements, increased linear concentration range, and the use of a more accurate digestion procedure. The linear concentration range for arsenic and selenium is 1 to 50 micrograms per liter in solution; the current method detection limit for arsenic in solution is 0.9 microgram per liter; the method detection limit for selenium in solution is 1 microgram per liter. This report describes results that were obtained using stop-flow and low-flow conditions during atomization. The bias and variability of the simultaneous determination of arsenic and selenium by GF-AAS under both conditions are supported with results from standard reference materials--water and sediment, real water samples, and spike recovery measurements. Arsenic and selenium results for all Standard Reference Water Samples analyzed were within one standard deviation of the most probable values. Long-term spike recoveries at 6.25, 25.0, 37.5 micrograms per liter in reagent-, ground-, and surface-water samples for arsenic averaged 103 plus or minus 2 percent using low-flow conditions and 104 plus or minus 4 percent using stop-flow conditions. Corresponding recoveries for selenium were 98 plus or minus 13 percent using low-flow conditions and 87 plus or minus 24 percent using stop-flow conditions. Spike recoveries at 25 micrograms per liter in 120 water samples ranged from 97 to 99 percent for arsenic and from 82 to 93 percent for selenium, depending on the flow conditions used. Statistical analysis of dissolved and whole-water recoverable analytical results for the same set of water samples indicated that there is no significant difference between the GF-AAS and HG-AAS methods. Interferences related to various chemical constituents were also identified. Although sulfate and chloride in association with various cations might interfere with the determination of arsenic and selenium by GF-AAS, the use of a magnesium nitrate/palladium matrix modifier and low-flow argon during atomization helped to minimize such interferences. When using stabilized temperature platform furnace conditions where stop flow is used during atomization, the addition of hydrogen (5 percent volume/volume) to the argon minimized chemical interferences. Nevertheless, stop flow during atomization was found to be less effective than low flow in reducing interference effects.

Selenium analysis by an integrated microwave digestion-needle trap device with hydride sorption on carbon nanotubes and electrothermal atomic absorption spectrometry determination

NASA Astrophysics Data System (ADS)

Maratta Martínez, Ariel; Vázquez, Sandra; Lara, Rodolfo; Martínez, Luis Dante; Pacheco, Pablo

2018-02-01

An integrated microwave assisted digestion (MW-AD) - needle trap device (NTD) for selenium determination in grape pomace samples is presented. The NTD was filled with oxidized multiwall carbon nanotubes (oxMWCNTS) where Se hydrides were preconcentrated. Determination was carried out by flow injection-electrothermal atomic absorption spectrometry (FI-ETAAS). The variables affecting the system were established by a multivariate design (Plackett Burman), indicating that the following variables significantly affect the system: sample amount, HNO3 digestion solution concentration, NaBH4 volume and elution volume. A Box-Behnken design was implemented to determine the optimized values of these variables. The system improved Se atomization in the graphite furnace, since only trapped hydrides reached the graphite furnace, and the pyrolysis stage was eliminated according to the aqueous matrix of the eluate. Under optimized conditions the system reached a limit of quantification of 0.11 μg kg- 1, a detection limit of 0.032 μg kg- 1, a relative standard deviation of 4% and a preconcentration factor (PF) of 100, reaching a throughput sample of 5 samples per hour. Sample analysis show Se concentrations between 0.34 ± 0.03 μg kg- 1 to 0.48 ± 0.03 μg kg- 1 in grape pomace. This system provides minimal reagents and sample consumption, eliminates discontinuous stages between samples processing reaching a simpler and faster Se analysis.

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.

Major- and Trace-Element Concentrations in Soils from Two Geochemical Surveys (1972 and 2005) of the Denver, Colorado, Metropolitan Area

USGS Publications Warehouse

Kilburn, James E.; Smith, David B.; Closs, L. Graham; Smith, Steven M.

2007-01-01

Introduction This report contains major- and trace-element concentration data for soil samples collected in 1972 and 2005 from the Denver, Colorado, metropolitan area. A total of 405 sites were sampled in the 1972 study from an area approximately bounded by the suburbs of Golden, Thornton, Aurora, and Littleton to the west, north, east, and south, respectively. This data set included 34 duplicate samples collected in the immediate vicinity of the primary sample. In 2005, a total of 464 sites together with 34 duplicates were sampled from the same approximate localities sampled in 1972 as well as additional sites in east Aurora and the area surrounding the Rocky Mountain Arsenal. Sample density for both surveys was on the order of 1 site per square mile. At each site, sample material was collected from a depth of 0-5 inches. Each sample collected was analyzed for near-total major- and trace-element composition by the following methods: (1) inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) for aluminum, antimony, arsenic, barium, beryllium, bismuth, cadmium, calcium, cerium, cesium, chromium, cobalt, copper, gallium, indium, iron, lanthanum, lead, lithium, magnesium, manganese, molybdenum, nickel, niobium, phosphorus, potassium, rubidium, scandium, silver, sodium, strontium, sulfur, tellurium, thallium, thorium, tin, titanium, tungsten, uranium, vanadium, yttrium, and zinc; and (2) hydride generation-atomic absorption spectrometry for selenium. The samples collected in 2005 were also analyzed by a cold vapor-atomic absorption method for mercury. This report makes available the analytical results of these studies.

Discussion of parameters associated with the determination of arsenic by electrothermal atomic absorption spectrometry in slurried environmental samples.

PubMed

Vassileva, E; Baeten, H; Hoenig, M

2001-01-02

A slurry sampling-fast program procedure has been developed for the determination of arsenic in plants, soils and sediments by electrothermal atomic absorption spectrometry. Efficiencies of various single and mixed modifiers for thermal stabilization of arsenic and for a better removal of the matrix during pyrolysis step were compared. The influence of the slurry concentration, amounts of modifier and parameters of the pyrolysis step on the As integrated absorbance signals have been studied and a comparison between fast and conventional furnace programs was also made. The ultrasonic agitation of the slurry followed by a fast electrothermal program using an Ir/Mg modifier provides the most consistent performance in terms of precision and accuracy. The reliability of the whole procedure has been compared with results obtained after application of a wet digestion method with an HF step and validated by analyzing eleven certified reference materials. Arsenic detection and quantitation limits expressed on dry sample matter were about 30 and 100 micrograms kg-1, respectively.

[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.

Analysis of beryllium and depleted uranium: An overview of detection methods in aerosols and soils

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

Camins, I.; Shinn, J.H.

We conducted a survey of commercially available methods for analysis of beryllium and depleted uranium in aerosols and soils to find a reliable, cost-effective, and sufficiently precise method for researchers involved in environmental testing at the Yuma Proving Ground, Yuma, Arizona. Criteria used for evaluation include cost, method of analysis, specificity, sensitivity, reproducibility, applicability, and commercial availability. We found that atomic absorption spectrometry with graphite furnace meets these criteria for testing samples for beryllium. We found that this method can also be used to test samples for depleted uranium. However, atomic absorption with graphite furnace is not as sensitive amore » measurement method for depleted uranium as it is for beryllium, so we recommend that quality control of depleted uranium analysis be maintained by testing 10 of every 1000 samples by neutron activation analysis. We also evaluated 45 companies and institutions that provide analyses of beryllium and depleted uranium. 5 refs., 1 tab.« less

Solvent microextraction-flame atomic absorption spectrometry (SME-FAAS) for determination of ultratrace amounts of cadmium in meat and fish samples.

PubMed

Goudarzi, Nasser

2009-02-11

A simple, low cost and highly sensitive method based on solvent microextraction (SME) for separation/preconcentration and flame atomic absorption spectrometry (FAAS) was proposed for the determination of ultratrace amounts of cadmium in meat and fish samples. The analytical procedure involved the formation of a hydrophobic complex by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution. In suitable conditions, the complex of cadmium-APDC entered the micro organic phase, and thus, separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, a detection limit (3 sigma) of 0.8 ng L(-1) and an enrichment factor of 93 were achieved. The relative standard deviation for the method was found to be 2.2% for Cd. The interference effects of some anions and cations were also investigated. The developed method has been applied to the determination of trace Cd in meat and fish samples.

[Determination of total mercury in water samples, sediments and solids in suspension in aquatic systems by cold-vapor atomic absorption spectrophotometry].

PubMed

Vieira, J L; Passarelli, M M

1996-06-01

The use of metallic mercury in the extraction and concentration of gold causes the discarding of tons of this metal in the environment, leading to a considerable increase in the natural levels of the same and the contamination of the surrounding areas. Thus it is extremely important to monitor the presence of this metal in various sectors of the environment with a view aiming to preventing human exposure to excessive concentrations which can result in serious episodes of mercury poisoning. It is also important to estimate the possibility of river sediments becoming potential sources of contamination of human beings. The determination of total mercury was undertaken by using cold vapor atomic absorption spectrometry. River waters, as well as sediments and suspended solids were used as samples for the standardization of the analytical procedure. Later on, this method was tested on samples originating in gold mining areas for the purpose of assessing its validity.

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…

Vortex-assisted switchable liquid-liquid microextraction for the preconcentration of cadmium in environmental samples prior to its determination with flame atomic absorption spectrometry.

PubMed

Fırat, Merve; Bodur, Süleyman; Tışlı, Büşra; Özlü, Cansu; Chormey, Dotse Selali; Turak, Fatma; Bakırdere, Sezgin

2018-06-12

In this study, a switchable solvent was used to preconcentrate trace amounts of Cd from aqueous solution for its determination by flame atomic absorption spectrometry (FAAS). Protonation of N,N-dimethylbenzylamine by dry ice (solid CO 2 ) made it water soluble, and addition of sodium hydroxide converted it back to its original nonionic state for phase separation and subsequent extraction of Cd. A slotted quartz tube (SQT) was attached to the flame burner head to increase the residence time of Cd atoms in the light path. Under the optimum conditions, limits of detection and quantification were determined as 0.7 and 2.6 μg L -1 , respectively. Low relative standard deviations calculated from seven replicate measurements of the lowest concentration indicated high precision. Accuracy of the developed method was checked by using a standard reference material (SRM 1633c). Spiked recovery tests were also performed on lake water and wastewater samples at different concentrations to check the applicability of the developed method, and the results obtained (90-103%) established high recovery.

A series of BCN nanosheets with enhanced photoelectrochemical performances

NASA Astrophysics Data System (ADS)

Li, Junqi; Lei, Nan; Hao, Hongjuan; Zhou, Jian

2017-03-01

A series of flake-like BCN compounds were produced by calcination at different reaction temperatures via thermal substitution of C atoms with B atoms of boric acid substructures in graphitic carbon nitrides (g-C3N4). The structural and optical properties of the samples were characterized by XRD, TEM, HRTEM, XPS and UV-vis absorption. The photoelectrochemical (PEC) performance of all samples were characterized through photocurrent and electrochemical impedance spectroscopy (EIS) measurement. The test results demonstrated that BCN nanosheets exhibited higher PEC performance with increasing substituted amount of boron.

Tungsten devices in analytical atomic spectrometry

NASA Astrophysics Data System (ADS)

Hou, Xiandeng; Jones, Bradley T.

2002-04-01

Tungsten devices have been employed in analytical atomic spectrometry for approximately 30 years. Most of these atomizers can be electrically heated up to 3000 °C at very high heating rates, with a simple power supply. Usually, a tungsten device is employed in one of two modes: as an electrothermal atomizer with which the sample vapor is probed directly, or as an electrothermal vaporizer, which produces a sample aerosol that is then carried to a separate atomizer for analysis. Tungsten devices may take various physical shapes: tubes, cups, boats, ribbons, wires, filaments, coils and loops. Most of these orientations have been applied to many analytical techniques, such as atomic absorption spectrometry, atomic emission spectrometry, atomic fluorescence spectrometry, laser excited atomic fluorescence spectrometry, metastable transfer emission spectroscopy, inductively coupled plasma optical emission spectrometry, inductively coupled plasma mass spectrometry and microwave plasma atomic spectrometry. The analytical figures of merit and the practical applications reported for these techniques are reviewed. Atomization mechanisms reported for tungsten atomizers are also briefly summarized. In addition, less common applications of tungsten devices are discussed, including analyte preconcentration by adsorption or electrodeposition and electrothermal separation of analytes prior to analysis. Tungsten atomization devices continue to provide simple, versatile alternatives for analytical atomic spectrometry.

Flow injection for the determination of Se(IV) and Se(VI) by hydride generation atomic absorption spectrometry with microwave oven on-line prereduction of Se(VI) to Se(IV)

NASA Astrophysics Data System (ADS)

Burguera, J. L.; Carrero, P.; Burguera, M.; Rondon, C.; Brunetto, M. R.; Gallignani, M.

1996-12-01

An on-line flow injection system has been developed for the selective determination of Se(IV) and Se(VI) in citric fruit juices and geothermal waters by hydride generation atomic absorption spectrometry with microwave-aided heating prereduction of Se(VI) to Se(IV). The samples and the prereductant solutions (4 mol l -1 HCl for Se(IV) and 12 mol l -1 HCl for Se(VI)) which circulated in a closed-flow circuit were injected by means of a time-based injector. This mixture was displaced by a carrier solution of 1% v/v of hydrochloric acid through a PTFE coil located inside the focused microwave oven and mixed downstream with a borohydride solution to generate the hydride. The linear ranges were 0-120 and 0-100 μg l -1 of Se(IV) and Se(VI), respectively. The detection limits were 1.0 μg l -1 for Se(IV) and 1.5 μg l -1 for Se(VI). The precision (about 2.0-2.5% RSD) and recoveries (96-98% for Se(IV) and 94-98% for Se(VI)) were good. Total selenium values were also obtained by electrothermal atomic absorption spectrometry which agreed with the content of both selenium species. The sample throughput was about 50 measurements per hour. The main advantage of the method is that the selective determination of Se(IV) and Se(VI) in citric fruit juices and geothermal waters is performed in a closed system with a minimum sample manipulation, exposure to the environment, minimum sample waste and operator attention.

Cu determination in crude oil distillation products by atomic absorption and inductively coupled plasma mass spectrometry after analyte transfer to aqueous solution

NASA Astrophysics Data System (ADS)

Kowalewska, Zofia; Ruszczyńska, Anna; Bulska, Ewa

2005-03-01

Cu was determined in a wide range of petroleum products from crude oil distillation using flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). Different procedures of sample preparation were evaluated: (i) mineralization with sulfuric acid in an open system, (ii) mineralization in a closed microwave system, (iii) combustion in hydrogen-oxygen flame in the Wickbold's apparatus, (iv) matrix evaporation followed by acid dissolution, and (v) acidic extraction. All the above procedures led to the transfer of the analyte into an aqueous solution for the analytical measurement step. It was found that application of FAAS was limited to the analysis of the heaviest petroleum products of high Cu content. In ICP-MS, the use of internal reference method (with Rh or In as internal reference element) was required to eliminate the matrix effects in the analysis of extracts and the concentrated solutions of mineralized heavy petroleum products. The detection limits (in original samples) were equal to, respectively, 10, 86, 3.3, 0.9 and 0.4 ng g - 1 in procedures i-v with ETAAS detection and 10, 78, 1.1 and 0.5 ng g - 1 in procedures i-iii and v with ICP-MS detection. The procedures recommended here were validated by recovery experiments, certified reference materials analysis and comparison of results, obtained for a given sample, in different ways. The Cu content in the analyzed samples was: 50-110 ng g - 1 in crude oil, < 0.4-6 ng g - 1 in gasoline, < 0.5-2 ng g - 1 in atmospheric oil, < 6-100 ng g - 1 in heavy vacuum oil and 140-300 ng g - 1 in distillation residue.

Multicomutation flow system for manganese speciation by solid phase extraction and flame atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Tobiasz, Anna; Sołtys, Monika; Kurys, Ewa; Domagała, Karolina; Dudek-Adamska, Danuta; Walas, Stanisław

2017-08-01

In the paper an application of solid phase extraction technique for speciation analysis of manganese in water samples with the use of flame atomic absorption spectrometry is presented. Two types of sorbents, activated silica gel and Dowex 1 × 4, were used respectively for simultaneously Mn2 + and MnO42 - retention and preconcentration. The whole procedure was realized in multicomutation flow system. Different conditions like: type and concentration of eluent, sample pH and loading time were tested during the study. Under appropriate conditions, it was possible to obtained enrichment factors of 20 and 16 for Mn(II) and Mn(VII), respectively. Precision of the procedure was close to 4% (measured as relative standard deviation), whereas the detection limit (3σ) was 1.4 μg·L- 1 for Mn(II) and 4.8 μg·L- 1 for Mn(VII).

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

USGS Publications Warehouse

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

1981-01-01

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

Speciation of chromium (VI) and total chromium determination in welding dust samples by flow-injection analysis coupled to atomic absorption spectrometry.

PubMed

Girard, L; Hubert, J

1996-11-01

We have studied the speciation of chromium (VI) in stainless-steel welding dusts. The approach used for the analysis of Cr(VI) and total Cr relies on a flow-injection analyzer (FIA) equipped with two different sequential detectors. The system measures Cr(VI). by colorimetry (with 1,5-diphenyl carbohydrazide) and total chromium content by flame atomic absorption spectroscopy (AAS). The extraction of the samples of welding-fume dusts is achieved in a buffer solution (acetic acid and sodium acetate at pH 4). This extraction procedure gives a 96% recovery of chromium (VI). The FIA-AAS system that has been described is also more sensitive, has a lower detection limit (0.005 mug ml(-1)) and gives a better precision (< 1%) than other equivalent systems that have been previously described.

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

ERIC Educational Resources Information Center

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

2011-01-01

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

Percutaneous absorption of selenium sulfide

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

Farley, J.; Skelly, E.M.; Weber, C.B.

1986-01-01

The purpose of this study was to determine selenium levels in the urine of Tinea patients before and after overnight application of a 2.5% selenium sulfide lotion. Selenium was measured by atomic absorption spectroscopy (AAS). Hydride generation and carbon rod atomization were studied. It was concluded from this study that selenium is absorbed through intact skin. Selenium is then excreted, at least partially, in urine, for at least a week following treatment. The data show that absorption and excretion of selenium vary on an individual basis. Selenium levels in urine following a single application of selenium sulfide lotion do notmore » indicate that toxic amounts of selenium are being absorbed. Repeated treatments with SeS/sub 2/ result in selenium concentrations in urine which are significantly higher than normal. Significant matrix effects are observed in the carbon rod atomization of urine samples for selenium determinations, even in the presence of a matrix modifier such as nickel. The method of standard additions is required to obtain accurate results in the direct determination of selenium in urine by carbon rod AAS.« less

Column preconcentration and electrothermal atomic absorption spectrometric determination of rhodium in some food and standard samples.

PubMed

Taher, Mohammad Ali; Pourmohammad, Fatemeh; Fazelirad, Hamid

2015-12-01

In the present work, an electrothermal atomic absorption spectrometric method has been developed for the determination of ultra-trace amounts of rhodium after adsorption of its 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol/tetraphenylborate ion associated complex at the surface of alumina. Several factors affecting the extraction efficiency such as the pH, type of eluent, sample and eluent flow rates, sorption capacity of alumina and sample volume were investigated and optimized. The relative standard deviation for eight measurements of 0.1 ng/mL of rhodium was ±6.3%. In this method, the detection limit was 0.003 ng/mL in the original solution. The sorption capacity of alumina and the linear range for Rh(III) were evaluated as 0.8 mg/g and 0.015-0.45 ng/mL in the original solution, respectively. The proposed method was successfully applied for the extraction and determination of rhodium content in some food and standard samples with high recovery values. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Novel visualization studies of lignocellulosic oxidation chemistry by application of C-near edge X-ray absorption fine structure spectroscopy

Treesearch

Douglas G. Mancosky; Lucian A. Lucia; Hiroki Nanko; Sue Wirick; Alan W. Rudie; Robert Braun

2005-01-01

The research presented herein is the first attempt to probe the chemical nature of lignocellulosic samples by the application of carbon near edge X-ray absorption fine structure spectroscopy (C-NEXAFS). C-NEXAFS is a soft X-ray technique that principally provides selective interrogation of discrete atomic moieties using photoelectrons of variable energies. The X1A beam...

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

PubMed

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

1991-05-01

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

Determination and Uncertainty Analysis of Inorganic Arsenic in Husked Rice by Solid Phase Extraction and Atomic Absorption Spectrometry with Hydride Generation.

PubMed

Saxena, Sushil Kumar; Karipalli, Agnes Raju; Krishnan, Anoop A; Rangasamy, Rajesh; Malekadi, Praveen; Singh, Dhirendra P; Vasu, Vimesh; Singh, Vijay K

2017-05-01

This study enables the selective determination of inorganic arsenic (iAs) with a low detection limit using an economical instrument [atomic absorption spectrometer with hydride generation (HG)] to meet the regulatory requirements as per European Commission (EC) and Codex guidelines. Dry rice samples (0.5 g) were diluted using 0.1 M HNO3-3% H2O2 and heated in a water bath (90 ± 2°C) for 60 min. Through this process, all the iAs is solubilized and oxidized to arsenate [As(V)]. The centrifuged extract was loaded onto a preconditioned and equilibrated strong anion-exchange SPE column (silica-based Strata SAX 500 mg/6 mL), followed by selective and sequential elution of As(V), enabling the selective quantification of iAs using atomic absorption spectrometry with HG. In-house validation showed a mean recovery of 94% and an LOQ of 0.025 mg/kg. The repeatability (HorRatr) and reproducibility (HorRatR) values were <2, meeting the performance criteria mandated by the EC. The combined standard measurement uncertainty by this method was less than the maximum standard measurement uncertainty; thus, the method can be considered for official control purposes. The method was applied for the determination of iAs in husked rice samples and has potential applications in other food commodities.

Integrating bio-inorganic and analytical chemistry into an undergraduate biochemistry laboratory.

PubMed

Erasmus, Daniel J; Brewer, Sharon E; Cinel, Bruno

2015-01-01

Undergraduate laboratories expose students to a wide variety of topics and techniques in a limited amount of time. This can be a challenge and lead to less exposure to concepts and activities in bio-inorganic chemistry and analytical chemistry that are closely-related to biochemistry. To address this, we incorporated a new iron determination by atomic absorption spectroscopy exercise as part of a five-week long laboratory-based project on the purification of myoglobin from beef. Students were required to prepare samples for chemical analysis, operate an atomic absorption spectrophotometer, critically evaluate their iron data, and integrate these data into a study of myoglobin. © 2015 The International Union of Biochemistry and Molecular Biology.

Flameless Atomic Absorption Spectroscopy: Effects of Nitrates and Sulfates.

DTIC Science & Technology

1980-05-01

ATTACHED DDJ~P 1413 EDITION 01 INO, 6 5 IabSoLEr J UjN!LbAa~ A- i SELU 0 IONOF I tG 651 J Flameless Atomic Absorption Spectroscopy: Effects of Nitrates...analytical techniques, flameless atomic absorption is subject to matrix or interference effects. Upon heating, nitrate and sulfate salts decompose to...Eklund and J.E. Smith, Anal Chem, 51, 1205 (1979) R.H. Eklund and J.A. Holcombe, Anal Chim. Acta, 109, 97 (1979) FLAMELESS ATOMIC ABSORPTION

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. Copyright © 2014 Elsevier Ltd. All rights reserved.

[Study on lead absorption in pumpkin by atomic absorption spectrophotometry].

PubMed

Li, Zhen-Xia; Sun, Yong-Dong; Chen, Bi-Hua; Li, Xin-Zheng

2008-07-01

A study was carried out on the characteristic of lead absorption in pumpkin via atomic absorption spectrophotometer. The results showed that lead absorption amount in pumpkin increased with time, but the absorption rate decreased with time; And the lead absorption amount reached the peak in pH 7. Lead and cadmium have similar characteristic of absorption in pumpkin.

Unraveling the atomic structure of biogenic silica: evidence of the structural association of Al and Si in diatom frustules

NASA Astrophysics Data System (ADS)

Gehlen, M.; Beck, L.; Calas, G.; Flank, A.-M.; Van Bennekom, A. J.; Van Beusekom, J. E. E.

2002-05-01

We used X-ray absorption spectroscopy at the Al K-edge to investigate the atomic structure of biogenic silica and to assess the effect of Al on its crystal chemistry. Our study provides the first direct evidence for a structural association of Al and Si in biogenic silica. In samples of cultured diatoms, Al is present exclusively in fourfold coordination. The location and relative intensity of X-ray absorption near-edge structure (XANES) features suggests the structural insertion of tetrahedral Al inside the silica framework synthesized by the organism. In diatom samples collected in the marine environment, Al is present in mixed six- and fourfold coordination. The relative intensity of XANES structures indicates the coexistence of structural Al with a clay component, which most likely reflects sample contamination by adhering mineral particles. Extended X-ray absorption fine structure spectroscopy has been used to get Al-O distances in biogenic silica of cultured diatoms, confirming a tetrahedral coordination. Because of its effect on solubility and reaction kinetics of biogenic silica, the structural association between Al and biogenic silica at the stage of biosynthesis has consequences for the use of sedimentary biogenic silica as an indicator of past environmental conditions.

21 CFR 862.2850 - Atomic absorption spectrophotometer for clinical use.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Atomic absorption spectrophotometer for clinical... HUMAN SERVICES (CONTINUED) MEDICAL DEVICES CLINICAL CHEMISTRY AND CLINICAL TOXICOLOGY DEVICES Clinical Laboratory Instruments § 862.2850 Atomic absorption spectrophotometer for clinical use. (a) Identification...

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.

Preconcentration and determination of boron in milk, infant formula, and honey samples by solid phase extraction-electrothermal atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

López-García, I.; Viñas, P.; Romero-Romero, R.; Hernández-Córdoba, M.

2009-02-01

This work presents alternative procedures for the electrothermal atomic absorption spectrometric determination of boron in milk, infant formulas, and honey samples. Honey samples (10% m/v) were diluted in a medium containing 1% v/v HNO 3 and 50% v/v H 2O 2 and introduced in the atomizer. A mixture of 20 µg Pd and 0.5 µg Mg was used for chemical modification. Calibration was carried out using aqueous solutions prepared in the same medium, in the presence of 10% m/v sucrose. The detection limit was 2 µg g - 1 , equivalent to three times the standard error of the estimate ( sy/ x) of the regression line. For both infant formulas and milk samples, due to their very low boron content, we used a procedure based on preconcentration by solid phase extraction (Amberlite IRA 743), followed by elution with 2 mol L - 1 hydrochloric acid. Detection limits were 0.03 µg g - 1 for 4% m/v honey, 0.04 µg g - 1 for 5% m/v infant formula and 0.08 µg mL - 1 for 15% v/v cow milk. We confirmed the accuracy of the procedure by comparing the obtained results with those found via a comparable independent procedure, as well by the analysis of four certified reference materials.

Midinfrared absorption measured at a lambda/400 resolution with an atomic force microscope.

PubMed

Houel, Julien; Homeyer, Estelle; Sauvage, Sébastien; Boucaud, Philippe; Dazzi, Alexandre; Prazeres, Rui; Ortéga, Jean-Michel

2009-06-22

Midinfrared absorption can be locally measured using a detection combining an atomic force microscope and a pulsed excitation. This is illustrated for the midinfrared bulk GaAs phonon absorption and for the midinfrared absorption of thin SiO(2) microdisks. We show that the signal given by the cantilever oscillation amplitude of the atomic force microscope follows the spectral dependence of the bulk material absorption. The absorption spatial resolution achieved with microdisks is around 50 nanometer for an optical excitation around 22 micrometer wavelength.

Absorption and emission spectra of Li atoms trapped in rare gas matrices

NASA Astrophysics Data System (ADS)

Wright, J. J.; Balling, L. C.

1980-10-01

Pulsed-dye-laser excitation has been used to investigate the optical absorption and emission spectra of Li atoms trapped in Ar, Kr, and Xe matrices at 10 °K. Attempts to stabilize Li atoms in a Ne matrix at 2 °K were unsuccessful. Results for all three rare gases were qualitatively the same. White light absorption scans showed a single absorption with three peaks centered near the free-atom 2s→2p transition wavelength. The intensity of fluorescence produced by dye-laser excitation within this absorption band was measured as a function of emission wavelength. Excitation of the longest- and shortest-wavelength absorption peaks produced identical emission profiles, but no distinct fluorescence signal was detected when the laser was tuned to the central absorption peaks, indicating that the apparent absorption triplet is actually the superposition of a singlet and a doublet absorption originating from two different trapping sites. No additional absorption bands were detected.

Reduced-temperature crystallization of thin amorphous Fe80B20 films studied via empirical modeling of extended x-ray absorption fine structure

NASA Astrophysics Data System (ADS)

Harris, V. G.; Oliver, S. A.; Ayers, J. D.; Das, B. N.; Koon, N. C.

1996-04-01

The evolution of the local atomic environment around Fe atoms in very thin (15 nm), amorphous, partially crystallized and fully crystallized films of Fe80B20 was studied using extended x-ray absorption fine structure (EXAFS) measurements. The relative atomic fraction of each crystalline phase present in the annealed samples was extracted from the Fe EXAFS data by a least-squares fitting procedure, using data collected from t-Fe3B, t-Fe2B, and α-Fe standards. The type and relative fraction of the crystallization products follows the trends previously measured in Fe80B20 melt-spun ribbons, except for the fact that crystallization temperatures are ≊200 K lower than those measured in bulk equivalents. This greatly reduced crystallization temperature may arise from the dominant role of surface nucleation sites in the crystallization of very thin amorphous films.

An automated flow injection system for metal determination by flame atomic absorption spectrometry involving on-line fabric disk sorptive extraction technique.

PubMed

Anthemidis, A; Kazantzi, V; Samanidou, V; Kabir, A; Furton, K G

2016-08-15

A novel flow injection-fabric disk sorptive extraction (FI-FDSE) system was developed for automated determination of trace metals. The platform was based on a minicolumn packed with sol-gel coated fabric media in the form of disks, incorporated into an on-line solid-phase extraction system, coupled with flame atomic absorption spectrometry (FAAS). This configuration provides minor backpressure, resulting in high loading flow rates and shorter analytical cycles. The potentials of this technique were demonstrated for trace lead and cadmium determination in environmental water samples. The applicability of different sol-gel coated FPSE media was investigated. The on-line formed complex of metal with ammonium pyrrolidine dithiocarbamate (APDC) was retained onto the fabric surface and methyl isobutyl ketone (MIBK) was used to elute the analytes prior to atomization. For 90s preconcentration time, enrichment factors of 140 and 38 and detection limits (3σ) of 1.8 and 0.4μgL(-1) were achieved for lead and cadmium determination, respectively, with a sampling frequency of 30h(-1). The accuracy of the proposed method was estimated by analyzing standard reference materials and spiked water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis, characterization and application of a new chelating resin for solid phase extraction, preconcentration and determination of trace metals in some dairy samples by flame atomic absorption spectrometry.

PubMed

Daşbaşı, Teslima; Saçmacı, Şerife; Çankaya, Nevin; Soykan, Cengiz

2016-11-15

In this study, a simple and rapid solid phase extraction/preconcentration procedure was developed for determination of Cd(II), Co(II), Cr(III), Cu(II), Fe(III), Mn(II), Pb(II), and Zn(II) trace metals by flame atomic absorption spectrometry (FAAS). A new chelating resin, poly(N-cyclohexylacrylamide-co-divinylbenzene-co-2-acrylamido-2-methyl-1-propanesulfonic acid) (NCA-co-DVB-co-AMPS) (hereafter CDAP) was synthesized and characterized. The influences of the analytical parameters such as pH of the sample solution, type and concentration of eluent, flow rates of the sample and eluent, volume of the sample and eluent, amount of chelating resin, and interference of ions were examined. The limit of detection (LOD) of analytes were found (3s) to be in the range of 0.65-1.90μgL(-1). Preconcentration factor (PF) of 200 and the relative standard deviation (RSD) of ⩽2% were achieved (n=11). The developed method was applied for determination of analytes in some dairy samples and certified reference materials. Copyright © 2016 Elsevier Ltd. All rights reserved.

In-situ suspended aggregate microextraction of gold nanoparticles from water samples and determination by electrothermal atomic absorption spectrometry.

PubMed

Choleva, Tatiana G; Kappi, Foteini A; Tsogas, George Z; Vlessidis, Athanasios G; Giokas, Dimosthenis L

2016-05-01

This work describes a new method for the extraction and determination of gold nanoparticles in environmental samples by means of in-situ suspended aggregate microextraction and electrothermal atomic absorption spectrometry. The method relies on the in-situ formation of a supramolecular aggregate phase through ion-association between a cationic surfactant and a benzene sulfonic acid derivative. Gold nanoparticles are physically entrapped into the aggregate phase which is separated from the bulk aqueous solution by vacuum filtration on the surface of a cellulose filter in the form of a thin film. The film is removed from the filter surface and is dissociated into an acidified methanolic solution which is used for analysis. Under the optimized experimental conditions, gold nanoparticles can be efficiently extracted from water samples with recovery rates between 81.0-93.3%, precision 5.4-12.0% and detection limits as low as 75femtomolL(-1) using only 20mL of sample volume. The satisfactory analytical features of the method along with the simplicity indicate the efficiency of this new approach to adequately collect and extract gold nanoparticle species from water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Application of Internal Standard Method for Several 3d-Transition Metallic Elements in Flame Atomic Absorption Spectrometry Using a Multi-wavelength High-resolution Spectrometer.

PubMed

Toya, Yusuke; Itagaki, Toshiko; Wagatsuma, Kazuaki

2017-01-01

We investigated a simultaneous internal standard method in flame atomic absorption spectrometry (FAAS), in order to better the analytical precision of 3d-transition metals contained in steel materials. For this purpose, a new spectrometer system for FAAS, comprising a bright xenon lamp as the primary radiation source and a high-resolution Echelle monochromator, was employed to measure several absorption lines at a wavelength width of ca. 0.3 nm at the same time, which enables the absorbances of an analytical line and also an internal standard line to be estimated. In considering several criteria for selecting an internal standard element and the absorption line, it could be suggested that platinum-group elements: ruthenium, rhodium, or palladium, were suitable for an internal standard element to determine the 3d-transition metal elements, such as titanium, iron, and nickel, by measuring an appropriate pair of these absorption lines simultaneously. Several variances of the absorption signal, such as a variation in aspirated amounts of sample solution and a short-period drift of the primary light source, would be corrected and thus reduced, when the absorbance ratio of the analytical line to the internal standard line was measured. In Ti-Pd, Ni-Rh, and Fe-Ru systems chosen as typical test samples, the repeatability of the signal respnses was investigated with/without the internal standard method, resulting in better precision when the internal standard method was applied in the FAAS with a nitrous oxide-acetylene flame rather than an air-acetylene flame.

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)…

DIRECT MERCURY ANALYSIS IN ENVIRONMENTAL SOLIDS BY ICPMS WITH ON-LINE SAMPLE ASHING AND MERCURY PRE-CONCENTRATION USING THE DIRECT MERCURY ANALYZER

EPA Science Inventory

A Direct Mercury Analyzer based on sample combustion and mercury concentration by gold amalgamation, followed by atomic absorption determination, was interfaced with a quadrupole and a magnet sector ICPMS. In this paper, we discuss design and operating parameters and eval...

Solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for gold determination in geological samples after preconcentration onto carbon nanotubes

NASA Astrophysics Data System (ADS)

Dobrowolski, Ryszard; Mróz, Agnieszka; Dąbrowska, Marzena; Olszański, Piotr

2017-06-01

A novelty method for the determination of gold in geological samples by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GF AAS) after solid-phase extraction onto modified carbon nanotubes (CNT) was described. The methodology developed is based on solid phase extraction of Au(III) ions from digested samples to eliminate strong interference caused by iron compounds and problems related to inhomogeneities of the samples. The use of aqueous or solid standard for calibration was studied and the slope of calibration curve was the same for both of these modes. This statement indicates the possibility to perform the calibration of the method using aqueous standard solutions. Under optimum conditions the absolute detection limit for gold was equal to 2.24 · 10- 6 μg g- 1 while the adsorption capacity of modified carbon nanotubes was 264 mg g- 1. The proposed procedure was validated by the application of certified reference materials (CRMs) with different content of gold and different matrix, the results were in good agreement with certified values. The method was successfully applied for separation and determination of gold ions in complex geological samples, with precision generally better than 8%.

Absorption spectroscopy of heavy alkaline earth metals Ba and Sr in rare gas matrices—CCSD(T) calculations and atomic site occupancies

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

Davis, Barry M.; McCaffrey, John G., E-mail: john.mccaffrey@nuim.ie

2016-01-28

Isolation of the heavier alkaline earth metals Ba and Sr in the solid rare gases (RGs) Ar, Kr, and Xe is analysed with absorption spectroscopy and interpreted partly with the assistance of ab initio calculations of the diatomic M ⋅ RG ground state interaction potentials. The y{sup 1}P←a{sup 1}S resonance transitions in the visible spectral region are used to compare the isolation conditions of these two metal atom systems and calcium. Complex absorption bands were recorded in all three metal atom systems even after extensive sample annealing. Coupled cluster calculations conducted on the ground states of the nine M ⋅more » RG diatomics (M = Ca, Sr, and Ba; RG = Ar, Kr, and Xe) at the coupled cluster single, double, and non-iterative triple level of theory revealed long bond lengths (>5 Å) and shallow bound regions (<130 cm{sup −1}). All of the M ⋅ RG diatomics have bond lengths considerably longer than those of the rare gas dimers, with the consequence that isolation of these metal atoms in a single substitutional site of the solid rare gas is unlikely, with the possible exception of Ca/Xe. The luminescence of metal dimer bands has been recorded for Ba and Sr revealing very different behaviours. Resonance fluorescence with a lifetime of 15 ns is observed for the lowest energy transition of Sr{sub 2} while this transition is quenched in Ba{sub 2}. This behaviour is consistent with the absence of vibrational structure on the dimer absorption band in Ba{sub 2} indicating lifetime broadening arising from efficient relaxation to low-lying molecular states. More extensive 2D excitation-emission data recorded for the complex site structures present on the absorption bands of the atomic Ba and Sr systems will be presented in future publications.« less

Determination of arsenic and cadmium in crude oil by direct sampling graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

de Jesus, Alexandre; Zmozinski, Ariane Vanessa; Damin, Isabel Cristina Ferreira; Silva, Márcia Messias; Vale, Maria Goreti Rodrigues

2012-05-01

In this work, a direct sampling graphite furnace atomic absorption spectrometry method has been developed for the determination of arsenic and cadmium in crude oil samples. The samples were weighed directly on the solid sampling platforms and introduced into the graphite tube for analysis. The chemical modifier used for both analytes was a mixture of 0.1% Pd + 0.06% Mg + 0.06% Triton X-100. Pyrolysis and atomization curves were obtained for both analytes using standards and samples. Calibration curves with aqueous standards could be used for both analytes. The limits of detection obtained were 5.1 μg kg- 1 for arsenic and 0.2 μg kg- 1 for cadmium, calculated for the maximum amount of sample that can be analyzed (8 mg and 10 mg) for arsenic and cadmium, respectively. Relative standard deviations lower than 20% were obtained. For validation purposes, a calibration curve was constructed with the SRM 1634c and aqueous standards for arsenic and the results obtained for several crude oil samples were in agreement according to paired t-test. The result obtained for the determination of arsenic in the SRM against aqueous standards was also in agreement with the certificate value. As there is no crude oil or similar reference material available with a certified value for cadmium, a digestion in an open vessel under reflux using a "cold finger" was adopted for validation purposes. The use of paired t-test showed that the results obtained by direct sampling and digestion were in agreement at a 95% confidence level. Recovery tests were carried out with inorganic and organic standards and the results were between 88% and 109%. The proposed method is simple, fast and reliable, being appropriated for routine analysis.

Determination of band gap in epitaxial delafossite Cu oxide using optical techniques

NASA Astrophysics Data System (ADS)

Cabrera, Alejandro; Wheatley, R.; Seifert, B.; Wallentowitz, S.; Joshi, T.; Lederman, D.

Highly epitaxial delafossite CuFeO2 and CuFe1-xGaxO2 films were grown using Pulsed Laser Deposition techniques. The sample thicknesses were estimated to be 21 nm, 75 nm.The estimated gallium fraction of substituted ferric atoms was x =0.25 for the composite sample. We present the study of the fundamental band gap(s) for each sample via observation of their respective optical absorption properties in the NIR-VIS region using transmittance and diffuse reflection spectroscopy. Predominant absorption edges measured were between 1.1eV and 3.1eV from transmittance spectra. The sample of CuFe1-xGaxO2 showed measurable absorption features located at 2.4eV and 2.8eV. This study also found evidence of changes between apparent absorption edges between transmittance and diffuse reflectance spectroscopies of each sample and it may be resultant from absorption channels via surface states. Future photoluminescence experiments are planned to determine the photo-induced semiconductor behavior of these materials. ACNOWLEDGEMENTS: This work was supported by FONDECyT 1130372 and Proyecto Anillo ACT1409 at PUC and supported in part by the WV Higher Education Policy Commission (Grant HEPC.dsr.12.29) and by FAME sponsored by MARCO and DARPA (contract # 2013-MA-2382).

Optical spectroscopy of laser-produced plasmas for standoff isotopic analysis

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

Harilal, Sivanandan S.; Brumfield, Brian E.; LaHaye, Nicole L.

2018-04-20

This review article covers the present status of isotope detection through emission, absorption, and fluorescence spectroscopy of atoms and molecules in a laser-produced plasma formed from a solid sample. A description of the physics behind isotope shifts in atoms and molecules is presented, followed by the physics behind solid sampling of laser ablation plumes, optical methods for isotope measurements, the suitable physical conditions of laser-produced plasma plumes for isotopic analysis, and the current status. Finally, concluding remarks will be made on the existing gaps between previous works in the literature and suggestions for future work.

