icp atomic emission: Topics by Science.gov

Sample records for icp atomic emission

Comparison of analytical performances of inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry for trace analysis of bismuth and bismuth oxide

NASA Astrophysics Data System (ADS)

Medvedev, Nickolay S.; Shaverina, Anastasiya V.; Tsygankova, Alphiya R.; Saprykin, Anatoly I.

2018-04-01

The paper presents а comparison of analytical performances of inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) for trace analysis of high purity bismuth and bismuth oxide. Matrix effects in the ICP-MS and ICP-AES methods were studied as a function of Bi concentration, ICP power and nebulizer flow rate. For ICP-MS the strong dependence of the matrix effects versus the atomic mass of analytes was observed. For ICP-AES the minimal matrix effects were achieved for spectral lines of analytes with low excitation potentials. The optimum degree of sample dilution providing minimum values of the limits of detection (LODs) was chosen. Both methods let us to reach LODs from n·10-7 to n·10-4 wt% for more than 50 trace elements. For most elements the LODs of ICP-MS were lower in comparison to ICP-AES. Validation of accuracy of the developed techniques was performed by "added-found" experiments and by comparison of the results of ICP-MS and ICP-AES analysis of high-purity bismuth oxide.
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.
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.
Ultra-Shallow Depth Profiling of Arsenic Implants in Silicon by Hydride Generation-Inductively Coupled Plasma Atomic Emission Spectrometry

NASA Astrophysics Data System (ADS)

Matsubara, Atsuko; Kojima, Hisao; Itoga, Toshihiko; Kanehori, Keiichi

1995-08-01

High resolution depth profiling of arsenic (As) implanted into silicon wafers by a chemical technique is described. Silicon wafers are precisely etched through repeated oxidation by hydrogen peroxide solution and dissolution of the oxide by hydrofluoric acid solution. The etched silicon thickness is determined by inductively-coupled plasma atomic emission spectrometry (ICP-AES). Arsenic concentration is determined by hydride generation ICP-AES (HG-ICP-AES) with prereduction using potassium iodide. The detection limit of As in a 4-inch silicon wafer is 2.4×1018 atoms/cm3. The etched silicon thickness is controlled to less than 4±2 atomic layers. Depth profiling of an ultra-shallow As diffusion layer with the proposed method shows good agreement with profiling using the four-probe method or secondary ion mass spectrometry.
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.
Boron detection from blood samples by ICP-AES and ICP-MS during boron neutron capture therapy.

PubMed

Linko, S; Revitzer, H; Zilliacus, R; Kortesniemi, M; Kouri, M; Savolainen, S

2008-01-01

The concept of boron neutron capture therapy (BNCT) involves infusion of a (10)B containing tracer into the patient's bloodstream followed by local neutron irradiation(s). Accurate estimation of the blood boron level for the treatment field before irradiation is required. Boron concentration can be quantified by inductively coupled plasma atomic emission spectrometry (ICP-AES), mass spectrometry (ICP-MS), spectrofluorometric and direct current atomic emission spectrometry (DCP-AES) or by prompt gamma photon detection methods. The blood boron concentrations were analysed and compared using ICP-AES and ICP-MS to ensure congruency of the results if the analysis had to be changed during the treatment, e.g. for technical reasons. The effect of wet-ashing on the results was studied in addition. The mean of all samples analysed with ICP-MS was 5.8 % lower than with ICP-AES coupled to wet-ashing (R (2) = 0.88). Without wet-ashing, the mean of all samples analysed with ICP-MS was 9.1 % higher than with ICP-AES (R (2) = 0.99). Boron concentration analysed from whole blood samples with ICP-AES correlated well with the values of ICP-MS with wet-ashing of the sample matrix, which is generally considered the reference method. When using these methods in parallel at certain intervals during the treatments, reliability of the blood boron concentration values remains satisfactory, taking into account the required accuracy of dose determination in the irradiation of cancer patients.
Spectroscopic Characteristic and Analytical Capability of Ar-N₂ Inductively Coupled Plasma in Axially Viewing Optical Emission Spectrometry.

PubMed

Ohata, Masaki

2016-01-01

The spectroscopic characteristics and analytical capability of argon-nitrogen (Ar-N2) inductively coupled plasma (ICP) in axially viewing optical emission spectrometry (OES) were examined and figures of merit were determined in the present study. The spectroscopic characteristics such as the emission intensity profile and the excitation temperature observed from the analytical zone of Ar-N2 ICP in axially viewing ICPOES, in order to elucidate the enhancement of the emission intensity of elements obtained in our previous study, were evaluated and compared to those of the standard ICP. The background and emission intensities of elements as well as their excitation behavior for both atom and ion lines were also examined. As results, a narrower emission intensity profile and an increased excitation temperature as well as enhancements for both background and emission intensities of elements, which could be due to the ICP shrunken as well as the enhancement of the interaction between the central channel of the ICP and samples introduced, were observed for Ar-N2 ICP in axially viewing OES. In addition, the elements with relatively higher excitation and ionization energies such as As, Bi, Cd, Ni, P, and Zn revealed larger enhancements of the emission intensities as well as improved limits of detection (LODs), which were also attributed to the enhanced interaction between Ar-N2 ICP and the samples. Since the Ar-N2 ICP could be obtained easily only by the addition of a small amount of N2 gas to the Ar plasma gas of the standard ICP and no optimization on the alignment between Ar-N2 ICP and the spectrometer in commercially available ICPOES instruments was needed, it could be utilized as simple and optional excitation and ionization sources in axially viewing ICPOES.
Exploration geochemical technique for the determination of preconcentrated organometallic halides by ICP-AES

USGS Publications Warehouse

Motooka, J.M.

1988-01-01

An atomic absorption extraction technique which is widely used in geochemical exploration for the determination of Ag, As, Au, Bi, Cd, Cu, Mo, Pb, Sb, and Zn has been modified and adapted to a simultaneous inductively coupled plasma-atomic emission instrument. the experimental and operating parameters are described for the preconcentration of the metals into their organometallic halides and for the determination of the metals. Lower limits of determination are equal to or improved over those for flame atomic absorption (except Au) and ICP results are very similar to the accepted AA values, with precision for the ICP data in excess of that necessary for exploration purposes.
Spectral emission from the alkali inductively-coupled plasma: Theory and experiment

NASA Astrophysics Data System (ADS)

Bazurto, R.; Huang, M.; Camparo, J.

2018-04-01

The weakly-ionized, alkali inductively-coupled plasma (ICP) has a long history as the light source for optical pumping. Today, its most significant application is perhaps in the rubidium atomic frequency standard (RAFS), arguably the workhorse of atomic timekeeping in space, where it is crucial to the RAFS' functioning and performance (and routinely referred to as the RAFS' "rf-discharge lamp"). In particular, the photon flux from the lamp determines the signal-to-noise ratio of the device, and variations in ICP brightness define the long-term frequency stability of the atomic clock as a consequence of the ac-Stark shift (i.e., the light-shift). Given the importance of Rb atomic clocks to diverse satellite navigation systems (e.g., GPS, Galileo, BeiDou) - and thereby the importance of alkali ICPs to these systems - it is somewhat surprising to find that the physical processes occurring within the discharge are not well understood. As a consequence, researchers do not understand how to improve the spectral emission from the lamp except at a trial-and-error level, nor do they fully understand the nonlinear mechanisms that result in ICP light instability. Here, we take a first step in developing an intuitive, semi-quantitative model of the alkali rf-discharge lamp, and we perform a series of experiments to validate the theory's predictions.
Analytical performance of a low-gas-flow torch optimized for inductively coupled plasma atomic emission spectrometry

USGS Publications Warehouse

Montaser, A.; Huse, G.R.; Wax, R.A.; Chan, S.-K.; Golightly, D.W.; Kane, J.S.; Dorrzapf, A.F.

1984-01-01

An inductively coupled Ar plasma (ICP), generated in a lowflow torch, was investigated by the simplex optimization technique for simultaneous, multielement, atomic emission spectrometry (AES). The variables studied included forward power, observation height, gas flow (outer, intermediate, and nebulizer carrier) and sample uptake rate. When the ICP was operated at 720-W forward power with a total gas flow of 5 L/min, the signal-to-background ratios (S/B) of spectral lines from 20 elements were either comparable or inferior, by a factor ranging from 1.5 to 2, to the results obtained from a conventional Ar ICP. Matrix effect studies on the Ca-PO4 system revealed that the plasma generated in the low-flow torch was as free of vaporizatton-atomizatton interferences as the conventional ICP, but easily ionizable elements produced a greater level of suppression or enhancement effects which could be reduced at higher forward powers. Electron number densities, as determined via the series until line merging technique, were tower ht the plasma sustained in the low-flow torch as compared with the conventional ICP. ?? 1984 American Chemical Society.
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.
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.
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...
Effects of liquid chromatography mobile phases and buffer salts on phosphorus inductively coupled plasma atomic emission and mass spectrometries utilizing ultrasonic nebulization and membrane desolvation.

PubMed

Carr, John E; Kwok, Kaho; Webster, Gregory K; Carnahan, Jon W

2006-01-23

Atomic spectrometry, specifically inductively coupled plasma atomic emission spectrometry (ICP-AES) and mass spectrometry (ICP-MS) show promise for heteroatom-based detection of pharmaceutical compounds. The combination of ultrasonic nebulization (USN) with membrane desolvation (MD) greatly enhances detection limits with these approaches. Because pharmaceutical analyses often incorporate liquid chromatography, the study herein was performed to examine the effects of solvent composition on the analytical behaviors of these approaches. The target analyte was phosphorus, introduced as phosphomycin. AES response was examined at the 253.7 nm atom line and mass 31 ions were monitored for the MS experiments. With pure aqueous solutions, detection limits of 5 ppb (0.5 ng in 0.1 mL injection volumes) were obtained with ICP-MS. The ICP-AES detection limit was 150 ppb. Solvent compositions were varied from 0 to 80% organic (acetonitrile and methanol) with nine buffers at concentrations typically used in liquid chromatography. In general, solvents and buffers had statistically significant, albeit small, effects on ICP-AES sensitivities. A few exceptions occurred in cases where typical liquid chromatography buffer concentrations produced higher mass loadings on the plasma. Indications are that isocratic separations can be reliably performed. Within reasonable accuracy tolerances, it appears that gradient chromatography can be performed without the need for signal response normalization. Organic solvent and buffer effects were more significant with ICP-MS. Sensitivities varied significantly with different buffers and organic solvent content. In these cases, gradient chromatography will require careful analytical calibration as solvent and buffer content is varied. However, for most buffer and solvent combinations, signal and detection limits are only moderately affected. Isocratic separations and detection are feasible.
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...
Final report on CCQM-K125: elements in infant formula

NASA Astrophysics Data System (ADS)

Merrick, J.; Saxby, D.; Dutra, E. S.; Sena, R. C.; Araújo, T. O.; Almeida, M. D.; Yang, L.; Pihillagawa, I. G.; Mester, Z.; Sandoval, S.; Wei, C.; Castillo, M. E. D.; Oster, C.; Fisicaro, P.; Rienitz, O.; Pape, C.; Schulz, U.; Jährling, R.; Görlitz, V.; Lampi, E.; Kakoulides, E.; Sin, D. W. M.; Yip, Y. C.; Tsoi, Y. T.; Zhu, Y.; Okumu, T. O.; Yim, Y. H.; Heo, S. W.; Han, M.; Lim, Y.; Osuna, M. A.; Regalado, L.; Uribe, C.; Buzoianu, M. M.; Duta, S.; Konopelko, L.; Krylov, A.; Shin, R.; Linsky, M.; Botha, A.; Magnusson, B.; Haraldsson, C.; Thiengmanee, U.; Klich, H.; Can, S. Z.; Coskun, F. G.; Tunc, M.; Entwisle, J.; O'Reilly, J.; Hill, S.; Goenaga-Infante, H.; Winchester, M.; Rabb, S. A.; Pérez, R.

2017-01-01

CCQM-K125 was organized by the Inorganic Analysis Working Group (IAWG) of CCQM to assess and document the capabilities of the national metrology institutes (NMIs) or the designated institutes (DIs) to measure the mass fractions of trace elements (K, Cu and I) in infant formula. Government Laboratory, Hong Kong SAR (GLHK) acted as the coordinating laboratory. In CCQM-K125, 25 institutes submitted the results for potassium, 24 institutes submitted the results for copper and 8 institutes submitted the results for iodine. For examination of potassium and copper, most of the participants used microwave-assisted acid digestion methods for sample dissolution. A variety of instrumental techniques including inductively coupled plasma mass spectrometry (ICP-MS), isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS), inductively coupled plasma optical emission spectrometry (ICP-OES), atomic absorption spectrometry (AAS), flame atomic emission spectrometry (FAES) and microwave plasma atomic emission spectroscopy (MP-AES) were employed by the participants for determination. For analysis of iodine, most of the participants used alkaline extraction methods for sample preparation. ICP-MS and ID-ICP-MS were used by the participants for the determination. Generally, the participants' results of CCQM-K125 were found consistent for all measurands according to their equivalence statements. Except with some extreme values, most of the participants obtained the values of di/U(di) within +/- 1 for the measurands. Main text To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).
Methods for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry

DOEpatents

Chan, George C. Y. [Bloomington, IN; Hieftje, Gary M [Bloomington, IN

2010-08-03

A method for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry (ICP-AES). ICP-AES analysis is performed across a plurality of selected locations in the plasma on an unknown sample, collecting the light intensity at one or more selected wavelengths of one or more sought-for analytes, creating a first dataset. The first dataset is then calibrated with a calibration dataset creating a calibrated first dataset curve. If the calibrated first dataset curve has a variability along the location within the plasma for a selected wavelength, errors are present. Plasma-related errors are then corrected by diluting the unknown sample and performing the same ICP-AES analysis on the diluted unknown sample creating a calibrated second dataset curve (accounting for the dilution) for the one or more sought-for analytes. The cross-over point of the calibrated dataset curves yields the corrected value (free from plasma related errors) for each sought-for analyte.
U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION, AND MAINTENANCE OF THE JOBIN-YVON MODEL 70 INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETER (BCO-L-7.1)

EPA Science Inventory

The purpose of this SOP is to detail the operation and maintenance of an Instruments, SA Inc., Jobin-Yvon Model 70 (JY-70) inductively coupled plasma atomic emissions spectrometry (ICP-AES). This procedure was followed to ensure consistent data retrieval during the Arizona NHEXA...
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.
Analysis of high-purity germanium dioxide by ETV-ICP-AES with preliminary concentration of trace elements.

PubMed

Medvedev, Nickolay S; Shaverina, Anastasiya V; Tsygankova, Alphiya R; Saprykin, Anatoly I

2016-08-01

The paper presents a combined technique of germanium dioxide analysis by inductively coupled plasma atomic emission spectrometry (ICP-AES) with preconcentration of trace elements by distilling off matrix and electrothermal (ETV) introduction of the trace elements concentrate into the ICP. Evaluation of metrological characteristics of the developed technique of high-purity germanium dioxide analysis was performed. The limits of detection (LODs) for 25 trace elements ranged from 0.05 to 20ng/g. The accuracy of proposed technique is confirmed by "added-found" («or spiking») experiment and comparing the results of ETV-ICP-AES and ICP-AES analysis of high purity germanium dioxide samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Lead isotope ratios in lichen samples evaluated by ICP-ToF-MS to assess possible atmospheric pollution sources in Havana, Cuba.

PubMed

Alvarez, Alfredo Montero; Estévez Alvarez, Juan R; do Nascimento, Clístenes Williams Araújo; González, Iván Pupo; Rizo, Oscar Díaz; Carzola, Lázaro Lima; Torres, Roberto Ayllón; Pascual, Jorge Gómez

2017-01-01

Epiphytic lichens, collected from 119 sampling sites grown over "Roistonea Royal Palm" trees, were used to assess the spatial distribution pattern of lead (Pb) and identify possible pollution sources in Havana (Cuba). Lead concentrations in lichens and topsoils were determined by flame atomic absorption spectrophotometry and inductively coupled plasma (ICP) atomic emission spectrometry, respectively, while Pb in crude oils and gasoline samples were measured by ICP-time of flight mass spectrometry (ICP-ToF-MS). Lead isotopic ratios measurements for lichens, soils, and crude oils were obtained by ICP-ToF-MS. We found that enrichment factors (EF) reflected a moderate contamination for 71% of the samples (EF > 10). The 206 Pb/ 207 Pb ratio values for lichens ranged from 1.17 to 1.20 and were a mixture of natural radiogenic and industrial activities (e.g., crude oils and fire plants). The low concentration of Pb found in gasoline (<7.0 μg L -1 ) confirms the official statement that leaded gasoline is no longer used in Cuba.
Preparation And Analysis Of Specimens Of Ablative Materials

NASA Technical Reports Server (NTRS)

Solomon, William C.

1994-01-01

Procedure for chemical analysis of specimens of silicone-based ablative thermal-insulation materials SLA-561 and MA25 involves acid digestion of specimens to prepare them for analysis by inductively-coupled-plasma/atomic-emission spectroscopy (ICP/AES). In comparison with atomic-absorption spectroscopy (AAS), ICP/AES is faster and more accurate than AAS. Results of analyses stored in data base, used to trace variations in concentrations of chemical elements in materials during long-term storage, and used in timely manner in investigations of failures. Acid-digestion portion of procedure applied to other thermal-insulation materials containing room-temperature-vulcanizing silicones and enables instrumental analysis of these materials.
Environmental Indicators of Metal Pollution and Emission: An Experiment for the Instrumental Analysis Laboratory

ERIC Educational Resources Information Center

Bowden, John A.; Nocito, Brian A.; Lowers, Russell H.; Guillette, Louis J., Jr.; Williams, Kathryn R.; Young, Vaneica Y.

2012-01-01

This experiment enlightens students on the use of environmental indicators and inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and demonstrates the ability of these monitoring tools to measure metal deposition in environmental samples (both as a result of lab-simulated and real events). In this two-part study, the initial…
Development of Desolvation System for Single-cell Analysis Using Droplet Injection Inductively Coupled Plasma Atomic Emission Spectroscopy.

PubMed

Ishihara, Yukiko; Aida, Mari; Nomura, Akito; Miyahara, Hidekazu; Hokura, Akiko; Okino, Akitoshi

2015-01-01

With a view to enhance the sensitivity of analytical instruments used in the measurement of trace elements contained in a single cell, we have now equipped the previously reported micro-droplet injection system (M-DIS) with a desolvation system. This modified M-DIS was coupled to inductively coupled plasma atomic emission spectroscopy (ICP-AES) and evaluated for its ability to measure trace elements. A flow rate of 100 mL/min for the additional gas and a measurement point -7.5 mm above the load coil (ALC) have been determined to be the optimal parameters for recording the emission intensity of the Ca(II) spectral lines. To evaluate the influence of the desolvation system, we recorded the emission intensities of the Ca(I), Ca(II), and H-β spectral lines with and without inclusion of the desolvation system. The emission intensity of the H-β spectral line reduces and the magnitude of the Ca(II)/Ca(I) emission intensity ratio increases four-fold with inclusion of the desolvation system. Finally, the elements Ca, Mg, and Fe present in a single cell of Pseudococcomyxa simplex are simultaneously determined by coupling the M-DIS equipped with the desolvation system to ICP-AES.
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.
Surface Modification of Polyimide for Improving Adhesion Strength by Inductively Coupled Plasma

NASA Astrophysics Data System (ADS)

Byun, Tae Joon; Kim, Sung Il; Kim, Youn Joon; Choi, Yoon Suk; Choi, In Sik; Setsuhara, Yuichi; Geon Han, Jeon

2009-08-01

This study examined the effect of an inductively coupled plasma (ICP) treatment using an argon and helium gas mixture on the adhesion between polyimide and a copper film. Optical emission spectroscopy (OES) of the ICP revealed the emission intensity of helium and argon at various intensities with the helium mixing ratio. The treated polyimide surface was analyzed using a contact angle analyzer, Atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The contact angle and RMS roughness ranged from 66 to 31° and 2.3 to 4.1 nm, respectively. XPS showed an increase in C-O bonding. The highest peel strength was 0.43 kgf/cm at a 40% of helium mixing ratio, which contained the highest level of activate species. Overall, an ICP treatment of a polyimide surface with a 40% helium gas mixture improves the adhesion strength between copper and polyimide significantly.
NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION AND MAINTENANCE OF THE JOBIN-YVON MODEL 70 INDUCTIVELY COUPLED PLASMA ATOMIC ABSORPTION SPECTROMETER (BCO-L-7.1)

EPA Science Inventory

The purpose of this SOP is to detail the operation and maintenance of an Instruments, SA Inc., Jobin-Yvon Model 70 (JY-70) inductively coupled plasma atomic emissions spectrometry (ICP-AES). This procedure was followed to ensure consistent data retrieval during the Arizona NHEXA...
Experimental evaluation of analyte excitation mechanisms in the inductively coupled plasma

NASA Astrophysics Data System (ADS)

Lehn, Scott A.; Hieftje, Gary M.