Optical spectroscopy of laser-produced plasmas for standoff isotopic analysis

DOE PAGES

Harilal, S. S.; Brumfield, B. E.; LaHaye, N. L.; ...

2018-04-20

This review article covers the present status of isotope detection through emission, absorption, and fluorescence spectroscopy of atoms and molecules in a laser-produced plasma formed from a solid sample. A description of the physics behind isotope shifts in atoms and molecules is presented, followed by the physics behind solid sampling of laser ablation plumes, optical methods for isotope measurements, the suitable physical conditions of laser-produced plasma plumes for isotopic analysis, and the current status. Lastly, concluding remarks will be made on the existing gaps between previous works in the literature and suggestions for future work.

Optical spectroscopy of laser-produced plasmas for standoff isotopic analysis

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

Harilal, S. S.; Brumfield, B. E.; LaHaye, N. L.

This review article covers the present status of isotope detection through emission, absorption, and fluorescence spectroscopy of atoms and molecules in a laser-produced plasma formed from a solid sample. A description of the physics behind isotope shifts in atoms and molecules is presented, followed by the physics behind solid sampling of laser ablation plumes, optical methods for isotope measurements, the suitable physical conditions of laser-produced plasma plumes for isotopic analysis, and the current status. Finally, concluding remarks will be made on the existing gaps between previous works in the literature and suggestions for future work.

Optical spectroscopy of laser-produced plasmas for standoff isotopic analysis

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

Harilal, S. S.; Brumfield, B. E.; LaHaye, N. L.

This review article covers the present status of isotope detection through emission, absorption, and fluorescence spectroscopy of atoms and molecules in a laser-produced plasma formed from a solid sample. A description of the physics behind isotope shifts in atoms and molecules is presented, followed by the physics behind solid sampling of laser ablation plumes, optical methods for isotope measurements, the suitable physical conditions of laser-produced plasma plumes for isotopic analysis, and the current status. Lastly, concluding remarks will be made on the existing gaps between previous works in the literature and suggestions for future work.

Optical spectroscopy of laser-produced plasmas for standoff isotopic analysis

DOE PAGES

Harilal, S. S.; Brumfield, B. E.; LaHaye, N. L.; ...

2018-06-01

This review article covers the present status of isotope detection through emission, absorption, and fluorescence spectroscopy of atoms and molecules in a laser-produced plasma formed from a solid sample. A description of the physics behind isotope shifts in atoms and molecules is presented, followed by the physics behind solid sampling of laser ablation plumes, optical methods for isotope measurements, the suitable physical conditions of laser-produced plasma plumes for isotopic analysis, and the current status. Finally, concluding remarks will be made on the existing gaps between previous works in the literature and suggestions for future work.

Solid sampling determination of total fluorine in baby food samples by high-resolution continuum source graphite furnace molecular absorption spectrometry.

PubMed

Ozbek, Nil; Akman, Suleyman

2016-11-15

This study describes the applicability of solid sampling technique for the determination of fluorine in various baby foods via molecular absorption of calcium monofluoride generated in a graphite furnace of high-resolution continuum source atomic absorption spectrometry. Fluorine was determined at CaF wavelength, 606.440nm in a graphite tube applying a pyrolysis temperature of 1000°C and a molecule forming temperature of 2200°C. The limit of detection and characteristic mass of the method were 0.20ng and 0.17ng of fluorine, respectively. The fluorine concentrations determined in standard reference sample (bush branches and leaves) were in good agreement with the certified values. By applying the optimized parameters, the concentration of fluorine in various baby foods were determined. The fluorine concentrations were ranged from

Direct analysis of environmental and biological samples for total mercury with comparison of sequential atomic absorption and fluorescence measurements from a single combustion event

NASA Astrophysics Data System (ADS)

Cizdziel, James V.; Tolbert, Candice; Brown, Garry

2010-02-01

A Direct Mercury Analyzer (DMA) based on sample combustion, concentration of mercury by amalgamation with gold, and cold vapor atomic absorption spectrometry (CVAAS) was coupled to a mercury-specific cold vapor atomic fluorescence spectrometer (CVAFS). The purpose was to evaluate combustion-AFS, a technique which is not commercially available, for low-level analysis of mercury in environmental and biological samples. The experimental setup allowed for comparison of dual measurements of mercury (AAS followed by AFS) for a single combustion event. The AFS instrument control program was modified to properly time capture of mercury from the DMA, avoiding deleterious combustion products from reaching its gold traps. Calibration was carried out using both aqueous solutions and solid reference materials. The absolute detection limits for mercury were 0.002 ng for AFS and 0.016 ng for AAS. Recoveries for reference materials ranged from 89% to 111%, and the precision was generally found to be <10% relative standard deviation (RSD). The two methods produced similar results for samples of hair, finger nails, coal, soil, leaves and food stuffs. However, for samples with mercury near the AAS detection limit (e.g., filter paper spotted with whole blood and segments of tree rings) the signal was still quantifiable with AFS, demonstrating the lower detection limit and greater sensitivity of AFS. This study shows that combustion-AFS is feasible for the direct analysis of low levels of mercury in solid samples that would otherwise require time-consuming and contamination-prone digestion.

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. Copyright © 2015 Elsevier B.V. All rights reserved.

Speciation of Mn(II), Mn(VII) and total manganese in water and food samples by coprecipitation-atomic absorption spectrometry combination.

PubMed

Citak, Demirhan; Tuzen, Mustafa; Soylak, Mustafa

2010-01-15

A speciation procedure based on the coprecipitation of manganese(II) with zirconium(IV) hydroxide has been developed for the investigation of levels of manganese species. The determination of manganese levels was performed by flame atomic absorption spectrometry (FAAS). Total manganese was determined after the reduction of Mn(VII) to Mn(II) by ascorbic acid. The analytical parameters including pH, amount of zirconium(IV), sample volume, etc., were investigated for the quantitative recoveries of manganese(II). The effects of matrix ions were also examined. The recoveries for manganese(II) were in the range of 95-98%. Preconcentration factor was calculated as 50. The detection limit for the analyte ions based on 3 sigma (n=21) was 0.75 microg L(-1) for Mn(II). The relative standard deviation was found to be lower than 7%. The validation of the presented procedure was performed by analysis of certified reference material having different matrices, NIST SRM 1515 (Apple Leaves) and NIST SRM 1568a (Rice Flour). The procedure was successfully applied to natural waters and food samples.

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

PubMed

Tuzen, Mustafa; Pekiner, Ozlem Zeynep

2015-12-01

A rapid and environmentally friendly ultrasound assisted ionic liquid dispersive liquid liquid microextraction (USA-IL-DLLME) was developed for the speciation of inorganic selenium in beverages and total selenium in food samples by using graphite furnace atomic absorption spectrometry. Some analytical parameters including pH, amount of complexing agent, extraction time, volume of ionic liquid, sample volume, etc. were optimized. Matrix effects were also investigated. Enhancement factor (EF) and limit of detection (LOD) for Se(IV) were found to be 150 and 12 ng L(-1), respectively. The relative standard deviation (RSD) was found 4.2%. The accuracy of the method was confirmed with analysis of LGC 6010 Hard drinking water and NIST SRM 1573a Tomato leaves standard reference materials. Optimized method was applied to ice tea, soda and mineral water for the speciation of Se(IV) and Se(VI) and some food samples including beer, cow's milk, red wine, mixed fruit juice, date, apple, orange, grapefruit, egg and honey for the determination of total selenium. Copyright © 2015 Elsevier Ltd. All rights reserved.

Mercury(II) and methyl mercury determinations in water and fish samples by using solid phase extraction and cold vapour atomic absorption spectrometry combination.

PubMed

Tuzen, Mustafa; Karaman, Isa; Citak, Demirhan; Soylak, Mustafa

2009-07-01

A method has been developed for mercury(II) and methyl mercury speciation on Staphylococcus aureus loaded Dowex Optipore V-493 micro-column in the presented work, by using cold vapour atomic absorption spectrometry. Selective and sequential elution with 0.1 molL(-1) HCl for methyl mercury and 2 molL(-1) HCl for mercury(II) were performed at the pH range of 2-6. Optimal analytical conditions including pH, amounts of biosorbent, sample volumes were investigated. The detection limits of the analytes were 2.5 ngL(-1) for Hg(II) and 1.7 ngL(-1) for methyl mercury. The capacity of biosorbent for mercury(II) and methyl mercury was 6.5 and 5.4 mgg(-1), respectively. The validation of the presented procedure is performed by the analysis of standard reference material. The speciation procedure established was successfully applied to the speciation of mercury(II) and methyl mercury in natural water and microwave digested fish samples.

Analyses and descriptions of geochemical samples from the Rich Mountain Roadless Area, Fannin and Gilmer counties, Georgia

USGS Publications Warehouse

Sears, C.M.; Foose, M.P.; Day, G.W.; Ericksen, M.S.

1983-01-01

Semi-quantitative spectrographic analyses for 31 elements on rock, soil, fine-grained stream sediment, bulk stream sediment, and panned stream sediment samples collected in the Rich Mountain Roadless Area, Fannin and Gilmer Counties, Georgia, are reported here. Atomic absorption analyses for gold and fluorometric analyses for uranium are also reported. Brief descriptions of all rock samples analyzed are included.

Determination of iridium in mafic rocks by atomic absorption

USGS Publications Warehouse

Grimaldi, F.S.; Schnepfe, M.M.

1970-01-01

Iridium is determined in mineralized mafic rocks by atomic absorption after fire-assay concentration into a gold bead. Interelement interferences in the atomic-absorption determination are removed and Ir sensitivity is increased by buffering the solutions with a mixture of copper and sodium sulphates. Substantial amounts of Ag, Al, Au, Bi, Ca, Cd, Co, Cr, Fe, Ho, Hg, K, La, Mg, Mn, Mo, Ni, Pb, Te, Ti, V, Y, Zn and platinum metals can be tolerated in the atomic-absorption determination. The sensitivity and detection limits are 3.2 and 0.25 ppm of Ir, respectively. ?? 1970.

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. © 2011 Institute of Food Technologists®

Chemometric evaluation of Cd, Co, Cr, Cu, Ni (inductively coupled plasma optical emission spectrometry) and Pb (graphite furnace atomic absorption spectrometry) concentrations in lipstick samples intended to be used by adults and children.

PubMed

Batista, Érica Ferreira; Augusto, Amanda dos Santos; Pereira-Filho, Edenir Rodrigues

2016-04-01

A method was developed for determining the concentrations of Cd, Co, Cr, Cu, Ni and Pb in lipstick samples intended to be used by adults and children using inductively coupled plasma optical emission spectrometry (ICP OES) and graphite furnace atomic absorption spectrometry (GF AAS) after treatment with dilute HNO3 and hot block. The combination of fractional factorial design and Desirability function was used to evaluate the ICP OES operational parameters and the regression models using Central Composite and Doehlert designs were calculated to stablish the best working condition for all analytes. Seventeen lipstick samples manufactured in different countries with different colors and brands were analyzed. Some samples contained high concentrations of toxic elements, such as Cr and Pb, which are carcinogenic and cause allergic and eczematous dermatitis. The maximum concentration detected was higher than the permissible safe limits for human use, and the samples containing these high metal concentrations were intended for use by children. Principal component analysis (PCA) was used as a chemometrics tool for exploratory analysis to observe the similarities between samples relative to the metal concentrations (a correlation between Cd and Pb was observed). Copyright © 2015 Elsevier B.V. All rights reserved.

Use of slurry sampling for the direct determination of zinc in yogurt by high resolution-continuum source flame atomic absorption spectrometry.

PubMed

Brandao, Geovani C; de Jesus, Raildo M; da Silva, Erik G P; Ferreira, Sergio L C

2010-06-15

This paper presents an analytical procedure for the direct determination of zinc in yogurt employing sampling slurry and high resolution-continuum source flame atomic absorption spectrometry (HR-CS FAAS). The step optimization established the experimental conditions of: 2.0molL(-1) hydrochloric acid, a sonication time of 20min and a sample mass of 1.0g for a slurry volume of 25mL. This method allows the determination of zinc with a limit of quantification of 0.32microgg(-1). The precision expressed as relative standard deviation (RSD) were 0.82 and 2.08% for yogurt samples containing zinc concentrations of 4.85 and 2.49microgg(-1), respectively. The accuracy was confirmed by the analysis of a certified reference material of non-fat milk powder furnished by the National Institute of Standard and Technology. The proposed method was applied for the determination of zinc in seven yogurt samples. The zinc content was varied from 2.19 to 4.85microgg(-1). These results agreed with those reported in the literature. The samples were also analyzed after acid digestion and zinc determination by FAAS. No statistical difference was observed between the results obtained by both of the procedures performed.

On-line ionic liquid-based preconcentration system coupled to flame atomic absorption spectrometry for trace cadmium determination in plastic food packaging materials.

PubMed

Martinis, Estefanía M; Olsina, Roberto A; Altamirano, Jorgelina C; Wuilloud, Rodolfo G

2009-05-15

A novel on-line preconcentration method based on liquid-liquid (L-L) extraction with room temperature ionic liquids (RTILs) coupled to flame atomic absorption spectrometry (FAAS) was developed for cadmium determination in plastic food packaging materials. The methodology is based on the complexation of Cd with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) reagent after sample digestion followed by extraction of the complex with the RTIL 1-butyl-3-methylimidazolium hexafluorophosphate ([C(4)mim][PF(6)]). The mixture was loaded into a flow injection analysis (FIA) manifold and the RTIL rich-phase was retained in a microcolumn filled with silica gel. The RTIL rich-phase was then eluted directly into FAAS. A enhancement factor of 35 was achieved with 20 mL of sample. The limit of detection (LOD), obtained as IUPAC recommendation, was 6 ng g(-1) and the relative standard deviation (R.S.D.) for 10 replicates at 10 microg L(-1) Cd concentration level was 3.9%, calculated at the peak heights. The calibration graph was linear and a correlation coefficient of 0.9998 was achieved. The accuracy of the method was evaluated by both a recovery study and comparison of results with direct determination by electrothermal atomic absorption spectrometry (ETAAS). The method was successfully applied for Cd determination in plastic food packaging materials and Cd concentrations found were in the range of 0.04-10.4 microg g(-1).

Collisional redistribution of radiation. II - The effects of degeneracy on the equations of motion for the density matrix. III - The equation of motion for the correlation function and the scattered spectrum

NASA Technical Reports Server (NTRS)

Burnett, K.; Cooper, J.

1980-01-01

The effect of correlations between an absorber atom and perturbers in the binary-collision approximation are applied to degenerate atomic systems. A generalized absorption profile which specifies the final state of the atom after an absorption event is related to the total intensities of Rayleigh scattering and fluorescence from the atom. It is suggested that additional dynamical information to that obtainable from ordinary absorption experiments is required in order to describe redistributed atomic radiation. The scattering of monochromatic radiation by a degenerate atom is computed in a binary-collision approximation; an equation of motion is derived for the correlation function which is valid outside the quantum-regression regime. Solutions are given for the weak-field conditions in terms of generalized absorption and emission profiles that depend on the indices of the atomic multipoles.

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

PubMed

Ramamurthy, N; Thillaivelavan, K

2005-01-01

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

Flame atomic absorption spectrometric determination of trace amounts of nickel after extraction and preconcentration onto natural modified analcime zeolite loaded with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol.

PubMed

Afzali, Darush; Taher, Mohammad Ali; Mostafavi, Ali; Mahani, Mohammad Khayatzadeh

2005-01-01

Nickel is a moderately toxic element compared with other transition metals. However, inhalation of nickel and its compounds leads to serious problems, including cancer of the respiratory system and a skin disorder, nickel-eczema. Thus, attention has focused on the toxicity of nickel at low concentrations, and the development of reliable, analytical approaches for the determination of trace amounts of nickel is needed. This paper describes a simple, rapid, and sensitive flame atomic absorption spectrometric method for the determination of trace amounts of nickel in various samples after adsorption of its 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex on a modified Analcime column in the pH range of 7.5-10.5. The retained analyte on the Analcime is recovered with 5.0 mL 2 M nitric acid and determined by flame atomic absorption spectrometry. The detection limit is 20 ng/mL, and the calibration curve is linear for analyte concentrations in the range of 0.1-8 microg/mL final solution, with a correlation coefficient of 0.9993. Eight replicate determinations of nickel at 2 microg/mL in the final solution gave an absorbance of 0.1222, with a relative standard deviation (RSD) of +/-1.2%. The interference of a large number of anions and cations was studied, and the proposed method was used for the determination of nickel in various standard reference samples. The accuracy of the proposed method was evaluated by analyzing standard reference samples, and the results were satisfactory (recoveries of >96%; RSD of <3.5%).

Screening Technique for Lead and Cadmium in Toys and Other Materials Using Atomic Absorption Spectroscopy

ERIC Educational Resources Information Center

Brouwer, Henry

2005-01-01

A simple procedure to quickly screen different consumer products for the presence of lead, cadmium, and other metals is described. This screening technique avoids expending a lot of preparation time on samples known to contain low levels of hazardous metals where only samples testing positive for the desired elements need to be analyzed…

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.

Dispersive liquid-liquid microextraction based on solidification of floating organic drop for preconcentration and determination of trace amounts of copper by flame atomic absorption spectrometry.

PubMed

Karadaş, Cennet; Kara, Derya

2017-04-01

A novel, simple, rapid, sensitive, inexpensive and environmentally friendly dispersive liquid-liquid microextraction method based on the solidification of a floating organic drop (DLLME-SFO) was developed for the determination of copper by flame atomic absorption spectrometry (FAAS). N-o-Vanillidine-2-amino-p-cresol was used as a chelating ligand and 1-undecanol was selected as an extraction solvent. The main parameters affecting the performance of DLLME-SFO, such as sample pH, volume of extraction solvent, extraction time, concentration of the chelating ligand, salt effect, centrifugation time and sample volume were investigated and optimized. The effect of interfering ions on the recovery of copper was also examined. Under the optimum conditions, the detection limit (3σ) was 0.93μgL -1 for Cu using a sample volume of 20mL, yielding a preconcentration factor of 20. The proposed method was successfully applied to the determination of Cu in tap, river and seawater, rice flour and black tea samples as well as certified reference materials. Copyright © 2016. Published by Elsevier Ltd.

Solid-phase extraction of copper(II) in water and food samples using silica gel modified with bis(3-aminopropyl)amine and determination by flame atomic absorption spectrometry.

PubMed

Cagirdi, Duygu; Altundag, Hüseyin; Imamoglu, Mustafa; Tuzen, Mustafa

2014-01-01

A simple and selective separation and preconcentration method was developed for the determination of Cu(ll) ions. This method is based on adsorption of Cu(ll) ions from aqueous solution on a bis(3-aminopropyl)amine modified silica gel column and flame atomic absorption spectrometric determination after desorption. Various analytical parameters such as pH, type of eluent solution and its volume, flow rate of sample and eluent, and sample volume were optimized. Effects of some cation, anion, and transition metal ions on the recoveries of Cu(ll) ions were also investigated. Cu(ll) ions were quantitatively recovered at pH 6; 5.0 mL of 2 M HCI was used as the eluent. The preconcentration factor was found to be 150. The LOD was 0.12 microg/L for Cu(ll). The accuracy of the method was confirmed by analysis of Tea Leaves (INCT-TL-1) and Fish Protein (DORM-3) certified reference materials. The optimized method was applied to various water and food samples for the determination of Cu(ll).

Determination of mercury by multisyringe flow injection system with cold-vapor atomic absorption spectrometry.

PubMed

Leal, L O; Elsholz, O; Forteza, R; Cerdà, V

2006-07-28

A new software-controlled time-based multisyringe flow injection system for mercury determination by cold-vapor atomic absorption spectrometry is proposed. Precise known volumes of sample, reducing agent (1.1% SnCl2 in 3% HCl) and carrier (3% HCl) are dispensed into a gas-liquid separation cell with a multisyringe burette coupled with one three-way solenoid valve. An argon flow delivers the reduced mercury to the spectrometer. The optimization of the system was carried out testing reaction coils and gas-liquid separators of different design as well as changing parameters, such as sample and reagents volumes, reagent concentrations and carrier gas flow rate, among others. The analytical curves were obtained within the range 50-5000 ng L(-1). The detection limit (3sigma(b)/S) achieved is 5 ng L(-1). The relative standard deviation (R.S.D.) was 1.4%, evaluated from 16 successive injections of 250 ng L(-1) Hg standard solution. The injection and sample throughput per hour were 44 and 11, respectively. This technique was validated by means of solid and water reference materials with good agreement with the certified values and was successfully applied to fish samples.

Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based-preconcentration and flow injection-cold vapor atomic absorption spectrometry.

PubMed

Martinis, Estefanía M; Bertón, Paula; Olsina, Roberto A; Altamirano, Jorgelina C; Wuilloud, Rodolfo G

2009-08-15

A liquid-liquid extraction procedure (L-L) based on room temperature ionic liquid (RTIL) was developed for the preconcentration and determination of mercury in different water samples. The analyte was quantitatively extracted with 1-butyl-3-methylimidazolium hexafluorophosphate ([C(4)mim][PF(6)]) under the form of Hg-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Hg-5-Br-PADAP) complex. A volume of 500 microl of 9.0 mol L(-1) hydrochloric acid was used to back-extract the analyte from the RTIL phase into an aqueous media prior to its analysis by flow injection-cold vapor atomic absorption spectrometry (FI-CV-AAS). A preconcentration factor of 36 was achieved upon preconcentration of 20 mL of sample. The limit of detection (LOD) obtained under the optimal conditions was 2.3ngL(-1) and the relative standard deviation (RSD) for 10 replicates at 1 microg L(-1) Hg(2+) was 2.8%, calculated with peaks height. The method was successfully applied to the determination of mercury in river, sea, mineral and tap water samples and a certified reference material (CRM).

Determination of Calcium in Cereal with Flame Atomic Absorption Spectroscopy: An Experiment for a Quantitative Methods of Analysis Course

ERIC Educational Resources Information Center

Bazzi, Ali; Kreuz, Bette; Fischer, Jeffrey

2004-01-01

An experiment for determination of calcium in cereal using two-increment standard addition method in conjunction with flame atomic absorption spectroscopy (FAAS) is demonstrated. The experiment is intended to introduce students to the principles of atomic absorption spectroscopy giving them hands on experience using quantitative methods of…

The use of emulsions for the determination of methylmercury and inorganic mercury in fish-eggs oil by cold vapor generation in a flow injection system with atomic absorption spectrometric detection.

PubMed

Burguera, J L; Quintana, I A; Salager, J L; Burguera, M; Rondón, C; Carrero, P; Anton de Salager, R; Petit de Peña, Y

1999-04-01

An on-line time based injection system used in conjunction with cold vapor generation atomic absorption spectrometry and microwave-aided oxidation with potassium persulfate has been developed for the determination of the different mercury species in fish-eggs oil samples. A three-phase surfactant-oil-water emulsion produced an advantageous flow when a peristaltic pump was used to introduce the highly viscous sample into the system. The optimum proportion of the oil-water mixture ratio was 2:3 v/v with a Tween 20 surfactant concentration in the emulsion of 0.008% v/v. Inorganic mercury was determined after reduction with sodium borohydride while total mercury was determined after an oxidation step with persulfate prior to the reduction step to elemental mercury with the same reducing agent. The difference between total and inorganic mercury determined the organomercury content in samples. A linear calibration graph was obtained in the range 0.1-20 micrograms l-1 of Hg2+ by injecting 0.7 ml of samples. The detection limits based on 3 sigma of the blank signals were 0.11 and 0.12 microgram l-1 for total and inorganic mercury, respectively. The relative standard deviation of ten independent measurements were 2.8 and 2.2% for 10 micrograms l-1 and 8.8 and 9.0% for 0.1 microgram l-1 amounts of total and inorganic mercury, respectively. The recoveries of 0.3, 0.6 and 8 micrograms l-1 of inorganic and organic mercury added to fish-eggs oil samples ranged from 93.0 to 94.8% and from 100 to 106%, respectively. Good agreement with those values obtained for total mercury content in real samples by electrothermal atomic absorption spectrometry was also obtained, differences between mean values were < 7%. With the proposed procedure, 22 proteropterous catfish-eggs oil samples from the northwestern coast of Venezuela were measured; while the organic mercury lay in the range 2.0 and 3.3 micrograms l-1, inorganic mercury was not detected.

Analyses and description of soil samples from Mountain Lake and Peters Mountain Wilderness Study areas, Virginia and West Virginia

USGS Publications Warehouse

Motooka, J.M.; Curtis, Craig A.; Lesure, Frank Gardner

1978-01-01

Semiquantitative emission spectrographic analyses for 30 elements and atomic absorption analysis for zinc on 98 soil samples are reported here in detail. Location for all samples are in Universal Transverse Mercator (UTM) coordinates. A few samples of soil developed on Lower Devonian sandstone and chert contain more barium and zinc than soils on other formations but do not suggest the occurrence of economic concentrations of either element.

A green analytical method using ultrasound in sample preparation for the flow injection determination of iron, manganese, and zinc in soluble solid samples by flame atomic absorption spectrometry.

PubMed

Yebra, M Carmen

2012-01-01

A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5-30 mg) at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2-4.6%) and a sample throughput of ca. 25 samples h(-1) were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee) and pharmaceutical preparations (multivitamin tablets). The ranges of concentrations found were 21.4-25.61 μg g(-1) for iron, 5.74-18.30 μg g(-1) for manganese, and 33.27-57.90 μg g(-1) for zinc in soluble solid food samples and 3.75-9.90 μg g(-1) for iron, 0.47-5.05 μg g(-1) for manganese, and 1.55-15.12 μg g(-1) for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors.

Effects of atomic oxygen and ultraviolet radiation on candidate elastomeric materials for long duration missions. Test series no.1

NASA Technical Reports Server (NTRS)

Linton, R. C.; Finckenor, M. M.; Kamenetzky, R. R.; Gray, P.

1993-01-01

Research was conducted at MSFC on the behavior of elastomeric materials after exposure to simulated space environment. Silicone S383 and Viton V747 samples were exposed to thermal vacuum, ultraviolet radiation, and atomic oxygen and then evaluated for changes in material properties. Characterization of the elastomeric materials included weight, hardness, optical inspection under normal and black light, spectrofluorescence, solar absorptance and emittance, Fourier transform infrared spectroscopy, and permeability. These results indicate a degree of sensitivity to exposure and provided some evidence of UV and atomic oxygen synergism.

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. Copyright © 2013 The Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved.

Organic palladium and palladium-magnesium chemical modifiers in direct determination of lead in fractions from distillation of crude oil by electrothermal atomic absorption analysis

NASA Astrophysics Data System (ADS)

Kowalewska, Zofia; Bulska, Ewa; Hulanicki, Adam

1999-05-01

Platinum reforming catalysts are easily poisoned by increased levels of lead, therefore a sensitive atomic absorption spectrometric procedure for lead determination in fractions from crude oil distillation was developed. Lead was present in organic form in the samples analysed therefore the behaviour of various lead compounds (Pb-alkylarylsulphonate, Pb-4-cyclohexanobutyrate, tetraethyllead, Pb in fuel oil) was studied. The best procedure for the determination of lead in different petroleum products, including those containing asphaltenes includes a pretreatment with iodine and methyltrioctylammonium chloride, followed by the use of an organic Pd-Mg modifier. Under these conditions an effective matrix removal is possible at a pyrolysis temperature up to approximately 1100°C and the behaviour of lead present in different forms is unified. The characteristic mass is 11-12 pg Pb, corresponding to a detection limit of 0.25 ng g -1 for 20 μl sample solution. This can be lowered by multiple injection.

[Determination of soil exchangeable base cations by using atomic absorption spectrophotometer and extraction with ammonium acetate].

PubMed

Zhang, Yu-ge; Xiao, Min; Dong, Yi-hua; Jiang, Yong

2012-08-01

A method to determine soil exchangeable calcium (Ca), magnesium (Mg), potassium (K), and sodium (Na) by using atomic absorption spectrophotometer (AAS) and extraction with ammonium acetate was developed. Results showed that the accuracy of exchangeable base cation data with AAS method fits well with the national standard referential soil data. The relative errors for parallel samples of exchangeable Ca and Mg with 66 pair samples ranged from 0.02%-3.14% and 0.06%-4.06%, and averaged to be 1.22% and 1.25%, respectively. The relative errors for exchangeable K and Na with AAS and flame photometer (FP) ranged from 0.06%-8.39% and 0.06-1.54, and averaged to be 3.72% and 0.56%, respectively. A case study showed that the determination method for exchangeable base cations by using AAS was proven to be reliable and trustable, which could reflect the real situation of soil cation exchange properties in farmlands.

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

USGS Publications Warehouse

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

1981-01-01

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

Efficient atom localization via probe absorption in an inverted-Y atomic system

NASA Astrophysics Data System (ADS)

Wu, Jianchun; Wu, Bo; Mao, Jiejian

2018-06-01

The behaviour of atom localization in an inverted-Y atomic system is theoretically investigated. For the atoms interacting with a weak probe field and several orthogonal standing-wave fields, their position information can be obtained by measuring the probe absorption. Compared with the traditional scheme, we couple the probe field to the transition between the middle and top levels. It is found that the probe absorption sensitively depends on the detuning and strength of the relevant light fields. Remarkably, the atom can be localized at a particular position in the standing-wave fields by coupling a microwave field to the transition between the two ground levels.

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

PubMed

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

2013-11-15

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

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION AND MAINTENANCE OF THE PERKIN-ELMER ZEEMAN/5000 SYSTEM ATOMIC ABSORPTION SPECTROMETER (BCO-L-6.0)

EPA Science Inventory

The purpose of this SOP is to outline the start-up, calibration, operation, and maintenance procedures for the Perkin-Elmer 5000 atomic absorption spectrophotometer (PE 5000 AA), and the Perkin Elmer 5000 Zeeman graphite furnace atomic absorption spectrophotometer (PE 5000Z GFAA)...

Use of filler limestone and construction and demolition residues for remediating soils contaminated with heavy metals: an assessment by means of plant uptake.

NASA Astrophysics Data System (ADS)

Banegas, Ascension; Martinez-Sanchez, Maria Jose; Agudo, Ines; Perez-Sirvent, Carmen

2010-05-01

A greenhouse trial was carried out to evaluate the assimilation of heavy metals by three types of horticultural plants (lettuce, broccoli and alfalfa), different parts of which are destined for human and animal consumption (leaves, roots, fruits). The plants were cultivated in four types of soil, one uncontaminated (T1), one soil collected in the surrounding area of Sierra Minera (T2), the third being remediated with residues coming from demolition and construction activities (T3) and the four remediated with filler limestone (T4). To determine the metal content, soil samples were first ground to a fine powder using an agate ball mill. Fresh vegetable samples were separated into root and aboveground biomass and then lyophilized. The DTPA-extractable content was also determined to calculate the bioavailable amount of metal. Finally, the translocation factor (TF) and bioconcentration factor (BCF) were calculated. Arsenic levels were obtained by using atomic fluorescence spectrometry with an automated continuous flow hydride generation (HG-AFS) spectrometer and Cd, Pb and Zn was determined by electrothermal atomization atomic absorption spectrometry (ETAAS) or flame atomic absorption spectrometry (FAAS). Samples of the leached water were also obtained and analyzed. According to our results, the retention of the studied elements varies with the type of plant and is strongly decreased by the incorporation of filler limestone and/or construction and demolition residues to the soils. This practice represents a suitable way to reduce the risk posed to the biota by the presence of high levels of heavy metal in soil.

Separation and Enrichment of Gold in Water, Geological and Environmental Samples by Solid Phase Extraction on Multiwalled Carbon Nanotubes Prior to its Determination by Flame Atomic Absorption Spectrometry.

PubMed

Duran, Ali; Tuzen, Mustafa; Soylak, Mustafa

2015-01-01

This study proposes the application of multi-walled carbon nanotubes as a solid sorbent for the preconcentration of gold prior to its flame atomic absorption spectrometry determination. Extraction was achieved by using a glass column (15.0 cm in length and 1.0 cm in diameter). Quantitative recoveries were obtained in the pH range of 2.5-4.0; the elution step was carried out with 5.0 ml of 1.0 mol/L HNO3 in acetone. In the ligand-free study, variables such as pH, eluent type, sample volume, flow rates, and matrix effect were examined for the optimum recovery of gold ions. The gold ions were able to be pre-concentrated by a factor of 150 and their LOD was determined to be 1.71 μg/L. In order to evaluate the accuracy of the developed method, addition-recovery tests were applied for the tap water, mineral water, and sea water samples. Gold recovery studies were implemented using a wet digestion technique for mine and soil samples taken from various media, and this method was also applied for anodic slime samples taken from the factories located in the Kayseri Industrial Zone of Turkey.

Magnetic stirrer induced dispersive ionic-liquid microextraction for the determination of vanadium in water and food samples prior to graphite furnace atomic absorption spectrometry.

PubMed

Naeemullah; Kazi, Tasneem Gul; Tuzen, Mustafa

2015-04-01

A new dispersive liquid-liquid microextraction, magnetic stirrer induced dispersive ionic-liquid microextraction (MS-IL-DLLME) was developed to quantify the trace level of vanadium in real water and food samples by graphite furnace atomic absorption spectrometry (GFAAS). In this extraction method magnetic stirrer was applied to obtained a dispersive medium of 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6] in aqueous solution of (real water samples and digested food samples) to increase phase transfer ratio, which significantly enhance the recovery of vanadium - 4-(2-pyridylazo) resorcinol (PAR) chelate. Variables having vital role on desired microextraction methods were optimised to obtain the maximum recovery of study analyte. Under the optimised experimental variables, enhancement factor (EF) and limit of detection (LOD) were achieved to be 125 and 18 ng L(-1), respectively. Validity and accuracy of the desired method was checked by analysis of certified reference materials (SLRS-4 Riverine water and NIST SRM 1515 Apple leaves). The relative standard deviation (RSD) for 10 replicate determinations at 0.5 μg L(-1) of vanadium level was found to be <5.0%. This method was successfully applied to real water and acid digested food samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

Oxidation and crystal field effects in uranium

NASA Astrophysics Data System (ADS)

Tobin, J. G.; Yu, S.-W.; Booth, C. H.; Tyliszczak, T.; Shuh, D. K.; van der Laan, G.; Sokaras, D.; Nordlund, D.; Weng, T.-C.; Bagus, P. S.

2015-07-01

An extensive investigation of oxidation in uranium has been pursued. This includes the utilization of soft x-ray absorption spectroscopy, hard x-ray absorption near-edge structure, resonant (hard) x-ray emission spectroscopy, cluster calculations, and a branching ratio analysis founded on atomic theory. The samples utilized were uranium dioxide (U O2) , uranium trioxide (U O3) , and uranium tetrafluoride (U F4) . A discussion of the role of nonspherical perturbations, i.e., crystal or ligand field effects, will be presented.

Method development for the determination of fluorine in toothpaste via molecular absorption of aluminum mono fluoride using a high-resolution continuum source nitrous oxide/acetylene flame atomic absorption spectrophotometer.

PubMed

Ozbek, Nil; Akman, Suleyman

2012-05-30

Fluorine was determined via the rotational molecular absorption line of aluminum mono fluoride (AlF) generated in C(2)H(2)/N(2)O flame at 227.4613 nm using a high-resolution continuum source flame atomic absorption spectrophotometer (HR-CS-FAAS). The effects of AlF wavelength, burner height, fuel rate (C(2)H(2)/N(2)O) and amount of Al on the accuracy, precision and sensitivity were investigated and optimized. The Al-F absorption band at 227.4613 nm was found to be the most suitable analytical line with respect to sensitivity and spectral interferences. Maximum sensitivity and a good linearity were obtained in acetylene-nitrous oxide flame at a flow rate of 210 L h(-1) and a burner height of 8mm using 3000 mg L(-1) of Al for 10-1000 mg L(-1)of F. The accuracy and precision of the method were tested by analyzing spiked samples and waste water certified reference material. The results were in good agreement with the certified and spiked amounts as well as the precision of several days during this study was satisfactory (RSD<10%). The limit of detection and characteristic concentration of the method were 5.5 mg L(-1) and 72.8 mg L(-1), respectively. Finally, the fluorine concentrations in several toothpaste samples were determined. The results found and given by the producers were not significantly different. The method was simple, fast, accurate and sensitive. Copyright © 2012 Elsevier B.V. All rights reserved.

Electrothermal atomisation atomic absorption conditions and matrix modifications for determining antimony, arsenic, bismuth, cadmium, gallium, gold, indium, lead, molybdenum, palladium, platinum, selenium, silver, tellurium, thallium and tin following back-extraction of organic aminohalide extracts

USGS Publications Warehouse

Clark, J.R.

1986-01-01

A multi-element organic-extraction and back-extraction procedure, that had been developed previously to eliminate matrix interferences in the determination of a large number of trace elements in complex materials such as geological samples, produced organic and aqueous solutions that were complex. Electrothermal atomisation atomic absorption conditions and matrix modifications have been developed for 13 of the extracted elements (Ag, As, Au, Bi, Cd, Ga, In, Pb, Sb, Se, Sn, Te and Tl) that enhance sensitivity, alleviate problems resulting from the complex solutions and produce acceptable precision. Platinum, Pd and Mo can be determined without matrix modification directly on the original unstripped extracts.

Trace and Essential Elements Analysis in Cymbopogon citratus (DC.) Stapf Samples by Graphite Furnace-Atomic Absorption Spectroscopy and Its Health Concern

PubMed Central

Anal, Jasha Momo H.

2014-01-01

Cymbopogon citratus (DC.) Stapf commonly known as lemon grass is used extensively as green tea and even as herbal tea ingredient across the world. Plants have the ability to uptake metals as nutrient from the soil and its environment which are so essential for their physiological and biochemical growth. Concentrations of these twelve trace elements, namely, Mg, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Mo, As, Cd, and Pb, are analysed by graphite furnace-atomic absorption spectroscopy (GF-AAS) and are compared with the permissible limits of FAO/WHO, ICMR, and NIH, USA, which are found to be within permissible limits. Toxic metals like As, Cd, and Pb, analysed are within the tolerable daily diet limit and at low concentration. PMID:25525430

Development of a flow system for the determination of cadmium in fuel alcohol using vermicompost as biosorbent and flame atomic absorption spectrometry.

PubMed

Bianchin, Joyce Nunes; Martendal, Edmar; Mior, Renata; Alves, Vanessa Nunes; Araújo, Cleide Sandra Tavares; Coelho, Nívia Maria Melo; Carasek, Eduardo

2009-04-30

In this study a method for the determination of cadmium in fuel alcohol using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry was developed. The sorbent material used was a vermicompost commonly used as a garden fertilizer. The chemical and flow variables of the on-line preconcentration system were optimized by means of a full factorial design. The selected factors were: sorbent mass, sample pH, buffer concentration and sample flow rate. The optimum extraction conditions were obtained using sample pH in the range of 7.3-8.3 buffered with tris(hydroxymethyl)aminomethane at 50 mmol L(-1), a sample flow rate of 4.5 mL min(-1) and 160 mg of sorbent mass. With the optimized conditions, the preconcentration factor, limit of detection and sample throughput were estimated as 32 (for preconcentration of 10 mL sample), 1.7 microg L(-1) and 20 samples per hour, respectively. The analytical curve was linear from 5 up to at least 50 microg L(-1), with a correlation coefficient of 0.998 and a relative standard deviation of 2.4% (35 microg L(-1), n=7). The developed method was successfully applied to spiked fuel alcohol, and accuracy was assessed through recovery tests, with recovery ranging from 94% to 100%.

Determination of indium in geological materials by electrothermal-atomization atomic absorption spectrometry with a tungsten-impregnated graphite furance

USGS Publications Warehouse

Zhou, L.; Chao, T.T.; Meier, A.L.

1984-01-01

The sample is fused with lithium metaborate and the melt is dissolved in 15% (v/v) hydrobromic acid. Iron(III) is reduced with ascorbic acid to avoid its coextraction with indium as the bromide into methyl isobutyl ketone. Impregnation of the graphite furnace with sodium tungstate, and the presence of lithium metaborate and ascorbic acid in the reaction medium improve the sensitivity and precision. The limits of determination are 0.025-16 mg kg-1 indium in the sample. For 22 geological reference samples containing more than 0.1 mg kg-1 indium, relative standard deviations ranged from 3.0 to 8.5% (average 5.7%). Recoveries of indium added to various samples ranged from 96.7 to 105.6% (average 100.2%). ?? 1984.

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

PubMed

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

2016-06-20

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

Electron density and effective atomic number (Zeff) determination through x-ray Moiré deflectometry

NASA Astrophysics Data System (ADS)

Valdivia Leiva, Maria Pia; Stutman, Dan; Finkenthal, Michael

2014-10-01

Talbot-Lau based Moiré deflectometry is a powerful density diagnostic capable of delivering refraction information and attenuation from a single image, through the accurate detection of X-ray phase-shift and intensity. The technique is able to accurately measure both the real part of the index of refraction δ (directly related to electron density) and the attenuation coefficient μ of an object placed in the x-ray beam. Since the atomic number Z (or Zeff for a composite sample) is proportional to these quantities, an elemental map of the effective atomic number can be obtained with the ratio of the phase and the absorption image. The determination of Zeff from refraction and attenuation measurements with Moiré deflectometry could be of high interest in various fields of HED research such as shocked materials and ICF experiments as Zeff is linked, by definition, to the x-ray absorption properties of a specific material. This work is supported by U.S. DoE/NNSA Grant No. 435 DENA0001835.

Investigation of an alternating current plasma as an element selective atomic emission detector for high-resolution capillary gas chromatography and as a source for atomic absorption and atomic emission spectrometry

NASA Astrophysics Data System (ADS)

Ombaba, Jackson M.