2003-10-01

The inductively coupled plasma (ICP) is a justifiably popular source for atomic emission spectrometry. However, despite its popularity, the ICP is still only partially understood. Even the mechanisms of analyte excitation remain unclear; some energy levels are quite clearly populated by charge transfer while others might be populated by electron-ion recombination, by electron impact, or by Penning processes. Distinguishing among these alternatives is possible by means of a steady-state kinetics approach that examines correlations between the emission of a selected atom, ion, or level and the local number densities of species assumed to produce the excitation. In an earlier investigation, strong correlations were found between either calcium atom or ion emission and selected combinations of calcium atom or ion number densities and electron number densities in the plasma. However, all radially resolved data employed in the earlier study were produced from Abel inversion and from measurements that were crude by today's standards. Now, by means of tomographic imaging, laser-saturated atomic fluorescence, and Thomson and Rayleigh scattering, it is possible to measure the required radially resolved data without Abel inversion and with far greater fidelity. The correlations previously studied for calcium have been investigated with these more reliable data. Ion-electron recombination, either radiative or with argon as a third body, was determined to be the most likely excitation mechanism for calcium atom, while electron impact appeared to be the most important process to produce excite-state calcium ions. These results were consistent with the previous study. However, the present study suggests that collisional deactivation, rather than radiative decay, is the most likely mode of returning both calcium atoms and ions to the ground state.
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.
STATISTICAL VALIDATION OF SULFATE QUANTIFICATION METHODS USED FOR ANALYSIS OF ACID MINE DRAINAGE

EPA Science Inventory

Turbidimetric method (TM), ion chromatography (IC) and inductively coupled plasma atomic emission spectrometry (ICP-AES) with and without acid digestion have been compared and validated for the determination of sulfate in mining wastewater. Analytical methods were chosen to compa...
A comparison of reliability of soil Cd determination by standard spectrometric methods

PubMed Central

McBride, M.B.

2015-01-01

Inductively coupled plasma emission spectrometry (ICP-OES) is the most common method for determination of soil Cd, yet spectral and matrix interferences affect measurements at the available analytical wavelengths for this metal. This study evaluated the severity of the interference over a range of total soil Cd by comparing ICP-OES and ICP-MS measurements of Cd in acid digests. ICP-OES using the emission at 226.5 nm generally unable to quantify soil Cd at low (near-background) levels, and gave unreliable values compared to ICP-MS. Using the line at 228.nm, a marked positive bias in Cd measurement (relative to the 226.5 nm measurement) was attributable to As interference even at soil As concentrations below 10 mg/kg. This spectral interference in ICP-OES was severe in As-contaminated orchard soils, giving a false value for soil total Cd near 2 mg kg−1 when soil As was 100–150 mg kg−1. In attempting to avoid these ICP emission-specific interferences, we evaluated a method to estimate total soil Cd using 1 M HNO3 extraction followed by determination of Cd by flame atomic absorption (FAA), either with or without pre-concentration of Cd using an Aliquat-heptanone extractant. The 1 M HNO3 extracted an average of 82% of total soil Cd. The FAA method had no significant interferences, and estimated the total Cd concentrations in all soils tested with acceptable accuracy. For Cd-contaminated soils, the Aliquat-heptanone pre-concentration step was not necessary, as FAA sensitivity was adequate for quantification of extractable soil Cd and reliable estimation of total soil Cd. PMID:22031569
Evaluation of a direct injection nebulizer interface for flow injection analysis and high performance liquid chromatography with inductively coupled plasma-atomic emission spectroscopic detection

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

LaFreniere, K.E.

A direct injection nebulizer (DIN) was designed, developed and evaluated to determine its potential utilization as an effective interface for flow injection analysis (FIA) and high performance liquid chromatography (HPLC) coupled with inductively coupled plasma-atomic emission spectroscopic detection. The analytical figures of merit for the DIN when used as an interface for FIA-ICP-AES were found to be comparable to or better than those obtained with conventional pneumatic nebulization in terms of limits of detection (LODs), reproducibility, linearity, and interelement effects. In the HPLC mode, the LODDs were found to be comparable to those obtained by continuous-flow sample introduction into themore » ICP, or inferior by up to only a factor of four. Stable plasma operation was maintained for the DIN sample introduction of a variety of pure organic solvents, including acetonitrile, methanol, methyl-isobutylketone, and pyridine. The HPLC-DIN-ICP-AES facility was specifically applied for the speciation of inorganic and organo-metallic species contained in synthetic mixtures, vanilla extracts and a variety of energy-related materials, such as shale oil process water, coal extracts, shale oil, crude oil, and an SRC II. Suggestions for future research are also considered.« less
Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; preparation procedure for aquatic biological material determined for trace metals

USGS Publications Warehouse

Hoffman, Gerald L.

1996-01-01

A method for the chemical preparation of tissue samples that are subsequently analyzed for 22 trace metals is described. The tissue-preparation procedure was tested with three National Institute of Standards and Technology biological standard reference materials and two National Water Quality Laboratory homogenized biological materials. A low-temperature (85 degrees Celsius) nitric acid digestion followed by the careful addition of hydrogen peroxide (30-percent solution) is used to decompose the biological material. The solutions are evaporated to incipient dryness, reconstituted with 5 percent nitric acid, and filtered. After filtration the solutions were diluted to a known volume and analyzed by inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), and cold vapor-atomic absorption spectrophotometry (CV-AAS). Many of the metals were determined by both ICP-MS and ICP-AES. This report does not provide a detailed description of the instrumental procedures and conditions used with the three types of instrumentation for the quantitation of trace metals determined in this study. Statistical data regarding recovery, accuracy, and precision for individual trace metals determined in the biological material tested are summarized.
Atlas of Atomic Spectral Lines of Neptunium Emitted by Inductively Coupled Plasma

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

DeKalb, E.L. and Edelson, M. C.

1987-08-01

Optical emission spectra from high-purity Np-237 were generated with a glovebox-enclosed inductively coupled plasma (ICP) source. Spectra covering the 230-700 nm wavelength range are presented along with general commentary on the methodology used in collecting the data. The Ames Laboratory Nuclear Safeguards and Security Program has been charged with the task of developing optical spectroscopic methods to analyze the composition of spent nuclear fuels. Such materials are highly radioactive even after prolonged 'cooling' and are chemically complex. Neptunium (Np) is a highly toxic by-product of nuclear power generation and is found, in low abundance, in spent nuclear fuels. This atlasmore » of the optical emission spectrum of Np, as produced by an inductively coupled plasma (ICP) spectroscopic source, is part of a general survey of the ICP emission spectra of the actinide elements. The ICP emission spectrum of the actinides originates almost exclusively from the electronic relaxation of excited, singly ionized species. Spectral data on the Np ion emission spectrum (i.e., the Np II spectrum) have been reported by Tomkins and Fred [1] and Haaland [2]. Tomkins and Fred excited the Np II spectrum with a Cu spark discharge and identified 114 Np lines in the 265.5 - 436.3 nm spectral range. Haaland, who corrected some spectral line misidentifications in the work of Tomkins and Fred, utilized an enclosed Au spark discharge to excite the Np II spectrum and reported 203 Np lines within the 265.4 - 461.0 nm wavelength range.« less
Improved documentation of spectral lines for inductively coupled plasma emission spectrometry

NASA Astrophysics Data System (ADS)

Doidge, Peter S.

2018-05-01

An approach to improving the documentation of weak spectral lines falling near the prominent analytical lines used in inductively coupled plasma optical emission spectrometry (ICP-OES) is described. Measurements of ICP emission spectra in the regions around several hundred prominent lines, using concentrated solutions (up to 1% w/v) of some 70 elements, and comparison of the observed spectra with both recent published work and with the output of a computer program that allows calculation of transitions between the known energy levels, show that major improvements can be made in the coverage of spectral atlases for ICP-OES, with respect to "classical" line tables. It is argued that the atomic spectral data (wavelengths, energy levels) required for the reliable identification and documentation of a large majority of the weak interfering lines of the elements detectable by ICP-OES now exist, except for most of the observed lines of the lanthanide elements. In support of this argument, examples are provided from a detailed analysis of a spectral window centered on the prominent Pb II 220.353 nm line, and from a selected line-rich spectrum (W). Shortcomings in existing analyses are illustrated with reference to selected spectral interferences due to Zr. This approach has been used to expand the spectral-line library used in commercial ICP-ES instruments (Agilent 700-ES/5100-ES). The precision of wavelength measurements is evaluated in terms of the shot-noise limit, while the absolute accuracy of wavelength measurement is characterised through comparison with a small set of precise Ritz wavelengths for Sb I, and illustrated through the identification of Zr III lines; it is further shown that fractional-pixel absolute wavelength accuracies can be achieved. Finally, problems with the wavelengths and classifications of certain Au I lines are discussed.
Inductively coupled plasma atomic emission spectrometric determination of tin in canned food.

PubMed

Sumitani, H; Suekane, S; Nakatani, A; Tatsuka, K

1993-01-01

Various canned foods were digested sequentially with HNO3 and HCl, diluted to 100 mL, and filtered, and then tin was determined by inductively coupled plasma atomic emission spectrometry (ICP/AES). Samples of canned Satsuma mandarin, peach, apricot, pineapple, apple juice, mushroom, asparagus, evaporated milk, short-necked clam, spinach, whole tomato, meat, and salmon were evaluated. Sample preparations did not require time-consuming dilutions, because ICP/AES has wide dynamic range. The standard addition method was used to determine tin concentration. Accuracy of the method was tested by analyzing analytical standards containing tin at 2 levels (50 and 250 micrograms/g). The amounts of tin found for the 50 and 250 micrograms/g levels were 50.5 and 256 micrograms/g, respectively, and the repeatability coefficients of variation were 4.0 and 3.8%, respectively. Recovery of tin from 13 canned foods spiked at 2 levels (50 and 250 micrograms/g) ranged from 93.9 to 109.4%, with a mean of 99.2%. The quantitation limit for tin standard solution was about 0.5 microgram/g.
Evaluation of a direct injection nebulizer interface for flow injection analysis and high performance liquid chromatography with inductively coupled plasma-atomic emission spectroscopic detection

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

LaFreniere, K.E.

A direct injection nebulizer (DIN) was designed, developed, and evaluated to determine its potential utilization as an effective interface for flow injection analysis (FIA) and high performance liquid chromatography (HPLC) coupled with inductively coupled plasma-atomic emission spectroscopic detection. The analytical figures of merit for the DIN when used as an interface for FIA-ICP-AES were found to be comparable to or better than those obtained with conventional pneumatic nebulization in terms of limits of detection (LODs), reproducibility, linearity, and interelement effects. Stable plasma operation was maintained for the DIN sample introduction of a variety of pure organic solvents, including acetonitrile, methanol,more » methylisobutylketone, and pyridine. The HPLC-DIN-ICP-AES facility was specifically applied for the speciation of inorganic and organometallic species contained in synthetic mixtures, vanilla extracts, and a variety of energy-related materials, such as shale oil process water, coal extracts, shale oil, crude oil, and an SRC II. Suggestions for future research are also considered. 227 refs., 44 figs., 15 tabs.« less
[Analytical figures of merit of Hildebrand grid and ultrasonic nebulizations in inductively coupled plasma atomic emission].

PubMed

Tian, Mei; Han, Xiao-yuan; Zhuo, Shang-jun; Zhang, Rui-rong

2012-05-01

Hildebrand grid nebulizer is a kind of improved Babington nebulizer, which can nebulize solutions with high total dissolved solids. And the ultrasonic nebulizer (USN) possesses advantage of high nebulization efficiency and fine droplets. In the present paper, the detection limits, matrix effects, ICP robustness and memory effects of Hildebrand grid and ultrasonic nebulizers for ICP-AES were studied. The results show that the detection limits using USN are improved by a factor of 6-23 in comparison to Hildebrand grid nebulizer for Cu, Pb, Zn, Cr, Cd and Ni. With the USN the matrix effects were heavier, and the degree of intensity enhancement and lowering depends on the element line, the composition and concentrations of matrices. Moreover, matrix effects induced by Ca and Mg are more significant than those caused by Na and Mg, and intensities of ionic lines are affected more easily than those of atomic lines. At the same time, with the USN ICP has less robustness. In addition, memory effect of the USN is also heavier than that of Hildebrand grid nebulizer.
The determination of mercury in mushrooms by CV-AAS and ICP-AES techniques.

PubMed

Jarzynska, Grazyna; Falandysz, Jerzy

2011-01-01

This research presents an example of an excellent applied study on analytical problems due to hazardous mercury determination in environmental materials and validity of published results on content of this element in wild growing mushrooms. The total mercury content has been analyzed in a several species of wild-grown mushrooms and some herbal origin certified reference materials, using two analytical methods. One method was commonly known and well validated the cold-vapour atomic absorption spectroscopy (CV-AAS) after a direct sample pyrolysis coupled to the gold wool trap, which was a reference method. A second method was a procedure that involved a final mercury measurement using the inductively-coupled plasma atomic emission spectroscopy (ICP-AES) at λ 194.163 nm, which was used by some authors to report on a high mercury content of a large sets of wild-grown mushrooms. We found that the method using the ICP-AES at λ 194.163 nm gave inaccurate and imprecise results. The results of this study imply that because of unsuitability of total mercury determination using the ICP-AES at λ 194.163 nm, the reports on great concentrations of this metal in a large sets of wild-grown mushrooms, when examined using this method, have to be studied with caution, since data are highly biased.
Lithogeochemistry of mineralized and altered rock samples from the northern Talkeetna Mountains, south-central Alaska

USGS Publications Warehouse

Light, Thomas D.; Schmidt, Jeanine M.

2011-01-01

Mineralized and altered rock samples collected from the northern Talkeetna Mountains, Alaska, were analyzed by two different inductively coupled plasma atomic-emission spectrometry (ICP-AES) methods for as many as 44 elements; by fire assay and either direct-coupled plasma (DCP) or atomic absorption spectrophotometry (AAS) for gold (Au); by cold vapor atomic absorption (CVAA) for mercury (Hg); and by irradiated neutron activation analysis (INAA) for tungsten (W). The analytical results showed that some samples contain high values of multiple elements and may be potential indicators of hydrothermal mineralization in the area.

ZnO synthesis by high vacuum plasma-assisted chemical vapor deposition using dimethylzinc and atomic oxygen

NASA Astrophysics Data System (ADS)

Barnes, Teresa M.; Hand, Steve; Leaf, Jackie; Wolden, Colin A.

2004-09-01

Zinc oxide thin films were produced by high vacuum plasma-assisted chemical vapor deposition (HVP-CVD) from dimethylzinc (DMZn) and atomic oxygen. HVP-CVD is differentiated from conventional remote plasma-enhanced CVD in that the operating pressures of the inductively coupled plasma (ICP) source and the deposition chamber are decoupled. Both DMZn and atomic oxygen effuse into the deposition chamber under near collisionless conditions. The deposition rate was measured as a function of DMZn and atomic oxygen flux on glass and silicon substrates. Optical emission spectroscopy and quadrupole mass spectrometry (QMS) were used to provide real time analysis of the ICP source and the deposition chamber. The deposition rate was found to be first order in DMZn pressure and zero order in atomic oxygen density. All films demonstrated excellent transparency and were preferentially orientated along the c-axis. The deposition chemistry occurs exclusively through surface-mediated reactions, since the collisionless transport environment eliminates gas-phase chemistry. QMS analysis revealed that DMZn was almost completely consumed, and desorption of unreacted methyl radicals was greatly accelerated in the presence of atomic oxygen. Negligible zinc was detected in the gas phase, suggesting that Zn was efficiently consumed on the substrate and walls of the reactor.
Cobalt as chemical modifier to improve chromium sensitivity and minimize matrix effects in tungsten coil atomic emission spectrometry.

PubMed

Silva, Sidnei G; Donati, George L; Santos, Luana N; Jones, Bradley T; Nóbrega, Joaquim A

2013-05-30

Cobalt is used as chemical modifier to improve sensitivity and minimize matrix effects in Cr determinations by tungsten coil atomic emission spectrometry (WCAES). The atomizer is a tungsten filament extracted from microscope light bulbs. A solid-state power supply and a handheld CCD-based spectrometer are also used in the instrumental setup. In the presence of 1000 mg L(-1) Co, WCAES limit of detection for Cr (λ=425.4 nm) is calculated as 0.070 mg L(-1); a 10-fold improvement compared to determinations without Co modifier. The mechanism involved in such signal enhancement is similar to the one observed in ICP OES and ICP-MS determinations of As and Se in the presence of C. Cobalt increases the population of Cr(+) by charge transfer reactions. In a second step, Cr(+)/e(-) recombination takes place, which results in a larger population of excited-state Cr atoms. This alternative excitation route is energetically more efficient than heat transfer from atomizer and gas phase to analyte atoms. A linear dynamic range of 0.25-10 mg L(-1) and repeatability of 3.8% (RSD, n=10) for a 2.0 mg L(-1) Cr solution are obtained with this strategy. The modifier high concentration also contributes to improving accuracy due to a matrix-matching effect. The method was applied to a certified reference material of Dogfish Muscle (DORM-2) and no statistically significant difference was observed between determined and certified Cr values at a 95% confidence level. Spike experiments with bottled water samples resulted in recoveries between 93% and 112%. Copyright © 2013 Elsevier B.V. All rights reserved.
The lateritic profile of Balkouin, Burkina Faso: Geochemistry, mineralogy and genesis

NASA Astrophysics Data System (ADS)

Giorgis, Ilaria; Bonetto, Sabrina; Giustetto, Roberto; Lawane, Abdou; Pantet, Anne; Rossetti, Piergiorgio; Thomassin, Jean-Hugues; Vinai, Raffaele

2014-02-01

This study reports on the geochemical and mineralogical characterization of a lateritic profile cropping out in the Balkouin area, Central Burkina Faso, aimed at obtaining a better understanding of the processes responsible for the formation of the laterite itself and the constraints to its development. The lateritic profile rests on a Paleoproterozoic basement mostly composed of granodioritic rocks related to the Eburnean magmatic cycle passing upwards to saprolite and consists of four main composite horizons (bottom to top): kaolinite and clay-rich horizons, mottled laterite and iron-rich duricrust. In order to achieve such a goal, a multi-disciplinary analytical approach was adopted, which includes inductively coupled plasma (ICP) atomic emission and mass spectrometries (ICP-AES and ICP-MS respectively), X-ray powder diffraction (XRPD), scanning electron microscopy with energy dispersive spectrometry (SEM-EDS) and micro-Raman spectroscopy.
[Determination of 24 metal elements and their compounds in air of workplace by ICP-AES].

PubMed

Wang, Xiang; Qiu, Jianguo; Zhao, Zhonglin; Guo, Ying

2014-06-01

To establish a method for determination of the levels of 24 metal elements and their compounds in the air of workplace by inductively coupled plasma-atomic emission spectroscopy (ICP- AES). Sampling filters were digested by microwave, and diluted to 25 ml. Twenty-four elements (Mg, Ni, K, Mo, Zn, Ca, Ba, Pb, Mn, Cd, Cr, Co, Cu, Sr, Bi, Tl, Sn, Li, Sb, Zr, In, V, Y, and Be) were simultaneously measured by ICP-AES. The detection limits for 24 elements were 0.001∼0.029 mg/L; liner correlation coefficient r values were all equal to or above 0.9994; the relative standard derivations were less than 5%; the recovery rates were 91.2%∼103.9%; the degradation rates in 7 days were less than 9.7%. ICP-AES technique is a simple, rapid, accurate, and reliable method, which can be used to measure 24 metal elements and their compounds in the air of workplace.
Determination of As in tree-rings of poplar (Populus alba L.) by U-shaped DC arc.