This thesis deals with the construction and evaluation of an alternating current plasma (ACP) as an element-selective detector for high resolution capillary gas chromatography (GC) and as an excitation source for atomic absorption spectrometry (AAS) and atomic emission spectrometry (AES). The plasma, constrained in a quartz discharge tube at atmospheric pressure, is generated between two copper electrodes and utilizes helium as the plasma supporting gas. The alternating current plasma power source consists of a step-up transformer with a secondary output voltage of 14,000 V at a current of 23 mA. The device exhibits a stable signal because the plasma is self-seeding and reignites itself every half cycle. A tesla coil is not required to commence generation of the plasma if the ac voltage applied is greater than the breakdown voltage of the plasma-supporting gas. The chromatographic applications studied included the following: (1) the separation and selective detection of the organotin species, tributyltin chloride (TBT) and tetrabutyltin (TEBT), in environmental matrices including mussels (Mvutilus edullus) and sediment from Boston Harbor, industrial waste water and industrial sludge, and (2) the detection of methylcyclopentadienyl manganesetricarbonyl (MMT) and similar compounds used as gasoline additives. An ultrasonic nebulizer (common room humidifier) was utilized as a sample introduction device for aqueous solutions when the ACP was employed as an atomization source for atomic absorption spectrometry and as an excitation source for atomic emission spectrometry. Plasma diagnostic parameters studied include spatial electron number density across the discharge tube, electronic, excitation and ionization temperatures. Interference studies both in absorption and emission modes were also considered. Figures of merits of selected elements both in absorption and emission modes are reported. The evaluation of a computer-aided optimization program, Drylab GC, using spearmint oil and Environmental Protection Agency (EPA) standard mixture as probes is also discussed. The program supplied by LC Resources (Lafayette, CA) is used for separation optimization and prediction of gas chromatographic parameters. Column dead-time and average plate number were used as input data in conjunction with the retention times and peak areas of solutes at two different temperature programming rates. Once input data are entered into an IBM or IBM compatible personal computer, the program produces a 'relative resolution map' (RRM) which guides the analyst in selecting the most favorable temperature programming rate for the separation.

2. VIEW IN ROOM 111, ATOMIC ABSORPTION BERYLLIUM ANALYSIS LABORATORY. ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

2. VIEW IN ROOM 111, ATOMIC ABSORPTION BERYLLIUM ANALYSIS LABORATORY. AIR FILTERS AND SWIPES ARE DISSOLVED WITH ACIDS AND THE REMAINING RESIDUES ARE SUSPENDED IN NITRIC ACID SOLUTION. THE SOLUTION IS PROCESSED THROUGH THE ATOMIC ABSORPTION SPECTROPHOTOMETER TO DETECT THE PRESENCE AND LEVELS OF BERYLLIUM. - Rocky Flats Plant, Health Physics Laboratory, On Central Avenue between Third & Fourth Streets, Golden, Jefferson County, CO

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION, AND MAINTENANCE OF THE PERKIN-ELMER ZEEMAN/5000 SYSTEM ATOMIC ABSORPTION SPECTROPHOTOMETER (BCO-L-6.0)

EPA Science Inventory

The purpose of this SOP is to outline the start-up, calibration, operation, and maintenance procedures for the Perkin-Elmer 5000 atomic absorption spectrophotometer (PE 5000 AA), and the Perkin Elmer 5000 Zeeman graphite furnace atomic absorption spectrophotometer (PE 5000Z GFAA)...

Spectral and non-spectral interferences in the determination of thallium in environmental materials using electrothermal atomization and vaporization techniques—a case study

NASA Astrophysics Data System (ADS)

Vale, Maria Goreti R.; Welz, Bernhard

2002-12-01

The literature on the determination of Tl in environmental samples using electrothermal atomization (ETA) and vaporization (ETV) techniques has been reviewed with special attention devoted to potential interferences and their control. Chloride interference, which is due to the formation of the volatile monochloride in the condensed phase, is the most frequently observed problem. Due to its high dissociation energy (88 kcal/mol), TlCl is difficult to dissociate in the gas phase and is easily lost. The best means of controlling this interference in ETA is atomization under isothermal conditions according to the stabilized temperature platform furnace concept, and the use of reduced palladium as a modifier. An alternative approach appears to be the 'fast furnace' concept, wherein both the use of a modifier and the pyrolysis stage are omitted. This concept requires an efficient background correction system, and high-resolution continuum-source atomic absorption spectrometry (HR-CS AAS) appears to offer the best results. This chloride interference can also cause significant problems when ETV techniques are used. Among the spectral interferences found in the determination of thallium are those due to Pd, the most efficient modifier, and Fe, which is frequently found at high concentrations in environmental samples. Both interferences are due to nearby atomic lines, and are observed only when deuterium background correction and relatively high atomization temperatures are used. A more serious spectral interference is that due to the molecular absorption spectrum of SO 2, which has a maximum around the Tl line and exhibits a pronounced rotational fine structure. HR-CS AAS again showed the best performance in coping with this interference.

[Analysis of effects of salt stress on absorption and accumulation of mineral elements in Elymus spp. using atomic absorption spectrophotometer].

PubMed

Jia, Ya-xiong; Sun, Lei; He, Feng; Wan, Li-qiang; Yuan, Qing-hua; Li, Xiang-lin

2008-12-01

Salinization contributes significantly to soil degradation and the growth and survival of plants. A high level of salts imposes both ionic and osmotic stresses on plants, resulting in an excessive accumulation of sodium (Na) in plant tissues. Na toxicity disrupts the uptake of soil nutrients. Plant uptake and absorption of macro-elements under salt stress have been studied in plants, but there is little literature addressing the effect of salt stress on plant accumulation and absorption of micro-elements. Species in Elymus genus are among the most important forage plants on high-salinity soils in China An experiment was conducted to study the effect of salt stress on accumulation and absorption of both macro- and micro-elements by wild plants of Elymus genus. Plant samples taken from two populations with different salt tolerance were tested and the level of 4 macro-elements, namely Na, K, Ca and Mg, and 4 micro-elements, namely Cu, Fe, Mn, Zn was determined using atomic absorption spectrophotometer. The relationship between the selection of elements in the process of absorption and accumulation and salt tolerance was also analyzed. The results showed that the level of Na in root and leaf tissues increased with increasing salt stress. The level of Na in leaf tissue of plants with high salt tolerance (HS) was significantly higher than that in plants with low salt tolerance (P<0.05). The level of K and Ca decreased in response to increasing salt stress, while that in HS was higher than in LS. The level of Fe and Zn in the tissues of both roots and leaves increased. No significant difference was detected between HS and LS samples in the level of Cu in root tissues, while that of Cu in leaf tissue of both samples increased. The level of Mn decreased with increasing salt stress, but was higher in HS than in LS. Fe and Zn in roots and leaves of HS were lower than in those of LS.

Major- and trace-element concentrations in soils from two continental-scale transects of the United States and Canada

USGS Publications Warehouse

Smith, David B.; Cannon, William F.; Woodruff, Laurel G.; Garrett, Robert G.; Klassen, Rodney; Kilburn, James E.; Horton, John D.; King, Harley D.; Goldhaber, Martin B.; Morrison, Jean M.

2005-01-01

This report contains major- and trace-element concentration data for soil samples collected from 265 sites along two continental-scale transects in North America. One of the transects extends from northern Manitoba to the United States-Mexico border near El Paso, Tex. and consists of 105 sites. The other transect approximately follows the 38th parallel from the Pacific coast of the United States near San Francisco, Calif., to the Atlantic coast along the Maryland shore and consists of 160 sites. Sampling sites were defined by first dividing each transect into approximately 40-km segments. For each segment, a 1-km-wide latitudinal strip was randomly selected; within each strip, a potential sample site was selected from the most representative landscape within the most common soil type. At one in four sites, duplicate samples were collected 10 meters apart to estimate local spatial variability. At each site, up to four separate soil samples were collected as follows: (1) material from 0-5 cm depth; (2) O horizon, if present; (3) a composite of the A horizon; and (4) C horizon. Each sample collected was analyzed for total major- and trace-element composition by the following methods: (1) inductively coupled plasmamass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICPAES) for aluminum, antimony, arsenic, barium, beryllium, bismuth, cadmium, calcium, cerium, cesium, chromium, cobalt, copper, gallium, indium, iron, lanthanum, lead, lithium, magnesium, manganese, molybdenum, nickel, niobium, phosphorus, potassium, rubidium, scandium, silver, sodium, strontium, sulfur, tellurium, thallium, thorium, tin, titanium, tungsten, uranium, vanadium, yttrium, and zinc; (2) cold vapor- atomic absorption spectrometry for mercury; (3) hydride generation-atomic absorption spectrometry for antimony and selenium; (4) coulometric titration for carbonate carbon; and (5) combustion for total carbon and total sulfur.

Determination of copper and mercury in phosphate fertilizers employing direct solid sampling analysis and high resolution continuum source graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

de Oliveira Souza, Sidnei; François, Luciane Luiza; Borges, Aline Rocha; Vale, Maria Goreti Rodrigues; Araujo, Rennan Geovanny Oliveira

2015-12-01

The present study proposes the determination of copper and mercury in phosphate fertilizers by direct solid sampling analysis (SS) employing high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). For Cu determination, two analytical lines were used: 327.3960 nm and 249.2146 nm. Hg determination was carried out on the line 253.6521 nm and 100 μg KMnO4 was used as chemical modifier. The optimal pyrolysis temperature for Cu determination was 1300 °C. Atomization temperatures for Cu and Hg were 2400 and 1100 °C, respectively. External calibration with aqueous standard solutions was adopted for both elements. The limits of quantification (LoQs) and characteristic mass (m0) obtained for Cu determination were 0.4 μg g- 1 and 1.12 ng, respectively, on line 249.2146 nm, and 64 μg g- 1 and 25 pg on 327.3960 nm. For mercury, LoQ and m0 were 4.8 ng g- 1 and 39 pg, respectively. The accuracy of the proposed methods was confirmed by the analysis of standard reference material (SRM) of Trace Elements in Multi-Nutrient Fertilizer (SRM NIST 695). The precision expressed as relative standard deviation (RSD), was better than 8.2% for Hg and 7.7% for the Cu (n = 5), considered satisfactory for microanalysis in solid sample. Four fertilizer samples acquired in commercial establishments in the city of Salvador, Bahia, Brazil, were analyzed. The optimized analytical methods were simple, fast, accurate, precise and free of spectral interferences for the determination of Cu and Hg in phosphate fertilizer samples by SS-HR-CS GF AAS, avoiding the dissolution of the sample, the use of harmful reagents and the generation of residues.

Neutron activation analysis for antimetabolites. [in food samples

NASA Technical Reports Server (NTRS)

1973-01-01

Determination of metal ion contaminants in food samples is studied. A weighed quantity of each sample was digested in a concentrated mixture of nitric, hydrochloric and perchloric acids to affect complete solution of the food products. The samples were diluted with water and the pH adjusted according to the specific analysis performed. The samples were analyzed by neutron activation analysis, polarography, and atomic absorption spectrophotometry. The solid food samples were also analyzed by neutron activation analysis for increased sensitivity and lower levels of detectability. The results are presented in tabular form.

Embedded dielectric water "atom" array for broadband microwave absorber based on Mie resonance

NASA Astrophysics Data System (ADS)

Gogoi, Dhruba Jyoti; Bhattacharyya, Nidhi Saxena

2017-11-01

A wide band microwave absorber at X-band frequency range is demonstrated numerically and experimentally by embedding a simple rectangular structured dielectric water "atom" in flexible silicone substrate. The absorption peak of the absorber is tuned by manipulating the size of the dielectric water "atom." The frequency dispersive permittivity property of the water "atom" shows broadband absorption covering the entire X-band above 90% efficiency with varying the size of the water "atom." Mie resonance of the proposed absorber provides the desired impedance matching condition at the air-absorber interface across a wide frequency range in terms of electric and magnetic resonances. Multipole decomposition of induced current densities is used to identify the nature of observed resonances. Numerical absorptivity verifies that the designed absorber is polarization insensitive for normal incidence and can maintain an absorption bandwidth of more than 2 GHz in a wide-angle incidence. Additionally, the tunability of absorption property with temperature is shown experimentally.

Method for quantitative determination and separation of trace amounts of chemical elements in the presence of large quantities of other elements having the same atomic mass

DOEpatents

Miller, C.M.; Nogar, N.S.

1982-09-02

Photoionization via autoionizing atomic levels combined with conventional mass spectroscopy provides a technique for quantitative analysis of trace quantities of chemical elements in the presence of much larger amounts of other elements with substantially the same atomic mass. Ytterbium samples smaller than 10 ng have been detected using an ArF* excimer laser which provides the atomic ions for a time-of-flight mass spectrometer. Elemental selectivity of greater than 5:1 with respect to lutetium impurity has been obtained. Autoionization via a single photon process permits greater photon utilization efficiency because of its greater absorption cross section than bound-free transitions, while maintaining sufficient spectroscopic structure to allow significant photoionization selectivity between different atomic species. Separation of atomic species from others of substantially the same atomic mass is also described.

Determination of selenium in the environment and in biological material.

PubMed Central

Bem, E M

1981-01-01

This paper reviews the following problems, sampling, decomposition procedures and most important analytical methods used for selenium determination, e.g., neutron activation analysis, atomic absorption spectrometry, gas-liquid chromatography, spectrophotometry, fluorimetry, and x-ray fluorescence. This review covers the literature mainly from 1975 to 1977. PMID:7007035

Microwave Digestion and Furnace Atomic Absorption Method for the Quantification of Nano-scale TiO2 in Aqueous Samples

EPA Science Inventory

Many nanomaterials posses physical, and potentially biological, activity that is unique relative to their macro-scaled or soluble forms. One such property is surface plasmon resonance; a phenomenon that can generate or facilitate photoreactivity. Optimization of these properties ...

The Moss Techniques for Air Pollution Study in Bulgaria

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

Marinova, S.; Marinov, A.; Frontasyeva, M.

2010-01-21

The paper presents new results on atmospheric deposition of 41 elements in four areas of Bulgaria during the European moss survey in 2005. The results have been obtained by the moss biomonitoring technique. Ninety seven moss samples were analyzed by instrumental neutron activation analysis (ENAA) and atomic absorption spectrometry (AAS).

Do Atoms Really "Emit" Absorption Lines?

ERIC Educational Resources Information Center

Brecher, Kenneth

1991-01-01

Presents three absorption line sources that enhance student understanding of the phenomena associated with the interaction of light with matter and help dispel the misconception that atoms "emit" absorption lines. Sources include neodymium, food coloring and other common household liquids, and fluorescent materials. (MDH)

Hg-Xe exciplex formation in mixed Xe/Ar matrices: molecular dynamics and luminescence study.

PubMed

Lozada-García, Rolando; Rojas-Lorenzo, Germán; Crépin, Claudine; Ryan, Maryanne; McCaffrey, John G

2015-03-19

Luminescence of Hg((3)P1) atoms trapped in mixed Ar/Xe matrices containing a small amount of Xe is reported. Broad emission bands, strongly red-shifted from absorption are recorded which are assigned to strong complexes formed between the excited mercury Hg* and xenon atoms. Molecular dynamics calculations are performed on simulated Xe/Ar samples doped with Hg to follow the behavior of Hg* in the mixed rare gas matrices leading to exciplex formation. The role of Xe atoms in the first solvation shell (SS1) around Hg was investigated in detail, revealing the formation of two kinds of triatomic exciplexes; namely, Xe-Hg*-Xe and Ar-Hg*-Xe. The first species exists only when two xenon atoms are present in SS1 with specific geometries allowing the formation of a linear or quasi-linear exciplex. In the other geometries, or in the presence of only one Xe in SS1, a linear Ar-Hg*-Xe exciplex is formed. The two kinds of exciplexes have different emission bands, the most red-shifted being that involving two Xe atoms, whose emission is very close to that observed in pure Xe matrices. Simulations give a direct access to the analysis of the experimental absorption, emission, and excitation spectra, together with the dynamics of exciplexes formation.

Determination of Hg(II) in waters by on-line preconcentration using Cyanex 923 as a sorbent — Cold vapor atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Duan, Taicheng; Song, Xuejie; Xu, Jingwei; Guo, Pengran; Chen, Hangting; Li, Hongfei

2006-09-01

Using a solid phase extraction mini-column home-made from a neutral extractant Cyanex 923, inorganic Hg could be on-line preconcentrated and simultaneously separated from methyl mercury. The preconcentrated Hg (II) was then eluted with 10% HNO 3 and subsequently reduced by NaBH 4 to form Hg vapor before determination by cold vapor atomic absorption spectrometry (CVAAS). Optimal conditions for and interferences on the Hg preconcentration and measurement were at 1% HCl, for a 25 mL sample uptake volume and a 10 mL min - 1 sample loading rate. The detection limit was 0.2 ng L - 1 and much lower than that of conventional method (around 15.8 ng L - 1 ). The relative standard deviation (RSD) is 1.8% for measurements of 40 ng L - 1 of Hg and the linear working curve is from 20 to 2000 ng L - 1 (with a correlation coefficient of 0.9996). The method was applied in determination of inorganic Hg in city lake and deep well water (from Changchun, Jilin, China), and recovery test results for both samples were satisfactory.

Synthesis and application of a nanoporous ion-imprinted polymer for the separation and preconcentration of trace amounts of vanadium from food samples before determination by electrothermal atomic absorption spectrometry.

PubMed

Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Dehghanpoor Frashah, Shahab

2016-04-01

A vanadium ion-imprinted polymer was synthesized in the presence of V(V) and N-benzoyl-N-phenyl hydroxyl amine using 4-vinyl pyridine as the monomer, ethylene glycol dimethacrylate as the cross linker and 2,2'-azobis(isobutyronitrile) as the initiator. The imprinted V(V) ions were completely removed by leaching the polymer with 5 mol/L nitric acid, and the polymer structure was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The ion-imprinted polymer was used as the sorbent in the development of the solid-phase extraction method for V(V) prior to its determination by electrothermal atomic absorption spectrometry. The maximum sorption capacity for V(V) ions was 26.7 mg/g at pH 4.0. Under the optimum conditions, for a sample volume of 150.0 mL, an enrichment factor of 289.0 and a detection limit of 6.4 ng/L were obtained. The developed method was successfully applied to the determination of vanadium in parsley, zucchini, black tea, rice, and water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

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

2017-03-24

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

A new cloud point extraction procedure for determination of inorganic antimony species in beverages and biological samples by flame atomic absorption spectrometry.

PubMed

Altunay, Nail; Gürkan, Ramazan

2015-05-15

A new cloud-point extraction (CPE) for the determination of antimony species in biological and beverages samples has been established with flame atomic absorption spectrometry (FAAS). The method is based on the fact that formation of the competitive ion-pairing complex of Sb(III) and Sb(V) with Victoria Pure Blue BO (VPB(+)) at pH 10. The antimony species were individually detected by FAAS. Under the optimized conditions, the calibration range for Sb(V) is 1-250 μg L(-1) with a detection limit of 0.25 μg L(-1) and sensitive enhancement factor of 76.3 while the calibration range for Sb(III) is 10-400 μg L(-1) with a detection limit of 5.15 μg L(-1) and sensitive enhancement factor of 48.3. The precision as a relative standard deviation is in range of 0.24-2.35%. The method was successfully applied to the speciative determination of antimony species in the samples. The validation was verified by analysis of certified reference materials (CRMs). Copyright © 2014 Elsevier Ltd. All rights reserved.

Ligandless surfactant mediated solid phase extraction combined with Fe₃O₄ nano-particle for the preconcentration and determination of cadmium and lead in water and soil samples followed by flame atomic absorption spectrometry: multivariate strategy.

PubMed

Jalbani, N; Soylak, M

2014-04-01

In the present study, a microextraction technique combining Fe3O4 nano-particle with surfactant mediated solid phase extraction ((SM-SPE)) was successfully developed for the preconcentration/separation of Cd(II) and Pb(II) in water and soil samples. The analytes were determined by flame atomic absorption spectrometry (FAAS). The effective variables such as the amount of adsorbent (NPs), the pH, concentration of non-ionic (TX-114) and centrifugation time (min) were investigated by Plackett-Burman (PBD) design. The important variables were further optimized by central composite design (CCD). Under the optimized conditions, the detection limits (LODs) of Cd(II) and Pb(II) were 0.15 and 0.74 µg/L, respectively. The validation of the proposed procedure was checked by the analysis of certified reference materials of TMDA 53.3 fortified water and GBW07425 soil. The method was successfully applied for the determination of Cd(II) and Pb(II) in water and soil samples. Copyright © 2014 Elsevier Inc. All rights reserved.

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.

Maps showing mines, quarries, and prospects, with analyses of samples, Gee Creek Wilderness, Polk and Monroe counties, Tennessee

USGS Publications Warehouse

Gazdik, Gertrude C.; Behum, Paul T.

1983-01-01

During the recent U.S. Bureau of Mines field investigation, 21 samples were collected (fig. 2) and were submitted to the Bureau's Reno Metallurgy Research Center, Reno, Nev., for analysis. All samples were tested for 40 elements by semiquantitative spectrographic analyses. Additional testing by atomic absorption, neutron activation, and wet chemical techniques was performed for selected elements on some samples. Two shale samples were submitted to the Bureau of Mines, Tuscaloosa Metallurgy Research Center, Tuscaloosa, Ala., for the evaluation of ceramic properties. 

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.

Displacement-dispersive liquid-liquid microextraction based on solidification of floating organic drop of trace amounts of palladium in water and road dust samples prior to graphite furnace atomic absorption spectrometry determination.

PubMed

Ghanbarian, Maryam; Afzali, Daryoush; Mostafavi, Ali; Fathirad, Fariba

2013-01-01

A new displacement-dispersive liquid-liquid microextraction method based on the solidification of floating organic drop was developed for separation and preconcentration of Pd(ll) in road dust and aqueous samples. This method involves two steps of dispersive liquid-liquid microextraction based on solidification. In Step 1, Cu ions react with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which is extracted by dispersive liquid-liquid microextraction based on a solidification procedure using 1-undecanol (extraction solvent) and ethanol (dispersive solvent). In Step 2, the extracted complex is first dispersed using ethanol in a sample solution containing Pd ions, then a dispersive liquid-liquid microextraction based on a solidification procedure is performed creating an organic drop. In this step, Pd(ll) replaces Cu(ll) from the pre-extracted Cu-DDTC complex and goes into the extraction solvent phase. Finally, the Pd(ll)-containing drop is introduced into a graphite furnace using a microsyringe, and Pd(ll) is determined using atomic absorption spectrometry. Several factors that influence the extraction efficiency of Pd and its subsequent determination, such as extraction and dispersive solvent type and volume, pH of sample solution, centrifugation time, and concentration of DDTC, are optimized.

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

Ozkendir, Osman Murat, E-mail: ozkendir@gmail.com

Highlights: • Crystal and electronic structure properties of Nd{sub x}Ti{sub 1−x}BO{sub 2+d} structure were investigated. • New crystal structures for Nd–Ti complexes are determined. • Distortions in the crystal structure were observed as a result of Boron shortage. • Prominent change in electronic properties of the samples with the increasing Nd amount. - Abstract: Neodymium substituted TiBO{sub 3} samples were investigated according to their crystal, electric and electronic properties. Studies were conducted by X-ray absorption fine structure spectroscopy (XAFS) technique for the samples with different substitutions in the preparation processes. To achieve better crystal structure results during the study, XRDmore » pattern results were supported by extended-XAFS (EXAFS) analysis. The electronic structure analysis were studied by X-ray absorption near-edge structure spectroscopy (XANES) measurements at the room temperatures. Due to the substituted Nd atoms, prominent changes in crystal structure, new crystal geometries for Nd-Ti complexes, phase transitions in the crystals structure were detected according to the increasing Nd substitutions in the samples. In the entire stages of the substitutions, Nd atoms were observed as governing the whole phenomena due to their dominant characteristics in Ti geometries. Besides, electrical resistivity decay was determined in the materials with the increasing amount of Nd substitution.« less

Flow injection-hydride generation atomic absorption spectrometric determination of selenium, arsenic and bismuth.

PubMed

Zhang, Yanlin; Adeloju, Samuel B

2008-08-15

A simple and robust flow injection system which permits low sample and reagent consumption is described for rapid and reliable hydride generation atomic absorption spectrometric determination of selenium, arsenic and bismuth. The system, which composed of one peristaltic pump and one four channel solenoid valve, used water as the carrier streams for both sample and NaBH(4) solution. Rapid off-line pre-reduction of the analytes was achieved by using hydroxylamine hydrochloride for selenium and a mixture of potassium iodide and ascorbic acid for arsenic and bismuth. Transition metal interference was eliminated with the addition of thiourea and EDTA into the NaBH(4) solution and significant sensitivity enhancement was observed for selenium in the presence of thiourea in the reductant solution. Under optimised conditions, the method achieved detection limits of 0.2 ng mL(-1) for Se, 0.5 ng mL(-1) for As and 0.3 ng mL(-1) for Bi. The method was very reproducible, achieving relative standard deviations of 6.3% for Se, 3.6% for As and 4.7% for Bi, and has a sample throughput of 360 h(-1). Successful application of the method to the quantification of selenium, arsenic and bismuth in a certified reference river sediment sample is reported.

One-step displacement dispersive liquid-liquid microextraction coupled with graphite furnace atomic absorption spectrometry for the selective determination of methylmercury in environmental samples.

PubMed

Liang, Pei; Kang, Caiyan; Mo, Yajun

2016-01-01

A novel method for the selective determination of methylmercury (MeHg) was developed by one-step displacement dispersive liquid-liquid microextraction (D-DLLME) coupled with graphite furnace atomic absorption spectrometry. In the proposed method, Cu(II) reacted with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which was used as the chelating agent instead of DDTC for the dispersive liquid-liquid microextraction (DLLME) of MeHg. Because the stability of MeHg-DDTC is higher than that of Cu-DDTC, MeHg can displace Cu from the Cu-DDTC complex and be preconcentrated in a single DLLME procedure. MeHg could be extracted into the extraction solvent phase at pH 6 while Hg(II) remained in the sample solution. Potential interference from co-existing metal ions with lower DDTC complex stability was largely eliminated without the need of any masking reagent. Under the optimal conditions, the limit of detection of this method was 13.6ngL(-1) (as Hg), and an enhancement factor of 81 was achieved with a sample volume of 5.0mL. The proposed method was successfully applied for the determination of trace MeHg in some environmental samples with satisfactory results. Copyright © 2015 Elsevier B.V. All rights reserved.

Modified Activated Carbon Prepared from Acorn Shells as a New Solid-Phase Extraction Sorbent for the Preconcentration and Determination of Trace Amounts of Nickel in Food Samples Prior to Flame Atomic Absorption Spectrometry.

PubMed

Ebrahimi, Bahram

2017-03-01

A new solid-phase extraction (SPE) sorbent was introduced based on acidic-modified (AM) activated carbon (AC) prepared from acorn shells of native oak trees in Kurdistan. Hydrochloric acid (15%, w/w) and nitric acid (32.5%, w/w) were used to condition and modify AC. The IR spectra of AC and AM-AC showed that AM lead to the formation of increasing numbers of acidic functional groups on AM-AC. AM-AC was used in the SPE method for the extraction and preconcentration of Ni+2 prior to flame atomic absorption spectrometric determination at ng/mL levels in model and real food samples. Effective parameters of the SPE procedure, such as the pH of the solutions, sorbent dosage, extraction time, sample volume, type of eluent, and matrix ions, were considered and optimized. An enrichment factor of 140 was obtained. The calibration curve was linear with an R2 of 0.997 in the concentration range of 1-220 ng/mL. The RSD was 5.67% (for n = 7), the LOD was 0.352 ng/mL, and relative recoveries in vegetable samples ranged from 96.7 to 103.7%.

Flow injection/atomic absorption spectrometric determination of zineb in commercial formulations of pesticide based on slurry sampling.

PubMed

Cassella, Ricardo J; Salim, Verĵnica A; Garrigues, Salvador; Santelli, Ricardo E; de la Guardia, Miguel

2002-11-01

This paper reports on a new strategy for the slurry sampling determination of dithiocarbamate pesticide zineb [[ethylenebis(dithiocarbamato)]zinc] employing a FIA system with a flame atomic absorption spectrometry detector. In the flow system, an on-line alkaline hydrolysis of the pesticide is performed, allowing the release of Zn(II) ions to the solution, which are easily detected by a flame AAS technique. Several parameters that could affect the performance of the analytical methodology were studied, such as the concentration of NH3(aq) used in the hydrolysis step, the effect of the presence of Triton X-100 on the sensitivity and precision, and the FIA parameters (carrier flow rate and mixing coil volume). Under optimized conditions, aqueous slurries containing 2.5 to 25 microg ml(-1) zineb provided good linear calibration fits. From the obtained data, a detection limit (3sigma) of 1.0 microg ml(-1) zineb was found and a repeatability of 2.7% was obtained from 12 measurements of a slurry containing 2.5 microg m(-1) zineb. On the other hand, a precision (reproducibility) of 7.8% was achieved from three determinations of a sample containing 128 mg g(-1) of the pesticide. Also, the developed system provides a sampling frequency of 72 h(-1).

Ultrasound-Assisted Emulsification Microextraction Based on Solidification Floating Organic Drop Trace Amounts of Manganese Prior to Graphite Furnace Atomic Absorption Spectrometry Determination

PubMed Central

Mohadesi, Alireza; Falahnejad, Masoumeh

2012-01-01

In the present study, an ultrasound-assisted emulsification microextraction based on solidification floating organic drop method is described for preconcentration of trace amounts of Mn (II). 2-(5-Bromo-2-pyridylazo)-5 diethylaminophenol was added to a solution of Mn+2 at ph = 10.0. After this, 1-undecanol was added to the solution as an extraction solvent, and solution was stirred. Several factors influencing the microextraction efficiency, such as pH, the amount of chelating agent, nature and volume of extraction solvent, the volume of sample solution, stirring rate, and extraction time were investigated and optimized. Then sample vial was cooled by inserting into an ice bath, and the solidified was transferred into a suitable vial for immediate melting. Finally the sample was injected into a graphite furnace atomic absorption spectrometry. Under the optimum condition the linear dynamic range was 0.50–10.0 ng mL−1 with a correlation coefficient of 0.9926, and the detection limit of 0.3 ng mL−1 was obtained. The enrichment factor was 160. The proposed method was successfully applied for separation and determination of manganese in sea, rain, tap, and river water samples. PMID:22645504

A Green Analytical Method Using Ultrasound in Sample Preparation for the Flow Injection Determination of Iron, Manganese, and Zinc in Soluble Solid Samples by Flame Atomic Absorption Spectrometry

PubMed Central

Yebra, M. Carmen

2012-01-01

A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5–30 mg) at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2–4.6%) and a sample throughput of ca. 25 samples h–1 were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee) and pharmaceutical preparations (multivitamin tablets). The ranges of concentrations found were 21.4–25.61 μg g−1 for iron, 5.74–18.30 μg g−1 for manganese, and 33.27–57.90 μg g−1 for zinc in soluble solid food samples and 3.75–9.90 μg g−1 for iron, 0.47–5.05 μg g−1 for manganese, and 1.55–15.12 μg g−1 for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors. PMID:22567553

[Determination of trace cobalt in human urine by graphite furnace atomic absorption spectrometr].

PubMed

Zhong, L X; Ding, B M; Jiang, D; Liu, D Y; Yu, B; Zhu, B L; Ding, L

2016-05-20

To establish a method to determine cobalt in human urine by graphite furnace atomic absorption spectrometry. Urine with 2% nitric acid diluted two-fold, to quantify the curve, graphite furnace atomic absorption spectrometric detection. Co was linear within 2.5~40.0 ng/ml with r>0.999. Spike experiment showed that Co received good recovery rate, which was 90.8%~94.8%. Intra-assay precisions were 3.2%~5.1% for Co, inter-assay precisions were 4.4%~5.2% for Co. The method by using graphite furnace atomic absorption spectrometr to determine urine Co was fast, accurate and with low matrix effect. It could meet the requirement in GBZ/T 210.5-2008.

On-line preconcentration system for lead(II) determination in waste water by atomic absorption spectrometry using active carbon loaded with Pyrogallol Red.

PubMed

Ensafi, Ali A; Khayamian, Taghi; Karbasi, Mohammad H

2003-06-01

An on-line system for enrichment and determination of lead(II) is presented. It is based on the adsorption of lead(II) ions on a minicolumn packed with active carbon loaded with Pyrogallol Red. After preconcentration step, the metal ions are eluted automatically by 5.0 ml of 0.50 M nitric acid solution and the lead ion contents were determined by atomic absorption spectrometry. The influence of chemicals, pH and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, the lead ions in aqueous samples were concentrated about 100 fold by the column. The detection limit was 0.001 microg ml(-1). The recovery percent of spliced lead(II) was in the range of 98%-103%.

An induction furnace for the determination of cadmium in solutions and zinc-base metals by atomic-absorption spectroscopy.

PubMed

Headridge, J B; Smith, D R

1971-03-01

An induction furnace coupled to a Unicam SP90 atomic-absorption spectrophotometer is described for the determination of traces of volatile elements in solutions and volatile matrices. The apparatus has been used to obtain calibration graphs for 1-20 and 50-750 ng of cadmium in microl-volumes of solution, the 228.8 and 326.2 nm resonance lines respectively being used, and to determine cadmium in 5-mg samples of zinc-base metals within the concentration range 5-400 microg g by using the less sensitive 326-2-nm line. A furnace temperature of 1,350 degrees was used. Data on accuracy and precision are presented. The apparatus could readily be used to determine trace elements in volatile materials at concentrations of 10-1000 ng/g .

Growth and characterization of LiInSe2 single crystals

NASA Astrophysics Data System (ADS)

Ma, Tianhui; Zhu, Chongqiang; Lei, Zuotao; Yang, Chunhui; Sun, Liang; Zhang, Hongchen

2015-04-01

Large and crack-free LiInSe2 single crystals were obtained by the vertical gradient freezing method with adding a temperature oscillation technology in a two-zone furnace. X-ray diffraction data showed that the pure LiInSe2 compound was synthesized. The grown crystals had different color depending on melt composition. The atomic ratios of elements of LiInSe2 crystals were obtained by an Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES), and the structural formula were calculated according to the relative contents of elements. The average absorption coefficients were estimated by using average reflection indices. The absorption coefficients of the thermal annealing samples are 0.6 cm-1 at 2-3 μm. The transparent range of our LiInSe2 crystals is from 0.6 μm to 13.5 μm.

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.

A rapid, partial leach and organic separation for the sensitive determination of Ag, Bi, Cd, Cu, Mo, Pb, Sb, and Zn in surface geologic materials by flame atomic absorption

USGS Publications Warehouse

Viets, J.G.; Clark, J.R.; Campbell, W.L.

1984-01-01

A solution of dilute hydrochloric acid, ascorbic acid, and potassium iodide has been found to dissolve weakly bound metals in soils, stream sediments, and oxidized rocks. Silver, Bi, Cd, Cu, Mo, Pb, Sb, and Zn are selectively extracted from this solution by a mixture of Aliquat 336 (tricaprylyl methyl ammonium chloride) and MIBK (methyl isobutyl ketone). Because potentially interfering major and minor elements do not extract, the organic separation allows interference-free determinations of Ag and Cd to the 0.05 ppm level, Mo, Cu, and Zn to 0.5 ppm, and Bi, Pb, and Sb to 1 ppm in the sample using flame atomic absorption spectroscopy. The analytical absorbance values of the organic solution used in the proposed method are generally enhanced more than threefold as compared to aqueous solutions, due to more efficient atomization and burning characteristics. The leaching and extraction procedures are extremely rapid; as many as 100 samples may be analyzed per day, yielding 800 determinations, and the technique is adaptable to field use. The proposed method was compared to total digestion methods for geochemical reference samples as well as soils and stream sediments from mineralized and unmineralized areas. The partial leach showed better anomaly contrasts than did total digestions. Because the proposed method is very rapid and is sensitive to pathfinder elements for several types of ore deposits, it should be useful for reconnaissance surveys for concealed deposits. ?? 1984.

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).

Atomically designed precursors in optical fiber amplifiers: The thermal stability of the heterobimetallic ErAl3(OPri)12 in a solution-coated silica soot

NASA Astrophysics Data System (ADS)

Engholm, M.; Lashgari, K.; Edvardsson, S.; Westin, G.; Norin, L.

2005-06-01

The thermal stability of the bimetallic alkoxide ErAl3(OPri)12 doped in an unsintered silica (soot) has been investigated. Samples have been heated to different temperatures (up to 1500°C and analyzed by using ultraviolet-visible-near infrared absorption spectroscopy, infrared spectroscopy, scanning electron microscopy, energy dispersive spectroscopy, thermal gravimetric analysis, and powder x-ray diffraction. It is seen that the doped samples heated up to 1000°C show broad glasslike absorption spectra, indicating an amorphous structure, while the high-temperature sample shows an ordered crystallinelike structure with sharp characteristic absorption peaks. X-ray diffraction measurements indicate the formation of an ordered structure at temperatures of 1500°C, revealing a crystal phase of silica and phases of erbium and aluminosilicate. A comparison is also made with a sample doped with aqueous ErCl3 and Al(NO3)3. It is concluded that the local structure of the ErAl3 precursor is not preserved at temperatures above 1000°C. Alternative doping procedures are discussed.

Incorporation of Trace Elements in Ancient and Modern Human Bone: An X-Ray Absorption Spectroscopy Study

NASA Astrophysics Data System (ADS)

Pingitore, N. E.; Cruz-Jimenez, G.; Price, T. D.

2001-12-01

X-ray absorption spectroscopy (XAS) affords the opportunity to probe the atomic environment of trace elements in human bone. We are using XAS to investigate the mode(s) of incorporation of Sr, Zn, Pb, and Ba in both modern and ancient (and thus possibly altered) human and animal bone. Because burial and diagenesis may add trace elements to bone, we performed XAS analysis on samples of pristine contemporary and ancient, buried human and animal bone. We assume that deposition of these elements during burial occurs by processes distinct from those in vivo, and this will be reflected in their atomic environments. Archaeologists measure strontium in human and animal bone as a guide to diet. Carnivores show lower Sr/Ca ratios than their herbivore prey due to discrimination against Sr relative to Ca up the food chain. In an initial sample suite no difference was observed between modern and buried bone. Analysis of additional buried samples, using a more sensitive detector, revealed significant differences in the distance to the second and third neighbors of the Sr in some of the buried samples. Distances to the first neighbor, oxygen, were similar in all samples. Zinc is also used in paleo-diet studies. Initial x-ray absorption spectroscopy of a limited suite of bones did not reveal any differences between modern and buried samples. This may reflect the limited number of samples examined or the low levels of Zn in typical aqueous solutions in soils. Signals from barium and lead were too low to record useful XAS spectra. Additional samples will be studied for Zn, Ba, and Pb. We conducted our XAS experiments on beam lines 4-1 and 4-3 at the Stanford Synchrotron Radiation Laboratory. Data were collected in the fluorescence mode, using a Lytle detector and appropriate filter, and a solid state, 13-element Ge-detector.

Sampling and analysis techniques for monitoring serum for trace elements.

PubMed

Ericson, S P; McHalsky, M L; Rabinow, B E; Kronholm, K G; Arceo, C S; Weltzer, J A; Ayd, S W

1986-07-01

We describe techniques for controlling contamination in the sampling and analysis of human serum for trace metals. The relatively simple procedures do not require clean-room conditions. The atomic absorption and atomic emission methods used have been applied in studying zinc, copper, chromium, manganese, molybdenum, selenium, and aluminum concentrations. Values obtained for a group of 16 normal subjects agree with the most reliable values reported in the literature, obtained by much more elaborate techniques. All of these metals can be measured in 3 to 4 mL of serum. The methods may prove especially useful in monitoring concentrations of essential trace elements in blood of patients being maintained on total parenteral nutrition.

Inertial impaction air sampling device

DOEpatents

Dewhurst, Katharine H.

1990-01-01

An inertial impactor to be used in an air sampling device for collection of respirable size particles in ambient air which may include a graphite furnace as the impaction substrate in a small-size, portable, direct analysis structure that gives immediate results and is totally self-contained allowing for remote and/or personal sampling. The graphite furnace collects suspended particles transported through the housing by means of the air flow system, and these particles may be analyzed for elements, quantitatively and qualitatively, by atomic absorption spectrophotometry.

Inertial impaction air sampling device

DOEpatents

Dewhurst, K.H.

1987-12-10

An inertial impactor to be used in an air sampling device for collection of respirable size particles in ambient air which may include a graphite furnace as the impaction substrate in a small-size, portable, direct analysis structure that gives immediate results and is totally self-contained allowing for remote and/or personal sampling. The graphite furnace collects suspended particles transported through the housing by means of the air flow system, and these particles may be analyzed for elements, quantitatively and qualitatively, by atomic absorption spectrophotometry. 3 figs.

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

PubMed

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

2013-11-15

Vanadium(V) ions as 8-hydroxyquinoline chelates were loaded on multiwalled carbon nanotubes (MWNTs) in a mini chromatographic column. Vanadium was determined by graphite furnace atomic absorption spectrometry (GFAAS). Various analytical parameters including pH of the working solutions, amounts of 8-hydroxyquinoline, eluent type, sample volume, and flow rates were investigated. The effects of matrix ions and some transition metals were also studied. The column can be reused 250 times without any loss in its sorption properties. The preconcentration factor was found as 100. Detection limit (3 s) and limit of quantification (10 s) for the vanadium in the optimal conditions were observed to be 0.012 µg L(-1) and 0.040 μg L(-1), respectively. The capacity of adsorption was 9.6 mg g(-1). Relative standard deviation (RSD) was found to be 5%. The validation of the method was confirmed by using NIST SRM 1515 Apple leaves, NIST SRM 1570a Spinach leaves and GBW 07605 Tea certified reference materials. The procedure was applied to the determination of vanadium in tap water and bottled drinking water samples. The procedure was also successfully applied to microwave digested food samples including black tea, coffee, tomato, cabbage, zucchini, apple and chicken samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Krawczyk-Coda, Magdalena

2017-03-01

In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

Identification of B-K near edge x-ray absorption fine structure peaks of boron nitride thin films prepared by sputtering deposition

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

Niibe, Masahito; Miyamoto, Kazuyoshi; Mitamura, Tohru

2010-09-15

Four {pi}{sup *} resonance peaks were observed in the B-K near edge x-ray absorption fine structure spectra of boron nitride thin films prepared by magnetron sputtering. In the past, these peaks have been explained as the K-absorption of boron atoms, which are present in environment containing nitrogen vacancies, the number of which is 1-3 corresponding to the three peaks at higher photon energy. However, the authors found that there was a strong correlation between the intensities of these three peaks and that of O-K absorption after wide range scanning and simultaneous measurement of nitrogen and oxygen K-absorptions of the BNmore » films. Therefore, the authors conclude that these three peaks at the higher energy side correspond to boron atoms bound to one-to-three oxygen atoms instead of three nitrogen atoms surrounding the boron atom in the h-BN structure. The result of the first-principles calculation with a simple cluster model supported the validity of this explanation.« less

The Flame Spectrometric Determination of Calcium in Fruit Juice by Standard Addition.

ERIC Educational Resources Information Center

Strohl, Arthur N.

1985-01-01

Provides procedures to measure the calcium concentration in fruit juice by atomic absorption. Fruit juice is used because: (1) it is an important consumer product; (2) large samples are available; and (3) calcium exists in fruit juice at concentrations that do not require excessive dilution or preconcentration prior to measurement. (JN)

Ecological-Evaluation of Organotin-Contaminated Sediment.

DTIC Science & Technology

1985-07-01

the potential for bioaccumulation of cadmium, chromium, copper, mercury , silver, pesticides, PCBs, petroleum hydrocarbons, and organotins RESULTS The...tissues were frozen for subsequent bioaccumulation estimates. Tissues and sediment samples were analyzed for cadmium, chromium, copper, mercury , silver...spectroscopy; mercury was analyzed by cold vapor atomic absorption spectroscopy. Pesticides, PCBs, and petroleum hydrocarbons were measured by gas

Determination of total arsenic and arsenic(III) in phosphate fertilizers by hydride generation atomic absorption spectrometry after ultrasound-assisted extraction based on a control acid media.

PubMed

Rezende, Helen Cristine; Coelho, Nivia Maria Melo

2014-01-01

An ultrasound-assisted extraction procedure was developed for determination of inorganic arsenic (As) in phosphate fertilizer by hydride generation atomic absorption spectrometry. The variables that affect the hydride generation step were optimized, including the reducer, acid, sample flow rate, and concentrations of the acid and reducer. The determination of As(lll) was performed through the simple control of solution pH with a 0.5 M citric acid-sodium citrate buffer solution at pH 4.5, and total As was determined after a pre-reduction reaction with 1.0% (w/v) thiourea. Ultrasound-assisted acid extraction was performed, and the parameters sonication time and acid and Triton X-114 concentrations were optimized using a 23 factorial design and central composite design. LODs for As(lll) and total As were 0.029 and 0.022 microg/L, respectively. The accuracy of the method was confirmed with certified reference materials. The method was successfully applied in the determination of inorganic As in phosphate fertilizer samples.

A green and efficient procedure for the preconcentration and determination of cadmium, nickel and zinc from freshwater, hemodialysis solutions and tuna fish samples by cloud point extraction and flame atomic absorption spectrometry.

PubMed

Galbeiro, Rafaela; Garcia, Samara; Gaubeur, Ivanise

2014-04-01

Cloud point extraction (CPE) was used to simultaneously preconcentrate trace-level cadmium, nickel and zinc for determination by flame atomic absorption spectrometry (FAAS). 1-(2-Pyridilazo)-2-naphthol (PAN) was used as a complexing agent, and the metal complexes were extracted from the aqueous phase by the surfactant Triton X-114 ((1,1,3,3-tetramethylbutyl)phenyl-polyethylene glycol). Under optimized complexation and extraction conditions, the limits of detection were 0.37μgL(-1) (Cd), 2.6μgL(-1) (Ni) and 2.3μgL(-1) (Zn). This extraction was quantitative with a preconcentration factor of 30 and enrichment factor estimated to be 42, 40 and 43, respectively. The method was applied to different complex samples, and the accuracy was evaluated by analyzing a water standard reference material (NIST SRM 1643e), yielding results in agreement with the certified values. Copyright © 2013 Elsevier GmbH. All rights reserved.

Determination of lead at trace levels in mussel and sea water samples using vortex assisted dispersive liquid-liquid microextraction-slotted quartz tube-flame atomic absorption spectrometry.

PubMed

Erarpat, Sezin; Özzeybek, Gözde; Chormey, Dotse Selali; Bakırdere, Sezgin

2017-12-01

In this study, dispersive liquid-liquid microextraction (DLLME) and slotted quartz tube (SQT) were coupled to flame atomic absorption spectrometry (FAAS) to increase the sensitivity of lead. Conditions such as the formation of the lead-dithizone complex, efficiency of the DLLME method and the output of the SQT were systematically optimized to improve the detection limit for the analyte. The conventional FAAS system was improved upon by about 3.0 times with SQT-FAAS, 32 times with DLLME-FAAS and 142 times with DLLME-SQT-FAAS. The method was applicable over a wide linear range (10-500 μg L -1 ). The limit of detection (LOD) determined by DLLME-SQT-FAAS for seawater and mussel were 2.7 μg L -1 and 270 μg kg -1 , respectively. The percent recoveries obtained for mussel and seawater samples (spiked at 20 and 50 μg L -1 ) were 95-96% and 98-110%, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

Analysis of heavy metals concentration in water and sediment in the Hara biosphere reserve, southern Iran.

PubMed

Nowrouzi, Mohsen; Mansouri, Borhan; Nabizadeh, Sahar; Pourkhabbaz, Alireza

2014-02-01

This study determined the concentration of heavy metals (Al, Cr, Cu, and Zn) in water and sediments at nine sites in the Hara biosphere reserve of southern Iran during the summer and winter 2010. Determination of Al, Cr, Cu, and Zn in water was carried out by graphite furnace atomic absorption spectrometer (Shimadzu, AA 610s) and in sediment by flame atomic absorption spectrometer (Perkin Elmer, AA3030). Results showed that the heavy metal concentrations in the water samples decreased in the sequence of Zn > Al > Cu > Cr, while in sediment samples were Cr > Zn > Cu > Al. Data analysis indicated that with the exception of Al, there was a Pearson's correlation coefficient between pH and Cu, Zn, and Cr at α = 0.01, 0.05, and 0.001 in sediment (in winter), respectively. There were also significant differences between heavy metals of Cr, Cu, and Zn during the two seasons (p < 0.001) in the water and sediment.

Ligandless dispersive liquid--liquid microextraction of iron in biological and foodstuff samples and its determination by Electrothermal atomic absorption spectrometry.

PubMed

Madadizadeh, Mohadeseh; Taher, Mohammad Ali; Ashkenani, Hamid

2013-01-01

A new, simple, and efficient method comprising ligandless dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry is reported for the preconcentration and determination of ultratrace amounts of Fe(III). Carbon tetrachloride and acetone were used as the extraction and disperser solvents, respectively. Some effective parameters of the microextraction such as choice of extraction and disperser solvents, their volume, extraction time and temperature, salt and surfactant effect, and pH were optimized. Under the optimum conditions, the calibration curve was linear in the range of 0.02 to 0.46 microg/L of Fe(III), with LOD and LOQ of 5.2 and 17.4 ng/L, respectively. The RSD for seven replicated determinations of Fe(IIl) ion at 0.1 microg/L concentration level was 5.2%. Operational simplicity, rapidity, low cost, good repeatability, and low consumption of extraction solvent are the main advantages of the proposed method. The method was successfully applied to the determination of iron in biological, food, and certified reference samples.

Visualizing the Solute Vaporization Interference in Flame Atomic Absorption Spectroscopy

ERIC Educational Resources Information Center

Dockery, Christopher R.; Blew, Michael J.; Goode, Scott R.

2008-01-01

Every day, tens of thousands of chemists use analytical atomic spectroscopy in their work, often without knowledge of possible interferences. We present a unique approach to study these interferences by using modern response surface methods to visualize an interference in which aluminum depresses the calcium atomic absorption signal. Calcium…

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...

Major- and Trace-Element Concentrations in Rock Samples Collected in 2005 from the Taylor Mountains 1:250,000-scale Quadrangle, Alaska

USGS Publications Warehouse

Klimasauskas, Edward P.; Miller, Marti L.; Bradley, Dwight C.; Bundtzen, Tom K.; Hudson, Travis L.

2006-01-01

The data consist of major- and minor-element concentrations for rock samples collected during 2005 by the U.S. Geological Survey. Samples were analyzed by fire assay (Au, Pd, Pt), cold vapor atomic absorption spectroscopy (Hg), and the inductively coupled plasma mass spectrometry (ICPMS) 10 and 42 element methods. For details of sample preparation and analytical techniques see USGS Open File Report 02-0223 (Analytical methods for chemical analysis of geologic and other materials, U.S. Geological Survey), available at .

Determining gold in water by anion-exchange batch extraction

USGS Publications Warehouse

McHugh, J.B.

1986-01-01

This paper describes a batch procedure for determining gold in natural waters. It is completely adaptable to field operations. The water samples are filtered and acidified before they are equilibrated with an anion-exchange resin by shaking. The gold is then eluted with acetone-nitric acid solution, and the eluate evaporated to dryness. The residue is taken up in hydrobromic acid-bromine solution and the gold is extracted with methyl isobutyl ketone. The extract is electrothermally atomized in an atomic-absorption spectrophotometer. The limit of determination is 1 ng 1. ?? 1986.

A rapid method for determining tin and molybdenum in geological samples by flame atomic-absorption spectroscopy

USGS Publications Warehouse

Welsch, E.P.

1985-01-01

The proposed method uses a lithium metaborate fusion, dissolution of the fusion bead in 15% v v hydrochloric acid, extraction into a 4% solution of trioctylphosphine oxide in methyl isobutyl ketone, and aspiration into a nitrous oxide-acetylene flame. The limits of detection for tin and molybdenum are 1.0 and 0.5 ppm, respectively. Approximately 50 samples can be analysed per day. ?? 1985.

Nanoscale infrared (IR) spectroscopy and imaging of structural lipids in human stratum corneum using an atomic force microscope to directly detect absorbed light from a tunable IR laser source.

PubMed

Marcott, Curtis; Lo, Michael; Kjoller, Kevin; Domanov, Yegor; Balooch, Guive; Luengo, Gustavo S

2013-06-01

An atomic force microscope (AFM) and a tunable infrared (IR) laser source have been combined in a single instrument (AFM-IR) capable of producing ~200-nm spatial resolution IR spectra and absorption images. This new capability enables IR spectroscopic characterization of human stratum corneum at unprecendented levels. Samples of normal and delipidized stratum corneum were embedded, cross-sectioned and mounted on ZnSe prisms. A pulsed tunable IR laser source produces thermomechanical expansion upon absorption, which is detected through excitation of contact resonance modes in the AFM cantilever. In addition to reducing the total lipid content, the delipidization process damages the stratum corneum morphological structure. The delipidized stratum corneum shows substantially less long-chain CH2 -stretching IR absorption band intensity than normal skin. AFM-IR images that compare absorbances at 2930/cm (lipid) and 3290/cm (keratin) suggest that regions of higher lipid concentration are located at the perimeter of corneocytes in the normal stratum corneum. © 2013 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

The Free-Free Absorption Coefficients of the Negative Helium Ion

NASA Astrophysics Data System (ADS)

John, T. L.

1994-08-01

Free-free absorption coefficients of the negative helium ion are calculated by a phaseshift approximation, using continuum data that accurately account for electron-atom correlation and polarization. The approximation is considered to yield results within a few per cent of numerical values for wavelengths greater than 1 m, over the temperature range 1400-10080 K. These coefficients are expected to give the best current estimates of He - continuous absorption. Key words: atomic data - atomic processes - stars: atmospheres - infrared: general.

Absorption of infrared radiation by electrons in the field of a neutral hydrogen atom

NASA Technical Reports Server (NTRS)

Stallcop, J. R.

1974-01-01

An analytical expression for the absorption coefficient is developed from a relationship between the cross-section for inverse bremsstrahlung absorption and the cross-section for electron-atom momentum transfer; it is accurate for those photon frequencies v and temperatures such that hv/kT is small. The determination of the absorption of infrared radiation by free-free transitions of the negative hydrogen ion has been extended to higher temperatures. A simple analytical expression for the absorption coefficient has been derived.

Determining photon energy absorption parameters for different soil samples

PubMed Central

Kucuk, Nil; Tumsavas, Zeynal; Cakir, Merve

2013-01-01

The mass attenuation coefficients (μs) for five different soil samples were measured at 661.6, 1173.2 and 1332.5 keV photon energies. The soil samples were separately irradiated with 137Cs and 60Co (370 kBq) radioactive point gamma sources. The measurements were made by performing transmission experiments with a 2″ × 2″ NaI(Tl) scintillation detector, which had an energy resolution of 7% at 0.662 MeV for the gamma-rays from the decay of 137Cs. The effective atomic numbers (Zeff) and the effective electron densities (Neff) were determined experimentally and theoretically using the obtained μs values for the soil samples. Furthermore, the Zeff and Neff values of the soil samples were computed for the total photon interaction cross-sections using theoretical data over a wide energy region ranging from 1 keV to 15 MeV. The experimental values of the soils were found to be in good agreement with the theoretical values. Sandy loam and sandy clay loam soils demonstrated poor photon energy absorption characteristics. However, clay loam and clay soils had good photon energy absorption characteristics. PMID:23179375

Three-dimensional atom localization via electromagnetically induced transparency in a three-level atomic system.

PubMed

Wang, Zhiping; Cao, Dewei; Yu, Benli

2016-05-01

We present a new scheme for three-dimensional (3D) atom localization in a three-level atomic system via measuring the absorption of a weak probe field. Owing to the space-dependent atom-field interaction, the position probability distribution of the atom can be directly determined by measuring the probe absorption. It is found that, by properly varying the parameters of the system, the probability of finding the atom in 3D space can be almost 100%. Our scheme opens a promising way to achieve high-precision and high-efficiency 3D atom localization, which provides some potential applications in laser cooling or atom nano-lithography via atom localization.

Ultraviolet absorption experiment MA-059

NASA Technical Reports Server (NTRS)

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

1976-01-01

The ultraviolet absorption experiment performed during the Apollo Soyuz mission involved sending a beam of atomic oxygen and atomic nitrogen resonance radiation, strong unabsorbable oxygen and nitrogen radiation, and visual radiation, all filling the same 3 deg-wide field of view from the Apollo to the Soyuz. The radiation struck a retroreflector array on the Soyuz and was returned to a spectrometer onboard the Apollo. 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. Information concerning oxygen densities was also obtained by observation of resonantly fluorescent light. The absorption experiments for atomic oxygen and atomic nitrogen were successfully performed at a range of 500 meters, and abundant resonance fluorescence data were obtained.

Optical spectroscopy of laser-produced plasmas for standoff isotopic analysis

NASA Astrophysics Data System (ADS)

Harilal, S. S.; Brumfield, B. E.; LaHaye, N. L.; Hartig, K. C.; Phillips, M. C.

2018-06-01

Rapid, in-field, and non-contact isotopic analysis of solid materials is extremely important to a large number of applications, such as nuclear nonproliferation monitoring and forensics, geochemistry, archaeology, and biochemistry. Presently, isotopic measurements for these and many other fields are performed in laboratory settings. Rapid, in-field, and non-contact isotopic analysis of solid material is possible with optical spectroscopy tools when combined with laser ablation. Laser ablation generates a transient vapor of any solid material when a powerful laser interacts with a sample of interest. Analysis of atoms, ions, and molecules in a laser-produced plasma using optical spectroscopy tools can provide isotopic information with the advantages of real-time analysis, standoff capability, and no sample preparation requirement. Both emission and absorption spectroscopy methods can be used for isotopic analysis of solid materials. However, applying optical spectroscopy to the measurement of isotope ratios from solid materials presents numerous challenges. Isotope shifts arise primarily due to variation in nuclear charge distribution caused by different numbers of neutrons, but the small proportional nuclear mass differences between nuclei of various isotopes lead to correspondingly small differences in optical transition wavelengths. Along with this, various line broadening mechanisms in laser-produced plasmas and instrumental broadening generated by the detection system are technical challenges frequently encountered with emission-based optical diagnostics. These challenges can be overcome by measuring the isotope shifts associated with the vibronic emission bands from molecules or by using the techniques of laser-based absorption/fluorescence spectroscopy to marginalize the effect of instrumental broadening. Absorption and fluorescence spectroscopy probe the ground state atoms existing in the plasma when it is cooler, which inherently provides narrower lineshapes, as opposed to emission spectroscopy which requires higher plasma temperatures to be able to detect thermally excited emission. Improvements in laser and detection systems and spectroscopic techniques have allowed for isotopic measurements to be carried out at standoff distances under ambient atmospheric conditions, which have expanded the applicability of optical spectroscopy-based isotopic measurements to a variety of scientific fields. These technological advances offer an in-situ measurement capability that was previously not available. This review will focus on isotope detection through emission, absorption, and fluorescence spectroscopy of atoms and molecules in a laser-produced plasma formed from a solid sample. A description of the physics behind isotope shifts in atoms and molecules is presented, followed by the physics behind solid sampling of laser ablation plumes, optical methods for isotope measurements, the suitable physical conditions of laser-produced plasma plumes for isotopic analysis, and the current status. Finally, concluding remarks will be made on the existing knowledge/technological gaps identified from the current literature and suggestions for the future work.

Understanding the Structure of High-K Gate Oxides - Oral Presentation

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

Miranda, Andre

2015-08-25

Hafnium Oxide (HfO 2) amorphous thin films are being used as gate oxides in transistors because of their high dielectric constant (κ) over Silicon Dioxide. The present study looks to find the atomic structure of HfO 2 thin films which hasn’t been done with the technique of this study. In this study, two HfO 2 samples were studied. One sample was made with thermal atomic layer deposition (ALD) on top of a Chromium and Gold layer on a silicon wafer. The second sample was made with plasma ALD on top of a Chromium and Gold layer on a Silicon wafer.more » Both films were deposited at a thickness of 50nm. To obtain atomic structure information, Grazing Incidence X-ray diffraction (GIXRD) was carried out on the HfO 2 samples. Because of this, absorption, footprint, polarization, and dead time corrections were applied to the scattering intensity data collected. The scattering curves displayed a difference in structure between the ALD processes. The plasma ALD sample showed the broad peak characteristic of an amorphous structure whereas the thermal ALD sample showed an amorphous structure with characteristics of crystalline materials. This appears to suggest that the thermal process results in a mostly amorphous material with crystallites within. Further, the scattering intensity data was used to calculate a pair distribution function (PDF) to show more atomic structure. The PDF showed atom distances in the plasma ALD sample had structure up to 10 Å, while the thermal ALD sample showed the same structure below 10 Å. This structure that shows up below 10 Å matches the bond distances of HfO 2 published in literature. The PDF for the thermal ALD sample also showed peaks up to 20 Å, suggesting repeating atomic spacing outside the HfO 2 molecule in the sample. This appears to suggest that there is some crystalline structure within the thermal ALD sample.« less

Understanding the Structure of Amorphous Thin Film Hafnia - Final Paper

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

Miranda, Andre

2015-08-27

Hafnium Oxide (HfO 2) amorphous thin films are being used as gate oxides in transistors because of their high dielectric constant (κ) over Silicon Dioxide. The present study looks to find the atomic structure of HfO 2 thin films which hasn’t been done with the technique of this study. In this study, two HfO 2 samples were studied. One sample was made with thermal atomic layer deposition (ALD) on top of a Chromium and Gold layer on a silicon wafer. The second sample was made with plasma ALD on top of a Chromium and Gold layer on a Silicon wafer.more » Both films were deposited at a thickness of 50nm. To obtain atomic structure information, Grazing Incidence X-ray diffraction (GIXRD) was carried out on the HfO 2 samples. Because of this, absorption, footprint, polarization, and dead time corrections were applied to the scattering intensity data collected. The scattering curves displayed a difference in structure between the ALD processes. The plasma ALD sample showed the broad peak characteristic of an amorphous structure whereas the thermal ALD sample showed an amorphous structure with characteristics of crystalline materials. This appears to suggest that the thermal process results in a mostly amorphous material with crystallites within. Further, the scattering intensity data was used to calculate a pair distribution function (PDF) to show more atomic structure. The PDF showed atom distances in the plasma ALD sample had structure up to 10 Å, while the thermal ALD sample showed the same structure below 10 Å. This structure that shows up below 10 Å matches the bond distances of HfO 2 published in literature. The PDF for the thermal ALD sample also showed peaks up to 20 Å, suggesting repeating atomic spacing outside the HfO 2 molecule in the sample. This appears to suggest that there is some crystalline structure within the thermal ALD sample.« less

Determination of Copper by Graphite Furnace Atomic Absorption Spectrophotometry: A Student Exercise in Instrumental Methods of Analysis.

ERIC Educational Resources Information Center

Williamson, Mark A.

1989-01-01

Discusses a student exercise which requires the optimizing of the charring and atomization temperatures by producing a plot of absorbance versus temperature for each temperature parameter. Notes that although the graphite furnace atomic absorption spectroscopy technique has widespread industrial use, there are no published, structured experiments…

Direct determination of chromium in infant formulas employing high-resolution continuum source electrothermal atomic absorption spectrometry and solid sample analysis.

PubMed

Silva, Arlene S; Brandao, Geovani C; Matos, Geraldo D; Ferreira, Sergio L C

2015-11-01

The present work proposed an analytical method for the direct determination of chromium in infant formulas employing the high-resolution continuum source electrothermal atomic absorption spectrometry combined with the solid sample analysis (SS-HR-CS ET AAS). Sample masses up to 2.0mg were directly weighted on a solid sampling platform and introduced into the graphite tube. In order to minimize the formation of carbonaceous residues and to improve the contact of the modifier solution with the solid sample, a volume of 10 µL of a solution containing 6% (v/v) H2O2, 20% (v/v) ethanol and 1% (v/v) HNO3 was added. The pyrolysis and atomization temperatures established were 1600 and 2400 °C, respectively, using magnesium as chemical modifier. The calibration technique was evaluated by comparing the slopes of calibration curves established using aqueous and solid standards. This test revealed that chromium can be determined employing the external calibration technique using aqueous standards. Under these conditions, the method developed allows the direct determination of chromium with limit of quantification of 11.5 ng g(-1), precision expressed as relative standard deviation (RSD) in the range of 4.0-17.9% (n=3) and a characteristic mass of 1.2 pg of chromium. The accuracy was confirmed by analysis of a certified reference material of tomato leaves furnished by National Institute of Standards and Technology. The method proposed was applied for the determination of chromium in five different infant formula samples. The chromium content found varied in the range of 33.9-58.1 ng g(-1) (n=3). These samples were also analyzed employing ICP-MS. A statistical test demonstrated that there is no significant difference between the results found by two methods. The chromium concentrations achieved are lower than the maximum limit permissible for chromium in foods by Brazilian Legislation. Copyright © 2015. Published by Elsevier B.V.

Slurry sampling high-resolution continuum source electrothermal atomic absorption spectrometry for direct beryllium determination in soil and sediment samples after elimination of SiO interference by least-squares background correction.

PubMed

Husáková, Lenka; Urbanová, Iva; Šafránková, Michaela; Šídová, Tereza

2017-12-01

In this work a simple, efficient, and environmentally-friendly method is proposed for determination of Be in soil and sediment samples employing slurry sampling and high-resolution continuum source electrothermal atomic absorption spectrometry (HR-CS-ETAAS). The spectral effects originating from SiO species were identified and successfully corrected by means of a mathematical correction algorithm. Fractional factorial design has been employed to assess the parameters affecting the analytical results and especially to help in the development of the slurry preparation and optimization of measuring conditions. The effects of seven analytical variables including particle size, concentration of glycerol and HNO 3 for stabilization and analyte extraction, respectively, the effect of ultrasonic agitation for slurry homogenization, concentration of chemical modifier, pyrolysis and atomization temperature were investigated by a 2 7-3 replicate (n = 3) design. Using the optimized experimental conditions, the proposed method allowed the determination of Be with a detection limit being 0.016mgkg -1 and characteristic mass 1.3pg. Optimum results were obtained after preparing the slurries by weighing 100mg of a sample with particle size < 54µm and adding 25mL of 20% w/w glycerol. The use of 1μg Rh and 50μg citric acid was found satisfactory for the analyte stabilization. Accurate data were obtained with the use of matrix-free calibration. The accuracy of the method was confirmed by analysis of two certified reference materials (NIST SRM 2702 Inorganics in Marine Sediment and IGI BIL-1 Baikal Bottom Silt) and by comparison of the results obtained for ten real samples by slurry sampling with those determined after microwave-assisted extraction by inductively coupled plasma time of flight mass spectrometry (TOF-ICP-MS). The reported method has a precision better than 7%. Copyright © 2017 Elsevier B.V. All rights reserved.

On-line preconcentration and speciation of arsenic by flow injection hydride generation atomic absorption spectrophotometry.

PubMed

Narcise, Cristine Ingrid S; Coo, Lilibeth Dlc; Del Mundo, Florian R

2005-12-15

A flow injection-column preconcentration-hydride generation atomic absorption spectrophotometric (FI-column-HGAAS) method was developed for determining mug/l levels of As(III) and As(V) in water samples, with simultaneous preconcentration and speciation. The speciation scheme involved determining As(V) at neutral pH and As(III+V) at pH 12, with As(III) obtained by difference. The enrichment factor (EF) increased with increase in sample loading volume from 2.5 to 10ml, and for preconcentration using the chloride-form anion exchange column, EFs ranged from 5 to 48 for As(V) and 4 to 24 for As(III+V), with corresponding detection limits of 0.03-0.3 and 0.07-0.3mug/l. Linear concentration range (LCR) also varied with sample loading volume, and for a 5-ml sample was 0.3-5 and 0.2-8mug/l for As(V) and As(III+V), respectively. Sample throughput, which decreased with increase in sample volume, was 8-17 samples/h. For the hydroxide-form column, the EFS for 2.5-10ml samples were 3-23 for As(V) and 2-15 for As(III+V), with corresponding detection limits of 0.07-0.4 and 0.1-0.5mug/l. The LCR for a 5-ml sample was 0.3-10mug/l for As(V) and 0.2-20mug/l for As(III+V). Sample throughput was 10-20 samples/h. The developed method has been effectively applied to tap water and mineral water samples, with recoveries ranging from 90 to 102% for 5-ml samples passed through the two columns.

Poly(1-vinylimidazole) functionalized magnetic ion imprinted polymer for fast and selective extraction of trace gold in geological, environmental and biological samples followed by graphite furnace atomic absorption spectrometry detection

NASA Astrophysics Data System (ADS)

Zhao, Bingshan; He, Man; Chen, Beibei; Xu, Hongrun; Hu, Bin

2018-05-01

In this study, poly(1-vinylimidazole) functionalized gold ion imprinted polymer coated magnetic nanoparticles (MNPs@PVIM-Au-IIP) were prepared and characterized. The adsorption behaviors of the prepared MNPs@PVIM-Au-IIP toward gold ions (Au(III)) were studied, it was found that MNPs@PVIM-Au-IIP has good selectivity, high adsorption capacity (185.4 mg g-1) and fast adsorption kinetic for Au(III). Based on it, a new method of ion imprinted magnetic solid phase extraction (II-MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the analysis of trace Au(III) in real samples with complicated matrix. Factors affecting MSPE including sample pH, desorption reagent, elution concentration and volume, elution time, sample volume and adsorption time were optimized. With high enrichment factor of 100-fold, the detection limit of the proposed method is 7.9 ng L-1 for Au(III) with the relative standard deviation of 7.4% (c = 50 ng L-1, n = 7). In order to validate the accuracy of the proposed method, the Certified Reference Material of GBW07293 geological sample (platinpalladium ore) was analyzed, and the determined value was in good agreement with the certified value. The proposed II-MSPE-GFAAS method is simple, fast, selective, sensitive and has been successfully applied in the determination of trace Au in ore, sediment, environmental water and human urine samples with satisfactory results.

Pigment identification in artwork using graphite furnace atomic absorption spectrometry.

PubMed

Goltz, D M; Coombs, J; Marion, C; Cloutis, E; Gibson, J; Attas, M; Choo-Smith, L-P; Collins, C

2004-06-17

The use of a sampling technique is described for the identification of metals from inorganic pigments in paint. The sampling technique involves gently contacting a cotton swab with the painted surface to physically remove a minute quantity ( approximately 1-2mug) of pigment. The amount of material removed from the painted surface is invisible to the unaided eye and does not cause any visible effect to the painted surface. The cotton swab was then placed in a 1.5ml polystyrene beaker containing HNO(3) to extract pigment metals prior to analysis using graphite furnace atomic absorption spectrometry (GFAAS). GFAAS is well suited for identifying pigment metals since it requires small samples and many pigments consist of main group elements (e.g. Al) as well as transition metals (e.g. Zn, Fe and Cd). Using Cd (cadmium red) as the test element, the reproducibility of sampling a paint surface with the cotton swab was approximately 13% in either a water or oil medium. To test the feasibility of cotton sampling for pigment identification, samples were obtained from paintings (watercolour and oil) of a local collection. Raman spectra provided complementary information to the GFAAS, which together are essential for positive identification of some pigments. For example, GFAAS indicated the presence of Cu, but the Raman spectra positively identified the modern copper pigment phthalocyanine green (Cu(C(32)Cl(16)N(8)). Both Raman spectroscopy and GFAAS were useful for identifying ZnO as a white pigment.

Photon absorption potential coefficient as a tool for materials engineering

NASA Astrophysics Data System (ADS)

Akande, Raphael Oluwole; Oyewande, Emmanuel Oluwole

2016-09-01

Different atoms achieve ionizations at different energies. Therefore, atoms are characterized by different responses to photon absorption in this study. That means there exists a coefficient for their potential for photon absorption from a photon source. In this study, we consider the manner in which molecular constituents (atoms) absorb photon from a photon source. We observe that there seems to be a common pattern of variation in the absorption of photon among the electrons in all atoms on the periodic table. We assume that the electrons closest to the nucleus (En) and the electrons closest to the outside of the atom (Eo) do not have as much potential for photon absorption as the electrons at the middle of the atom (Em). The explanation we give to this effect is that the En electrons are embedded within the nuclear influence, and similarly, Eo electrons are embedded within the influence of energies outside the atom that there exists a low potential for photon absorption for them. Unlike En and Eo, Em electrons are conditioned, such that there is a quest for balance between being influenced either by the nuclear force or forces external to the atom. Therefore, there exists a higher potential for photon absorption for Em electrons than for En and Eo electrons. The results of our derivations and analysis always produce a bell-shaped curve, instead of an increasing curve as in the ionization energies, for all elements in the periodic table. We obtained a huge data of PAPC for each of the several materials considered. The point at which two or more PAPC values cross one another is termed to be a region of conflicting order of ionization, where all the atoms absorb equal portion of the photon source at the same time. At this point, a greater fraction of the photon source is pumped into the material which could lead to an explosive response from the material. In fact, an unimaginable and unreported phenomenon (in physics) could occur, when two or more PAPCs cross, and the material is able to absorb more than that the photon source could provide, at this point. These resulting effects might be of immense materials engineering applications.

Attosecond transient absorption of argon atoms in the vacuum ultraviolet region: line energy shifts versus coherent population transfer

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

Cao, Wei; Warrick, Erika R.; Neumark, Daniel M.

Using attosecond transient absorption, the dipole response of an argon atom in the vacuum ultraviolet (VUV) region is studied when an external electromagnetic field is present. An isolated attosecond VUV pulse populates Rydberg states lying 15 eV above the argon ground state. A synchronized few-cycle near infrared (NIR) pulse modifies the oscillating dipoles of argon impulsively, leading to alterations in the VUV absorption spectra. As the NIR pulse is delayed with respect to the VUV pulse, multiple features in the absorption profile emerge simultaneously including line broadening, sideband structure, sub-cycle fast modulations, and 5-10 fs slow modulations. These features indicatemore » the coexistence of two general processes of the light-matter interaction: the energy shift of individual atomic levels and coherent population transfer between atomic eigenstates, revealing coherent superpositions. Finally, an intuitive formula is derived to treat both effects in a unifying framework, allowing one to identify and quantify the two processes in a single absorption spectrogram.« less

Attosecond transient absorption of argon atoms in the vacuum ultraviolet region: line energy shifts versus coherent population transfer

NASA Astrophysics Data System (ADS)

Cao, Wei; Warrick, Erika R.; Neumark, Daniel M.; Leone, Stephen R.

2016-01-01

Using attosecond transient absorption, the dipole response of an argon atom in the vacuum ultraviolet (VUV) region is studied when an external electromagnetic field is present. An isolated attosecond VUV pulse populates Rydberg states lying 15 eV above the argon ground state. A synchronized few-cycle near infrared (NIR) pulse modifies the oscillating dipoles of argon impulsively, leading to alterations in the VUV absorption spectra. As the NIR pulse is delayed with respect to the VUV pulse, multiple features in the absorption profile emerge simultaneously including line broadening, sideband structure, sub-cycle fast modulations, and 5-10 fs slow modulations. These features indicate the coexistence of two general processes of the light-matter interaction: the energy shift of individual atomic levels and coherent population transfer between atomic eigenstates, revealing coherent superpositions. An intuitive formula is derived to treat both effects in a unifying framework, allowing one to identify and quantify the two processes in a single absorption spectrogram.

Attosecond transient absorption of argon atoms in the vacuum ultraviolet region: line energy shifts versus coherent population transfer

DOE PAGES

Cao, Wei; Warrick, Erika R.; Neumark, Daniel M.; ...

2016-01-18

Using attosecond transient absorption, the dipole response of an argon atom in the vacuum ultraviolet (VUV) region is studied when an external electromagnetic field is present. An isolated attosecond VUV pulse populates Rydberg states lying 15 eV above the argon ground state. A synchronized few-cycle near infrared (NIR) pulse modifies the oscillating dipoles of argon impulsively, leading to alterations in the VUV absorption spectra. As the NIR pulse is delayed with respect to the VUV pulse, multiple features in the absorption profile emerge simultaneously including line broadening, sideband structure, sub-cycle fast modulations, and 5-10 fs slow modulations. These features indicatemore » the coexistence of two general processes of the light-matter interaction: the energy shift of individual atomic levels and coherent population transfer between atomic eigenstates, revealing coherent superpositions. Finally, an intuitive formula is derived to treat both effects in a unifying framework, allowing one to identify and quantify the two processes in a single absorption spectrogram.« less

Removal of iron interferences by solvent extraction for geochemical analysis by atomic-absorption spectrophotometry

USGS Publications Warehouse

Zhou, L.; Chao, T.T.; Sanzolone, R.F.

1985-01-01

Iron is a common interferent in the determination of many elements in geochemical samples. Two approaches for its removal have been taken. The first involves removal of iron by extraction with methyl isobutyl ketone (MIBK) from hydrochloric acid medium, leaving the analytes in the aqueous phase. The second consists of reduction of iron(III) to iron(II) by ascorbic acid to minimize its extraction into MIBK, so that the analytes may be isolated by extraction. Elements of interest can then be determined using the aqueous solution or the organic extract, as appropriate. Operating factors such as the concentration of hydrochloric acid, amounts of iron present, number of extractions, the presence or absence of a salting-out agent, and the optimum ratio of ascorbic acid to iron have been determined. These factors have general applications in geochemical analysis by atomic-absorption spectrophotometry. ?? 1985.

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.

The standard calibration instrument automation system for the atomic absorption spectrophotometer. Part 3: Program documentation

NASA Astrophysics Data System (ADS)

Ryan, D. P.; Roth, G. S.

1982-04-01

Complete documentation of the 15 programs and 11 data files of the EPA Atomic Absorption Instrument Automation System is presented. The system incorporates the following major features: (1) multipoint calibration using first, second, or third degree regression or linear interpolation, (2) timely quality control assessments for spiked samples, duplicates, laboratory control standards, reagent blanks, and instrument check standards, (3) reagent blank subtraction, and (4) plotting of calibration curves and raw data peaks. The programs of this system are written in Data General Extended BASIC, Revision 4.3, as enhanced for multi-user, real-time data acquisition. They run in a Data General Nova 840 minicomputer under the operating system RDOS, Revision 6.2. There is a functional description, a symbol definitions table, a functional flowchart, a program listing, and a symbol cross reference table for each program. The structure of every data file is also detailed.

Rapid Determination of Trace Palladium in Active Pharmaceutical Ingredients by Magnetic Solid-Phase Extraction and Flame Atomic Absorption Spectrometry

NASA Astrophysics Data System (ADS)

Yin, Q. H.; Zhu, D. M.; Yang, D. Z.; Hu, Q. F.; Yang, Y. L.

2018-01-01

Clutaraldehyde cross-linked magnetic chitosan nanoparticles were synthesized and used as an adsorbent for the dispersive solid-phase extraction of palladium in active pharmaceutical ingredients (APIs) prior to analysis by a flame atomic absorption spectrophotometer. FT-IR, X-ray diffraction, and TEM were used to characterize the adsorbent. Various parameters of experimental performance, such as adsorbent amount, pH, adsorption time, desorption solutions, coexisting ions, and adsorbent reusability, were investigated and optimized. Under the optimized conditions, good linearity was achieved in the 5.0-500 μg/L concentration range, with correlation coefficients of 0.9989. The limit of detection is 2.8 μg/L and the recoveries of spiked samples ranged from 91.7 to 97.6%. It was confirmed that the GMCNs nanocomposite was a promising adsorbing material for extraction and preconcentration of Pd in APIs.

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.

Speciation of organic and inorganic selenium in selenium-enriched rice by graphite furnace atomic absorption spectrometry after cloud point extraction.

PubMed

Sun, Mei; Liu, Guijian; Wu, Qianghua

2013-11-01

A new method was developed for the determination of organic and inorganic selenium in selenium-enriched rice by graphite furnace atomic absorption spectrometry detection after cloud point extraction. Effective separation of organic and inorganic selenium in selenium-enriched rice was achieved by sequentially extracting with water and cyclohexane. Under the optimised conditions, the limit of detection (LOD) was 0.08 μg L(-1), the relative standard deviation (RSD) was 2.1% (c=10.0 μg L(-1), n=11), and the enrichment factor for selenium was 82. Recoveries of inorganic selenium in the selenium-enriched rice samples were between 90.3% and 106.0%. The proposed method was successfully applied for the determination of organic and inorganic selenium as well as total selenium in selenium-enriched rice. Copyright © 2013 Elsevier Ltd. All rights reserved.

Diode Lasers and Practical Trace Analysis.

ERIC Educational Resources Information Center

Imasaka, Totaro; Nobuhiko, Ishibashi

1990-01-01

Applications of lasers to molecular absorption spectrometry, molecular fluorescence spectrometry, visible semiconductor fluorometry, atomic absorption spectrometry, and atomic fluorescence spectrometry are discussed. Details of the use of the frequency-doubled diode laser are provided. (CW)

Determination of ultratrace elements in natural waters by solid-phase extraction and atomic spectrometry methods.

PubMed

Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Frache, Roberto

2003-01-01

A study was carried out on the preconcentration of ultratrace amounts of cadmium, lead, manganese, copper and iron from high-salinity aqueous samples and determination by atomic spectrometry methods. Sample volume, amount of resin, loading flow rate, and elution volume were optimized in order to obtain the simultaneous preconcentration of all the analytes. Quantitative recoveries were obtained by using 200 mg of iminodiacetic resin with a loading flow rate of 2 mL min(-1), elution volume of 3 mL and sample volume of 50-450 mL. Only copper in seawater samples was not completely retained by the resin (60-70% recovery), due to unfavorable competition of iminodiacetic-active groups with organically bound metal.To quantify the metals in the eluates, two atomic spectrometry techniques were compared: electrothermal atomization atomic absorption spectrometry (ETAAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) with simultaneous CCD detection system. Both techniques are suitable for sample analysis with detection limits of 1.0, 4.7, 3.3, 6.8, and 53 ng L(-1) using ETAAS and 12, 122, 3.4, 17, and 21 ng L(-1) using ICP-OES for Cd, Pb, Mn, Cu, and Fe, respectively. Relative standard deviations of the procedures ranged from 1.7 to 14% at the sub-microg L(-1) concentration level. The accuracy of both methods was verified by analyzing various certified reference materials (river water, estuarine water, coastal and off-shore seawater).

Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

2015-08-01

A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L- 1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L- 1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract.

Interference of nitrite and nitrogen dioxide on mercury and selenium determination by chemical vapor generation atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Nunes, Dayana Lopes; dos Santos, Eliane Pereira; Barin, Juliano Smanioto; Mortari, Sergio Roberto; Dressler, Valderi Luiz; de Moraes Flores, Érico Marlon

2005-06-01

In this study, a systematic investigation was performed concerning the interference of nitrogen oxides on the determination of selenium and mercury by hydride generation atomic absorption spectrometry (HG AAS) and cold vapor atomic absorption spectrometry (CV AAS). The effect of nitrate, nitrite and NO 2 dissolved in the condensed phase was evaluated. No effect of NO 3- on Se and Hg determination was observed up to 100 mg of sodium nitrate added to the reaction vessel. The Se signal was reduced by about 80% upon the addition of 6.8 mg NO 2-. For Hg, no interference of nitrite was observed up to 20 mg of NO 2-. A complete suppression of the Se signal was observed when gaseous NO 2 was introduced into analytical solutions. For Hg, a signal decrease between 8 and 13% occurred. For Se, bubbling argon or heating the solution was not able to recover the original absorbance values, whereas Hg signals were recovered with these procedures. When gaseous NO 2 was passed directly into the atomizer, Se signals decreased similarly to when NO 2 was bubbled in analytical solutions. The addition of urea, hydroxylamine hydrochloride and sulfamic acid (SA) was investigated to reduce the NO 2 effect in sample digests containing residual NO 2, but only SA was effective in reducing the interference. Based on the results, it is possible to propose the use of SA to prevent interferences in Se and Hg determinations by HG AAS and CV AAS, respectively.