PubMed

Marković, D M; Novović, I; Vilotić, D; Ignjatović, Lj

2009-04-01

An argon-stabilized U-shaped DC arc with a system for aerosol introduction was used for determination of As in poplar (Populus alba L.) tree-rings. After optimization of the operating parameters and selection of the most appropriate signal integration time (30 s), the limit of detection for As was reduced to 15.0 ng/mL. This detection limit obtained with the optimal integration time was compared with those for other methods: inductively coupled plasma-atomic emission spectrometry (ICP-AES), direct coupled plasma-atomic emission spectrometry (DCP-AES), microwave induced plasma-atomic emission spectrometry (MIP-AES) and improved thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS). Arsenic is toxic trace element which can adversely affect plant, animal and human health. As an indicator of environment pollution we collected poplar tree-rings from two locations. The first area was close to the "Nikola Tesla" (TENT-A) power plant, Obrenovac, while the other was in the urban area of Novi Sad. In all cases elevated average concentrations of As were registered in poplar tree-rings from the Obrenovac location.
Database creation, data quality assessment, and geochemical maps (phase V, deliverable 59)—Final report on compilation and validation of geochemical data: Chapter D in Second projet de renforcement institutionnel du secteur minier de la République Islamique de Mauritanie (PRISM-II)

USGS Publications Warehouse

Eppinger, Robert G.; Giles, Stuart A.; Lee, Gregory K.; Smith, Steven M.

2015-01-01

The geochemical sample media collected by the BGS and BRGM under the PRISM-I contract included rock, sediment, regolith, and soil samples. Details on sample collection procedures are in unpublished reports available from PRISM. These samples were analyzed under PRISM-I contract by ALS Chemex Laboratories using various combinations of modern methods including fire-assay inductively coupled plasma-atomic emission spectrometry (ICPAES) and ICP-mass spectrometry (ICP-MS) for Au; multi-acid digestion, atomic absorption spectroscopy (AAS) for Ag and As; 47-element, four-acid digestion, ICP-MS; 27-element, fouracid digestion, ICP-AES; special four-acid ICP-MS techniques for Pt and B; fire assay followed by ICP-AES for platinum-group elements; whole-rock analyses by wavelength dispersive X-ray fluorescence (XRF); special techniques for loss-on-ignition, inorganic C, and total S; and special ore-grade AAS techniques for Ag, Au, Cu, Ni, Pb, and Zn. Around 30,000 samples were analyzed by at least one technique. However, it is stressed here that: (1) there was no common sample medium collected at all sites, likely due to the vast geological and geomorphologic differences across the country, (2) the sample site distribution is very irregular, likely due in part to access constraints and sand dune cover, and (3) there was no common across-the-board trace element analytical package used for all samples. These three aspects fundamentally affect the ability to produce country-wide geochemical maps of Mauritania. Gold (Au), silver (Ag), and arsenic (As) were the three elements that were most commonly analyzed.
Determination of aluminium in groundwater samples by GF-AAS, ICP-AES, ICP-MS and modelling of inorganic aluminium complexes.

PubMed

Frankowski, Marcin; Zioła-Frankowska, Anetta; Kurzyca, Iwona; Novotný, Karel; Vaculovič, Tomas; Kanický, Viktor; Siepak, Marcin; Siepak, Jerzy

2011-11-01

The paper presents the results of aluminium determinations in ground water samples of the Miocene aquifer from the area of the city of Poznań (Poland). The determined aluminium content amounted from <0.0001 to 752.7 μg L(-1). The aluminium determinations were performed using three analytical techniques: graphite furnace atomic absorption spectrometry (GF-AAS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The results of aluminium determinations in groundwater samples for particular analytical techniques were compared. The results were used to identify the ascent of ground water from the Mesozoic aquifer to the Miocene aquifer in the area of the fault graben. Using the Mineql+ program, the modelling of the occurrence of aluminium and the following aluminium complexes: hydroxy, with fluorides and sulphates was performed. The paper presents the results of aluminium determinations in ground water using different analytical techniques as well as the chemical modelling in the Mineql+ program, which was performed for the first time and which enabled the identification of aluminium complexes in the investigated samples. The study confirms the occurrence of aluminium hydroxy complexes and aluminium fluoride complexes in the analysed groundwater samples. Despite the dominance of sulphates and organic matter in the sample, major participation of the complexes with these ligands was not stated based on the modelling.
Direct solid analysis of powdered tungsten carbide hardmetal precursors by laser-induced argon spark ablation with inductively coupled plasma atomic emission spectrometry.

PubMed

Holá, Markéta; Kanický, Viktor; Mermet, Jean-Michel; Otruba, Vítezslav

2003-12-01

The potential of the laser-induced argon spark atomizer (LINA-Spark atomizer) coupled with ICP-AES as a convenient device for direct analysis of WC/Co powdered precursors of sintered hardmetals was studied. The samples were presented for the ablation as pressed pellets prepared by mixing with powdered silver binder containing GeO2 as internal standard. The pellets were ablated with the aid of a Q-switched Nd:YAG laser (1064 nm) focused 16 mm behind the target surface with a resulting estimated power density of 5 GW cm(-2). Laser ablation ICP-AES signals were studied as a function of ablation time, and the duration of time prior to measurement (pre-ablation time) which was necessary to obtain reliable results was about 40 s. Linear calibration plots were obtained up to 10% (m/m) Ti, 9% Ta and 3.5% Nb both without internal standardization and by using germanium as an added internal standard or tungsten as a contained internal standard. The relative uncertainty at the centroid of the calibration line was in the range from +/- 6% to +/- 11% for Nb, Ta and Ti both with and without internal standardisation by Ge. A higher spread of points about the regression was observed for cobalt for which the relative uncertainty at the centroid was in the range from +/- 9% to +/- 14%. Repeatability of results was improved by the use of both Ge and W internal standards. The lowest determinable quantities calculated for calibration plots were 0.060% Co, 0.010% Nb, 0.16% Ta and 0.030% Ti with internal standardization by Ge. The LA-ICP-AES analyses of real samples led to good agreement with the results obtained by solution-based ICP determination with a relative bias not exceeding 10%. The elimination of the dissolution procedure of powdered tungsten (Nb, Ta, Ti) carbide is the principal advantage of the developed LA-ICP-AES method.
Multielement extraction system for determining 19 trace elements in gold exploration samples

USGS Publications Warehouse

Clark, J. Robert; Viets, John G.; ,

1990-01-01

A multielement extraction system is being used successfully to provide essentially interference-free geochemical analyses to aid in gold exploration. The Methyl isobutyl ketone-Amine synerGistic Iodide Complex (MAGIC) extraction system separates Ag, As, Au, Bi, Cd, Cu, Ga, Hg, In, Mo, Pb, Pd, Pt, Sb, Se, Sn, Te, Tl, and Zn from interfering geological matrices. Quantitative extraction of these elements is accomplished over a broad range of acid normality making it possible to economically determine all 19 elements from a single digestion or leach solution. The resulting organic extracts are amenable to analysis by inductively coupled plasma atomic emission spectroscopy (ICP-AES) and flame atomic absorption spectroscopy (FAAS). For many years the principal shortcoming of ICP-AES was the complex spectral and stray-light interferences that were caused by the extreme variability of components such as Fe, Na, and Ca in common geological matrices. The MAGIC extraction allows determination of the extracted elements with enhanced sensitivity, from a virtually uniform matrix, by ICP-AES and FAAS. Because of its simultaneous multichannel capabilities, ICP-AES is the ideal instrumental technique for determining these 19 extracted elements. Ultratrace (sub-part-per-billion) determinations of Au and many of the other extracted elements can be made by graphite furnace atomic absorption spectroscopy (GFAAS), following back stripping of the extracts. The combination of the extraction followed by stripping of the organic phase eliminates 99.999% of potential interferences for Au. Gold determination by GFAAS from these extracts under the specified conditions yields a fourfold improvement in sensitivity over conventional GFAAS methods. This sensitivity enhancement and the interference-free matrix allow highly reliable determinations well into the parts-per-trillion range.
Feasibility of laser-induced breakdown spectroscopy (LIBS) for classification of sea salts.

PubMed

Tan, Man Minh; Cui, Sheng; Yoo, Jonghyun; Han, Song-Hee; Ham, Kyung-Sik; Nam, Sang-Ho; Lee, Yonghoon

2012-03-01

We have investigated the feasibility of laser-induced breakdown spectroscopy (LIBS) as a fast, reliable classification tool for sea salts. For 11 kinds of sea salts, potassium (K), magnesium (Mg), calcium (Ca), and aluminum (Al), concentrations were measured by inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and the LIBS spectra were recorded in the narrow wavelength region between 760 and 800 nm where K (I), Mg (I), Ca (II), Al (I), and cyanide (CN) band emissions are observed. The ICP-AES measurements revealed that the K, Mg, Ca, and Al concentrations varied significantly with the provenance of each salt. The relative intensities of the K (I), Mg (I), Ca (II), and Al (I) peaks observed in the LIBS spectra are consistent with the results using ICP-AES. The principal component analysis of the LIBS spectra provided the score plot with quite a high degree of clustering. This indicates that classification of sea salts by chemometric analysis of LIBS spectra is very promising. Classification models were developed by partial least squares discriminant analysis (PLS-DA) and evaluated. In addition, the Al (I) peaks enabled us to discriminate between different production methods of the salts. © 2012 Society for Applied Spectroscopy
Gunshot residue testing in suicides: Part II: Analysis by inductive coupled plasma-atomic emission spectrometry.

PubMed

Molina, D Kimberley; Castorena, Joe L; Martinez, Michael; Garcia, James; DiMaio, Vincent J M

2007-09-01

Several different methods can be employed to test for gunshot residue (GSR) on a decedent's hands, including scanning electron microscopy with energy dispersive x-ray (SEM/EDX) and inductive coupled plasma-atomic emission spectrometry (ICP-AES). In part I of this 2-part series, GSR results performed by SEM/EDX in undisputed cases of suicidal handgun wounds were studied. In part II, the same population was studied, deceased persons with undisputed suicidal handgun wounds, but GSR testing was performed using ICP-AES. A total of 102 cases were studied and analyzed for caliber of weapon, proximity of wound, and the results of the GSR testing. This study found that 50% of cases where the deceased was known to have fired a handgun immediately prior to death had positive GSR results by ICP/AES, which did not differ from the results of GSR testing by SEM/EDX. Since only 50% of cases where the person is known to have fired a weapon were positive for GSR by either method, this test should not be relied upon to determine whether someone has discharged a firearm and is not useful as a determining factor of whether or not a wound is self-inflicted or non-self-inflicted. While a positive GSR result may be of use, a negative result is not helpful in the medical examiner setting as a negative result indicates that either a person fired a weapon prior to death or a person did not fire a weapon prior to death.
Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis

NASA Astrophysics Data System (ADS)

Papadopoulou, D. N.; Zachariadis, G. A.; Anthemidis, A. N.; Tsirliganis, N. C.; Stratis, J. A.