An x-ray absorption spectroscopy study of Ni-Mn-Ga shape memory alloys.

PubMed

Sathe, V G; Dubey, Aditi; Banik, Soma; Barman, S R; Olivi, L

2013-01-30

The austenite to martensite phase transition in Ni-Mn-Ga ferromagnetic shape memory alloys was studied by extended x-ray absorption fine structure (EXAFS) and x-ray absorption near-edge structure (XANES) spectroscopy. The spectra at all the three elements', namely, Mn, Ga and Ni, K-edges in several Ni-Mn-Ga samples (with both Ni and Mn excess) were analyzed at room temperature and low temperatures. The EXAFS analysis suggested a displacement of Mn and Ga atoms in opposite direction with respect to the Ni atoms when the compound transforms from the austenite phase to the martensite phase. The first coordination distances around the Mn and Ga atoms remained undisturbed on transition, while the second and subsequent shells showed dramatic changes indicating the presence of a modulated structure. The Mn rich compounds showed the presence of antisite disorder of Mn and Ga. The XANES results showed remarkable changes in the unoccupied partial density of states corresponding to Mn and Ni, while the electronic structure of Ga remained unperturbed across the martensite transition. The post-edge features in the Mn K-edge XANES spectra changed from a double peak like structure to a flat peak like structure upon phase transition. The study establishes strong correlation between the crystal structure and the unoccupied electronic structure in these shape memory alloys.

Solubility of Lead Sulfate in Water and in Sodium Sulfate Solutions: An Experiment in Atomic Absorption Spectrophotometry.

ERIC Educational Resources Information Center

Lehman, Thomas A.; Everett, Wayne W.

1982-01-01

Describes a set of undergraduate laboratory experiments which provide experience in deuteration and derivatization procedures applied to infrared spectroscopy. Basic skills in vacuum-line technique are also taught while measuring infrared spectra of deuterated solid samples and demonstrating the value of derivatization as an aid to interpreting…

Modeling the Oxygen K Absorption in the Interstellar Medium: An XMM-Newton View of Sco X-1

NASA Technical Reports Server (NTRS)

Garcia, J.; Ramirez, J. M.; Kallman, T. R.; Witthoeft, M.; Bautista, M. A.; Mendoza, C.; Palmeri, P.; Quinet, P.

2011-01-01

We investigate the absorption structure of the oxygen in the interstellar medium by analyzing XMM-Newton observations of the low mass X-ray binary Sco X-1. We use simple models based on the O I atomic cross section from different sources to fit the data and evaluate the impact of the atomic data in the interpretation of astrophysical observations. We show that relatively small differences in the atomic calculations can yield spurious results. We also show that the most complete and accurate set of atomic cross sections successfully reproduce the observed data in the 21 - 24.5 Angstrom wavelength region of the spectrum. Our fits indicate that the absorption is mainly due to neutral gas with an ionization parameter of Epsilon = 10(exp -4) erg/sq cm, and an oxygen column density of N(sub O) approx. = 8-10 x 10(exp 17)/sq cm. Our models are able to reproduce both the K edge and the K(alpha) absorption line from O I, which are the two main features in this region. We find no conclusive evidence for absorption by other than atomic oxygen.

Electrothermal atomic absorption spectrometric determination of arsenic in essential lavender and rose oils.

PubMed

Karadjova, Irina B; Lampugnani, Leonardo; Tsalev, Dimiter L

2005-02-28

Analytical procedures for electrothermal atomic absorption spectrometric (ETAAS) determination of arsenic in essential oils from lavender (Lavendula angustifolia) and rose (Rosa damascena) are described. For direct ETAAS analysis, oil samples are diluted with ethanol or i-propanol for lavender and rose oil, respectively. Leveling off responses of four different arsenic species (arsenite, arsenate, monomethylarsonate and dimethylarsinate) is achieved by using a composite chemical modifier: l-cysteine (0.05gl(-1)) in combination with palladium (2.5mug) and citric acid (100mug). Transverse-heated graphite atomizer (THGA) with longitudinal Zeeman-effect background correction and 'end-capped' graphite tubes with integrated pyrolytic graphite platforms, pre-treated with Zr-Ir for permanent modification are employed as most appropriate atomizer. Calibration with solvent-matched standard solutions of As(III) is used for four- and five-fold diluted samples of lavender and rose oil, respectively. Lower dilution factors required standard addition calibration by using aqueous (for lavender oil) or i-propanol (for rose oil) solutions of As(III). The limits of detection (LOD) for the whole analytical procedure are 4.4 and 4.7ngg(-1) As in levender and rose oil, respectively. The relative standard deviation (R.S.D.) for As at 6-30ngg(-1) levels is between 8 and 17% for both oils. As an alternative, procedure based on low temperature plasma ashing in oxygen with ETAAS, providing LODs of 2.5 and 2.7ngg(-1) As in levender and rose oil, respectively, and R.S.D. within 8-12% for both oils has been elaborated. Results obtained by both procedures are in good agreement.

Flame and flameless atomic-absorption determination of tellurium in geological materials

USGS Publications Warehouse

Chao, T.T.; Sanzolone, R.F.; Hubert, A.E.

1978-01-01

The sample is digested with a solution of hydrobromic acid and bromine and the excess of bromine is expelled. After dilution of the solution to approximately 3 M in hydrobromic acid, ascorbic acid is added to reduce iron(III) before extraction of tellurium into methyl isobutyl ketone (MIBK). An oxidizing air-acetylene flame is used to determine tellurium in the 0.1-20 ppm range. For samples containing 4-200 ppb of tellurium, a carbon-rod atomizer is used after the MIBK extract has been washed with 0.5 M hydrobromic acid to remove the residual iron. The flame procedure is useful for rapid preliminary monitoring, and the flameless procedure can determine tellurium at very low concentrations. ?? 1978.

Air pollution assessment of Salé's city (Morocco)

NASA Astrophysics Data System (ADS)

Bounakhla, M.; Fatah, A.; Embarch, K.; Ibn Majah, M.; Azami, R.; Sabir, A.; Nejjar, A.; Cherkaoui, R.; Gaudry, A.

2003-05-01

Four sites were selected in Sale's city in Morocco in order to contribute in air pollution level assessment and determination of its effects on public health. The sites were selected so that they are close to the most important industrialized areas, they have a very high demographic density and they cover a heavy traffic. Two approaches of air sampling and subsequent analysis methods of elements in atmospheric aerosols have been performed. The first is a classical approach, which consists in sampling total airborne materials with a High Volume Sampler and analysing the samples using Atomic Absorption Spectroscopy (AAS). The second is having its interest for studies relating effects of particles on human health. It consists in employing a Dichotomous Sampler to collect inhalable particles and the X-ray Fluorescence (XRF) for elemental analysis. With such system, it was possible to collect separately respirable and inhalable aerosols. The ED-XRF analysis method used is appropriate for monitoring airborne polluants in living and working areas with advantage of simple preparation, nondestructive nature, rapidity and suitable limits of detection. Using this method, it was possible to identify and quantify S, Ca, CI, Fe, Cu, and Pb. With Atomic Absorption Spectroscopy Analysis Method, we quantified Cd. This study have been completed by measuring NOx SO2 and solid suspended particles or airborne particulate matter (APM).

A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

PubMed

Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

2013-01-01

A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples.

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

PubMed

Rezvani, Seyyed Ahmad; Soleymanpour, Ahmad

2016-03-04

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

Modifications of the optical properties for DAM-ADC nuclear track detector exposed to alpha particles

NASA Astrophysics Data System (ADS)

Rammah, Y. S.; Awad, E. M.

2018-05-01

Modifications of the optical properties of diallyl maleate-allyl diglycol carbonate (DAM-ADC) nuclear detector induced by alpha particles are described. DAM-ADC samples were irradiated perpendicularly by thin 241Am disk source that emits alpha particles with 5.48 MeV. The optical absorption has been measured using the ultraviolet-visible (UV-1100) spectroscopy. It was found that DAM-ADC polymer shows substantial modifications in its optical characteristics upon irradiated with alpha particles with different energies. The optical energy band gap (Egap) for the detector was calculated for the direct and the indirect allowed transitions in K-space using two approaches (Tauc's model and absorption spectrum fitting (ASF) method). Urbach's energy (Ea), number of carbon atoms per conjugated length (N), number of carbon atoms per cluster (M), and refractive index (n) for the present samples were determined. Results reveal that the values of energy gap in direct transition are greater than those of indirect, before and after irradiation. (Egap), (Ea), (N), (M), and (n) of the present samples are changed significantly with irradiation time and value of alpha energy. Results reflect the possibility of using DAM-ADC polymer track detectors to estimate alpha particle energies using the variation of the absorbance.

Species selective preconcentration and quantification of gold nanoparticles using cloud point extraction and electrothermal atomic absorption spectrometry.

PubMed

Hartmann, Georg; Schuster, Michael

2013-01-25

The determination of metallic nanoparticles in environmental samples requires sample pretreatment that ideally combines pre-concentration and species selectivity. With cloud point extraction (CPE) using the surfactant Triton X-114 we present a simple and cost effective separation technique that meets both criteria. Effective separation of ionic gold species and Au nanoparticles (Au-NPs) is achieved by using sodium thiosulphate as a complexing agent. The extraction efficiency for Au-NP ranged from 1.01 ± 0.06 (particle size 2 nm) to 0.52 ± 0.16 (particle size 150 nm). An enrichment factor of 80 and a low limit of detection of 5 ng L(-1) is achieved using electrothermal atomic absorption spectrometry (ET-AAS) for quantification. TEM measurements showed that the particle size is not affected by the CPE process. Natural organic matter (NOM) is tolerated up to a concentration of 10 mg L(-1). The precision of the method expressed as the standard deviation of 12 replicates at an Au-NP concentration of 100 ng L(-1) is 9.5%. A relation between particle concentration and the extraction efficiency was not observed. Spiking experiments showed a recovery higher than 91% for environmental water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Separation and preconcentration of Ag(I) in aqueous samples by flotation as an ion-associate using iodide and ferroin followed the determination by flame atomic absorption spectrometry.

PubMed

Hosseini, Mohammad Saeid; Hashemi-Moghaddam, Hamid; Kardan-Moghaddam, Gholamreza

2007-01-01

A simple method for separation/preconcentration and determination of Ag(I) in aqueous samples is described. The method is based on formation of an ion-associate between Ag(I)-iodide complex and ferroin, which can be floated at the interface of the aqueous/n-heptane phases. The flotation process was carried out using 500-ml aliquot of the aqueous solution and the floated layer was dissolved in 5 ml of 1 M HNO3 containing methanol (50% v/v) as the solvent. The Ag(I) content was then determined by flame atomic absorption spectrometry (FAAS). The method so could be considered as an enrichment process, was achieved to a quantitative feature, when the pH of the solution was adjusted to 4 and the concentrations of iodide and ferroin were about 3.2 x 10(-4) M and 6.25 x 10(-5) M, respectively. The LOD and RSD (n = 7) were obtained 1.0 x 10(-8) M and 2.4%, respectively. It was found that a large number of cations and anions even at high considerably foreign ion/Ag(I) ratios were not interfered. The method was applied satisfactorily to recovery of Ag(I) from different aqueous samples.

Determination of sub-microgram amounts of selenium in geological materials by atomic-absorption spectrophotometry with electrothermal atomisation after solvent extraction

USGS Publications Warehouse

Sanzolone, R.F.; Chao, T.T.

1981-01-01

An atomic-absorption spectrophotometric method with electrothermal atomisation has been developed for the determination of selenium in geological materials. The sample is decomposed with a mixture of nitric, perchloric and hydrofluoric acids and heated with hydrochloric acid to reduce selenium to selenium (IV). Selenium is then extracted into toluene from a hydrochloric acid - hydrobromic acid medium containing iron. A few microlitres of the toluene extract are injected into a carbon rod atomiser, using a nickel solution as a matrix modifier. The limits of determination are 0.2-200 p.p.m. of selenium in a geological sample. For concentrations between 0.05 and 0.2 p.p.m., back-extraction of the selenium into dilute hydrochloric acid is employed before atomisation. Selenium values for reference samples obtained by replicate analysis are in general agreement with those reported by other workers, with relative standard deviations ranging from 4.1 to 8.8%. Recoveries of selenium spiked at two levels were 98-108%. Major and trace elements commonly encountered in geological materials do not interfere. Arsenic has a suppressing effect on the selenium signals, but only when its concentration is greater than 1000 p.p.m. Nitric acid interferes seriously with the extraction of selenium and must be removed by evaporation in the sample-digestion step.

Methods for analysis of selected metals in water by atomic absorption

USGS Publications Warehouse

Fishman, Marvin J.; Downs, Sanford C.

1966-01-01

This manual describes atomic-absorption-spectroscopy methods for determining calcium, copper, lithium, magnesium, manganese, potassium, sodium, strontium and zinc in atmospheric precipitation, fresh waters, and brines. The procedures are intended to be used by water quality laboratories of the Water Resources Division of the U.S. Geological Survey. Detailed procedures, calculations, and methods for the preparation of reagents are given for each element along with data on accuracy, precision, and sensitivity. Other topics discussed briefly are the principle of atomic absorption, instrumentation used, and special analytical techniques.

Simultaneous determination of V, Ni and Fe in fuel fly ash using solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry.

PubMed

Cárdenas Valdivia, A; Vereda Alonso, E; López Guerrero, M M; Gonzalez-Rodriguez, J; Cano Pavón, J M; García de Torres, A

2018-03-01

A green and simple method has been proposed in this work for the simultaneous determination of V, Ni and Fe in fuel ash samples by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GFAAS). The application of fast programs in combination with direct solid sampling allows eliminating pretreatment steps, involving minimal manipulation of sample. Iridium treated platforms were applied throughout the present study, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9931. The concentrations found in the fuel ash samples analysed ranged from 0.66% to 4.2% for V, 0.23-0.7% for Ni and 0.10-0.60% for Fe. Precision (%RSD) were 5.2%, 10.0% and 9.8% for V, Ni and Fe, respectively, obtained as the average of the %RSD of six replicates of each fuel ash sample. The optimum conditions established were applied to the determination of the target analytes in fuel ash samples. In order to test the accuracy and applicability of the proposed method in the analysis of samples, five ash samples from the combustion of fuel in power stations, were analysed. The method accuracy was evaluated by comparing the results obtained using the proposed method with the results obtained by ICP OES previous acid digestion. The results showed good agreement between them. The goal of this work has been to develop a fast and simple methodology that permits the use of aqueous standards for straightforward calibration and the simultaneous determination of V, Ni and Fe in fuel ash samples by direct SS HR CS GFAAS. Copyright © 2017 Elsevier B.V. All rights reserved.

Enhanced Reverse Saturable Absorption and Optical Limiting in Heavy-Atom Substituted Phthalocyanines

NASA Technical Reports Server (NTRS)

Perry, J. W.; Mansour, K.; Marder, S. R.; Alvarez, D., Jr.; Perry, K. J.; Choong, I.

1994-01-01

The reverse saturable absorption and optical limiting response of metal phthalocyaninies can be enhanced by using the heavy-atom effect. Phthalocyanines containing heavy metal atoms, such as In, Sn, and Pb show nearly a factor of two enhancement in the ratio of effective excited-state to ground-state absorption cross sections compared to those containing lighter atoms, such as Al and Si. In an f/8 optical geometry, homogeneous solutions of heavy metal phthalocyanines, at 30% linear transmission, limit 8-ns, 532-nm laser pulses to less than or equal to 3 (micro)J (the energy for 50% probability of eye damage) for incident pulses up to 800 (micro)J.

Mini-Column Ion-Exchange Separation and Atomic Absorption Quantitation of Nickel, Cobalt, and Iron: An Undergraduate Quantitative Analysis Experiment.

ERIC Educational Resources Information Center

Anderson, James L.; And Others

1980-01-01

Presents an undergraduate quantitative analysis experiment, describing an atomic absorption quantitation scheme that is fast, sensitive and comparatively simple relative to other titration experiments. (CS)

Inertial impaction air sampling device

DOEpatents

Dewhurst, K.H.

1990-05-22

An inertial impactor is designed which is to be used in an air sampling device for collection of respirable size particles in ambient air. The device may include a graphite furnace as the impaction substrate in a small-size, portable, direct analysis structure that gives immediate results and is totally self-contained allowing for remote and/or personal sampling. The graphite furnace collects suspended particles transported through the housing by means of the air flow system, and these particles may be analyzed for elements, quantitatively and qualitatively, by atomic absorption spectrophotometry. 3 figs.

40 CFR Appendix G to Part 50 - Reference Method for the Determination of Lead in Suspended Particulate Matter Collected From...

Code of Federal Regulations, 2010 CFR

2010-07-01

... Absorption Spectroscopy.” Published by Interscience Company, New York, NY (1968). 5. Kirkbright, G. F., and Sargent, M., “Atomic Absorption and Fluorescence Spectroscopy.” Published by Academic Press, New York, NY... County, IL, by Atomic Absorption Spectroscopy.” Envir. Sci. and Tech., 3, 472-475 (1969). 7. “Proposed...

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of low-level silver by graphite furnace atomic absorption spectrophotometry

USGS Publications Warehouse

Damrau, D.L.

1993-01-01

Increased awareness of the quality of water in the United States has led to the development of a method for determining low levels (0.2-5.0 microg/L) of silver in water samples. Use of graphite furnace atomic absorption spectrophotometry provides a sensitive, precise, and accurate method for determining low-level silver in samples of low ionic-strength water, precipitation water, and natural water. The minimum detection limit determined for low-level silver is 0.2 microg/L. Precision data were collected on natural-water samples and SRWS (Standard Reference Water Samples). The overall percent relative standard deviation for natural-water samples with silver concentrations more than 0.2 microg/L was less than 40 percent throughout the analytical range. For the SRWS with concentrations more than 0.2 microg/L, the overall percent relative standard deviation was less than 25 percent throughout the analytical range. The accuracy of the results was determined by spiking 6 natural-water samples with different known concentrations of the silver standard. The recoveries ranged from 61 to 119 percent at the 0.5-microg/L spike level. At the 1.25-microg/L spike level, the recoveries ranged from 92 to 106 percent. For the high spike level at 3.0 microg/L, the recoveries ranged from 65 to 113 percent. The measured concentrations of silver obtained from known samples were within the Branch of Quality Assurance accepted limits of 1 1/2 standard deviations on the basis of the SRWS program for Inter-Laboratory studies.

High enthalpy arc-heated plasma flow diagnostics by tunable diode laser absorption spectroscopy

NASA Astrophysics Data System (ADS)

Lin, Xin; Chen, Lianzhong; Zeng, Hui; Ou, Dongbin; Dong, Yonghui

2017-05-01

This paper reports the laser absorption measurements of atomic oxygen in the FD04 arc-heater at China Academy of Aerospace Aerodynamics (CAAA). An atomic oxygen absorption line at 777.19 nm is utilizied for detecting the population of electronically excited oxygen atom in an air plasma flow. A scanned-wavelength direct absorption mode is used in this study. The laser is scanned in wavelength across the absorption feature at a rate of 200 Hz. Under the assumption of thermal equilibrium, time-resolved temperature measurements are obtained on one line-of-sight in the arc-heater. The good agreement of the temperature inferred from the sonic throat method suggests the equilibrium assumption is valid. These results illustrate the feasibility of the diode laser sensors for flow parameters in high enthalpy arc-heated facilities.

Trends in tungsten coil atomic spectrometry

NASA Astrophysics Data System (ADS)

Donati, George L.

Renewed interest in electrothermal atomic spectrometric methods based on tungsten coil atomizers is a consequence of a world wide increasing demand for fast, inexpensive, sensitive, and portable analytical methods for trace analysis. In this work, tungsten coil atomic absorption spectrometry (WCAAS) and tungsten coil atomic emission spectrometry (WCAES) are used to determine several different metals and even a non-metal at low levels in different samples. Improvements in instrumentation and new strategies to reduce matrix effects and background signals are presented. Investigation of the main factors affecting both WCAAS and WCAES analytical signals points to the importance of a reducing, high temperature gas phase in the processes leading to atomic cloud generation. Some more refractory elements such as V and Ti were determined for the first time by double tungsten coil atomic emission spectrometry (DWCAES). The higher temperatures provided by two atomizers in DWCAES also allowed the detection of Ag, Cu and Sn emission signals for the first time. Simultaneous determination of several elements by WCAES in relatively complex sample matrices was possible after a simple acid extraction. The results show the potential of this method as an alternative to more traditional, expensive methods for fast, more effective analyses and applications in the field. The development of a new metallic atomization cell is also presented. Lower limits of detection in both WCAAS and WCAES determinations were obtained due to factors such as better control of background signal, smaller, more isothermal system, with atomic cloud concentration at the optical path for a longer period of time. Tungsten coil-based methods are especially well suited to applications requiring low sample volume, low cost, sensitivity and portability. Both WCAAS and WCAES have great commercial potential in fields as diverse as archeology and industrial quality control. They are simple, inexpensive, effective methods for trace metal determinations in several different samples, representing an important asset in today's analytical chemistry.

Evaluation of Low Earth Orbit Environmental Effects on International Space Station Thermal Control Materials

NASA Technical Reports Server (NTRS)

Dever, Joyce A.; Rutledge, Sharon K.; Hasegawa, Mark M.; Reed, Charles K.

1998-01-01

Samples of International Space Station (ISS) thermal control coatings were exposed to simulated low Earth orbit (LEO) environmental conditions to determine effects on optical properties. In one test, samples of the white paint coating Z-93P were coated with outgassed products from Tefzel(R) (ethylene tetrafluoroethylene copolymer) power cable insulation as-may occur on ISS. These samples were then exposed, along with an uncontaminated Z-93P witness sample, to vacuum ultraviolet (VUV) radiation to determine solar absorptance degradation. The Z-93P samples coated with Tefzel(R) outgassing products experienced greater increases in solar absorptance than witness samples not coated with Tefzel(R) outgassing products. In another test, samples of second surface silvered Teflon(R) FEP (fluorinated ethylene propylene), SiO. (where x=2)-coated silvered Teflon(R) FEP, and Z-93P witness samples were exposed to the combined environments of atomic oxygen and VLTV radiation to determine optical properties changes due to these simulated ISS environmental effects. This test verified the durability of these materials in the absence of contaminants.

Determination of metals in lubricating oils by flame atomic absorption spectrometry using a single-bore high-pressure pneumatic nebulizer.

PubMed

Mora, J; Todolí, J L; Sempere, F J; Canals, A; Hernandis, V

2000-12-01

The behaviour of a single-bore high-pressure pneumatic nebulizer (SBHPPN) as a tool for the analysis of lubricating oils by flame atomic absorption spectrometry (FAAS) was investigated. The effects of the sample oil content [from 10% to 100% (w/w) oil in 4-methylpentan-2-one, IBMK] and the carrier nature (IBMK and methanol) on the characteristics of the aerosols generated, on the analyte transport efficiency and on the analytical figures of merit in FAAS were studied. A pneumatic concentric nebulizer (PCN) was used for comparison. Increasing the oil content increases the viscosity of the sample. With the PCN this gives rise to coarser aerosols, making it impossible to nebulize samples with an oil content higher than 70% (w/w). Using the SBHPPN, the viscosity of the sample scarcely affects the characteristics of the primary aerosols. Hence, the SBHPPN is able, by using the appropriate carrier, to nebulize pure lubricating oils. Among the carriers tested, IBMK is the most advisable because it is fully miscible with all the oil samples. The SBHPPN provides higher sensitivities and lower limits of detection than the PCN. Compared with a method based on organic dilution, the use of the SBHPPN for the direct analysis of lubricating oils by FAAS makes it possible, in addition to increasing the analysis throughput, to detect elements at lower concentrations. Moreover, the SBHPPN provides similar results to those obtained using a previous acid digestion step.

Novel ion imprinted magnetic mesoporous silica for selective magnetic solid phase extraction of trace Cd followed by graphite furnace atomic absorption spectrometry detection

NASA Astrophysics Data System (ADS)

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

2015-05-01

Determination of trace Cd in environmental, biological and food samples is of great significance to toxicological research and environmental pollution monitoring. While the direct determination of Cd in real-world samples is difficult due to its low concentration and the complex matrix. Herein, a novel Cd(II)-ion imprinted magnetic mesoporous silica (Cd(II)-II-MMS) was prepared and was employed as a selective magnetic solid-phase extraction (MSPE) material for extraction of trace Cd in real-world samples followed by graphite furnace atomic absorption spectrometry (GFAAS) detection. Under the optimized conditions, the detection limit of the proposed method was 6.1 ng L- 1 for Cd with the relative standard deviation (RSD) of 4.0% (c = 50 ng L- 1, n = 7), and the enrichment factor was 50-fold. To validate the proposed method, Certified Reference Materials of GSBZ 50009-88 environmental water, ZK018-1 lyophilized human urine and NIES10-b rice flour were analyzed and the determined values were in a good agreement with the certified values. The proposed method exhibited a robust anti-interference ability due to the good selectivity of Cd(II)-II-MMS toward Cd(II). It was successfully employed for the determination of trace Cd(II) in environmental water, human urine and rice samples with recoveries of 89.3-116%, demonstrating that the proposed method has good application potential in real world samples with complex matrix.

Sample preparation for arsenic speciation analysis in baby food by generation of substituted arsines with atomic absorption spectrometry detection.

PubMed

Huber, Charles S; Vale, Maria Goreti R; Dessuy, Morgana B; Svoboda, Milan; Musil, Stanislav; Dědina, Jiři

2017-12-01

A slurry sampling procedure for arsenic speciation analysis in baby food by arsane generation, cryogenic trapping and detection with atomic absorption spectrometry is presented. Several procedures were tested for slurry preparation, including different reagents (HNO 3 , HCl and tetramethylammonium hydroxide - TMAH) and their concentrations, water bath heating and ultrasound-assisted agitation. The best results for inorganic arsenic (iAs) and dimethylarsinate (DMA) were reached when using 3molL -1 HCl under heating and ultrasound-assisted agitation. The developed method was applied for the analysis of five porridge powder and six baby meal samples. The trueness of the method was checked with a certified reference material (CRM) of total arsenic (tAs), iAs and DMA in rice (ERM-BC211). Arsenic recoveries (mass balance) for all samples and CRM were performed by the determination of the tAs by inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted digestion and its comparison against the sum of the results from the speciation analysis. The relative limits of detection were 0.44, 0.24 and 0.16µgkg -1 for iAs, methylarsonate and DMA, respectively. The concentrations of the most toxic arsenic species (iAs) in the analyzed baby food samples ranged between 4.2 and 99µgkg -1 which were below the limits of 300, 200 and 100µgkg -1 set by the Brazilian, Chinese and European legislation, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of silicon in biomass and products of pyrolysis process via high-resolution continuum source atomic absorption spectrometry.

PubMed

Nakadi, Flávio V; Prodanov, Caroline; Boschetti, Wiliam; Vale, Maria Goreti R; Welz, Bernhard; de Andrade, Jailson B

2018-03-01

Thermochemical processes can convert the biomass into fuels, such as bio-oil. The biomass submitted to pyrolysis process, such as fibers, are generally rich in silicon, an element that can lead to damages in an engine when there is high concentration in a fuel. High-resolution continuum source atomic absorption spectrometry (HR-CS AAS) is an interesting alternative for Si determination in the products and byproducts of the pyrolysis process because, besides the flame (F) and graphite furnace (GF) atomizers, it has enhanced the application of direct analysis of solid samples (SS) within GF. This study aimed the development of methods to determine Si in biomass samples, their products and byproducts using HR-CS AAS. A high-resolution continuum source atomic absorption spectrometer contrAA 700 equipped with F and GF atomizers was used throughout the study. HR-CS F AAS (λ = 251.611nm, 1 detection pixel, N 2 O/C 2 H 2 flame) was used to evaluate Si content in biomass and ash, after a microwave-assisted acid digestion with HNO 3 and HF. HR-CS GF AAS (T pyr = 1400°C, T atom = 2650°C) has evaluated Si in pyrolysis water and bio-oil at 251.611nm, and in peach pit biomass and ash at 221.174nm using SS, both wavelengths with 1 detection pixel. Rhodium (300μg) was applied as permanent modifier and 10μgPd + 6μg Mg were pipetted onto the standards/samples at each analysis. Three different biomass samples were studied: palm tree fiber, coconut fiber and peach pit, and three certified reference materials (CRM) were used to verify the accuracy of the methods. The figures of merit were LOD 0.09-20mgkg -1 , and LOQ 0.3-20mgkg -1 , considering all the methods. There were no significant differences between the CRM certified values and the determined ones, using a Student t-test with a confidence interval of 95% (n = 5). Si concentration ranged from 0.11-0.92% mm -1 , 1.1-1.7mgkg -1 , 3.3-13mgkg -1 , and 0.41-1.4%mm -1 , in biomass, bio-oil, pyrolysis water and ash, respectively. Si remained mostly in the ash, leading to a mass fraction of up to 103%, even when the Si loss is not considered. Silicon concentration in bio-oil was below 1.7mgkg -1 , which is suitable for its application as a fuel. The developed methods using HR-CS AAS are suitable for Si determination in biomass, bio-oil, pyrolysis water, and ash. The application of bio-oil as an alternative fuel would be possible evaluating its Si content due to its low levels. The mass balance for Si has proved to be an important tool in order to evaluate the correct disposal of pyrolysis process byproducts. Copyright © 2017 Elsevier B.V. All rights reserved.

Lead determination at ng/mL level by flame atomic absorption spectrometry using a tantalum coated slotted quartz tube atom trap.

PubMed

Demirtaş, İlknur; Bakırdere, Sezgin; Ataman, O Yavuz

2015-06-01

Flame atomic absorption spectrometry (FAAS) still keeps its importance despite the relatively low sensitivity; because it is a simple and economical technique for determination of metals. In recent years, atom traps have been developed to increase the sensitivity of FAAS. Although the detection limit of FAAS is only at the level of µg/mL, with the use of atom traps it can reach to ng/mL. Slotted quartz tube (SQT) is one of the atom traps used to improve sensitivity. In atom trapping mode of SQT, analyte is trapped on-line in SQT for few minutes using ordinary sample aspiration, followed by the introduction of a small volume of organic solvent to effect the revolatilization and atomization of analyte species resulting in a transient signal. This system is economical, commercially available and easy to use. In this study, a sensitive analytical method was developed for the determination of lead with the help of SQT atom trapping flame atomization (SQT-AT-FAAS). 574 Fold sensitivity enhancement was obtained at a sample suction rate of 3.9 mL/min for 5.0 min trapping period with respect to FAAS. Organic solvent was selected as 40 µL of methyl isobutyl ketone (MIBK). To obtain a further sensitivity enhancement inner surface of SQT was coated with several transition metals. The best sensitivity enhancement, 1650 fold enhancement, was obtained by the Ta-coated SQT-AT-FAAS. In addition, chemical nature of Pb species trapped on quartz and Ta surface, and the chemical nature of Ta on quartz surface were investigated by X-ray photoelectron spectroscopy (XPS) and Raman Spectroscopy. Raman spectrometric results indicate that tantalum is coated on SQT surface in the form of Ta2O5. XPS studies revealed that the oxidation state of Pb in species trapped on both bare and Ta coated SQT surfaces is +2. For the accuracy check, the analyses of standard reference material were performed by use of SCP SCIENCE EnviroMAT Low (EU-L-2) and results for Pb were to be in good agreement with the certified value using SQT-AT-FAAS and Ta coated-SQT. Copyright © 2015 Elsevier B.V. All rights reserved.

High resolution x-ray fluorescence spectroscopy - a new technique for site- and spin-selectivity

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

Wang, Xin

1996-12-01

X-ray spectroscopy has long been used to elucidate electronic and structural information of molecules. One of the weaknesses of x-ray absorption is its sensitivity to all of the atoms of a particular element in a sample. Through out this thesis, a new technique for enhancing the site- and spin-selectivity of the x-ray absorption has been developed. By high resolution fluorescence detection, the chemical sensitivity of K emission spectra can be used to identify oxidation and spin states; it can also be used to facilitate site-selective X-ray Absorption Near Edge Structure (XANES) and site-selective Extended X-ray Absorption Fine Structure (EXAFS). Themore » spin polarization in K fluorescence could be used to generate spin selective XANES or spin-polarized EXAFS, which provides a new measure of the spin density, or the nature of magnetic neighboring atoms. Finally, dramatic line-sharpening effects by the combination of absorption and emission processes allow observation of structure that is normally unobservable. All these unique characters can enormously simplify a complex x-ray spectrum. Applications of this novel technique have generated information from various transition-metal model compounds to metalloproteins. The absorption and emission spectra by high resolution fluorescence detection are interdependent. The ligand field multiplet model has been used for the analysis of K{alpha} and K{beta} emission spectra. First demonstration on different chemical states of Fe compounds has shown the applicability of site selectivity and spin polarization. Different interatomic distances of the same element in different chemical forms have been detected using site-selective EXAFS.« less

Understanding of sub-band gap absorption of femtosecond-laser sulfur hyperdoped silicon using synchrotron-based techniques

PubMed Central

Limaye, Mukta V.; Chen, S. C.; Lee, C. Y.; Chen, L. Y.; Singh, Shashi B.; Shao, Y. C.; Wang, Y. F.; Hsieh, S. H.; Hsueh, H. C.; Chiou, J. W.; Chen, C. H.; Jang, L. Y.; Cheng, C. L.; Pong, W. F.; Hu, Y. F.

2015-01-01

The correlation between sub-band gap absorption and the chemical states and electronic and atomic structures of S-hyperdoped Si have been extensively studied, using synchrotron-based x-ray photoelectron spectroscopy (XPS), x-ray absorption near-edge spectroscopy (XANES), extended x-ray absorption fine structure (EXAFS), valence-band photoemission spectroscopy (VB-PES) and first-principles calculation. S 2p XPS spectra reveal that the S-hyperdoped Si with the greatest (~87%) sub-band gap absorption contains the highest concentration of S2− (monosulfide) species. Annealing S-hyperdoped Si reduces the sub-band gap absorptance and the concentration of S2− species, but significantly increases the concentration of larger S clusters [polysulfides (Sn2−, n > 2)]. The Si K-edge XANES spectra show that S hyperdoping in Si increases (decreased) the occupied (unoccupied) electronic density of states at/above the conduction-band-minimum. VB-PES spectra evidently reveal that the S-dopants not only form an impurity band deep within the band gap, giving rise to the sub-band gap absorption, but also cause the insulator-to-metal transition in S-hyperdoped Si samples. Based on the experimental results and the calculations by density functional theory, the chemical state of the S species and the formation of the S-dopant states in the band gap of Si are critical in determining the sub-band gap absorptance of hyperdoped Si samples. PMID:26098075

Effect of LEO Exposure on Aromatic Polymers Containing Phenylphosphine Oxide Groups

NASA Technical Reports Server (NTRS)

Watson, K. A.; Ghose, S.; Lillehei, P. T.; Smith, J. G., Jr.; Connell, J. W.

2007-01-01

As part of the Materials on The International Space Station Experiment (MISSE), aromatic polymers containing phenylphosphine oxide groups were exposed to low Earth orbit (LEO) for approximately 4 years. All of the aromatic polymers containing phenylphosphine oxide groups survived the exposure despite the high fluence of atomic oxygen that completely eroded other polymer films such as Kapton and Mylar of comparable or greater thickness. The samples consisted of a colorless polyimide film and a poly(arylene ether benzimidazole) film and thread. The samples were characterized for changes in physical properties, thermal/optical properties (i.e. solar absorptivity and thermal emissivity), surface chemistry (X-ray photoelectron spectroscopy), and surface topography (atomic force microscopy). The data from the polymer samples on MISSE were compared to samples from the same batch of material stored under ambient conditions on Earth. In addition, comparisons were made between the MISSE samples and those subjected to shorter term space flight exposures. The results of these analyses will be presented.

Mercury Pollution Exploration in Latvia with High-Sensitivity Zeeman Atomic Absorption Spectrometry

NASA Astrophysics Data System (ADS)

Bogans, Egils; Gavare, Zanda; Svagere, Anda; Poikane, Rita; Skudra, Jānis

2011-01-01

This research presents Hg pollution measurements performed in Latvia with sensitive method using Zeeman AAS analyzer RA-915+ and necessary attachments. Air in Riga city and water samples from a number of rivers and lakes of Latvia were analyzed for presence of low-level Hg concentrations. Ombrotrophic bog peat was analyzed to get insight into long-term trends. Environment in the sites sampled is relatively clean according to the results obtained, but there are local spots of pollution.

Sequential injection ionic liquid dispersive liquid-liquid microextraction for thallium preconcentration and determination with flame atomic absorption spectrometry.

PubMed

Anthemidis, Aristidis N; Ioannou, Kallirroy-Ioanna G

2012-08-01

A novel, automatic on-line sequential injection dispersive liquid-liquid microextraction (SI-DLLME) method, based on 1-hexyl-3-methylimidazolium hexafluorophosphate ([Hmim][PF(6)]) ionic liquid as an extractant solvent was developed and demonstrated for trace thallium determination by flame atomic absorption spectrometry. The ionic liquid was on-line fully dispersed into the aqueous solution in a continuous flow format while the TlBr(4)(-) complex was easily migrated into the fine droplets of the extractant due to the huge contact area of them with the aqueous phase. Furthermore, the extractant was simply retained onto the surface of polyurethane foam packed into a microcolumn. No specific conditions like low temperature are required for extractant isolation. All analytical parameters of the proposed method were investigated and optimized. For 15 mL of sample solution, an enhancement factor of 290, a detection limit of 0.86 μg L(-1) and a precision (RSD) of 2.7% at 20.0 μg L(-1) Tl(I) concentration level, was obtained. The developed method was evaluated by analyzing certified reference materials while good recoveries from environmental and biological samples proved that present method was competitive in practical applications.

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

PubMed

Sun, Mei; Wu, Qianghua

2010-04-15

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

Temperature dependence of Ti 1s near-edge spectra in Ti-based perovskites: theory and experiment

NASA Astrophysics Data System (ADS)

Shirley, Eric; Cockayne, Eric; Ravel, Bruce; Woicik, Joseph

Ti 1s near-edge spectra (around 4970 eV) in SrTiO3 and PbTiO3 reveal electric-dipole and quadrupole transitions to Ti 3d, 4p and mixed 3d-4p states. Crystal field-split pre-edge features attributed to 1s ->3d transitions are small compared to the main edge jump at the onset of the Ti 4s/4p continuum. Pre-edge and subsequent near-edge features are predicted to be weaker than what is observed, unless one accounts for ferroelectric polarization in PbTiO3 and thermal motion in both compounds. Using density-functional theory molecular dynamics simulations at various temperatures (including sampling two phases of PbTiO3), we capture the statistically averaged root-mean-square deviations of Ti4+ ions from the centers of their oxygen cages. By sampling appropriate snapshots of atomic configurations and averaging Ti 1s absorption spectra computed within a Bethe-Salpeter Equation framework, we obtain absorption spectra that agree well with experiment, including details related to ferroelectric polarization, phase transitions, and fluctuations of atomic coordinates.

Integrated lab-in-syringe platform incorporating a membraneless gas-liquid separator for automatic cold vapor atomic absorption spectrometry.

PubMed

Giakisikli, Georgia; Miró, Manuel; Anthemidis, Aristidis

2013-10-01

This manuscript reports the proof-of-concept of a novel integrated lab-in-syringe/gas-liquid separation (LIS/GLS) batch-flow system based on a programmable flow for automatic cold vapor atomic absorption spectrometric assays. Homogeneous mixing of metered volumes of sample and reagent solutions drawn up in a sandwich-type mode along with in situ vapor generation are accomplished inside the microsyringe in a closed manner, while the separation of vapor species is achieved via the membraneless GLS located at the top of the syringe's valve in the upright position. The potentials of the proposed manifold were demonstrated for trace inorganic mercury determination in drinking waters and seawater. For a 3.0 mL sample, the limit of detection and repeatability (RSD) were found to be 0.03 μg L(-1) Hg(II) and 3.1% (at the 2.0 μg L(-1) concentration level), respectively, with a dynamic range extending up to 10.0 μg L(-1). The proposed system fulfills the requirements of US-EPA, WHO, and EU Council Directives for measurements of the maximum allowed concentrations of inorganic mercury in drinking water.

Structural, Morphological, Optical and Photocatalytic Properties of Y, N-Doped and Codoped TiO2 Thin Films

PubMed Central

Hamden, Zeineb; Conceição, David; Boufi, Sami; Vieira Ferreira, Luís Filipe; Bouattour, Soraa

2017-01-01

Pure TiO2, Y-N single-doped and codoped TiO2 powders and thin films deposited on glass beads were successfully prepared using dip-coating and sol-gel methods. The samples were analyzed using grazing angle X-ray diffraction (GXRD), Raman spectroscopy, time resolved luminescence, ground state diffuse reflectance absorption and scanning electron microscopy (SEM). According to the GXRD patterns and micro-Raman spectra, only the anatase form of TiO2 was made evident. Ground state diffuse reflectance absorption studies showed that doping with N or codoping with N and Y led to an increase of the band gap. Laser induced luminescence analysis revealed a decrease in the recombination rate of the photogenerated holes and electrons. The photocatalytic activity of supported catalysts, toward the degradation of toluidine, revealed a meaningful enhancement upon codoping samples at a level of 2% (atomic ratio). The photocatalytic activity of the material and its reactivity can be attributed to a reduced, but significant, direct photoexcitation of the semiconductor by the halogen lamp, together with a charge-transfer-complex mechanism, or with the formation of surface oxygen vacancies by the N dopant atoms. PMID:28772962

Structural, Morphological, Optical and Photocatalytic Properties of Y, N-Doped and Codoped TiO₂ Thin Films.

PubMed

Hamden, Zeineb; Conceição, David; Boufi, Sami; Vieira Ferreira, Luís Filipe; Bouattour, Soraa

2017-05-31

Pure TiO₂, Y-N single-doped and codoped TiO₂ powders and thin films deposited on glass beads were successfully prepared using dip-coating and sol-gel methods. The samples were analyzed using grazing angle X-ray diffraction (GXRD), Raman spectroscopy, time resolved luminescence, ground state diffuse reflectance absorption and scanning electron microscopy (SEM). According to the GXRD patterns and micro-Raman spectra, only the anatase form of TiO₂ was made evident. Ground state diffuse reflectance absorption studies showed that doping with N or codoping with N and Y led to an increase of the band gap. Laser induced luminescence analysis revealed a decrease in the recombination rate of the photogenerated holes and electrons. The photocatalytic activity of supported catalysts, toward the degradation of toluidine, revealed a meaningful enhancement upon codoping samples at a level of 2% (atomic ratio). The photocatalytic activity of the material and its reactivity can be attributed to a reduced, but significant, direct photoexcitation of the semiconductor by the halogen lamp, together with a charge-transfer-complex mechanism, or with the formation of surface oxygen vacancies by the N dopant atoms.

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

Method 200.12 - Determination of Trace Elements in Marine Waters by StabilizedTemperature Graphite Furnace Atomic Absorption

EPA Science Inventory

This method provides procedures for the determination of total recoverable elements by graphite furnace atomic absorption (GFAA) in marine waters, including estuarine, ocean and brines with salinities of up to 35 ppt.

Assessing the engagement, learning, and overall experience of students operating an atomic absorption spectrophotometer with remote access technology.

PubMed

Erasmus, Daniel J; Brewer, Sharon E; Cinel, Bruno

2015-01-01

The use of internet-based technologies in the teaching of laboratories has emerged as a promising education tool. This study evaluated the effectiveness of using remote access technology to operate an atomic absorption spectrophotometer in analyzing the iron content in a crude myoglobin extract. Sixty-two students were surveyed on their level of engagement, learning, and overall experience. Feedback from students suggests that the use of remote access technology is effective in teaching students the principles of chemical analysis by atomic absorption spectroscopy. © 2014 The International Union of Biochemistry and Molecular Biology.

Gold in natural water: A method of determination by solvent extraction and electrothermal atomization

USGS Publications Warehouse

McHugh, J.B.

1984-01-01

A method has been developed using electrothermal atomization to effectively determine the amount of gold in natural water within the nanogram range. The method has four basic steps: (1) evaporating a 1-L sample; (2) putting it in hydrobromic acid-bromine solution; (3) extracting the sample with methyl-isobutyl-ketone; and (4) determining the amount of gold using an atomic absorption spectrophotometer. The limit of detection is 0.001 ??g gold per liter. Results from three studies indicate, respectively, that the method is precise, effective, and free of interference. Specifically, a precision study indicates that the method has a relative standard deviation of 16-18%; a recovery study indicates that the method recovers gold at an average of 93%; and an interference study indicates that the interference effects are eliminated with solvent extraction and background correction techniques. Application of the method to water samples collected from 41 sites throughout the Western United States and Alaska shows a gold concentration range of < 0.001 to 0.036 ??g gold per liter, with an average of 0.005 ??g/L. ?? 1984.

Optical Absorption and Electric Resistivity of an l-Cysteine Film

NASA Astrophysics Data System (ADS)

Kamada, Masao; Hideshima, Takuya; Azuma, Junpei; Yamamoto, Isamu; Imamura, Masaki; Takahashi, Kazutoshi

2016-12-01

The optical and electric properties of an l-cysteine film have been investigated to understand its applicability to bioelectronics. The fundamental absorption is the allowed transition having the threshold at 5.8 eV and the absorption is due to the charge-transfer type transition from sulfur-3sp to oxygen-2p and/or carbon-2p states, while absorptions more than 9 eV can be explained with intra-atomic transitions in the functional groups. The electric resistivity is 2.0 × 104 Ω m at room temperature and increases as the sample temperature decreases. The results indicate that the l-cysteine film is a p-type semiconductor showing the hole conduction caused by the sulfur-3sp occupied states and unknown impurity or defect states as acceptors. The electron affinity of the l-cysteine film is derived as ≦-0.3 eV.

Comparison of three different sample preparation procedures for the determination of traffic-related elements in airborne particulate matter collected on glass fiber filters.

PubMed

Castilho, Ivan N B; Welz, Bernhard; Vale, Maria Goreti R; de Andrade, Jailson B; Smichowski, Patricia; Shaltout, Abdallah A; Colares, Lígia; Carasek, Eduardo

2012-01-15

Three different procedures for sample preparation have been compared for the determination of Cu, Mo and Sb in airborne particulate matter (APM) collected on glass fiber filters using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). Direct solid sample analysis of the ground filters was compared with microwave-assisted acid leaching with aqua regia and ultrasound-assisted extraction also using aqua regia. The main absorption line at 324.754 nm or the secondary line at 216.509 nm was used for the determination of Cu, depending on the analyte content in the samples. The primary absorption line at 313.259 nm was used for Mo and the secondary line at 212.739 nm for Sb determination. The limits of detection (LOD, 3σ) found for the direct solid sampling method, based on ten atomizations of an unused filter were 15 μg g(-1) for all three analytes, corresponding to 40 ng m(-3) for a typical air volume of 1,440 m(3) collected over a period of 24h. The LOD for the other two methods were less than a factor of two inferior, but the total time required for an analysis was significantly longer. The repeatability of the measurements was between 3 and 9% (n=5), and the results obtained with the three methods did not show any significant difference. The ratio between the three analytes on the filters from areas of intense traffic was found to be around Cu:Mo:Sb≈4:1:1.4, which suggests that the source of all three elements is brake linings, i.e., related to automobile traffic. When the ratio deviated significantly from the above values, the source of contamination was assumed to be of different origin. Copyright © 2011 Elsevier B.V. All rights reserved.

Silver binding in argentiferous manganese oxide minerals investigated by synchrotron radiation X-ray absorption spectroscopy

NASA Astrophysics Data System (ADS)

Fan, Chenzi; Li, Qiaoying; Chu, Binbin; Lu, Guohui; Gao, Yuhong; Xu, Lingxiao

2018-02-01

The knowledge of the nature of silver occurrence and sites in argentiferous manganese oxides is significant for developing better process to extract silver from manganese-silver ores. Synchrotron radiation has been used to collect Ag K-edge X-ray absorption spectroscopy of three natural and five synthetic samples of silver-containing manganese oxide, basically in the phases of tunnel-type cryptomelane or todorokite and layer-type birnessite or chalcophanite. Data were also gathered on five standards including Ag foil, Ag2O, Ag2SO4, Ag2CO3, and AgNO3 to compare the local environments of Ag atoms with the samples. Ag K-edge XANES studies show that Ag is present in most of the samples in Ag+ oxidation state, except in the Ag-Tod sample through annealing step in the form of Ag0 nanoparticles which are also identified by TEM. The natural samples from Xiangguang manganese-silver ores exhibit similar coordination distances as the corresponding tunnel or layer structured synthetic samples. In the argentiferous cryptomelanes, silver cations do not occupy the tunnel centers like K+, but rather place on the common face sites of the cubic cage formed by MnO6 octahedra, coordinated with about four oxygen anions at 2.4 Å bond distances proved by the EXAFS results. In the silver-exchanged birnessites or natural argentiferous chalcophanite, silver cations probably occupy a tetrahedral coordination to interlayer O atoms and a position located above or below the vacant cavities in the Mn octahedra layers.

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.

Analyzing lead absorption by the sycamore tree species in the industrial park of Rasht, Iran.

PubMed

Hashemi, Seyed Armin; FallahChay, Mir Mozaffar; Tarighi, Fattaneh

2015-07-01

In this study, the subject of heavy metal concentration in soil, rock, sediment, surface water and groundwater, which can be caused by natural or man-posed pollution, was analyzed in the industrial park of Rasht. These concentrations were compared with the standard range of environmental data. Heavy metals are important environmental pollutants that can cause health hazards to humans, plants and microorganisms by entering food chain. This study aimed to investigate the absorption of lead by the leaves of sycamore tree species in the industrial park of Rasht. For this purpose, a sample of 32 sycamore tree species were randomly selected at a specified time, and the concentration of lead were measured using an atomic absorption device. Results showed that the amount of lead absorption by sycamore leaves is remarkable. The highest amount of lead absorption by sycamore leaves was detected at station 1 (Khazar Steel) and the lowest amount at station 2 (control station). © The Author(s) 2012.

Verification Of The Defense Waste Processing Facility's (DWPF) Process Digestion Methods For The Sludge Batch 8 Qualification Sample

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

Click, D. R.; Edwards, T. B.; Wiedenman, B. J.

2013-03-18

This report contains the results and comparison of data generated from inductively coupled plasma – atomic emission spectroscopy (ICP-AES) analysis of Aqua Regia (AR), Sodium Peroxide/Sodium Hydroxide Fusion Dissolution (PF) and Cold Chem (CC) method digestions and Cold Vapor Atomic Absorption analysis of Hg digestions from the DWPF Hg digestion method of Sludge Batch 8 (SB8) Sludge Receipt and Adjustment Tank (SRAT) Receipt and SB8 SRAT Product samples. The SB8 SRAT Receipt and SB8 SRAT Product samples were prepared in the SRNL Shielded Cells, and the SRAT Receipt material is representative of the sludge that constitutes the SB8 Batch ormore » qualification composition. This is the sludge in Tank 51 that is to be transferred into Tank 40, which will contain the heel of Sludge Batch 7b (SB7b), to form the SB8 Blend composition.« less

Two-photon absorption laser-induced fluorescence of atomic oxygen in the afterglow of pulsed positive corona discharge

NASA Astrophysics Data System (ADS)

Ono, Ryo; Takezawa, Kei; Oda, Tetsuji

2009-08-01

Atomic oxygen is measured in the afterglow of pulsed positive corona discharge using time-resolved two-photon absorption laser-induced fluorescence. The discharge occurs in a 14 mm point-to-plane gap in dry air. After the discharge pulse, the atomic oxygen density decreases at a rate of 5×104 s-1. Simultaneously, ozone density increases at almost the same rate, where the ozone density is measured using laser absorption method. This agreement between the increasing rate of atomic oxygen and decreasing rate of ozone proves that ozone is mainly produced by the well-known three-body reaction, O+O2+M→O3+M. No other process for ozone production such as O2(v)+O2→O3+O is observed. The spatial distribution of atomic oxygen density is in agreement with that of the secondary streamer luminous intensity. This agreement indicates that atomic oxygen is mainly produced in the secondary streamer channels, not in the primary streamer channels.

Observation of high-order quantum resonances in the kicked rotor.

PubMed

Kanem, J F; Maneshi, S; Partlow, M; Spanner, M; Steinberg, A M

2007-02-23

Quantum resonances in the kicked rotor are characterized by a dramatically increased energy absorption rate, in stark contrast to the momentum localization generally observed. These resonances occur when the scaled Planck's constant Planck's [over ]=r/s 4pi, for any integers r and s. However, only the variant Planck's [over ]=r2pi resonances are easily observable. We have observed high-order quantum resonances (s>2) utilizing a sample of low energy, noncondensed atoms and a pulsed optical standing wave. Resonances are observed for variant Planck's [over ]=r/16 4pi for integers r=2-6. Quantum numerical simulations suggest that our observation of high-order resonances indicate a larger coherence length (i.e., coherence between different wells) than expected from an initially thermal atomic sample.

Vacancy-hydrogen complexes in ammonothermal GaN

NASA Astrophysics Data System (ADS)

Tuomisto, F.; Kuittinen, T.; Zając, M.; Doradziński, R.; Wasik, D.

2014-10-01

We have applied positron annihilation spectroscopy to study in-grown vacancy defects in bulk GaN crystals grown by the ammonothermal method. We observe a high concentration of Ga vacancy related defects in n-type samples with varying free electron and oxygen content. The positron lifetimes found in these samples suggest that the Ga vacancies are complexed with hydrogen impurities. The number of hydrogen atoms in each vacancy decreases with increasing free electron concentration and oxygen and hydrogen content. The local vibrational modes observed in infrared absorption support this conclusion. Growth of high-quality ammonothermal GaN single crystals with varying electron concentrations. Identification of defect complexes containing a Ga vacancy and 1 or more hydrogen atoms, and possibly O. These vacancy complexes provide a likely explanation for electrical compensation in ammonothermal GaN.

Application of sodium carbonate prevents sulphur poisoning of catalysts in automated total mercury analysis

NASA Astrophysics Data System (ADS)

McLagan, David S.; Huang, Haiyong; Lei, Ying D.; Wania, Frank; Mitchell, Carl P. J.

2017-07-01

Analysis of high sulphur-containing samples for total mercury content using automated thermal decomposition, amalgamation, and atomic absorption spectroscopy instruments (USEPA Method 7473) leads to rapid and costly SO2 poisoning of catalysts. In an effort to overcome this issue, we tested whether the addition of powdered sodium carbonate (Na2CO3) to the catalyst and/or directly on top of sample material increases throughput of sulphur-impregnated (8-15 wt%) activated carbon samples per catalyst tube. Adding 5 g of Na2CO3 to the catalyst alone only marginally increases the functional lifetime of the catalyst (31 ± 4 g of activated carbon analyzed per catalyst tube) in relation to unaltered catalyst of the AMA254 total mercury analyzer (17 ± 4 g of activated carbon). Adding ≈ 0.2 g of Na2CO3 to samples substantially increases (81 ± 17 g of activated carbon) catalyst life over the unaltered catalyst. The greatest improvement is achieved by adding Na2CO3 to both catalyst and samples (200 ± 70 g of activated carbon), which significantly increases catalyst performance over all other treatments and enables an order of magnitude greater sample throughput than the unaltered samples and catalyst. It is likely that Na2CO3 efficiently sequesters SO2, even at high furnace temperatures to produce Na2SO4 and CO2, largely negating the poisonous impact of SO2 on the catalyst material. Increased corrosion of nickel sampling boats resulting from this methodological variation is easily resolved by substituting quartz boats. Overall, this variation enables an efficient and significantly more affordable means of employing automated atomic absorption spectrometry instruments for total mercury analysis of high-sulphur matrices.

Determination of lead and nickel in environmental samples by flame atomic absorption spectrometry after column solid-phase extraction on Ambersorb-572 with EDTA.

PubMed

Baytak, Sitki; Türker, A Rehber

2006-02-28

Lead and nickel were preconcentrated as their ethylenediaminetetraacedic acid (EDTA) complexes from aqueous sample solutions using a column containing Ambersorb-572 and determined by flame atomic absorption spectrometry (FAAS). pH values, amount of solid phase, elution solution and flow rate of sample solution have been optimized in order to obtain quantitative recovery of the analytes. The effect of interfering ions on the recovery of the analytes has also been investigated. The recoveries of Pb and Ni under the optimum conditions were 99 +/- 2 and 97 +/- 3%, respectively, at 95% confidence level. Seventy-five-fold (using 750 mL of sample solution and 10 mL of eluent) and 50-fold (using 500 mL of sample solution and 10 mL of eluent) preconcentration was obtained for Pb and Ni, respectively. Time of analysis is about 4.5 h (for obtaining enrichment factor of 75). By applying these enrichment factors, the analytical detection limits of Pb and Ni were found as 3.65 and 1.42 ng mL(-1), respectively. The capacity of the sorbent was found as 0.17 and 0.21 mmol g(-1) for Pb and Ni, respectively. The interferences of some cations, such as Mn2+, Co2+, Fe3+, Al3+, Zn2+, Cd2+, Ca2+, Mg2+, K+ and Na+ usually present in water samples were also studied. This procedure was applied to the determination of lead and nickel in parsley, green onion, sea water and waste water samples. The accuracy of the procedure was checked by determining Pb and Ni in standard reference tea leaves sample (GBW-07605). The results demonstrated good agreement with the certified values.

VUV absorption spectroscopy measurements of the role of fast neutral atoms in a high-power gap breakdown

NASA Astrophysics Data System (ADS)

Filuk, A. B.; Bailey, J. E.; Cuneo, M. E.; Lake, P. W.; Nash, T. J.; Noack, D. D.; Maron, Y.

2000-12-01

The maximum power achieved in a wide variety of high-power devices, including electron and ion diodes, z pinches, and microwave generators, is presently limited by anode-cathode gap breakdown. A frequently discussed hypothesis for this effect is ionization of fast neutral atoms injected throughout the anode-cathode gap during the power pulse. We describe a newly developed diagnostic tool that provides a direct test of this hypothesis. Time-resolved vacuum-ultraviolet absorption spectroscopy is used to directly probe fast neutral atoms with 1-mm spatial resolution in the 10-mm anode-cathode gap of the SABRE 5 MV, 1 TW applied-B ion diode. Absorption spectra collected during Ar RF glow discharges and with CO2 gas fills confirm the reliability of the diagnostic technique. Throughout the 50-100 ns ion diode pulses no measurable neutral absorption was seen, setting upper limits of (0.12-1.5)×1014 cm-3 for ground-state fast neutral atom densities of H, C, N, O, and F. The absence of molecular absorption bands also sets upper limits of (0.16-1.2)×1015 cm-3 for common simple molecules. These limits are low enough to rule out ionization of fast neutral atoms as a breakdown mechanism. Breakdown due to ionization of molecules is also found to be unlikely. This technique can now be applied to quantify the role of neutral atoms in other high-power devices.

Depth Resolution Dependence on Sample Thickness and Incident Energy in On-Axis Transmission Kikuchi Diffraction in Scanning Electron Microscope (SEM).

PubMed

Brodu, Etienne; Bouzy, Emmanuel

2017-12-01

Transmission Kikuchi diffraction is an emerging technique aimed at producing orientation maps of the structure of materials with a nanometric lateral resolution. This study investigates experimentally the depth resolution of the on-axis configuration, via a twinned silicon bi-crystal sample specifically designed and fabricated. The measured depth resolution varies from 30 to 65 nm in the range 10-30 keV, with a close to linear dependence with incident energy and no dependence with the total sample thickness. The depth resolution is explained in terms of two mechanisms acting concomitantly: generation of Kikuchi diffraction all along the thickness of the sample, associated with continuous absorption on the way out. A model based on the electron mean free path is used to account for the dependence with incident energy of the depth resolution. In addition, based on the results in silicon, the use of the mean absorption coefficient is proposed to predict the depth resolution for any atomic number and incident energy.

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...

DETERMINING BERYLLIUM IN DRINKING WATER BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROSCOPY

EPA Science Inventory

A direct graphite furnace atomic absorption spectroscopy method for the analysis of beryllium in drinking water has been derived from a method for determining beryllium in urine. Ammonium phosphomolybdate and ascorbic acid were employed as matrix modifiers. The matrix modifiers s...

The extreme wings of atomic emission and absorption lines. [in low pressure gases

NASA Technical Reports Server (NTRS)

Dalgarno, A.; Sando, K. M.

1973-01-01

Consideration of the extreme wings of atomic and molecular emission and absorption lines in low pressure gases. Classical and semiclassical results are compared with accurate quantal calculations of the self-broadening of Lyman-alpha in the hydrogen absorption spectrum that arises from quasimolecular transition. The results of classical, quantal, and semiclassical calculations of the absorption coefficient in the red wing are shown for temperatures of 500, 200, and 100 K. The semiclassical and quantal spectra agree well in shape at 500 K. Various other findings are discused.

Precision atomic beam density characterization by diode laser absorption spectroscopy

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

Oxley, Paul; Wihbey, Joseph

2016-09-15

We provide experimental and theoretical details of a simple technique to determine absolute line-of-sight integrated atomic beam densities based on resonant laser absorption. In our experiments, a thermal lithium beam is chopped on and off while the frequency of a laser crossing the beam at right angles is scanned slowly across the resonance transition. A lock-in amplifier detects the laser absorption signal at the chop frequency from which the atomic density is determined. The accuracy of our experimental method is confirmed using the related technique of wavelength modulation spectroscopy. For beams which absorb of order 1% of the incident lasermore » light, our measurements allow the beam density to be determined to an accuracy better than 5% and with a precision of 3% on a time scale of order 1 s. Fractional absorptions of order 10{sup −5} are detectable on a one-minute time scale when we employ a double laser beam technique which limits laser intensity noise. For a lithium beam with a thickness of 9 mm, we have measured atomic densities as low as 5 × 10{sup 4} atoms cm{sup −3}. The simplicity of our technique and the details we provide should allow our method to be easily implemented in most atomic or molecular beam apparatuses.« less

Precision atomic beam density characterization by diode laser absorption spectroscopy.

PubMed

Oxley, Paul; Wihbey, Joseph

2016-09-01

We provide experimental and theoretical details of a simple technique to determine absolute line-of-sight integrated atomic beam densities based on resonant laser absorption. In our experiments, a thermal lithium beam is chopped on and off while the frequency of a laser crossing the beam at right angles is scanned slowly across the resonance transition. A lock-in amplifier detects the laser absorption signal at the chop frequency from which the atomic density is determined. The accuracy of our experimental method is confirmed using the related technique of wavelength modulation spectroscopy. For beams which absorb of order 1% of the incident laser light, our measurements allow the beam density to be determined to an accuracy better than 5% and with a precision of 3% on a time scale of order 1 s. Fractional absorptions of order 10 -5 are detectable on a one-minute time scale when we employ a double laser beam technique which limits laser intensity noise. For a lithium beam with a thickness of 9 mm, we have measured atomic densities as low as 5 × 10 4 atoms cm -3 . The simplicity of our technique and the details we provide should allow our method to be easily implemented in most atomic or molecular beam apparatuses.

Vibrational properties of gold nanoparticles obtained by green synthesis

NASA Astrophysics Data System (ADS)

Alvarez, Ramón A. B.; Cortez-Valadez, M.; Bueno, L. Oscar Neira; Britto Hurtado, R.; Rocha-Rocha, O.; Delgado-Beleño, Y.; Martinez-Nuñez, C. E.; Serrano-Corrales, Luis Ivan; Arizpe-Chávez, H.; Flores-Acosta, M.

2016-10-01

This study reports the synthesis and characterization of gold nanoparticles through an ecological method to obtain nanostructures from the extract of the plant Opuntia ficus-indica. Colloidal nanoparticles show sizes that vary between 10-20 nm, and present various geometric morphologies. The samples were characterized through optical absorption, Raman Spectroscopy and Transmission Electron Microscopy (TEM). Additionally, low energy metallic clusters of Aun (n=2-20 atoms) were modeled by computational quantum chemistry. The theoretical results were obtained with Density Functional Theory (DFT). The predicted results of Au clusters show a tendency and are correlated with the experimental results concerning the optical absorption bands and Raman spectroscopy in gold nanoparticles.

Two-dimensional fluorescence spectroscopy of uranium isotopes in femtosecond laser ablation plumes

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

Phillips, Mark C.; Brumfield, Brian E.; LaHaye, Nicole

Here, we demonstrate measurement of uranium isotopes in femtosecond laser ablation plumes using two-dimensional fluorescence spectroscopy (2DFS). The high-resolution, tunable CW-laser spectroscopy technique clearly distinguishes atomic absorption from 235U and 238U in natural and highly enriched uranium metal samples. We present analysis of spectral resolution and analytical performance of 2DFS as a function of ambient pressure. Simultaneous measurement using time-resolved absorption spectroscopy provides information on temporal dynamics of the laser ablation plume and saturation behavior of fluorescence signals. The rapid, non-contact measurement is promising for in-field, standoff measurements of uranium enrichment for nuclear safety and security.

Two-dimensional fluorescence spectroscopy of uranium isotopes in femtosecond laser ablation plumes

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

Phillips, Mark C.; Brumfield, Brian E.; LaHaye, Nicole L.

We demonstrate measurement of uranium isotopes in femtosecond laser ablation plumes using two-dimensional fluorescence spectroscopy (2DFS). The high-resolution, tunable CW-laser spectroscopy technique clearly distinguishes atomic absorption from 235U and 238U in natural and highly enriched uranium metal samples. We present analysis of spectral resolution and analytical performance of 2DFS as a function of ambient pressure. Simultaneous measurement using time-resolved absorption spectroscopy provides information on temporal dynamics of the laser ablation plume and saturation behavior of fluorescence signals. The rapid, non-contact measurement is promising for in-field, standoff measurements of uranium enrichment for nuclear safety and security applications.

Two-dimensional fluorescence spectroscopy of uranium isotopes in femtosecond laser ablation plumes

DOE PAGES

Phillips, Mark C.; Brumfield, Brian E.; LaHaye, Nicole; ...

2017-06-19

Here, we demonstrate measurement of uranium isotopes in femtosecond laser ablation plumes using two-dimensional fluorescence spectroscopy (2DFS). The high-resolution, tunable CW-laser spectroscopy technique clearly distinguishes atomic absorption from 235U and 238U in natural and highly enriched uranium metal samples. We present analysis of spectral resolution and analytical performance of 2DFS as a function of ambient pressure. Simultaneous measurement using time-resolved absorption spectroscopy provides information on temporal dynamics of the laser ablation plume and saturation behavior of fluorescence signals. The rapid, non-contact measurement is promising for in-field, standoff measurements of uranium enrichment for nuclear safety and security.

Disentangling atomic-layer-specific x-ray absorption spectra by Auger electron diffraction spectroscopy

NASA Astrophysics Data System (ADS)

Matsui, Fumihiko; Matsushita, Tomohiro; Kato, Yukako; Hashimoto, Mie; Daimon, Hiroshi

2009-11-01

In order to investigate the electronic and magnetic structures of each atomic layer at subsurface, we have proposed a new method, Auger electron diffraction spectroscopy, which is the combination of x-ray absorption spectroscopy (XAS) and Auger electron diffraction (AED) techniques. We have measured a series of Ni LMM AED patterns of the Ni film grown on Cu(001) surface for various thicknesses. Then we deduced a set of atomic-layer-specific AED patterns in a numerical way. Furthermore, we developed an algorithm to disentangle XANES spectra from different atomic layers using these atomic-layer-specific AED patterns. Surface and subsurface core level shift were determined for each atomic layer.

Fast arsenic speciation in water by on-site solid phase extraction and high-resolution continuum source graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Mihucz, Victor G.; Bencs, László; Koncz, Kornél; Tatár, Enikő; Weiszburg, Tamás; Záray, Gyula

2017-02-01

A method of high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS), combined with on-site separation/solid phase extraction (SPE) has been developed for the speciation of inorganic As (iAs) in geothermal and drinking water samples. The HR-CS-GFAAS calibration curves were linear up to 200 μg/L As, but using second order polynomial fitting, accurate calibration could be performed up to 500 μg/L. It has been demonstrated that sample pH should not be higher than 8 for an accurate speciation of As(V) with a recovery of ≈ 95%. Geothermal water had fairly high salt content (≈ 2200 mg/L) due to the presence of chlorides and sulfates at mg/L levels. Therefore, a two-fold dilution of these types of samples before SPE is recommended, especially, for total As determinations, when the As concentration is as high as 400 μg/L. For drinking water, sampled from public wells with records of As concentrations higher than the 10 μg/L in the past, the reduction of As contamination below the WHO's health limit value could be observed. However, the electrical conductivity was close to 2500 μS/cm, i.e., the guideline limit for drinking water, which was due to their higher chloride content. The proposed fit-for-purpose SPE-HR-CS-GFAAS method could be a candidate for screening drinking water quality.

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

PubMed

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

2010-09-15

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

Comparison of palladium and zirconium treated graphite tubes for in-atomizer trapping of hydrogen selenide in hydride generation electrothermal atomization atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Laborda, Francisco; Medrano, Jesús; Cortés, José I.; Mir, José M.; Castillo, Juan R.

1999-02-01

Zirconium treated graphite tubes were investigated and compared with non-treated and palladium coated ones for in situ trapping of selenium hydride generated in a flow injection system. Selenium was effectively trapped on zirconium treated tubes at trapping temperatures of 300-600°C, similar to those observed for palladium, whereas trapping temperatures higher than 600°C had to be used with non-treated tubes. Zirconium treated tubes used in this work showed good stability up to 300 trapping/atomization cycles, with precision better than 5%, characteristic masses of 42 (peak height) and 133 pg (peak area) of selenium were obtained. Sensitivity of zirconium and palladium treatments were similar, but zirconium offered the advantage of a single application per tube. Detection limits were 0.11 (peak height) and 0.23 ng (peak area) for a 1 ml sample volume.

Laser-induced breakdown spectroscopy (LIBS) technique for the determination of the chemical composition of complex inorganic materials

NASA Astrophysics Data System (ADS)

Łazarek, Łukasz; Antończak, Arkadiusz J.; Wójcik, Michał R.; Kozioł, Paweł E.; Stepak, Bogusz; Abramski, Krzysztof M.

2014-08-01

Laser-induced breakdown spectroscopy (LIBS) is a fast, fully optical method, that needs little or no sample preparation. In this technique qualitative and quantitative analysis is based on comparison. The determination of composition is generally based on the construction of a calibration curve namely the LIBS signal versus the concentration of the analyte. Typically, to calibrate the system, certified reference materials with known elemental composition are used. Nevertheless, such samples due to differences in the overall composition with respect to the used complex inorganic materials can influence significantly on the accuracy. There are also some intermediate factors which can cause imprecision in measurements, such as optical absorption, surface structure, thermal conductivity etc. This paper presents the calibration procedure performed with especially prepared pellets from the tested materials, which composition was previously defined. We also proposed methods of post-processing which allowed for mitigation of the matrix effects and for a reliable and accurate analysis. This technique was implemented for determination of trace elements in industrial copper concentrates standardized by conventional atomic absorption spectroscopy with a flame atomizer. A series of copper flotation concentrate samples was analyzed for contents of three elements, that is silver, cobalt and vanadium. It has been shown that the described technique can be used to qualitative and quantitative analyses of complex inorganic materials, such as copper flotation concentrates.

Determining the arsenic, cadmium, lead, copper and chromium contents by atomic absorption spectrometry in Pangasius fillets from Vietnam.

PubMed

Molognoni, Luciano; Vitali, Luciano; Ploêncio, Leandro As; Santos, Jacson N; Daguer, Heitor

2016-07-01

Pangasius is a fish produced on a large scale in Vietnam and exported to many countries. Since river contamination from human activities can affect the safety of this food, fish consumption can cause exposure to potentially toxic elements for humans. The aim of this study, therefore, was to assess arsenic, cadmium, lead, copper and chromium contents by atomic absorption spectrometry in Pangasius fillet produced in the provinces of Dong Thap and Can Tho (Vietnam) and exported to Brazil. The limits of detection were: arsenic 0.5443 µg kg(-1) , cadmium 0.0040 mg kg(-1) , chromium 0.0004 mg kg(-1) , copper 0.0037 mg kg(-1) and lead 0.0284 mg kg(-1) . Analysis of 20 samples showed results below the limit of detection for arsenic, chromium and lead, while copper average concentration was 0.0234 mg kg(-1) . Cadmium average concentration was 0.0547 mg kg(-1) , with no significant difference between the two regions studied. The samples of Pangasius had no detectable concentrations of arsenic, chromium, copper and lead, and do not represent a hazard to public health. However, cadmium analysis revealed non-compliant samples, demonstrating the importance of monitoring the quality of imported Pangasius fish. © 2015 Society of Chemical Industry. © 2015 Society of Chemical Industry.

Flotation separation and electrothermal atomic absorption spectrometric determination of thallium in wastewater samples.

PubMed

Hosseini, Mohammad Saeid; Chamsaz, Mahmoud; Raissi, Heidar; Naseri, Yousef

2006-01-01

The proposed method is a simple process for the determination of trace amount of thallium(I) in the environmental wastewater samples by electrothermal atomic absorption spectrometry. The wastewater samples were obtained from the environment of a cement plant and subjected to a simple treatment, such as adjusting pH and masking the interfering ions, to prepare for the flotation process in which the thallium(I) content was floated as an ion-association complex using iodide and Rhodamine B at the interface of aqueous/cyclohexane layers. The floated layer was then separated and dissolved in 2 ml of a solution, which was 1% to H2SO4 and 50% to methanol, respectively. Aliquots of 10-microl of this solution were subjected to the graphite furnace to determine the thallium(I) content. The flotation process can be carried in a weak acidic medium in which the interfering effects owing to certain metal ions were eliminated by masking them as neutral citrate chelates. The dynamic range for the determination was found to be 1.0 x 10(-8) - 1.0 x 10(-7) mol l(-1). The RSD was 3.2% and the DL was 2.5 x 10(-9) mol l(-1) (calculated as 3SD of the blank). The reliability of the method is demonstrated by the analysis of a synthetic wastewater in which the recovery was found to be 94%.

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

PubMed

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

2014-01-01

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

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

PubMed Central

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

2014-01-01

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

The use of mosses as environmental metal pollution indicators.

PubMed

Aceto, Maurizio; Abollino, Ornella; Conca, Raffaele; Malandrino, Mery; Mentasti, Edoardo; Sarzanini, Corrado

2003-01-01

The possibility of using mosses as environmental indicators of metal pollution has been investigated. Mosses of the species Bryum argenteum were collected from different parts of Piedmont (Italy), ranging from highly polluted areas to nearly uncontaminated mountain areas. Periodical samplings were planned in every site on a monthly base, in order to check variations of metal uptake throughout one year; correlations with pluviometric and thermal patterns were investigated for all sampling stations. On every moss sample 20 elements, ranging from major (K, P, Al, Ca, Fe and Mg) to minor (Mn, Na, Ti and Zn) and trace (As, Ba, Cd, Co, Cr, Cu, Li, Ni, Pb and Sr), were quantitatively determined by inductively coupled plasma-atomic emission spectrometry or graphite furnace-atomic absorption spectrometry, depending on the needed sensitivity. Statistical analyses, carried out with principal component analysis and cluster analysis methods, revealed that a good correlation exists between metal content in mosses and pollution degree in the areas sampled.

Atomic Absorption Spectroscopy. The Present and the Future.

ERIC Educational Resources Information Center

Slavin, Walter

1982-01-01

The status of current techniques and methods of atomic absorption (AA) spectroscopy (flame, hybrid, and furnace AA) is discussed, including limitations. Technological opportunities and how they may be used in AA are also discussed, focusing on automation, microprocessors, continuum AA, hybrid analyses, and others. (Author/JN)

Concurrent determination of total serum calcium and magnesium by thermometric titration with ethylenediaminetetraacetate.

PubMed

Callicott, R H; Carr, P W

1976-07-01

Total serum calcium and magnesium may be determined in one thermometric titration, with disodium ethylenediaminetetraacetate as the titrant. A 1-ml serum sample is diluted with 1 ml of tris(hydroxymethyl)aminomethane buffer (pH 8) and titrated at a constant rate with a motorized syringe buret. Results by the thermometric method compared well with those by atomic absorption spectroscopy.

Coping with effects of high dissolved salt samples on the inductively coupled plasma spectrometer

Treesearch

Jane E. Hislop; James W. Hornbeck; James W. Hornbeck

2002-01-01

Research on acidic forest soils typically uses unbuffered salt solutions as extractants for exchangeable cations. Our lab uses 1 M NH4C1 extractant for exchangeable cations (Ca, K, Mg, and Na) and 1 M KC1 for exchangeable aluminum. The resulting high dissolved salt solutions presented chronic analytical problems on flame atomic absorption spectrophotometer (AAS) and...

The remarkable chemical uniformity of Apollo 16 layered deep drill core section 60002

NASA Technical Reports Server (NTRS)

Nava, D. F.; Philpotts, J. A.; Lindstrom, M. M.; Schuhmann, P. J.; Lindstrom, D. J.

1976-01-01

Atomic absorption and colorimetric spectrophotometers were used to determine major- and minor-element abundances in 12 samples from layered section 60002 of the Apollo 16 deep drill core. It is suggested that gardening of a relatively thick local unit produced the layering in this section in such a manner that the proportions of materials of different compositions remained virtually unchanged.

Analysis of arsenical metabolites in biological samples.

PubMed

Hernandez-Zavala, Araceli; Drobna, Zuzana; Styblo, Miroslav; Thomas, David J

2009-11-01

Quantitation of iAs and its methylated metabolites in biological samples provides dosimetric information needed to understand dose-response relations. Here, methods are described for separation of inorganic and mono-, di-, and trimethylated arsenicals by thin layer chromatography. This method has been extensively used to track the metabolism of the radionuclide [(73)As] in a variety of in vitro assay systems. In addition, a hydride generation-cryotrapping-gas chromatography-atomic absorption spectrometric method is described for the quantitation of arsenicals in biological samples. This method uses pH-selective hydride generation to differentiate among arsenicals containing trivalent or pentavalent arsenic.

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.

Paleodiet characterisation of an Etrurian population of Pontecagnano (Italy) by Isotope Ratio Mass Spectrometry (IRMS) and Atomic Absorption Spectrometry (AAS)(#).

PubMed

Scarabino, Carla; Lubritto, Carmine; Proto, Antonio; Rubino, Mauro; Fiengo, Gilda; Marzaioli, Fabio; Passariello, Isabella; Busiello, Gaetano; Fortunato, Antonietta; Alfano, Davide; Sabbarese, Carlo; Rogalla, Detlef; De Cesare, Nicola; d'Onofrio, Antonio; Terrasi, Filippo

2006-06-01

Human bones recovered from the archaeological site of Pontecagnano (Salerno, Italy) have been studied to reconstruct the diet of an Etrurian population. Two different areas were investigated, named Library and Sant' Antonio, with a total of 44 tombs containing human skeletal remains, ranging in age from the 8th to the 3rd century B.C. This time span was confirmed by 14C dating obtained using Accelerator Mass Spectrometry (AMS) on one bone sample from each site. Atomic Absorption Spectrometry (AAS) was used to extract information about the concentration of Sr, Zn, Ca elements in the bone inorganic fraction, whilst stable isotope ratio measurements (IRMS) were carried out on bone collagen to obtain the delta13C and delta15N. A reliable technique has been used to extract and separate the inorganic and organic fractions of the bone remains. Both IRMS and AAS results suggest a mixed diet including C3 plant food and herbivore animals, consistent with archaeological indications.

Study of zinc-induced changes in lymphocyte membranes using atomic force microscopy, luminescence, and light scattering methods

NASA Astrophysics Data System (ADS)

Filimonenko, D. S.; Khairullina, A. Ya.; Yasinskii, V. M.; Kozlova, N. M.; Zubritskaja, G. P.; Slobozhanina, E. I.

2011-07-01

Changes in the surface structure of lymphocyte membranes exposed to various concentrations of zinc ions are studied. It is found by atomic force microscopy that increasing the concentration of zinc ions leads to a reduction in the correlation length of the autocorrelation function of the roughness profile of a lymphocyte compared to control samples; this may indicate the existence of fine structure in the membrane surface. Fluorescence markers are used to observe a reduction in the microviscosity of the lipids in the outer monolayer of the lipid bilayer after lymphocytes are exposed to Zn ions, as well as the exposure of phosphatidylserine on the surface membrane, and the oxidation of HS-groups of membrane proteins. Calculations of the absorption coefficients of lymphocytes modified with zinc reveal the existence of absorption bands owing to the formation of metal-protein complexes and zinc oxide nanoparticles. These results indicate significant changes in the structural and functional state of lymphocyte membranes exposed to zinc ions.

An improved method for the determination of trace levels of arsenic and antimony in geological materials by automated hydride generation-atomic absorption spectroscopy

USGS Publications Warehouse

Crock, J.G.; Lichte, F.E.

1982-01-01

An improved, automated method for the determination of arsenic and antimony in geological materials is described. After digestion of the material in sulfuric, nitric, hydrofluoric and perchloric acids, a hydrochloric acid solution of the sample is automatically mixed with reducing agents, acidified with additional hydrochloric acid, and treated with a sodium tetrahydroborate solution to form arsine and stibine. The hydrides are decomposed in a heated quartz tube in the optical path of an atomic absorption spectrometer. The absorbance peak height for arsenic or antimony is measured. Interferences that exist are minimized to the point where most geological materials including coals, soils, coal ashes, rocks and sediments can be analyzed directly without use of standard additions. The relative standard deviation of the digestion and the instrumental procedure is less than 2% at the 50 ??g l-1 As or Sb level. The reagent-blank detection limit is 0.2 ??g l-1 As or Sb. ?? 1982.

Reduction of matrix interferences in furnace atomic absorption with the L'vov Platform

USGS Publications Warehouse

Kaiser, M.L.; Koirtyohann, S.R.; Hinderberger, E.J.; Taylor, Howard E.

1981-01-01

Use of a modified L'vov Platform and ammonium phosphate as a matrix modifier greatly reduced matrix interferences in a commercial Massmann-type atomic absorption furnace. Platforms were readily fabricated from furnace tubes and, once positioned in the furnace, caused no inconvenience in operation. Two volatile elements (Pb, Cd), two of intermediate volatility (Co, Cr) and two which form stable oxides (Al, Sn) were tested in natural water and selected synthetic matrices. In every case for which there was a significant matrix effect during atomization from the tube wall, the platform and platform plus modifier gave improved performance. With lead, for example, an average ratio of 0.48 ?? 0.11 was found when the slope of the standard additions plot for six different natural water samples was compared to the slope of the standard working curve in dilute acid. The average slope ratio between the natural water matrices and the dilute acid matrix was 0.94 ?? 0.03 with the L'vov Platform and 0.96 ?? 0.03 with the platform and matrix modifier. In none of the cases studied did the use of the platform or platform plus modifier cause an interference problem where none existed while atomizing from the tube wall. An additional benefit of the platform was a factor of about two improvement in peak height precision. ?? 1981.