2004-12-01

Two multielement instrumental methods of analysis, micro X-ray fluorescence spectrometry (micro-XRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were applied for the analysis of 7th and 5th century B.C. ancient ceramic sherds in order to evaluate the above two methods and to assess the potential to use the current compact and portable micro-XRF instrument for the in situ analysis of ancient ceramics. The distinguishing factor of interest is that micro-XRF spectrometry offers the possibility of a nondestructive analysis, an aspect of primary importance in the compositional analysis of cultural objects. Micro-XRF measurements were performed firstly directly on the ceramic sherds with no special pretreatment apart from surface cleaning (micro-XRF on sherds) and secondly on pressed pellet disks which were prepared for each ceramic sherd (micro-XRF on pellet). For the ICP-AES determination of elements, test solutions were prepared by the application of a microwave-assisted decomposition procedure in closed high-pressure PFA vessels. Also, the standard reference material SARM 69 was used for the efficiency calibration of the micro-XRF instrument and was analysed by both methods. In order to verify the calibration, the standard reference materials NCS DC 73332 and SRM620 as well as the reference materials AWI-1 and PRI-1 were analysed by micro-XRF. Elemental concentrations determined by the three analytical procedures (ICP-AES, micro-XRF on sherds and micro-XRF on pellets) were statistically treated by correlation analysis and Student's t-test (at the 95% confidence level).
Optimized laser-induced breakdown spectroscopy for determination of xenobiotic silver in monosodium glutamate and its verification using ICP-AES.

PubMed

Rehan, I; Gondal, M A; Rehan, K

2018-04-20

Laser-induced breakdown spectroscopy (LIBS) was applied as a potential tool for the determination of xenobiotic metal in monosodium glutamate (MSG). In order to achieve a high-sensitivity LIBS system required to determine trace amounts of metallic silver in MSG and to attain the best detection limit, the parameters used in our experiment (impact of focusing laser energy on the intensity of LIBS emission signals, the influence of focusing lens distance on the intensity of LIBS signals, and time responses of the plasma emissions) were optimized. The spectra of MSG were obtained in air using a suitable detector with an optical resolution of 0.06 nm, covering a spectral region from 220 to 720 nm. Along with the detection of xenobiotic silver, other elements such as Ca, Mg, S, and Na were also detected in MSG. To determine the concentration of xenobiotic silver in MSG, the calibration curve was plotted by preparing standard samples having different silver abundances in an MSG matrix. The LIBS results of each sample were cross-verified by analyzing with a standard analytical technique such as inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Both (LIBS and ICP-AES) results were in mutual agreement. The limit of detection of the LIBS setup was found to be 0.57 ppm for silver present in MSG samples.
Noninvasive intracranial pressure measurement using infrasonic emissions from the tympanic membrane.

PubMed

Stettin, Eduard; Paulat, Klaus; Schulz, Chris; Kunz, Ulrich; Mauer, Uwe Max

2011-06-01

We investigated whether ICP can be assessed by measuring infrasonic emissions from the tympanic membrane. An increase in ICP was induced in 22 patients with implanted ICP pressure sensors. ICP waveforms that were obtained invasively and continuously were compared with infrasonic emission waveforms. In addition, the noninvasive method was used in a control group of 14 healthy subjects. In a total of 83 measurements, the changes in ICP that were observed in response to different types of stimulation were detected in the waveforms obtained noninvasively as well as in those acquired invasively. Low ICP was associated with an initial high peak and further peaks with smaller amplitudes. High ICP was associated with a marked decrease in the number of peaks and in the difference between the amplitudes of the initial and last peaks. The assessment of infrasonic emissions, however, does not yet enable us to provide exact figures. It is conceivable that the assessment of infrasonic emissions will become suitable both as a screening tool and for the continuous monitoring of ICP in an intensive care environment.
Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of whole-water recoverable arsenic, boron, and vanadium using inductively coupled plasma-mass spectrometry

USGS Publications Warehouse

Garbarino, John R.

2000-01-01

Analysis of in-bottle digestate by using the inductively coupled plasma?mass spectrometric (ICP?MS) method has been expanded to include arsenic, boron, and vanadium. Whole-water samples are digested by using either the hydrochloric acid in-bottle digestion procedure or the nitric acid in-bottle digestion procedure. When the hydrochloric acid in-bottle digestion procedure is used, chloride must be removed from the digestate by subboiling evaporation before arsenic and vanadium can be accurately determined. Method detection limits for these elements are now 10 to 100 times lower than U.S. Geological Survey (USGS) methods using hydride generation? atomic absorption spectrophotometry (HG? AAS) and inductively coupled plasma? atomic emission spectrometry (ICP?AES), thus providing lower variability at ambient concentrations. The bias and variability of the methods were determined by using results from spike recoveries, standard reference materials, and validation samples. Spike recoveries in reagent-water, surface-water, ground-water, and whole-water recoverable matrices averaged 90 percent for seven replicates; spike recoveries were biased from 25 to 35 percent low for the ground-water matrix because of the abnormally high iron concentration. Results for reference material were within one standard deviation of the most probable value. There was no significant difference between the results from ICP?MS and HG?AAS or ICP?AES methods for the natural whole-water samples that were analyzed.
Road Environments: Impact of Metals on Human Health in Heavily Congested Cities of Poland

PubMed Central

Adamiec, Ewa

2017-01-01

Road dust as a by-product of exhaust and non-exhaust emissions can be a major cause of systemic oxidative stress and multiple disorders. Substantial amounts of road dust are repeatedly resuspended, in particular at traffic lights and junctions where more braking is involved, causing potential threat to pedestrians, especially children. In order to determine the degree of contamination in the heavily traffic-congested cities of Poland, a total of 148 samples of road dust (RD), sludge from storm drains (SL) and roadside soil (RS) were collected. Sixteen metals were analysed using inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectroscopy (ICP-OES) and atomic absorption spectroscopy (AAS) in all samples. Chemical evaluation followed by Principal Component Analysis (PCA) revealed that road environments have been severely contaminated with traffic-related elements. Concentration of copper in all road-environment samples is even higher, exceeding even up to 15 times its average concentrations established for the surrounding soils. Non-carcinogenic health risk assessment revealed that the hazard index (HI) for children in all road-environment samples exceeds the safe level of 1. Therefore, greater attention should be paid to potential health risks caused by the ingestion of traffic-related particles during outdoor activities. PMID:28661464
Road Environments: Impact of Metals on Human Health in Heavily Congested Cities of Poland.

PubMed

Adamiec, Ewa

2017-06-29

Road dust as a by-product of exhaust and non-exhaust emissions can be a major cause of systemic oxidative stress and multiple disorders. Substantial amounts of road dust are repeatedly resuspended, in particular at traffic lights and junctions where more braking is involved, causing potential threat to pedestrians, especially children. In order to determine the degree of contamination in the heavily traffic-congested cities of Poland, a total of 148 samples of road dust (RD), sludge from storm drains (SL) and roadside soil (RS) were collected. Sixteen metals were analysed using inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectroscopy (ICP-OES) and atomic absorption spectroscopy (AAS) in all samples. Chemical evaluation followed by Principal Component Analysis (PCA) revealed that road environments have been severely contaminated with traffic-related elements. Concentration of copper in all road-environment samples is even higher, exceeding even up to 15 times its average concentrations established for the surrounding soils. Non-carcinogenic health risk assessment revealed that the hazard index (HI) for children in all road-environment samples exceeds the safe level of 1. Therefore, greater attention should be paid to potential health risks caused by the ingestion of traffic-related particles during outdoor activities.
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.
[Application of AOTF in spectral analysis. 3. Application of AOTF in atomic emission spectral analysis].

PubMed

Chen, Ze-yong; Peng, Rong-fei; Zhang, Zhan-xia

2002-06-01

An atomic emission spectrometer based on acousto-optic tunable filter (AOTF) was self-constructed and was used to evaluate its practical use in atomic emission analysis. The AOTF used was of model TEAF5-0.36-0.52-S (Brimrose, USA) and the frequency of the direct digital RF synthesizer ranges from 100 MHz to 200 MHz. ICP and PMT were used as light source and detector respectively. The software, written in Visual C++ and running on the Windows 98 platform, is of an utility program system having two data banks and multiwindows. The wavelength calibration was performed with 14 emission lines of Ca, Y, Li, Eu, Sr and Ba using a tenth-order polynomial for line fitting method. The absolute error of the peak position was less than 0.1 nm, and the peak deviation was only 0.04 nm as the PMT varied from 337.5 V to 412.5 V. The scanning emission spectra and the calibration curves of Ba, Y, Eu, Sc and Sr are presented. Their average correlation coefficient was 0.9991 and their detection limits were in the range of 0.051 to 0.97 micrograms.mL-1 respectively. The detection limit can be improved under optimized operating conditions. However, the spectral resolution is only 2.1 nm at the wavelength of 488 nm. Evidently, this poor spectral resolution would restrict the application of AOTF in atomic emission spectral analysis, unless an enhancing techniques is integrated in it.
Analysis of ZDDP Content and Thermal Decomposition in Motor Oils Using NAA and NMR

NASA Astrophysics Data System (ADS)

Ferguson, S.; Johnson, J.; Gonzales, D.; Hobbs, C.; Allen, C.; Williams, S.

Zinc dialkyldithiophosphates (ZDDPs) are one of the most common anti-wear additives present in commercially-available motor oils. The ZDDP concentrations of motor oils are most commonly determined using inductively coupled plasma atomic emission spectroscopy (ICP-AES). As part of an undergraduate research project, we have determined the Zn concentrations of eight commercially-available motor oils and one oil additive using neutron activation analysis (NAA), which has potential for greater accuracy and less sensitivity to matrix effects as compared to ICP-AES. The 31P nuclear magnetic resonance (31P-NMR) spectra were also obtained for several oil additive samples which have been heated to various temperatures in order to study the thermal decomposition of ZDDPs.