Investigation of Teflon FEP Embrittlement on Spacecraft in Low-Earth Orbit

NASA Technical Reports Server (NTRS)

deGroh, Kim K.; Banks, Bruce A.

1997-01-01

Teflon fluorinated ethylene propylene (FEP) (DuPont) is commonly used on exterior spacecraft surfaces for thermal control in the low-Earth orbit environment. Silverized or aluminized Teflon FEP is used for the outer layers of the thermal control blanket because of its high reflectance, low solar absorptance, and high thermal emittance. Teflon FEP is also desirable because, compared with other spacecraft polymers (such as Kapton), it has relatively high resistance to atomic oxygen erosion. Because of its comparably low atomic oxygen erosion yield, Teflon FEP has been used unprotected in the space environment. Samples of Teflon FEP from the Long Duration Exposure Facility (LDEF) and the Hubble Space Telescope (retrieved during its first servicing mission) were evaluated for solar-induced embrittlement and for synergistic effects of solar degradation and atomic oxygen.

Near-neighbor mixing and bond dilation in mechanically alloyed Cu-Fe

NASA Astrophysics Data System (ADS)

Harris, V. G.; Kemner, K. M.; Das, B. N.; Koon, N. C.; Ehrlich, A. E.; Kirkland, J. P.; Woicik, J. C.; Crespo, P.; Hernando, A.; Garcia Escorial, A.

1996-09-01

Extended x-ray-absorption fine-structure (EXAFS) measurements were used to obtain element-specific, structural, and chemical information of the local environments around Cu and Fe atoms in high-energy ball-milled CuxFe1-x samples (x=0.50 and 0.70). Analysis of the EXAFS data shows both Fe and Cu atoms reside in face-centered-cubic sites where the first coordination sphere consists of a mixture of Fe and Cu atoms in a ratio which reflects the as-prepared stoichiometry. The measured bond distances indicate a dilation in the bonds between unlike neighbors which accounts for the lattice expansion measured by x-ray diffraction. These results indicate that metastable alloys having a positive heat of mixing can be prepared via the high-energy ball-milling process.

[Determination of lead in microemulsified rapeseed oil and bio-diesel oil by GFAAS].

PubMed

Li, Sheng-qing; He, Xiao-min; Du, Ping; Wang, Min; Chen, Hao; Wu, Mou-cheng

2008-10-01

Bio-diesel oil has attracted much attention as a substitutable energy sources for its renewable and eco-friendly property. However, problems of lead contamination in fuel are also emphasized increasingly at present. So it was of quite significance to determine the contents of lead in bio-diesel oil and its raw material rapeseed oil. An effective method was developed for the rapid determination of lead in rapeseed oil and bio-diesel oil by graphite furnace atomic absorption spectrometry (GFAAS) after their stabilization as microemulsions. In this research work, polyethyleneglycol octyl phenyl ether and n-butanol were used for emulsifier and auxiliary emulsifying agent, respectively. For Pb, efficient thermal stabilization was obtained using NH4H2PO4 as matrix modifier. Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling. Excellent long-term sample stabilization and the influence of the microemulsion composition on the GFAAS response were observed by mixing different organic solvents. The ashing and atomization temperature and ramp rate influenced the sensitivity obtained for Ph. Take this into account, the optimum conditions of the graphite furnace atomic absorption spectrometric determination of Pb in rapeseed oil and bio-diesel oil samples were investigated. The results showed that the microemulsion was quite stable when the value of V(20% polyethyleneglycol octyl phenyl ether), V(n-butanol), V(oil) and V(water) was 0.1: 8.9: 0.5: 0.5, without matrix interference effect. The determination limit of the proposed method was 126.2 microg x L(-1) for Pb, comfortably below the values found in the analyzed samples. The recoveries were from 81.8% to 109.0%, which performed using the addition of different concentrations of lead to bio-diesel oil, rapeseed oil and petrochemical diesel samples. The relative standard deviation of determination was 5.84%. This work showed the great efficiency of the microemulsion, indicating that it is possible to extract lead from the oil phase. The method was applied to the determination of lead in oil samples with satisfactory results.

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

NASA Technical Reports Server (NTRS)

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

1988-01-01

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

The determination of specific forms of aluminum in natural water

USGS Publications Warehouse

Barnes, R.B.

1975-01-01

A procedure for analysis and pretreatment of natural-water samples to determine very low concentrations of Al is described which distinguishes the rapidly reacting equilibrium species from the metastable or slowly reacting macro ions and colloidal suspended material. Aluminum is complexed with 8-hydroxyquinoline (oxine), pH is adjusted to 8.3 to minimize interferences, and the aluminum oxinate is extracted with methyl isobutyl ketone (MIBK) prior to analysis by atomic absorption. To determine equilibrium species only, the contact time between sample and 8-hydroxyquinoline is minimized. The Al may be extracted at the sample site with a minimum of equipment and the MIBK extract stored for several weeks prior to atomic absorption analysis. Data obtained from analyses of 39 natural groundwater samples indicate that filtration through a 0.1-??m pore size filter is not an adequate means of removing all insoluble and metastable Al species present, and extraction of Al immediately after collection is necessary if only dissolved and readily reactive species are to be determined. An average of 63% of the Al present in natural waters that had been filtered through 0.1-??m pore size filters was in the form of monomeric ions. The total Al concentration, which includes all forms that passed through a 0.1-??m pore size filter, ranged 2-70 ??g/l. The concentration of Al in the form of monomeric ions ranged from below detection to 57 ??g/l. Most of the natural water samples used in this study were collected from thermal springs and oil wells. ?? 1975.

An x ray scatter approach for non-destructive chemical analysis of low atomic numbered elements

NASA Technical Reports Server (NTRS)

Ross, H. Richard

1993-01-01

A non-destructive x-ray scatter (XRS) approach has been developed, along with a rapid atomic scatter algorithm for the detection and analysis of low atomic-numbered elements in solids, powders, and liquids. The present method of energy dispersive x-ray fluorescence spectroscopy (EDXRF) makes the analysis of light elements (i.e., less than sodium; less than 11) extremely difficult. Detection and measurement become progressively worse as atomic numbers become smaller, due to a competing process called 'Auger Emission', which reduces fluorescent intensity, coupled with the high mass absorption coefficients exhibited by low energy x-rays, the detection and determination of low atomic-numbered elements by x-ray spectrometry is limited. However, an indirect approach based on the intensity ratio of Compton and Rayleigh scattered has been used to define light element components in alloys, plastics and other materials. This XRS technique provides qualitative and quantitative information about the overall constituents of a variety of samples.

Atomic and Molecular Gas Phase Spectrometry.

DTIC Science & Technology

1983-09-30

between the thermometric levels, k is the Boltzmann constant (k = 0.695 cm-I K-1 ), Aik (s- 1) is the transition probability for spontaneous emission from...monitoring of the atomic absorption of M; information about the reaction processes were deduced from the shapes of the titration curves; (5) measure- ment of...Changes During Titration Based Upon The Releasing Effect Atomic Absorption Spectroscopy," D. Stojanovic and J.D. Winefordner, Anal Chim. Acta, 114, 295

X-ray absorption spectroscopy and X-ray photoelectron spectroscopy studies of CaSO 4:Dy thermoluminescent phosphors

NASA Astrophysics Data System (ADS)

Bakshi, A. K.; Jha, S. N.; Olivi, L.; Phase, D. M.; Kher, R. K.; Bhattacharyya, D.

2007-11-01

Extended X-ray absorption fine structure (EXAFS) measurements have been carried out on CaSO4:Dy phosphor samples at the Dy L3 edge with synchrotron radiation. Measurements were carried out on a set of samples which were subjected to post-preparation annealing at different temperatures and for different cycles. The EXAFS data have been analysed to find the Dy-S and Dy-O bond lengths in the neighbourhood of the Dy atoms in a CaSO4 matrix. The observations from EXAFS measurements were verified with XANES and XPS techniques. On the basis of these measurements, efforts were made to explain the loss of thermoluminescence sensitivity of CaSO4:Dy phosphors after repeated cycles of annealing at 400 °C in air for 1 h.

Spin noise spectroscopy of rubidium atomic gas under resonant and non-resonant conditions

NASA Astrophysics Data System (ADS)

Ma, Jian; Shi, Ping; Qian, Xuan; Li, Wei; Ji, Yang

2016-11-01

The spin fluctuation in rubidium atom gas is studied via all-optical spin noise spectroscopy (SNS). Experimental results show that the integrated SNS signal and its full width at half maximum (FWHM) strongly depend on the frequency detuning of the probe light under resonant and non-resonant conditions. The total integrated SNS signal can be well fitted with a single squared Faraday rotation spectrum and the FWHM dependence may be related to the absorption profile of the sample. Project supported by the National Natural Science Foundation of China (Grant Nos. 91321310 and 11404325) and the National Basic Research Program of China (Grant No. 2013CB922304).

The Use of an Air-Natural Gas Flame in Atomic Absorption.

ERIC Educational Resources Information Center

Melucci, Robert C.

1983-01-01

Points out that excellent results are obtained using an air-natural gas flame in atomic absorption experiments rather than using an air-acetylene flame. Good results are obtained for alkali metals, copper, cadmium, and zinc but not for the alkaline earths since they form refractory oxides. (Author/JN)

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...

[Atomic absorption in mercury determination by "Julia-2" analyzer and urine mercury level in children of Moscow suburbs].

PubMed

Pavlovskaia, N A; Vagina, E N; Stepanova, E V

2000-01-01

The authors report on atomic absorption method determining mercury in urine. Being sensitive, with lower determination threshold of 10 nmole/l and correctness of 95.5%, the method was tested on children living in two districts of Moscow suburb.

Determination of essential elements in beverages, herbal infusions and dietary supplements using a new straightforward sequential approach based on flame atomic absorption spectrometry.

PubMed

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

2017-03-15

A simple method based on FAAS was developed for the sequential multi-element determination of Cu, Zn, Mn, Mg and Si in beverages and food supplements with successful results. The main absorption lines for Cu, Zn and Si and secondary lines for Mn and Mg were selected to carry out the measurements. The sample introduction was performed using a flow injection system. Using the choice of the absorption line wings, the upper limit of the linear range increased up to 110mgL -1 for Mg, 200mgL -1 for Si and 13mgL -1 for Zn. The determination of the five elements was carried out, in triplicate, without the need of additional sample dilutions and/or re-measurements, using less than 3.5mL of sample to perform the complete analysis. The LODs were 0.008mgL -1 for Cu, 0.017mgL -1 for Zn, 0.011mgL -1 for Mn, 0.16mgL -1 for Si and 0.11mgL -1 for Mg. Copyright © 2016 Elsevier Ltd. All rights reserved.

Questa baseline and pre-mining ground-water quality investigation. 2. Low-flow (2001) and snowmelt (2002) synoptic/tracer water chemistry for the Red River, New Mexico

USGS Publications Warehouse

McCleskey, R. Blaine; Nordstrom, D. Kirk; Steiger, Judy I.; Kimball, Briant A.; Verplanck, Philip L.

2003-01-01

Water analyses are reported for 259 samples collected from the Red River, New Mexico, and its tributaries during low-flow(2001) and spring snowmelt (2002) tracer studies. Water samples were collected along a 20-kilometer reach of the Red River beginning just east of the town of Red River and ending at the U.S. Geological Survey streamflow-gaging station located east of Questa, New Mexico. The study area was divided into three sections where separate injections and synoptic sampling events were performed during the low-flow tracer study. During the spring snowmelt tracer study, three tracer injections and synoptic sampling events were performed bracketing the areas with the greatest metal loading into the Red River as determined from the low-flow tracer study. The lowflow tracer synoptic sampling events were August 17, 20, and 24, 2001. The synoptic sampling events for the spring snowmelt tracer were March 30, 31, and April 1, 2002. Stream and large inflow water samples were sampled using equal-width and depth-integrated sampling methods and composited into half-gallon bottles. Grab water samples were collected from smaller inflows. Stream temperatures were measured at the time of sample collection. Samples were transported to a nearby central processing location where pH and specific conductance were measured and the samples processed for chemical analyses. Cations, trace metals, iron redox species, and fluoride were analyzed at the U.S. Geological Survey laboratory in Boulder, Colorado. Cations and trace metal concentrations were determined using inductively coupled plasma-optical emission spectrometry and graphite furnace atomic absorption spectrometry. Arsenic concentrations were determined using hydride generation atomic absorption spectrometry, iron redox species were measured using ultraviolet-visible spectrometry, and fluoride concentrations were determined using an ion-selective electrode. Alkalinity was measured by automated titration, and sulfate, chloride, and bromide were analyzed by ion chromatography at the U.S. Geological Survey laboratory in Salt Lake City, Utah.

VUV absorption spectroscopy measurements of the role of fast neutral atoms in a high-power gap breakdown

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

Filuk, A. B.; Bailey, J. E.; Cuneo, M. E.

The maximum power achieved in a wide variety of high-power devices, including electron and ion diodes, z pinches, and microwave generators, is presently limited by anode-cathode gap breakdown. A frequently discussed hypothesis for this effect is ionization of fast neutral atoms injected throughout the anode-cathode gap during the power pulse. We describe a newly developed diagnostic tool that provides a direct test of this hypothesis. Time-resolved vacuum-ultraviolet absorption spectroscopy is used to directly probe fast neutral atoms with 1-mm spatial resolution in the 10-mm anode-cathode gap of the SABRE 5 MV, 1 TW applied-B ion diode. Absorption spectra collected duringmore » Ar RF glow discharges and with CO{sub 2} gas fills confirm the reliability of the diagnostic technique. Throughout the 50--100 ns ion diode pulses no measurable neutral absorption was seen, setting upper limits of (0.12--1.5)x10{sup 14}cm{sup -3} for ground-state fast neutral atom densities of H, C, N, O, and F. The absence of molecular absorption bands also sets upper limits of (0.16--1.2)x10{sup 15}cm{sup -3} for common simple molecules. These limits are low enough to rule out ionization of fast neutral atoms as a breakdown mechanism. Breakdown due to ionization of molecules is also found to be unlikely. This technique can now be applied to quantify the role of neutral atoms in other high-power devices.« less

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.

Confocal absorption spectral imaging of MoS2: optical transitions depending on the atomic thickness of intrinsic and chemically doped MoS2.

PubMed

Dhakal, Krishna P; Duong, Dinh Loc; Lee, Jubok; Nam, Honggi; Kim, Minsu; Kan, Min; Lee, Young Hee; Kim, Jeongyong

2014-11-07

We performed a nanoscale confocal absorption spectral imaging to obtain the full absorption spectra (over the range 1.5-3.2 eV) within regions having different numbers of layers and studied the variation of optical transition depending on the atomic thickness of the MoS2 film. Three distinct absorption bands corresponding to A and B excitons and a high-energy background (BG) peak at 2.84 eV displayed a gradual redshift as the MoS2 film thickness increased from the monolayer, to the bilayer, to the bulk MoS2 and this shift was attributed to the reduction of the gap energy in the Brillouin zone at the K-point as the atomic thickness increased. We also performed n-type chemical doping of MoS2 films using reduced benzyl viologen (BV) and the confocal absorption spectra modified by the doping showed a strong dependence on the atomic thickness: A and B exciton peaks were greatly quenched in the monolayer MoS2 while much less effect was shown in larger thickness and the BG peak either showed very small quenching for 1 L MoS2 or remained constant for larger thicknesses. Our results indicate that confocal absorption spectral imaging can provide comprehensive information on optical transitions of microscopic size intrinsic and doped two-dimensional layered materials.

Method development for the determination of fluorine in water samples via the molecular absorption of strontium monofluoride formed in an electrothermal atomizer

NASA Astrophysics Data System (ADS)

Ozbek, Nil; Akman, Suleyman

The presence of fluorine (F) was detected via the rotational molecular absorption line of diatomic strontium-monofluoride (SrF) generated in the gas phase at 651.187 nm using high-resolution continuum source electrothermal atomic absorption spectrometry. Upon the addition of excess strontium (Sr) as the nitrate, the fluorine in the sample was converted to SrF in the gas phase of a graphite furnace. The effects on the accuracy, precision and sensitivity of variables such as the SrF wavelength, graphite furnace program, amount of Sr, coating of the graphite tube and platform with Zr and Ir and the use of a modifier were investigated and optimized. It was determined that there was no need to use a modifier or to cover the platform/tubes with Zr or Ir. Fluorine concentrations in various water samples (certified waste water, tap water, drinking water and mineral water) were determined using 20 μg of Sr as the molecule-forming reagent and applying a maximum pyrolysis temperature of 800 °C and a molecule-forming temperature of 2200 °C with a heating rate of 2000 °C s- 1. Good linearity was maintained up to 0.1 μg of F. The accuracy and precision of the method were tested by analyzing certified reference wastewater. The results were in good agreement with certified values, and the precision was satisfactory (RSD < 10%). The limit of detection and the characteristic mass for the method were 0.36 ng and 0.55 ng, respectively. Finally, the fluorine concentrations in several drinking water and mineral water samples taken from the market were determined. The results were in good agreement with the values supplied by the producers. No significant differences were found between the results from the linear calibration and standard addition techniques. The method was determined to be simple, fast, accurate and sensitive.

Method and apparatus for sampling atmospheric mercury

DOEpatents

Trujillo, Patricio E.; Campbell, Evan E.; Eutsler, Bernard C.

1976-01-20

A method of simultaneously sampling particulate mercury, organic mercurial vapors, and metallic mercury vapor in the working and occupational environment and determining the amount of mercury derived from each such source in the sampled air. A known volume of air is passed through a sampling tube containing a filter for particulate mercury collection, a first adsorber for the selective adsorption of organic mercurial vapors, and a second adsorber for the adsorption of metallic mercury vapor. Carbon black molecular sieves are particularly useful as the selective adsorber for organic mercurial vapors. The amount of mercury adsorbed or collected in each section of the sampling tube is readily quantitatively determined by flameless atomic absorption spectrophotometry.

The use of atomic spectroscopy in the pharmaceutical industry for the determination of trace elements in pharmaceuticals.

PubMed

Lewen, Nancy

2011-06-25

The subject of the analysis of various elements, including metals and metalloids, in the pharmaceutical industry has seen increasing importance in the last 10-15 years, as modern analytical instrumentation has afforded analysts with the opportunity to provide element-specific, accurate and meaningful information related to pharmaceutical products. Armed with toxicological data, compendial and regulatory agencies have revisited traditional approaches to the testing of pharmaceuticals for metals and metalloids, and analysts have begun to employ the techniques of atomic spectroscopy, such as flame- and graphite furnace atomic absorption spectroscopy (FAAS, Flame AA or FAA and GFAAS), inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and inductively coupled plasma-mass spectrometry (ICP-MS), to meet their analytical needs. Newer techniques, such as laser-induced breakdown spectroscopy (LIBS) and Laser Ablation ICP-MS (LAICP-MS) are also beginning to see wider applications in the analysis of elements in the pharmaceutical industry.This article will provide a perspective regarding the various applications of atomic spectroscopy in the analysis of metals and metalloids in drug products, active pharmaceutical ingredients (API's), raw materials and intermediates. The application of atomic spectroscopy in the analysis of metals and metalloids in clinical samples, nutraceutical, metabolism and pharmacokinetic samples will not be addressed in this work. Copyright © 2010 Elsevier B.V. All rights reserved.

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.

Toxic metals in imported fruits and vegetables marketed in Kuwait

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

Husain, A.; Baroon, Z.; Al-Khalafawi, M.

1995-12-31

The concentration of lead, cadmium, and mercury in 134 samples of imported fruits and vegetables marketed in Kuwait were determined using an atomic absorption spectrophotometer with a graphite furnace and the cold vapor technique. Results obtained showed that the concentration of these metal ions in most cases did not exceed the maximum permissible concentration of metals in fresh fruits and vegetables as restricted by some countries. Only a few samples of fruits and vegetables contained levels of mercury, cadmium, and lead which exceeded these maximum permissible levels.

Beyond the single-atom response in absorption line shapes: probing a dense, laser-dressed helium gas with attosecond pulse trains.

PubMed

Liao, Chen-Ting; Sandhu, Arvinder; Camp, Seth; Schafer, Kenneth J; Gaarde, Mette B

2015-04-10

We investigate the absorption line shapes of laser-dressed atoms beyond the single-atom response, by using extreme ultraviolet (XUV) attosecond pulse trains to probe an optically thick helium target under the influence of a strong infrared (IR) field. We study the interplay between the IR-induced phase shift of the microscopic time-dependent dipole moment and the resonant-propagation-induced reshaping of the macroscopic XUV pulse. Our experimental and theoretical results show that as the optical depth increases, this interplay leads initially to a broadening of the IR-modified line shape, and subsequently, to the appearance of new, narrow features in the absorption line.

Determination of the atomic density of rubidium-87

NASA Astrophysics Data System (ADS)

Zhao, Meng; Zhang, Kai; Chen, Li-Qing

2015-09-01

Atomic density is a basic and important parameter in quantum optics, nonlinear optics, and precision measurement. In the past few decades, several methods have been used to measure atomic density, such as thermionic effect, optical absorption, and resonance fluorescence. The main error of these experiments stemmed from depopulation of the energy level, self-absorption, and the broad bandwidth of the laser. Here we demonstrate the atomic density of 87Rb vapor in paraffin coated cell between 297 K and 334 K mainly using fluorescence measurement. Optical pumping, anti-relaxation coating, and absorption compensation approaches are used to decrease measurement error. These measurement methods are suitable for vapor temperature at dozens of degrees. The fitting function for the experimental data of 87Rb atomic density is given. Project supported by the Natural Science Foundation of China (Grant Nos. 11274118 and 11474095), the Innovation Program of Shanghai Municipal Education Commission of China (Grant No. 13ZZ036), and the Fundamental Research Funds for the Central Universities of China.

Determination of cadmium and lead in table salt by sequential multi-element flame atomic absorption spectrometry.

PubMed

Amorim, Fábio A C; Ferreira, Sérgio L C

2005-02-28

In the present paper, a simultaneous pre-concentration procedure for the sequential determination of cadmium and lead in table salt samples using flame atomic absorption spectrometry is proposed. This method is based on the liquid-liquid extraction of cadmium(II) and lead(II) ions as dithizone complexes and direct aspiration of the organic phase for the spectrometer. The sequential determination of cadmium and lead is possible using a computer program. The optimization step was performed by a two-level fractional factorial design involving the variables: pH, dithizone mass, shaking time after addition of dithizone and shaking time after addition of solvent. In the studied levels these variables are not significant. The experimental conditions established propose a sample volume of 250mL and the extraction process using 4.0mL of methyl isobutyl ketone. This way, the procedure allows determination of cadmium and lead in table salt samples with a pre-concentration factor higher than 80, and detection limits of 0.3ngg(-1) for cadmium and 4.2ngg(-1) for lead. The precision expressed as relative standard deviation (n = 10) were 5.6 and 2.6% for cadmium concentration of 2 and 20ngg(-1), respectively, and of 3.2 and 1.1% for lead concentration of 20 and 200ngg(-1), respectively. Recoveries of cadmium and lead in several samples, measured by standard addition technique, proved also that this procedure is not affected by the matrix and can be applied satisfactorily for the determination of cadmium and lead in saline samples. The method was applied for the evaluation of the concentration of cadmium and lead in table salt samples consumed in Salvador City, Bahia, Brazil.

Simple hollow fiber renewal liquid membrane extraction method for pre-concentration of Cd(II) in environmental samples and detection by flame atomic absorption spectrometry.

PubMed

Carletto, Jeferson Schneider; Luciano, Raquel Medeiros; Bedendo, Gizelle Cristina; Carasek, Eduardo

2009-04-06

A hollow fiber renewal liquid membrane (HFRLM) extraction method to determine cadmium (II) in water samples using Flame Atomic Absorption Spectrometry (FAAS) was developed. Ammonium O,O-diethyl dithiophosphate (DDTP) was used to complex cadmium (II) in an acid medium to obtain a neutral hydrophobic complex (ML(2)). The organic solvent introduced to the sample extracts this complex from the aqueous solution and carries it over the poly(dimethylsiloxane) (PDMS) membrane, that had their walls previously filled with the same organic solvent. The organic solvent is solubilized inside the PDMS membrane, leading to a homogeneous phase. The complex strips the lumen of the membrane where, at higher pH, the complex Cd-DDTP is broken down and cadmium (II) is released into the stripping phase. EDTA was used to complex the cadmium (II), helping to trap the analyte in the stripping phase. A multivariate procedure was used to optimize the studied variables. The optimized variables were: sample (donor phase) pH 3.25, DDTP concentration 0.05% (m/v), stripping (acceptor phase) pH 8.75, EDTA concentration 1.5x10(-2) mol L(-1), extraction temperature 40 degrees C, extraction time 40 min, a solvent mixture N-butyl acetate and hexane (60/40%, v/v) with a volume of 100 microL, and addition of ammonium sulfate to saturate the sample. The sample volume used was 20 mL and the stripping volume was 165 microL. The analyte enrichment factor was 120, limit of detection (LOD) 1.3 microg L(-1), relative standard deviation (RSD) 5.5% and the working linear range 2-30 microg L(-1).

Determination of palladium, platinum and rhodium in used automobile catalysts and active pharmaceutical ingredients using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis

NASA Astrophysics Data System (ADS)

Resano, Martín; Flórez, María del Rosario; Queralt, Ignasi; Marguí, Eva

2015-03-01

This work investigates the potential of high-resolution continuum source graphite furnace atomic absorption spectrometry for the direct determination of Pd, Pt and Rh in two samples of very different nature. While analysis of active pharmaceutical ingredients is straightforward and it is feasible to minimize matrix effects, to the point that calibration can be carried out against aqueous standard solutions, the analysis of used automobile catalysts is more challenging requiring the addition of a chemical modifier (NH4F·HF) to help in releasing the analytes, a more vigorous temperature program and the use of a solid standard (CRM ERM®-EB504) for calibration. However, in both cases it was possible to obtain accurate results and precision values typically better than 10% RSD in a fast and simple way, while only two determinations are needed for the three analytes, since Pt and Rh can be simultaneously monitored in both types of samples. Overall, the methods proposed seem suited for the determination of these analytes in such types of samples, offering a greener and faster alternative that circumvents the traditional problems associated with sample digestion, requiring a small amount of sample only (0.05 mg per replicate for catalysts, and a few milligrams for the pharmaceuticals) and providing sufficient sensitivity to easily comply with regulations. The LODs achieved were 6.5 μg g- 1 (Pd), 8.3 μg g- 1 (Pt) and 9.3 μg g- 1 (Rh) for catalysts, which decreased to 0.08 μg g- 1 (Pd), 0.15 μg g- 1 (Pt) and 0.10 μg g- 1 (Rh) for pharmaceuticals.

Method development for the control determination of mercury in seafood by solid-sampling thermal decomposition amalgamation atomic absorption spectrometry (TDA AAS).

PubMed

Torres, D P; Martins-Teixeira, M B; Silva, E F; Queiroz, H M

2012-01-01

A very simple and rapid method for the determination of total mercury in fish samples using the Direct Mercury Analyser DMA-80 was developed. In this system, a previously weighted portion of fresh fish is combusted and the released mercury is selectively trapped in a gold amalgamator. Upon heating, mercury is desorbed from the amalgamator, an atomic absorption measurement is performed and the mercury concentration is calculated. Some experimental parameters have been studied and optimised. In this study the sample mass was about 100.0 mg. The relative standard deviation was lower than 8.0% for all measurements of solid samples. Two calibration curves against aqueous standard solutions were prepared through the low linear range from 2.5 to 20.0 ng of Hg, and the high linear range from 25.0 to 200.0 ng of Hg, for which a correlation coefficient better than 0.997 was achieved, as well as a normal distribution of the residuals. Mercury reference solutions were prepared in 5.0% v/v nitric acid medium. Lyophilised fish tissues were also analysed; however, the additional procedure had no advantage over the direct analysis of the fresh fish, and additionally increased the total analytical process time. A fish tissue reference material, IAEA-407, was analysed and the mercury concentration was in agreement with the certified value, according to the t-test at a 95% confidence level. The limit of quantification (LOQ), based on a mercury-free sample, was 3.0 µg kg(-1). This LOQ is in accordance with performance criteria required by the Commission Regulation No. 333/2007. Simplicity and high efficiency, without the need for any sample preparation procedure, are some of the qualities of the proposed method.

Extraction method based on emulsion breaking for the determination of Cu, Fe and Pb in Brazilian automotive gasoline samples by high-resolution continuum source flame atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Leite, Clarice C.; de Jesus, Alexandre; Kolling, Leandro; Ferrão, Marco F.; Samios, Dimitrios; Silva, Márcia M.

2018-04-01

This work reports a new method for extraction of Cu, Fe and Pb from Brazilian automotive gasoline and their determination by high-resolution continuous source flame atomic absorption spectrometry (HR-CS FAAS). The method was based on the formation of water-in-oil emulsion by mixing 2.0 mL of extraction solution constituted by 12% (w/v) Triton X-100 and 5% (v/v) HNO3 with 10 mL of sample. After heating at 90 °C for 10 min, two well-defined phases were formed. The bottom phase (approximately 3.5 mL), composed of acidified water and part of the ethanol originally present in the gasoline sample, containing the extracted analytes was analyzed. The surfactant and HNO3 concentrations and the heating temperature employed in the process were optimized by Doehlert design, using a Brazilian gasoline sample spiked with Cu, Fe and Pb (organometallic compounds). The efficiency of extraction was investigated and it ranged from 80 to 89%. The calibration was accomplished by using matrix matching method. For this, the standards were obtained performing the same extraction procedure used for the sample, using emulsions obtained with a gasoline sample free of analytes and the addition of inorganic standards. Limits of detection obtained were 3.0, 5.0 and 14.0 μg L-1 for Cu, Fe and Pb, respectively. These limits were estimated for the original sample taking into account the preconcentration factor obtained. The accuracy of the proposed method was assured by recovery tests spiking the samples with organometallic standards and the obtained values ranged from 98 to 105%. Ten gasoline samples were analyzed and Fe was found in four samples (0.04-0.35 mg L-1) while Cu (0.28 mg L-1) and Pb (0.60 mg L-1) was found in just one sample.

Circuit Board Analysis for Lead by Atomic Absorption Spectroscopy in a Course for Nonscience Majors

ERIC Educational Resources Information Center

Weidenhammer, Jeffrey D.

2007-01-01

A circuit board analysis of the atomic absorption spectroscopy, which is used to measure lead content in a course for nonscience majors, is being presented. The experiment can also be used to explain the potential environmental hazards of unsafe disposal of various used electronic equipments.

Transition metal atomic multiplets in the ligand K-edge x-ray absorption spectra and multiple oxidation states in the L2,3 emission of strongly correlated compounds

NASA Astrophysics Data System (ADS)

Jiménez-Mier, J.; Olalde-Velasco, P.; Yang, W.-L.; Denlinger, J.

2014-07-01

We present results that show that atomic multiplet ligand field calculations are in very good agreement with experimental x-ray absorption spectra at the L2,3 edge of transition metal (TM) di-fluorides (MF2, MCrCu). For chromium more than one TM oxidation state is needed to achieve such an agreement. We also show that signature of the TM atomic multiplet can be found at the pre-edge of the fluorine K-edge x-ray absorption spectra. TM atomic multiplet ligand field calculations with a structureless core hole show good agreement with the observed pre-edges in the experimental fluorine absorption spectra. Preliminary results for the comparison between calculated and experimental resonant x-ray emission spectra for nominal CrF2 with more than one oxidation state indicate the presence of three chromium oxidation states in the bulk.

Evaluation of zirconium as a permanent chemical modifier using synchrotron radiation and imaging techniques for lithium determination in sediment slurry samples by ET AAS.

PubMed

Flores, Araceli V; Pérez, Carlos A; Arruda, Marco A Z

2004-02-27

In the present paper, lithium was determined in river sediment using slurry sampling and electrothermal atomic absorption spectrometry (ET AAS) after L'vov platform coating with zirconium (as a permanent chemical modifier). The performance of this modifier and its distribution on the L'vov platform after different heating cycles were evaluated using synchrotron radiation X-ray fluorescence (SRXRF) and imaging scanning electron microscopy (SEM) techniques. The analytical conditions for lithium determination in river sediment slurries were also investigated and the best conditions were obtained employing 1300 and 2300 degrees C for pyrolysis and atomization temperatures, respectively. In addition, 100mg of sediment samples were prepared using 4.0moll(-1) HNO(3). The Zr-coating permitted lithium determination with good precision and accuracy after 480 heating cycles using the same platform for slurry samples. The sediment samples were collected from five different points of the Cachoeira river, São Paulo, Brazil. The detection and quantification limits were, respectively, 0.07 and 0.23mugl(-1).

Mercury concentrations in estuarine sediments, Lavaca and Matagorda bays, Texas, 1992

USGS Publications Warehouse

Brown, David S.; Snyder, Grant L.; Taylor, R. Lynn

1998-01-01

U.S. Environmental Protection Agency Method 7471 (Cold Vapor Atomic Absorption) was an acceptable analytical method for determining the total mercury concentrations in the Lavaca-Matagorda Bays estuarine sediment samples. Measurement of additional trace metals would aid in the characterization of total mercury concentrations and in the identification of concentrator/collector relations that are principally responsible for the adsorption of mercurous compounds to particulates in the bottom sediments.

Levels of dissolved zinc and cadmium in some surface waters of western Nigeria

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

Fatoki, O.S.

1993-12-31

Dissolved zinc and cadmium in some surface waters of Western Nigeria were separated and quantified using anion exchange of their chloro-complexes and detected by atomic absorption spectrophotometry. Concentrations of zinc and cadmium found in tested water samples ranged from 0.99 to 2.97 mg L{sup {minus}1} and 0.13 to 0.17 mg L{sup {minus}1}, respectively. 35 refs., 2 tabs.

Determination of trace heavy metals in soil and sediments by atomic spectrometry following preconcentration with Schiff bases on Amberlite XAD-4.

PubMed

Kara, Derya; Fisher, Andrew; Hill, Steve J

2009-06-15

A matrix separation and analyte preconcentration system using Amberlite XAD copolymer resins functionalized by Schiff base reactions coupled with atomic spectrometry has been developed. Three different functionalized Amberlite XAD resins were synthesized using 4-phenylthiosemicarbazide, 2,3-dihydroxybenzaldehyde and 2-thiophenecarboxaldehyde as reagents. These resins could be used to preconcentrate transition and other trace heavy metal analytes from nitric acid digests of soil and sediment samples. Analyte retention was shown to work well at pH 6.0. After treatment of the digests with sodium fluoride and buffering to pH 6, samples that contain extremely large concentrations of iron were analysed for trace analytes without the excess iron overloading the capacity of the resin. The analytes Cd, Co, Cu, Ni and Pb were preconcentrated from acid extracts of certified soil/sediment samples and then eluted with 0.1M HNO(3) directly to the detection system. Flame atomic absorption spectrometry was used as a means of detection during the studies. The efficiency of the chelating resin and the accuracy of the proposed method were evaluated by the analysis of soil (SO-2) and sediment (LGC 6157 and MESS-3) certified reference materials.

Flow injection determination of Se in dietary supplements using TiO2 mediated ultraviolet-photochemical volatile species generation

NASA Astrophysics Data System (ADS)

Nováková, E.; Linhart, O.; Červený, V.; Rychlovský, P.; Hraníček, J.

2017-08-01

This paper proposes a method for determination of selenium content in samples of dietary supplements using TiO2 mediated UV-photochemical vapor generation with quartz furnace atomic spectrometric detection. The flow-injection method was optimized for determination of selenium in the form of selenite or selenate ions. The limits of detection of the proposed method are 0.89 ng mL- 1 and 0.68 ng mL- 1 for selenite and selenate, respectively. Extraction in neutral medium was used for the leaching of selenate and NaOH solution was used for the leaching of selenite. The methods accuracy was verified against the declared amounts of Se in five different samples of over-the-counter dietary supplements and on NIST SRM 3280. The method was also compared to results achieved with determination by electrothermal atomization atomic absorption spectrometry following microwave decomposition. The recovery of selenium during sample preparation was tested by spiking the tablets prior to extraction and estimated to be approximately 100%. An interference study has been carried out to estimate the effect of concomitant elements on the methods accuracy.

On-line separation and preconcentration of lead(II) by solid-phase extraction using activated carbon loaded with xylenol orange and its determination by flame atomic absorption spectrometry.

PubMed

Ensafi, Ali A; Shiraz, A Zendegi

2008-02-11

Activated carbon loaded with xylenol orange in a mini-column was used for the highly selective separation and preconcentration of Pb(II) ions. An on-line system for enrichment and the determination of Pb(II) was carried out on flame atomic absorption spectrometry. The conditions of preconcentration and quantitative recovery of Pb(II) from diluted solution, such as pH of aqueous phase, amount of the sorbent, volume of the solutions and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, Pb(II) in an aqueous sample was concentrated about 200-fold and the detection limit was 0.4 ng mL(-1) Pb(II). The adsorption capacity of the solid phase was 0.20mg of lead per one gram of the modified activated carbon. The modified activated carbon is stable for several treatments of sample solutions without the need for using any chemical reagent. The recovery of lead(II) from river water, waste water, tap water, and in the following reference materials: SRM 2711 Montana soil and GBW-07605 tea were obtained in the range of 97-104% by the proposed method.

Preparation of modified magnetic nanoparticles as a sorbent for the preconcentration and determination of cadmium ions in food and environmental water samples prior to flame atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Mirabi, Ali; Dalirandeh, Zeinab; Rad, Ali Shokuhi

2015-05-01

A new method has been developed for the separation/preconcentration of trace level cadmium ions using diphenyl carbazone/sodium dodecyl sulfate immobilized on magnetic nanoparticle Fe3O4 as a new sorbent SPE and their determination by flame atomic absorption spectrometry (FAAS). Synthesized nanoparticle was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). Various influencing parameters on the separation and preconcentration of trace level cadmium ions such as, pH value, amount of nanoparticles, amount of diphenyl carbazone, condition of eluting solution, the effects of matrix ions were examined. The cadmium ions can be eluted from the modified magnetic nanoparticle using 1 mol L-1 HCl as a desorption reagent. The detection limit of this method for cadmium was 3.71 ng ml-1 and the R.S.D. was 0.503% (n=6). The advantages of this new method include rapidity, easy preparation of sorbents and a high concentration factor. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, green tea, rice, tobacco, carrot, lettuce, ginseng, spice, tap water, river water, sea water with satisfactory results.

Remote laser evaporative molecular absorption spectroscopy

NASA Astrophysics Data System (ADS)

Hughes, Gary B.; Lubin, Philip; Cohen, Alexander; Madajian, Jonathan; Kulkarni, Neeraj; Zhang, Qicheng; Griswold, Janelle; Brashears, Travis

2016-09-01

We describe a novel method for probing bulk molecular and atomic composition of solid targets from a distant vantage. A laser is used to melt and vaporize a spot on the target. With sufficient flux, the spot temperature rises rapidly, and evaporation of surface materials occurs. The melted spot creates a high-temperature blackbody source, and ejected material creates a plume of surface materials in front of the spot. Molecular and atomic absorption occurs as the blackbody radiation passes through the ejected plume. Bulk molecular and atomic composition of the surface material is investigated by using a spectrometer to view the heated spot through the ejected plume. The proposed method is distinct from current stand-off approaches to composition analysis, such as Laser-Induced Breakdown Spectroscopy (LIBS), which atomizes and ionizes target material and observes emission spectra to determine bulk atomic composition. Initial simulations of absorption profiles with laser heating show great promise for Remote Laser-Evaporative Molecular Absorption (R-LEMA) spectroscopy. The method is well-suited for exploration of cold solar system targets—asteroids, comets, planets, moons—such as from a spacecraft orbiting the target. Spatial composition maps could be created by scanning the surface. Applying the beam to a single spot continuously produces a borehole or trench, and shallow subsurface composition profiling is possible. This paper describes system concepts for implementing the proposed method to probe the bulk molecular composition of an asteroid from an orbiting spacecraft, including laser array, photovoltaic power, heating and ablation, plume characteristics, absorption, spectrometry and data management.

VUV absorption spectroscopy measurements of the role of fast neutral atoms in high-power gap breakdown

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

FILUK,A.B.; BAILEY,JAMES E.; CUNEO,MICHAEL E.

The maximum power achieved in a wide variety of high-power devices, including electron and ion diodes, z pinches, and microwave generators, is presently limited by anode-cathode gap breakdown. A frequently-discussed hypothesis for this effect is ionization of fast neutral atoms injected throughout the anode-cathode gap during the power pulse. The authors describe a newly-developed diagnostic tool that provides the first direct test of this hypothesis. Time-resolved vacuum-ultraviolet absorption spectroscopy is used to directly probe fast neutral atoms with 1 mm spatial resolution in the 10 mm anode-cathode gap of the SABRE 5 MV, 1 TW applied-B ion diode. Absorption spectramore » collected during Ar RF glow discharges and with CO{sub 2} gas fills confirm the reliability of the diagnostic technique. Throughout the 50--100 ns ion diode pulses no measurable neutral absorption is seen, setting upper limits of 0.12--1.5 x 10{sup 14} cm{sup {minus}3} for ground state fast neutral atom densities of H, C, N, O, F. The absence of molecular absorption bands also sets upper limits of 0.16--1.2 x 10{sup 15} cm{sup {minus}3} for common simple molecules. These limits are low enough to rule out ionization throughout the gap as a breakdown mechanism. This technique can now be applied to quantify the role of neutral atoms in other high-power devices.« less

Low loss liquid crystal photonic bandgap fiber in the near-infrared region

NASA Astrophysics Data System (ADS)

Scolari, Lara; Wei, Lei; Gauza, Sebastian; Wu, Shin-Tson; Bjarklev, Anders

2011-01-01

We infiltrate a perdeuterated liquid crystal with a reduced infrared absorption in a photonic crystal fiber. The H atoms of this liquid crystal were substituted with D atoms in order to move the vibration bands which cause absorption loss to longer wavelengths and therefore reduce the absorption in the spectral range of 1-2 μm. We achieve in the middle of the near-infrared transmission bandgap the lowest loss (about 1 dB) ever reported for this kind of devices.

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

USGS Publications Warehouse

Hageman, Philip L.

2007-01-01

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

HD 62542: Probing the Bare, Dense Core of an Interstellar Cloud

NASA Astrophysics Data System (ADS)

Welty, Daniel; Sonnentrucker, Paule G.; Rachford, Brian; Snow, Theodore; York, Donald G.

2018-01-01

We discuss the interstellar absorption from many atomic and molecular species seen in high-resolution HST/STIS UV spectra of the moderately reddened B3-5 V star HD 62542 [E(B-V) ~ 0.35; AV ~ 1.2]. This remarkable sight line exhibits both very steep far-UV extinction and a high fraction of hydrogen in molecular form -- with strong absorption from CH, C2, CN, and CO but weak absorption from CH+ and most of the commonly observed diffuse interstellar bands. Most of the material appears to reside in a single narrow velocity component -- thus offering a rare opportunity to probe the relatively dense, primarily molecular core of a single interstellar cloud, with little associated diffuse atomic gas.Detailed analyses of the absorption-line profiles seen in the UV spectra reveal a number of properties of the main diffuse molecular cloud toward HD 62542:1) The depletions of Mg, Si, and Fe are more severe than those seen in any other sight line, but the depletions of Cl and Kr are very mild; the overall pattern of depletions differs somewhat from those derived from larger samples of Galactic sight lines.2) The rotational excitation of H2 and C2 indicates that the gas is fairly cold (Tk = 40-45 K) and moderately dense (nH > 420 cm-3) somewhat higher densities are suggested by the fine-structure excitation of neutral carbon.3) The excitation temperatures characterizing the rotational populations of both 12CO (11.7 K) and 13CO (7.7 K) are higher than those typically found for Galactic diffuse molecular clouds.4) Carbon is primarily singly ionized -- N(C+) > N(CO) > N(C).5) The relative abundances of various trace neutral atomic species reflect the effects of both the steep far-UV extinction and the severe depletions of some elements.6) Differences in line widths for the various atomic and molecular species are suggestive of differences in spatial distribution within the main cloud.Support for this study was provided by NASA, via STScI grant GO-12277.008-A.

Selective determination of arsenic(III) and arsenic(V) with ammonium pyrrolidinedithiocarbamate, sodium diethyldithiocarbamate and dithizone by means of flameless atomic-absorption spectrophotometry with a carbon-tube atomizer.

PubMed

Kamada, T

The extraction behaviour of arsenic(III) and arsenic(V) with ammonium pyrrolidinedithiocarbamate, sodium diethyldithiocarbamate and dithizone in organic solvents has been investigated by means of nameless atomic-absorption spectrophotometry with a carbon-tube atomizer. The selective extraction of arsenic(III) and differential determination of arsenic(III) and arsenic(V) have been developed. With ammonium pyrrolidinedithiocarbamate and methyl isobutyl ketone or nitrobenzene, when the aqueous phase/solvent volume ratio is 5 and the injection volume in the carbon tube is 20 mul, the sensitivities for 1% absorption are 0.4 and 0.5 part per milliard of arsenic, respectively. The relative standard deviations are ca. 3%. Interference by many metal ions can be prevented by masking with EDTA. The proposed methods are applied satisfactorily for determination of As(III) and As(V) in various types of water.

Cold atomic hydrogen in the inner galaxy

NASA Technical Reports Server (NTRS)

Dickey, J. M.; Garwood, R. W.

1986-01-01

The VLA is used to measure 21 cm absorption in directions with the absolute value of b less than 1 deg., the absolute value of 1 less than 25 deg. to probe the cool atomic gas in the inner galaxy. Abundant H I absorption is detected; typical lines are deep and narrow, sometimes blending in velocity with adjacent features. Unlike 21 cm emission not all allowed velocities are covered: large portions of the l-v diagram are optically thin. Although not similar to H I emission, the absorption shows a striking correspondence with CO emission in the inner galaxy: essentially every strong feature detected in one survey is seen in the other. The provisional conclusion is that in the inner galaxy most cool atomic gas is associated with molecular cloud complexes. There are few or no cold atomic clouds devoid of molecules in the inner galaxy, although these are common in the outer galaxy.

Magnetic states of Mn and Co atoms at Co2MnGe/MgO interfaces seen via soft x-ray magnetic circular dichroism

NASA Astrophysics Data System (ADS)

Asakura, D.; Koide, T.; Yamamoto, S.; Tsuchiya, K.; Shioya, T.; Amemiya, K.; Singh, V. R.; Kataoka, T.; Yamazaki, Y.; Sakamoto, Y.; Fujimori, A.; Taira, T.; Yamamoto, M.

2010-11-01

The magnetic states of Mn and Co atoms in Co-rich Co2MnGe Heusler alloy thin films facing an MgO barrier were studied by means of soft x-ray magnetic circular dichroism (XMCD). In particular, the Co2MnGe film-thickness dependence of the Mn and Co magnetic moments was investigated. With a decrease in the Co2MnGe film thickness to 1-2 monolayers (MLs), the spin magnetic moment of Mn decreased and the MnL2,3 -edge x-ray absorption spectra (XAS) showed a Mn2+ -like multiplet structure in MnO, in contrast to samples thicker than 4 ML, indicating that the Mn atoms of the 1 and 2 ML samples were oxidized. The Co spin magnetic moment increased slightly with decreasing thickness. A Co2+ -like multiplet structure in CoO was not observed in all the CoL2,3 -edge XAS and XMCD, indicating that, even in the ultrathin samples, the Co atoms were not oxidized, and were more strongly spin polarized than those in the thicker samples. Co spin magnetic moments of 1.40-1.77μB larger than the theoretical value for ideal stoichiometric Co2MnGe (˜1μB) and the Co-rich film composition imply the presence of Co antisites that would lower the spin polarization.

X-ray absorption spectroscopic studies of the active sites of nickel- and copper-containing metalloproteins

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

Tan, Grace O.

1993-06-01

X-ray absorption spectroscopy (XAS) is a useful tool for obtaining structural and chemical information about the active sites of metalloproteins and metalloenzymes. Information may be obtained from both the edge region and the extended X-ray absorption fine structure (EXAFS) or post-edge region of the K-edge X-ray absorption spectrum of a metal center in a compound. The edge contains information about the valence electronic structure of the atom that absorbs the X-rays. It is possible in some systems to infer the redox state of the metal atom in question, as well as the geometry and nature of ligands connected to it,more » from the features in the edge in a straightforward manner. The EXAFS modulations, being produced by the backscattering of the ejected photoelectron from the atoms surrounding the metal atom, provide, when analyzed, information about the number and type of neighbouring atoms, and the distances at which they occur. In this thesis, analysis of both the edge and EXAFS regions has been used to gain information about the active sites of various metalloproteins. The metalloproteins studied were plastocyanin (Pc), laccase and nickel carbon monoxide dehydrogenase (Ni CODH). Studies of Cu(I)-imidazole compounds, related to the protein hemocyanin, are also reported here.« less

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

2017-09-01

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. Copyright © 2016 Elsevier GmbH. All rights reserved.

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

Molecular dynamics study of the interaction between nanoscale interstitial dislocation loops and grain boundaries in BCC iron

NASA Astrophysics Data System (ADS)

Gao, N.; Perez, D.; Lu, G. H.; Wang, Z. G.

2018-01-01

Atomic simulations are used to investigate the interaction between nanoscale interstitial dislocation loops and grain boundaries (GBs), the subsequent evolution of the GBs' structures, and the resulting impact on mechanical properties, in BCC iron. The interaction between loops and GBs - Σ 3 { 111 } and Σ 3 { 112 } - is affected by the angle (θ) between the Burgers vector and the normal to the GB plane, as well as by the distribution of free volume (FV) and stress. Loops can be totally absorbed by Σ 3 { 111 } boundaries, while the interaction with Σ 3 { 112 } boundaries is found to change the Burgers vector and habit plane after absorption, but to otherwise leave the loop intact, resulting in selective absorption. When θ =90o , no absorption occurs in Σ 3 { 112 } . The stress accumulation induced by the absorption affects the local mechanical properties of GBs. In nanocrystalline iron sample, a similar phenomenon is also observed, resulting in rearrangement of GBs and grain growth.

Tank 40 Final SB7b Chemical Characterization Results

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

Bannochie, C. J.

2012-11-06

A sample of Sludge Batch 7b (SB7b) was taken from Tank 40 in order to obtain radionuclide inventory analyses necessary for compliance with the Waste Acceptance Product Specifications (WAPS). The SB7b WAPS sample was also analyzed for chemical composition including noble metals and fissile constituents. At the Savannah River National Laboratory (SRNL) the 3-L Tank 40 SB7b sample was transferred from the shipping container into a 4-L high density polyethylene bottle and solids were allowed to settle over the weekend. Supernate was then siphoned off and circulated through the shipping container to complete the transfer of the sample. Following thoroughmore » mixing of the 3-L sample, a 558 g sub-sample was removed. This sub-sample was then utilized for all subsequent analytical samples. Eight separate aliquots of the slurry were digested, four with HNO{sub 3}/HCl (aqua regia) in sealed Teflon vessels and four with NaOH/Na{sub 2}O{sub 2} (alkali or peroxide fusion) using Zr crucibles. Two Analytical Reference Glass ? 1 (ARG-1) standards were digested along with a blank for each preparation. Each aqua regia digestion and blank was diluted to 1:100 mL with deionized water and submitted to Analytical Development (AD) for inductively coupled plasma ? atomic emission spectroscopy (ICP-AES) analysis, inductively coupled plasma ? mass spectrometry (ICP-MS) analysis, atomic absorption spectroscopy (AA) for As and Se, and cold vapor atomic absorption spectroscopy (CV-AA) for Hg. Equivalent dilutions of the alkali fusion digestions and blank were submitted to AD for ICP-AES analysis. Tank 40 SB7b supernate was collected from a mixed slurry sample in the SRNL Shielded Cells and submitted to AD for ICP-AES, ion chromatography (IC), total base/free OH{sup -}/other base, total inorganic carbon/total organic carbon (TIC/TOC) analyses, and Cs-137 gamma scan. Weighted dilutions of slurry were submitted for IC, TIC/TOC, and total base/free OH-/other base analyses. Activities for U-233, U-235, and Pu-239 were determined from the ICP-MS data for the aqua regia digestions of the Tank 40 WAPS slurry using the specific activity of each isotope. The Pu-241 value was determined from a Pu-238/-241 method.« less

Determination of As(III) and total inorganic As in water samples using an on-line solid phase extraction and flow injection hydride generation atomic absorption spectrometry.

PubMed

Sigrist, Mirna; Albertengo, Antonela; Beldoménico, Horacio; Tudino, Mabel

2011-04-15

A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH(3) generation using 3.5 mol L(-1) HCl as carrier solution and 0.35% (m/v) NaBH(4) in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl(-), SO(4)(2-), NO(3)(-), HPO(4)(2-), HCO(3)(-) on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C(6)H(8)O(6) solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 μg L(-1) and 0.6 μg L(-1) for As(III) and inorganic total As, respectively, were obtained for a 500 μL sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samplesh(-1). The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species separation was performed through the employ of a serial connection of membrane filters and anion-exchange cartridges. Advantages derived from this approach were evaluated. HPLC-ICPMS was employed to study the consistency of the analytical results. Copyright © 2011 Elsevier B.V. All rights reserved.

SPECIES DETERMINATION OF ORGANOMETALLIC COMPOUNDS USING ZEEMAN ATOMIC ABSORPTION SPECTROSCOPY WITH LIQUID CHROMATOGRAPHY

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

Koizumi, H.; Hadeishi, T.; McLaughlin, R.

1978-01-01

Over the past several years we have devised and expanded the capabilities of Zeeman atomic absorption spectroscopy (ZAA). Using this technique, trace elements in a complex matrix can be directly analyzed with high accuracy even when there is only one atom of interest contained in several million atoms of the host material. Quantities in the nanogram, or in some cases picogram, range can be determined within IS seconds for more than 30 elements. Because of its high selectivity and high sensitivity, ZAA can be used as a new technique for organometallic species determination by interfacing with a high pressure liquidmore » chromatograph (HPLC). The HPLC separates various molecular species. Different kinds of mobil solvents can be directly introduced in the ZAA detection system; even organic solvents or high concentration salt solutions. Then, organometallic species in the ppb range are separately detected according to their retention times. This technique has a much larger field of application than HPLC coupled with conventional AA. The advantages of the ZAA technique are described in a recent publication. In this case, a steady magnetic field at 11 kgauss is applied to the sample vapor perpendicular to the incident light beam. The difference in absorption of the polarized constituents P{perpendicular} and P{parallel} is proportional to the atomic density, but is not affected by the various kind of spectral interferences caused by thermal decomposition of the eluants. The recently developed HPLC technique has many advantages over gas chromatography. Nonvolatile, polar, thermally unstable molecules or high molecular weight compounds can be separated. In the present system, the main requirement is that the solute be soluble in the mobile solvent. A demonstration of the operation of this system is provided by the analysis of a mixture of vitamin B12 and Co(No{sub 3}){sub 2}. As shown in Figure 1, vitamin B12 has a Co in its functional center. Sample 1 contained Co of 0.813 {micro}g/ml in the vitamin B12 (cyanocobalamine form) and the Co of 25.0 {micro}g/ml that was introduced as Co (NO{sub 3}){sub 2}. Sample 2 contained only vitamin B12 at the same concentration as that in Sample 1. 0.5 ml of the sample was eluted with CH{sub 3}COONH{sub 4} [2 M] through an anion exchange column at a flow rate of 1.0 ml/min. and pressure of 20 kg/cm{sup 2}. The separation between vitamin B12 and Co (NO{sub 3}){sub 2} was confirmed by using UV absorption and coulmetry at the same time as shown in Figure 1. The upper and lower traces in Figure 1 show the signals from the coulometric detector and the UV absorption detector, respectively. The first peak in the lower trace shows the appearance of the vitamin B12 and the second peak in the upper trace of the Co (NO{sub 3}){sub 2}. After separation, the mobile solvent was directly introduced into a ZAA spectrophotometer by utilizing an automatic injector to measure the concentration of Co with time. For Sample 1, two Co concentration peaks were observed at the retention times of the vitamin B12 and Co (NO{sub 3}){sub 2} For sample 2, only one peak corresponding to vitamin B12 was observed. Next, fractions A, B, C, with retention times between 2-5, 5-8, 8-11 min., respectively, were collected for both Sample 1 and Sample 2. 10 {micro}l from each fraction of 3 ml was introduced into the ZAA spectrophotometer and the concentration of Co was measured at the wavelength of 240.7 nm. Table 1 shows the concentration of Co in each fraction. The concentration of Co bound to vitamin B12 could be obtained without interference even through the coexisting inorganic Co concentration was 30 times larger than that of Co in vitamin B12. From Fraction A of both Sample 1 and Sample 2, about 0.12 ppm of Co was detected. This result shows that about 90% of Co bound to vitamin B12 was recovered in this experiment. The Co of 0.007 ppm in Fraction B shows the background level of this system. From the Fraction C of Sample 1, a comparatively high concentration of Co (3.63 ppm) was detected. However, in the Fraction C of Sample 2, only 0.127 ppm of Co, which might be attributed to the contamination from the reagents and HPLC, was observed. From Table 1 we can safely conclude that the concentration of Co bound to the vitamin B12 molecule could be obtained without any interference with the comparatively high concentration coexisting inorganic Co. Also the concentration of the inorganic Co could be obtained separately from the Co in vitamin B12. Species determinations by the present technique have application to the field of biochemistry because many enzymes and coenzymes have a metal atom in their functional center. This type of analysis is also important in the envjronmental field because the toxicity of a metal depends upon its chemical form.« less

Atomic and molecular gas phase spectrometry

NASA Astrophysics Data System (ADS)

Winefordner, J. D.

1985-10-01

The major goals of this research have been to develop diagnostical spectroscopic methods for measuring spatial/temporal temperatures and species of combustion flames and plasmas and to develop sensitive, selective, precise, reliable, rapid spectrometric methods of trace analysis of elements present in jet engine lubricating oils, metallurgical samples, and engine exhausts. The diagnostical approaches have been based upon the measurement of metal probes introduced into the flame or plasmas and the measurement of OH in flames. The measurement approaches have involved the use of laser-excited fluorescence, saturated absorption, polarization, and linear absorption. The spatial resolution in most studies is less than 1 cu mm and the temporal resolution is less than 10 ns with the use of pulsed lasers. Single pulse temperature and species measurements have also been carried out. Other diagnostical studies have involved the measurement of collisional redistribution of radiatively excited levels of Na and Tl in acetylene/02/Ar flames and the measurement of lifetimes and quantum efficiencies of atoms and ions in the inductively coupled plasmas, ICP. The latter studies indicate that the high electron number densities in ICPs are not efficient quenchers of excited atoms/ions. Temperatures of microwave atmospheric plasmas produced capacitatively and cool metastable N2 discharge produced by a dielectric discharge have also been measured.

[Determination of sulfur in plant using a high-resolution continuum source atomic absorption spectrometer].

PubMed

Wang, Yu; Li, Jia-xi

2009-05-01

A method for the analysis of sulfur (S) in plant by molecular absorption of carbon monosulfide (CS) using a high-resolution continuum source atomic absorption spectrometer (CS AAS) with a fuel-rich air/acetylene flame has been devised. The strong CS absorption band was found around 258 nm. The half-widths of some absorption bands were of the order of picometers, the same as the common atomic absorption lines. The experimental procedure in this study provided optimized instrumental conditions (the ratio of acetylene to air, the burner height) and parameters, and researched the spectral interferences and chemical interferences. The influence of the organic solvents on the CS absorption signals and the different digestion procedures for the determination of sulfur were also investigated. The limit of detection achieved for sulfur was 14 mg x L(-1), using the CS wavelength of 257. 961 nm and a measurement time of 3 s. The accuracy and precision were verified by analysis of two plant standard reference materials. The major applications of this method have been used for the determination of sulfur in plant materials, such as leaves. Compared to the others, this method for the analysis of sulfur is rapid, easy and simple for sulfur determination in plant.

Efficient control of ultrafast optical nonlinearity of reduced graphene oxide by infrared reduction

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

Bhattachraya, S.; Maiti, R.; Das, A. C.

Simultaneous occurrence of saturable absorption nonlinearity and two-photon absorption nonlinearity in the same medium is well sought for the devices like optical limiter and laser mode-locker. Pristine graphene sheet consisting entirely of sp{sup 2}-hybridized carbon atoms has already been identified having large optical nonlinearity. However, graphene oxide (GO), a precursor of graphene having both sp{sup 2} and sp{sup 3}-hybridized carbon atom, is increasingly attracting cross-discipline researchers for its controllable properties by reduction of oxygen containing groups. In this work, GO has been prepared by modified Hummers method, and it has been further reduced by infrared (IR) radiation. Characterization of reducedmore » graphene oxide (RGO) by means of Raman spectroscopy, X-ray photoelectron spectroscopy, and UV-Visible absorption measurements confirms an efficient reduction with infrared radiation. Here, we report precise control of non-linear optical properties of RGO in femtosecond regime with increased degrees of IR reduction measured by open aperture z-scan technique. Depending on the intensity, both saturable absorption and two-photon absorption effects are found to contribute to the non-linearity of all the samples. Saturation dominates at low intensity (∼127 GW/cm{sup 2}) while two-photon absorption becomes prominent at higher intensities (from 217 GW/cm{sup 2} to 302 GW/cm{sup 2}). The values of two-photon absorption co-efficient (∼0.0022–0.0037 cm/GW for GO, and ∼0.0128–0.0143 cm/GW for RGO) and the saturation intensity (∼57 GW/cm{sup 2} for GO, and ∼194 GW/cm{sup 2} for RGO) increase with increasing reduction, indicating GO and RGO as novel tunable photonic devices. We have also explained the reason of tunable nonlinear optical properties by using amorphous carbon model.« less

Water-chemistry data for selected springs, geysers, and streams in Yellowstone National Park, Wyoming, 1999-2000

USGS Publications Warehouse

Ball, James W.; McCleskey, R. Blaine; Nordstrom, D. Kirk; Holloway, JoAnn M.; Verplanck, Philip L.; Sturtevant, Sabin A.

2002-01-01

Sixty-seven water analyses are reported for samples collected from 44 hot springs and their overflow drainages and two ambient-temperature acid streams in Yellowstone National Park (YNP) during 1990-2000. Thirty-seven analyses are reported for 1999, 18 for June of 2000, and 12 for September of 2000. These water samples were collected and analyzed as part of research investigations in YNP on microbially mediated sulfur oxidation in stream water, arsenic and sulfur redox speciation in hot springs, and chemical changes in overflow drainages that affect major ions, redox species, and trace elements. Most samples were collected from sources in the Norris Geyser Basin. Two ambient-temperature acidic stream systems, Alluvium and Columbine Creeks and their tributaries in Brimstone Basin, were studied in detail. Analyses were performed at or near the sampling site, in an on-site mobile laboratory truck, or later in a USGS laboratory, depending on stability of the constituent and whether or not it could be preserved effectively. Water temperature, specific conductance, pH, Eh, dissolved oxygen (D.O.), and dissolved H2S were determined on-site at the time of sampling. Alkalinity, acidity, and F were determined within a few days of sample collection by titration with acid, titration with base, and ion-selective electrode or ion chromatography (IC), respectively. Concentrations of S2O3 and SxO6 were determined as soon as possible (minutes to hours later) by IC. Concentrations of Br, Cl, NH4, NO2, NO3, SO4, Fe(II), and Fe(total) were determined within a few days of sample collection. Densities were determined later in the USGS laboratory. Concentrations of Li and K were determined by flame atomic absorption spectrometry. Concentrations of Al, As(total), B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe(total), K, Li, Mg, Mn, Na, Ni, Pb, Se, Si, Sr, V, and Zn were determined by inductively-coupled plasma-optical emission spectrometry. Trace concentrations of Cd, Cr, Cu, Pb, and Sb were determined by Zeeman-corrected graphitefurnace atomic-absorption spectrometry. Trace concentrations of As(total) and As(III) were determined by hydride generation atomic-absorption spectrometry using a flow-injection analysis system. Concentrations of Cl, NO3, Br, and SO4 were determined by IC. Concentrations of Fe(II) and Fe(total) were determined by the ferrozine colorimetric method. Concentrations of NO2 were determined by colorimetry using matrix-matched standards. Concentrations of NH4 were determined by IC, with reanalysis by colorimetry where separation of Na and NH4 peaks was poor. Dissolved organic carbon (DOC) concentrations were determined by the wet persulfate oxidation method.

Microwave absorption properties of carbon nanocoils coated with highly controlled magnetic materials by atomic layer deposition.

PubMed

Wang, Guizhen; Gao, Zhe; Tang, Shiwei; Chen, Chaoqiu; Duan, Feifei; Zhao, Shichao; Lin, Shiwei; Feng, Yuhong; Zhou, Lei; Qin, Yong

2012-12-21

In this work, atomic layer deposition is applied to coat carbon nanocoils with magnetic Fe(3)O(4) or Ni. The coatings have a uniform and highly controlled thickness. The coated nanocoils with coaxial multilayer nanostructures exhibit remarkably improved microwave absorption properties compared to the pristine carbon nanocoils. The enhanced absorption ability arises from the efficient complementarity between complex permittivity and permeability, chiral morphology, and multilayer structure of the products. This method can be extended to exploit other composite materials benefiting from its convenient control of the impedance matching and combination of dielectric-magnetic multiple loss mechanisms for microwave absorption applications.

Copper, lead and zinc concentrations of human breast milk as affected by maternal dietary practices

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

Umoren, J.; Kies, C.

1986-03-01

Maternal dietary practices have been found to affect the concentrations of some nutrients in human breast milk. Lead toxicity is a concern in young children. Lead, copper and zinc are thought to compete for intestinal absorption sites. The objective of the current project was to compare copper, lead and zinc contents of breast milk from practicing lacto-vegetarian and omnivore, lactating women at approximately four months post-partum. Analyses were done by atomic absorption spectrophotometry using a carbon rod attachment. Copper concentrations were higher in milk samples from lacto-ovo-vegetarians. Milk samples from the omnivores had the highest lead and zinc concentrations. Leadmore » and copper concentrations in milk were negatively correlated. The higher zinc concentrations in the milk of the omnivore women may have been related to better utilization of zinc from meat than from plant food sources.« less

Fundamental Studies on Donor-acceptor Conjugated Polymers Containing 'Heavy' Group 14 and Group 16 Elements

NASA Astrophysics Data System (ADS)

Gibson, Gregory Laird

One advantage of conjugated polymers as organic materials is that their properties may be readily tuned through covalent modifications. This thesis presents studies on the structure-property relationships resulting from single- and double-atom substitutions on an alternating donor-acceptor conjugated polymer. Specifically, single selenium and tellurium atoms have been incorporated into the acceptor monomer in place of sulfur; silicon and germanium atoms have been substituted in place of carbon at the donor monomer bridge position. The carbon-donor/ tellurium-acceptor polymer was synthesized by a post-polymerization reaction sequence and demonstrated the utility of heavy group 16 atoms to red shift a polymer absorption spectrum. Density functional theory calculations point to a new explanation for this result invoking the lower heavy atom ionization energy and reduced aromaticity of acceptor monomers containing selenium and tellurium compared to sulfur. Absorption and emission experiments demonstrate that both silicon and germanium substitutions in the donor slightly blue shift the polymer absorption spectrum. Polymers containing sulfur in the acceptor are the strongest light absorbers of all polymers studied here. Molecular weight and phenyl end capping studies show that molecular weight appears to affect polymer absorption to the greatest degree in a medium molecular weight regime and that these effects have a significant aggregation component. Solar cell devices containing either the silicon- or germanium-donor/selenium-acceptor polymer display improved red light harvesting or hole mobility relative to their structural analogues. Overall, these results clarify the effects of single atom substitution on donor-acceptor polymers and aid in the future design of polymers containing heavy atoms.

Tables showing analyses of semiquantitative spectrometry and atomic-absorption spectrophotometry of rock samples collected in the Ugashik, Bristol Bay, and western part of the Karluk quadrangles, Alaska

USGS Publications Warehouse

Wilson, Frederic H.; O'Leary, Richard M.

1987-01-01

The accompanying tables list chemical analyses of 337 rock samples that were collected in 1979, 1980, and 1981 in conjunction with geologic mapping in the Ugashik, Bristol Bay, and part of Karluk quadrangles. This work was conducted under the auspices of the Alaska Mineral Resource Assessment Program (AMRAP). This report is to accompany Wilson and O'Leary (1986) which inadvertently is missing most of the data tables listed here. Together the two reports contain the complete data from all samples collected for the Ugashik AMRAP.

Synthesis and characterization of Zn-Mg ferrite

NASA Astrophysics Data System (ADS)

Singh, Shailndra; Barbar, S. K.; Ram, Sahi

2018-05-01

The Zn-Mg ferrite sample of general formula Zn0.5Mg0.5Fe2O4 have been prepared by standard solid state reaction technique using high purity oxides. X-ray diffraction analysis shows the formation of a zinc-magnesium ferrite cubic phase at room temperature with space group Fd3m. FTIR spectra show two significant absorption bands first at 665.15 cm-1 corresponding to tetrahedral (A) and second band at 434 cm-1 corresponding to octahedral (B) sites of the spinel. Morphology of the sample determined by the SEM measurement and EDS analysis has confirmed the composition of atoms in the sample.

Platinum-group elements (Rh, Pt, Pd) and Au distribution in snow samples from the Kola Peninsula, NW Russia

NASA Astrophysics Data System (ADS)

Gregurek, Dean; Melcher, Frank; Niskavaara, Heikki; Pavlov, Vladimir A.; Reimann, Clemens; Stumpfl, Eugen F.

In April 1996 snowpack samples were collected from the surroundings of the ore roasting and dressing plant at Zapoljarnij and the nickel smelters at Nikel and Monchegorsk, Kola Peninsula, NW Russia. In the laboratory, filter residues of snowpack samples (fraction>0.45 μm) from 15 localities (close to the nickel processing centres) were chemically for precious metals (Rh, Pt, Pd, Au) and Te by graphite furnace atomic absorption spectrometry (GFAAS) analysis, and for Cu and Ni by ICP-MS. Values up to 2770 ng/l Pd, 650 ng/l Pt and 186 ng/l Au were found in the filter residues. Additionally, platinum-group elements (PGE) and Au contents in ore samples from Noril'sk , as well as in technogenic products ("Cu-Ni-feinstein" and copper concentrate) processed at the Monchegorsk smelter complex, were analysed using flameless atomic absorption spectroscopy (FAAS) for comparison with results obtained from snow. Rh, Pt, Pd and Au distribution data show the presence of two ore components (Noril'sk and Pechenga). Concentrations of these metals decrease with distance from the industrial sources and with the prevailing wind direction (generally north-south). Microscopic investigations and electron microprobe analysis of polished sections of snow filter residues (>0.45 μm) also reveal differences between particles from the two sources. To avoid confusion the term "Noril'sk" is used throughout the paper to denote material and/or data from the Noril'sk area and its sub-district, Noril'sk while Pechenga relates to the local ore.

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. Copyright © 2013 Elsevier B.V. All rights reserved.

Development of new portable miniaturize solid phase microextraction of silver-APDC complex using micropipette tip in-syringe system couple with electrothermal atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Naeemullah; Kazi, Tasneem Gul; Afridi, Hassan Imran; Shah, Faheem; Arain, Sadaf Sadia; Arain, Salma Aslam; Panhwar, Abdul Haleem; Arain, Mariam Shahzadi; Samoon, Muhammad Kashif

2016-02-01

An innovative and simple miniaturized solid phase microextraction (M-SPME) method, was developed for preconcentration and determination of silver(I) in the fresh and waste water samples. For M-SPME, a micropipette tip packed with activated carbon cloth (ACC) as sorbent, in a syringe system. The size, morphology and elemental composition of ACC before and after adsorption of analyte have been characterized by scanning electron microscopy and energy dispersive spectroscopy. The sample solution treated with a complexing reagent, ammonium pyrrolidine dithiocarbamate (APDC), was drawn into the syringe filled with ACC and dispensed manually for 2 to 10 aspirating/dispensing cycle. Then the Ag- complex sorbed on the ACC in micropipette was quantitatively eluted by drawing and dispensing of different concentrations of acids for 2 to 5 aspirating/dispensing cycles. The extracted Ag ions with modifier were injected directly into the electrothermal atomic absorption spectrometry for analysis. The influence of different variables on the extraction efficiency, including the concentration of ligand, pH, sample volume, eluent type, concentration and volume was investigated. Validity and accuracy of the developed method was checked by the standard addition method. Reliability of the proposed methodology was checked by the relative standard deviation (%RSD), which was found to be < 5%. Under the optimized experimental variables, the limits of detection (LOD) and enhancement factors (EF), were obtained to be 0.86 ng L- 1 and 120, respectively. The proposed method was successfully applied for the determination of trace levels of silver ions in fresh and waste water samples.

Selective and sensitive speciation analysis of Cr(VI) and Cr(III), at sub-μgL-1 levels in water samples by electrothermal atomic absorption spectrometry after electromembrane extraction.

PubMed

Tahmasebi, Zeinab; Davarani, Saied Saeed Hosseiny

2016-12-01

In this work, electromembrane extraction in combination with electrothermal atomic absorption spectrometry (ET-AAS) was investigated for speciation, preconcentration and quantification of Cr(VI) and Cr(III) in water samples through the selective complexation of Cr(VI) with 1,5-diphenylcarbazide (DPC) as a complexing agent. DPC reduces Cr(VI) to Cr(III) ions and then Cr(III) species are extracted based on electrokinetic migration of their cationic complex (Cr(III)-DPC) toward the negative electrode placed in the hollow fiber. Also, once oxidized to Cr(VI), Cr(III) ions in initial sample were determined by this procedure. The influence of extraction parameters such as pH, type of organic solvent, chelating agent concentration, stirring rate, extraction time and applied voltage were evaluated following a one-at-a-time optimization approach. Under optimized conditions, the extracted analyte was quantified by ETAAS, with an acceptable linearity in the range of 0.05-5ngmL -1 (R 2 value=0.996), and a repeatability (%RSD) between 3.7% and 12.2% (n=4) for 5.0 and 1.0ngmL -1 of Cr(VI), respectively. Also, we obtained an enrichment factor of 110 that corresponded to the recovery of 66%. The detection limit (S/N ratio of 3:1) was 0.02ngmL -1 . Finally, this new method was successfully employed to determine Cr(III) and Cr(VI) species in real water samples. Copyright © 2016. Published by Elsevier B.V.

A Simplified Digestion Protocol for the Analysis of Hg in Fish by Cold Vapor Atomic Absorption Spectroscopy

ERIC Educational Resources Information Center

Kristian, Kathleen E.; Friedbauer, Scott; Kabashi, Donika; Ferencz, Kristen M.; Barajas, Jennifer C.; O'Brien, Kelly

2015-01-01

Analysis of mercury in fish is an interesting problem with the potential to motivate students in chemistry laboratory courses. The recommended method for mercury analysis in fish is cold vapor atomic absorption spectroscopy (CVAAS), which requires homogeneous analyte solutions, typically prepared by acid digestion. Previously published digestion…

Improved hopcalite procedure for the determination of mercury vapor in air by flameless atomic absorption.

PubMed

Rathje, A O; Marcero, D H

1976-05-01

Mercury vapor is efficiently trapped from air by passage through a small glass tube filled with hopcalite. The hopcalite and adsorbed mercury are dissolved in a mixture of nitric and hydrochloric acids. Solution is rapid and complete, with no loss of mercury. Analysis is completed by flameless atomic absorption.

Interstellar photoelectric absorption cross sections, 0.03-10 keV

NASA Technical Reports Server (NTRS)

Morrison, R.; Mccammon, D.

1983-01-01

An effective absorption cross section per hydrogen atom has been calculated as a function of energy in the 0.03-10 keV range using the most recent atomic cross section and cosmic abundance data. Coefficients of a piecewise polynomial fit to the numerical results are given to allow convenient application in automated calculations.

Direct Electrothermal Atomic Absorption Determination of Trace Elements in Body Fluids (Review)

NASA Astrophysics Data System (ADS)

Zacharia, A. N.; Arabadji, M. V.; Chebotarev, A. N.

2017-03-01

This review is focused on the state and development of tendencies of electrothermal atomic absorption spectroscopy over the last 25 years (from 1990 to 2016) in the direct determination of Cu, Zn, Pb, Cd, Mn, Se, As, Cr, Co, Ni, Al, and Hg in body fluids such as blood, urine, saliva, and breast milk.

Au Colloids Formed by Ion Implantation in Muscovite Mica Studied by Vibrational and Electronic Spectroscopes and Atomic Force Microscopy

NASA Technical Reports Server (NTRS)

Tung, Y. S.; Henderson, D. O.; Mu, R.; Ueda, A.; Collins, W. E.; White, C. W.; Zuhr, R. A.; Zhu, Jane G.

1997-01-01

Au was implanted into the (001) surface of Muscovite mica at an energy of 1.1 MeV and at doses of 1, 3, 6, and 10 x 10(exp 16) ions/cu cm. Optical spectra of the as-implanted samples revealed a peak at 2.28 eV (545 nm) which is attributed to the surface plasmon absorption of Au colloids. The infrared reflectance measurements show a decreasing reflectivity with increasing ion dose in the Si-O stretching region (900-1200 /cm). A new peak observed at 967 /cm increases with the ion dose and is assigned to an Si-O dangling bond. Atomic force microscopy images of freshly cleaved samples implanted with 6 and 10 x 10(exp 16) ions/sq cm indicated metal colloids with diameters between 0.9- 1.5 nm. AFM images of the annealed samples showed irregularly shaped structures with a topology that results from the fusion of smaller colloids.

Substrate temperature effect on the structural anisotropy in amorphous Tb-Fe films

NASA Astrophysics Data System (ADS)

Harris, V. G.; Hellman, F.; Elam, W. T.; Koon, N. C.

1993-05-01

Using extended x-ray absorption fine structures (EXAFS) measurements we have investigated the atomic environment around the Fe atom in a series of amorphous Tb0.26Fe0.74 films having different magnetic anisotropy energies owing to different deposition temperatures. The polarization properties of synchrotron radiation allowed the separate study of structure parallel and perpendicular to the sample plane. An anisotropy between these two structures was observed. Modeling results indicate this anisotropy is due to anisotropic pair correlations where the Fe-Fe pairs are statistically preferred in-plane and the Fe-Tb pairs out-of-plane. The amplitude of this anisotropy scales with both the substrate temperature and the magnetic anisotropy energy. A ≊1% in-plane compression of the Fe-Fe distance was measured between the in-plane and out-of-plane structure of the sample grown at 77 K. This sample had no detectable local chemical anisotropy suggesting that intrinsic stress plays an important role in determining its magnetic anisotropy.

Electronic structure study of Ce1-xAxO2 (A = Zr & Hf) nanoparticles: NEXAFS and EXAFS investigations.

PubMed

Sharma, Aditya; Varshney, Mayora; Shin, Hyun-Joon; Park, Yong Jun; Kim, Min-Gyu; Ha, Tae-Kyun; Chae, Keun Hwa; Gautam, Sanjeev

2014-10-07

Single phase nanoparticles (NPs) of CeO2, Ce0.5Zr0.5O2, Ce0.5Hf0.5O2 and Ce0.5Hf0.25Zr0.25O2 were successfully synthesized by co-precipitation method at constant pH and temperature. The X-ray diffraction results revealed that the additive atoms did not segregate to form secondary phases but led to grain size variation in the NPs. The 10 Dq values in the near edge X-ray absorption fine structure (NEXAFS) spectra at the O K-edge did not vary in the same way as the average grain size was changed for the doped CeO2 NPs. The deconvolution of Ce M5-edge and detailed analysis of O K pre-edge peak have shown the higher Ce(+3)/(Ce(+3) + Ce(+4)) ratio in the Zr- and Hf-doped samples. The local atomic structure around the Ce, Zr and Hf atoms was investigated using extended X-ray absorption fine structure (EXAFS) spectroscopy at Ce K-edge, Zr K-edge and Hf L3-edge, respectively, and the EXAFS data were fitted with the theoretical calculations. The 4f occupancy, Ce(+3)/(Ce(+3) + Ce(+4)) ratio of Ce ions, coordination number of Ce and Ce-Ce/Ce-O bond distances were sensitive to the additive atoms but not explicitly changed according to the grain size variation in the NPs.

Application of blood cadmium determination to industry using a punched disc technique.

PubMed Central

Cernik, A A; Sayers, M P

1975-01-01

A paper disc flameless atomic absorption spectroscopy (AAS) method is described for the determination of cadmium (Cd) in blood, enabling difficulties in sample preparation to be minimized. By control of the ashing step the matrix can be removed without loss of cadmium. Problems with the fast signal response during atomization can be met by spectral band width and temperature control. At the 106 pg level (471 nmol Cd/1 blood; 5-3 mug/100 ml) the relative standard deviation (RSD) was 0-06. Results in four industrial situations are reported. This description of the method should facilitate further investigation of its application to industry using capillary or venous blood. PMID:1131342

Multivessel system for cold-vapor mercury generation. Determination of mercury in hair and fish.

PubMed

Boaventura, G R; Barbosa, A C; East, G A

1997-01-01

A multivessel system for the determination of mercury (Hg) by cold-vapor atomic absorption spectrometry (CV-AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) was developed. The performance of the proposed device was tested by determining total Hg in quality-control samples of hair and fishes following acid digestion. Application of the apparatus to the determination of Hg by CV-AAS following alkaline digestion was studied as well. The detection limit obtained for CV-AAS was 0.11 ng/mL and for ICP-AES 1.39 ng/mL. The results show that the system is appropriate to be used in techniques involving cold-vapor generation of Hg.

Forced-flow chromatographic determination of calcium and magnesium with continuous spectrophotometric detection

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

Arguello, M.D.

1977-12-01

Modifications to the forced-flow chromatograph include a flow-through pH monitor to continuously monitor the pH of the final effluent and an active low-pass filter to eliminate noise in the spectrophotometric detector. All separations are performed using partially sulfonated XAD-2 as the ion exchanger. Elution of calcium and magnesium is accomplished using ammonium chloride and ethylenediammonium chloride solutions. Calcium and magnesium are detected by means of Arsenazo I and PAR-ZnEDTA color-forming reagents. Other metal ions are detected by means of PAR and Chromazurol S color-forming reagents. Calcium and magnesium distribution coefficients on partially sulfonated XAD-2 as functions of ammonium chloride andmore » ethylenediammonium chloride concentration are given together with distribution coefficients of other metal ions. Methods for the selective elution of interfering metal ions prior to the elution of calcium and magnesium are described. Beryllium and aluminum are selectively eluted with sulfosalicylic acid. Those elements forming anionic chloride complexes are selectively eluted with HCl-acetone. Nickel is selectively eluted with HCl-acetone-dimethylglyoxime. Synthetic samples containing calcium and magnesium, both alone and in combination with alkali metals, strontium, barium, beryllium, aluminum, transition metals, and rare earths, are analyzed. Hard water samples are analyzed for calcium and magnesium and the results compared to those obtained by EDTA titration, atomic absorption spectroscopy, and plasma emission spectroscopy. Several clinical serum samples are analyzed for calcium and magnesium and the results compared to those obtained by atomic absorption spectroscopy.« less