Late-paleozoic granitoid complexes of the southwest Primorye: geochemistry, age and typification

NASA Astrophysics Data System (ADS)

Veldemar, A. A.; Vovna, G. M.

2017-12-01

The article presents the first data of geochemical studies of the Late Permian granitoids of the Gamov Complex located in the southwestern part of the Voznesenskiy terrane. The purpose of the study was to identify the main geochemical features of the Late Paleozoic granitoids of the southwestern Primorye, which in the future will allow us to draw conclusions about the petrogenesis of these granitoids. Elemental analysis of 20 samples was carried out, conducted statistical and mathematical processing of the data, have been constructed representative diagrams and graphs for this group of rocks. Elemental analysis was performed by atomic emission (ICP-AES) and inductively-coupled-plasma (ICP-MS) mass spectrometry, at the Analytical Center FEGI FEB RAS.
Considerations in As analysis and speciation

USGS Publications Warehouse

Edwards, M.; Patel, S.; McNeil, L.; Chen, H.W.; Frey, M.; Eaton, A.D.; Antweiler, Ronald C.; Taylor, Howard E.

1998-01-01

This article summarizes recent experiences in arsenic (As) quantification, preservation, and speciation developed during AWWA Research Foundation (AWWARF) and Water Industry Technical Action Fund (WITAF) projects. The goal of this article is to alert analysts and decision-makers to potential problems in As analysis and speciation, because there appear to be several unresolved problems with routine analytical approaches. In true split drinking water samples As was quantified by three accepted analytical methods in three laboratories. The techniques used were graphite furnace atomic absorption spectrometry (GFAAS), inductively coupled plasma mass spectrometry (ICP-MS), and hydride generation inductively coupled plasma-emission spectrometry (HG-ICP-AES). Experimental findings are organized into sections on As analysis, particulate As in water supplies, and examination of As speciation methods.
Mapping Copper and Lead Concentrations at Abandoned Mine Areas Using Element Analysis Data from ICP-AES and Portable XRF Instruments: A Comparative Study.

PubMed

Lee, Hyeongyu; Choi, Yosoon; Suh, Jangwon; Lee, Seung-Ho

2016-03-30

Understanding spatial variation of potentially toxic trace elements (PTEs) in soil is necessary to identify the proper measures for preventing soil contamination at both operating and abandoned mining areas. Many studies have been conducted worldwide to explore the spatial variation of PTEs and to create soil contamination maps using geostatistical methods. However, they generally depend only on inductively coupled plasma atomic emission spectrometry (ICP-AES) analysis data, therefore such studies are limited by insufficient input data owing to the disadvantages of ICP-AES analysis such as its costly operation and lengthy period required for analysis. To overcome this limitation, this study used both ICP-AES and portable X-ray fluorescence (PXRF) analysis data, with relatively low accuracy, for mapping copper and lead concentrations at a section of the Busan abandoned mine in Korea and compared the prediction performances of four different approaches: the application of ordinary kriging to ICP-AES analysis data, PXRF analysis data, both ICP-AES and transformed PXRF analysis data by considering the correlation between the ICP-AES and PXRF analysis data, and co-kriging to both the ICP-AES (primary variable) and PXRF analysis data (secondary variable). Their results were compared using an independent validation data set. The results obtained in this case study showed that the application of ordinary kriging to both ICP-AES and transformed PXRF analysis data is the most accurate approach when considers the spatial distribution of copper and lead contaminants in the soil and the estimation errors at 11 sampling points for validation. Therefore, when generating soil contamination maps for an abandoned mine, it is beneficial to use the proposed approach that incorporates the advantageous aspects of both ICP-AES and PXRF analysis data.
Final Report on Jobin Yvon Contained Inductively Coupled Plasma Emission Spectrometer

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

Pennebaker, F.M.

2003-03-17

A new Inductively Coupled Plasma -- Emission Spectrometer (ICP-ES) was recently purchased and installed in Lab B-147/151 at SRTC. The contained JY Model Ultima 170-C ICP-ES has been tested and compared to current ADS ICP-ES instrumentation. The testing has included both performance tests to evaluate instrumental ability, and the measurement of matrix standards commonly analyzed by ICP-ES at Savannah River. In developing operating procedures for this instrument, we have implemented the use of internal standards and off-peak background subtraction. Both of these techniques are recommended by EPA SW-846 ICP-ES methods and are common to current ICP-ES operations. Based on themore » testing and changes, the JY Model Ultima 170-C ICP-ES provides improved performance for elemental analysis of radioactive samples in the Analytical Development Section.« less
Deformed space-time transformations in Mercury

NASA Astrophysics Data System (ADS)

Cardone, F.; Albertini, G.; Bassani, D.; Cherubini, G.; Guerriero, E.; Mignani, R.; Monti, M.; Petrucci, A.; Ridolfi, F.; Rosada, A.; Rosetto, F.; Sala, V.; Santoro, E.; Spera, G.

2017-09-01

A mole of Mercury was suitably treated by ultrasound in order to generate in it the same conditions of local Lorentz invariance violation that were generated in a sonicated cylindrical bar of AISI 304 steel and that are the cause of neutron emission during the sonication. After 3 min, part of the mercury turned into a solid material which turned out to contain isotopes having a different mass (higher and lower) with respect to the isotopes already present in the initial material (mercury). These transformations in the atomic weight without gamma production above the background are brought about during Deformed Space-Time reactions. We present the results of the analyses performed on samples taken from the transformation product. The analyses have been done in two groups, the first one using five different analytical techniques: ICP-OES, XRF, ESEM-EDS, ICP-MS, INAA. In the second group of analyses, we used only two techniques: INAA and ICP-MS. The second group of analyses confirmed the occurring of the transformations in mercury.
Two-dimensional on-line detection of brominated and iodinated volatile organic compounds by ECD and ICP-MS after GC separation.

PubMed

Schwarz, A; Heumann, K G

2002-09-01

Inductively coupled plasma-mass spectrometry (ICP-MS) was coupled to a gas chromatographic (GC) system with electron capture detector (ECD), which enables relatively easy characterization and quantification of brominated and iodinated (halogenated) volatile organic compounds (HVOCs) in aquatic and air samples. The GC-ECD system is connected in series with an ICP-MS by a directly heated transfer line and an outlet port-hole for elimination of the ECD make-up gas during ignition of the plasma. The hyphenated GC-ECD/ICP-MS system provides high selectivity and sensitivity for monitoring individual HVOCs under fast chromatographic conditions. The ECD is most sensitive for the detection of chlorinated and brominated but the ICP-MS for iodinated compounds. The greatest advantage of the use of an ICP-MS is its element-specific detection, which allows clear identification of compounds in most cases. The absolute detection limits for ICP-MS are 0.5 pg for iodinated, 10 pg for brominated, and 50 pg for chlorinated HVOCs with the additional advantage that calibration is almost independent on different compounds of the same halogen. In contrast to that detection limits for ECD vary for the different halogenated compounds and lie in the range of 0.03-11 pg. The two-dimensional GC-ECD/ICP-MS instrumentation is compared with electron impact mass spectrometry (EI-MS) and microwave induced plasma atomic emission detection (MIP-AED). Even if EI-MS has additional power in identifying unknown peaks by its scan mode, the detection limits are much higher compared with GC-ECD/ICP-MS, whereas the selective ion monitoring mode (SIM) reaches similar detection limits. The MIP-AED detection limits are at the same level as EI-MS in the scan mode.
Development of a certified reference material (NMIJ CRM 7505-a) for the determination of trace elements in tea leaves.

PubMed

Zhu, Yanbei; Narukawa, Tomohiro; Inagaki, Kazumi; Kuroiwa, Takayoshi; Chiba, Koichi

2011-01-01

A certified reference material (CRM) for trace elements in tea leaves has been developed in National Metrology Institute of Japan (NMIJ). The CRM was provided as a dry powder (<90 µm) after frozen pulverization of washed and dried fresh tea leaves from a tea plant farm in Shizuoka Prefecture, Japan. Characterization of the property value for each element was carried out exclusively by NMIJ with at least two independent analytical methods, including inductively coupled plasma mass spectrometry (ICP-MS), high-resolution (HR-) ICP-MS, isotope-dilution (ID-) ICP-MS, inductively coupled plasma optical emission spectrometry (ICP-OES), graphite-furnace atomic-absorption spectrometry (GF-AAS) and flame atomic-absorption spectrometry (FAAS). Property values were provided for 19 elements (Ca, K, Mg, P, Al, B, Ba, Cd, Cu, Fe, Li, Mn, Na, Ni, Pb, Rb, Sr, Zn and Co) and informative values for 18 elements (Ti, V, Cr, Y, and all of the lanthanides, except for Pm whose isotopes are exclusively radioactive). The concentration ranges of property values and informative values were from 1.59% (mass) of K to 0.0139 mg kg(-1) of Cd and from 0.6 mg kg(-1) of Ti to 0.0014 mg kg(-1) of Lu, respectively. Combined relatively standard uncertainties of the property values were estimated by considering the uncertainties of the homogeneity, analytical methods, characterization, calibration standard, and dry-mass correction factor. The range of the relative combined standard uncertainties was from 1.5% of Mg and K to 4.1% of Cd.
Quantification of immobilized Candida antarctica lipase B (CALB) using ICP-AES combined with Bradford method.

PubMed

Nicolás, Paula; Lassalle, Verónica L; Ferreira, María L

2017-02-01

The aim of this manuscript was to study the application of a new method of protein quantification in Candida antarctica lipase B commercial solutions. Error sources associated to the traditional Bradford technique were demonstrated. Eight biocatalysts based on C. antarctica lipase B (CALB) immobilized onto magnetite nanoparticles were used. Magnetite nanoparticles were coated with chitosan (CHIT) and modified with glutaraldehyde (GLUT) and aminopropyltriethoxysilane (APTS). Later, CALB was adsorbed on the modified support. The proposed novel protein quantification method included the determination of sulfur (from protein in CALB solution) by means of Atomic Emission by Inductive Coupling Plasma (AE-ICP). Four different protocols were applied combining AE-ICP and classical Bradford assays, besides Carbon, Hydrogen and Nitrogen (CHN) analysis. The calculated error in protein content using the "classic" Bradford method with bovine serum albumin as standard ranged from 400 to 1200% when protein in CALB solution was quantified. These errors were calculated considering as "true protein content values" the results of the amount of immobilized protein obtained with the improved method. The optimum quantification procedure involved the combination of Bradford method, ICP and CHN analysis. Copyright © 2016 Elsevier Inc. All rights reserved.
Development of a certified reference material (NMIJ CRM 7531-a) for the determination of trace cadmium and other elements in brown rice flour.

PubMed

Miyashita, Shin-ichi; Inagaki, Kazumi; Narukawa, Tomohiro; Zhu, Yanbei; Kuroiwa, Takayoshi; Hioki, Akiharu; Chiba, Koichi

2012-01-01

A certified reference material (CRM) for trace cadmium and other elements in brown rice flour was developed at the National Metrology Institute of Japan (NMIJ). The CRM was provided as a dry powder after drying and frozen pulverization of fresh brown rice obtained from a Japanese domestic market. Characterization of the property value for each element was carried out exclusively by NMIJ with at least two independent analytical methods, including inductively coupled plasma mass spectrometry (ICP-MS), ICP high-resolution mass spectrometry, isotope-dilution ICP-MS, ICP optical emission spectrometry, and graphite-furnace atomic-absorption spectrometry. Property values were provided for six elements (Mn, Fe, Cu, Zn, As, and Cd). The concentration range of the property values was from 0.280 mg kg(-1) of As to 31.8 mg kg(-1) of Zn. The combined relative standard uncertainties of the property values were estimated by considering the uncertainties of the homogeneity, characterization, difference among analytical methods, dry-mass correction factor, and calibration standard. The range of the relative combined standard uncertainties was from 1.1% of Zn to 1.6% of As.
Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: a tutorial review. Part I. Theoretical considerations.

PubMed

Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

2015-07-23

Due to their outstanding analytical performances, inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are widely used for multi-elemental measurements and also for isotopic characterization in the case of ICP-MS. While most studies are carried out in aqueous matrices, applications involving organic/hydro-organic matrices become increasingly widespread. This kind of matrices is introduced in ICP based instruments when classical "matrix removal" approaches such as acid digestion or extraction procedures cannot be implemented. Due to the physico-chemical properties of organic/hydro-organic matrices and their associated effects on instrumentation and analytical performances, their introduction into ICP sources is particularly challenging and has become a full topic. In this framework, numerous theoretical and phenomenological studies of these effects have been performed in the past, mainly by ICP-OES, while recent literature is more focused on applications and associated instrumental developments. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP-OES and ICP-MS. The present Part I, provides theoretical considerations in connection with the physico-chemical properties of organic/hydro-organic matrices, in order to better understand the induced phenomena. This focal point is divided in four chapters highlighting: (i) the impact of organic/hydro-organic matrices from aerosol generation to atomization/excitation/ionization processes; (ii) the production of carbon molecular constituents and their spatial distribution in the plasma with respect to analytes repartition; (iii) the subsequent modifications of plasma fundamental properties; and (iv) the resulting spectroscopic and non spectroscopic interferences. This first part of this tutorial review is addressed either to beginners or to more experienced scientists who are interested in the analysis of organic/hydro-organic matrices by ICP sources and would like to consider the theoretical background of effects induced by such matrices. The second part of this tutorial review will be dedicated to more practical consideration on instrumentation, such as adapted introductions devices, as well as instrumental and operating parameters optimization. The analytical strategies for elemental quantification in such matrices will also be addressed. Copyright © 2015 Elsevier B.V. All rights reserved.
Comparative measurements of mineral elements in milk powders with laser-induced breakdown spectroscopy and inductively coupled plasma atomic emission spectroscopy.

PubMed

Lei, W Q; El Haddad, J; Motto-Ros, V; Gilon-Delepine, N; Stankova, A; Ma, Q L; Bai, X S; Zheng, L J; Zeng, H P; Yu, J

2011-07-01

Mineral elements contained in commercially available milk powders, including seven infant formulae and one adult milk, were analyzed with inductively coupled plasma atomic emission spectrometry (ICP-AES) and laser-induced breakdown spectroscopy (LIBS). The purpose of this work was, through a direct comparison of the analytical results, to provide an assessment of the performance of LIBS, and especially of the procedure of calibration-free LIBS (CF-LIBS), to deal with organic compounds such as milk powders. In our experiments, the matrix effect was clearly observed affecting the analytical results each time laser ablation was employed for sampling. Such effect was in addition directly observed by determining the physical parameters of the plasmas induced on the different samples. The CF-LIBS procedure was implemented to deduce the concentrations of Mg and K with Ca as the internal reference element. Quantitative analytical results with CF-LIBS were validated with ICP-AES measurements and nominal concentrations specified for commercial milks. The obtained good results with the CF-LIBS procedure demonstrate its capacity to take into account the difference in physical parameters of the plasma in the calculation of the concentrations of mineral elements, which allows a significant reduction of the matrix effect related to laser ablation. We finally discuss the way to optimize the implementation of the CF-LIBS procedure for the analysis of mineral elements in organic materials.
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).
Micronutrient Composition of 35 Food Fishes from India and Their Significance in Human Nutrition.

PubMed

Mohanty, Bimal P; Sankar, T V; Ganguly, Satabdi; Mahanty, Arabinda; Anandan, R; Chakraborty, Kajal; Paul, B N; Sarma, Debajit; Dayal, J Syama; Mathew, Suseela; Asha, K K; Mitra, Tandrima; Karunakaran, D; Chanda, Soumen; Shahi, Neetu; Das, Puspita; Das, Partha; Akhtar, Md Shahbaz; Vijayagopal, P; Sridhar, N

2016-12-01

The micronutrients (vitamins and minerals) are required in small amounts but are essential for health, development, and growth. Micronutrient deficiencies, which affect over two billion people around the globe, are the leading cause of many ailments including mental retardation, preventable blindness, and death during childbirth. Fish is an important dietary source of micronutrients and plays important role in human nutrition. In the present investigation, micronutrient composition of 35 food fishes (includes both finfishes and shellfishes) was investigated from varying aquatic habitats. Macrominerals (Na, K, Ca, Mg) and trace elements (Fe, Cu, Zn, Mn, Se) were determined by either atomic absorption spectroscopy (AAS) or inductively coupled plasma mass spectrometry (ICP-MS)/atomic emission spectrometry (ICP-AES). Phosphorus content was determined either spectrophotometrically or by ICP-AES. Fat-soluble vitamins (A, D, E, K) were analyzed by high-performance liquid chromatography (HPLC). The analysis showed that, in general, the marine fishes were rich in sodium and potassium; small indigenous fishes (SIFs) in calcium, iron, and manganese; coldwater fishes in selenium; and the brackishwater fishes in phosphorous. The marine fishes Sardinella longiceps and Epinephelus spp. and the SIFs were rich in all fat-soluble vitamins. All these recommendations were made according to the potential contribution (daily value %) of the species to the recommended daily allowance (RDA). Information on the micronutrients generated would enhance the utility of fish in both community and clinical nutrition.
Comparison of several analytical methods for the determination of tin in geochemical samples as a function of tin speciation

USGS Publications Warehouse

Kane, J.S.; Evans, J.R.; Jackson, J.C.

1989-01-01

Accurate and precise determinations of tin in geological materials are needed for fundamental studies of tin geochemistry, and for tin prospecting purposes. Achieving the required accuracy is difficult because of the different matrices in which Sn can occur (i.e. sulfides, silicates and cassiterite), and because of the variability of literature values for Sn concentrations in geochemical reference materials. We have evaluated three methods for the analysis of samples for Sn concentration: graphite furnace atomic absorption spectrometry (HGA-AAS) following iodide extraction, inductively coupled plasma atomic emission spectrometry (ICP-OES), and energy-dispersive X-ray fluorescence (EDXRF) spectrometry. Two of these methods (HGA-AAS and ICP-OES) required sample decomposition either by acid digestion or fusion, while the third (EDXRF) was performed directly on the powdered sample. Analytical details of all three methods, their potential errors, and the steps necessary to correct these errors were investigated. Results showed that similar accuracy was achieved from all methods for unmineralized samples, which contain no known Sn-bearing phase. For mineralized samples, which contain Sn-bearing minerals, either cassiterite or stannous sulfides, only EDXRF and fusion ICP-OES methods provided acceptable accuracy. This summary of our study provides information which helps to assure correct interpretation of data bases for underlying geochemical processes, regardless of method of data collection and its inherent limitations. ?? 1989.
An analytical method for hydrogeochemical surveys: Inductively coupled plasma-atomic emission spectrometry after using enrichment coprecipitation with cobalt and ammonium pyrrolidine dithiocarbamate

USGS Publications Warehouse

Hopkins, D.M.

1991-01-01

Trace metals that are commonly associated with mineralization were concentrated and separated from natural water by coprecipitation with ammonium pyrollidine dithiocarbamate (APDC) and cobalt and determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The method is useful in hydrogeochemical surveys because it permits preconcentration near the sample sites, and selected metals are preserved shortly after the samples are collected. The procedure is relatively simple: (1) a liter of water is filtered; (2) the pH is adjusted; (3) Co chloride and APDC are added to coprecipitate the trace metals; and (4) later, the precipitate is filtered, dissolved, and diluted to 10 ml for a 100-fold concentration enrichment of the separated metals. Sb(III), As(III), Cd, Cr, Cu, Fe, Pb, Mo, Ni, Ag, V, and Zn can then be determined simultaneously by ICP-AES. In an experiment designed to measure the coprecipitation efficiency, Sb(III), Cd and Ag were recovered at 70 to 75% of their original concentration. The remaining metals were recovered at 85 to 100% of their original concentrations, however. The range for the lower limits of determination for the metals after preconcentration is 0.1 to 3.0 ??g/l. The precision of the method was evaluated by replicate analyses of a Colorado creek water and two simulated water samples. The accuracy of the method was estimated using a water reference standard (SRM 1643a) certified by the U.S. National Bureau of Standards. In addition, the method was evaluated by analyzing groundwater samples collected near a porphyry copper deposit in Arizona and by analyzing meltwater from glacier-covered areas favorable for mineralization in south-central Alaska. The results for the ICP-AES analyses compared favorably with those obtained using the sequential technique of GFAAS on the acidified but unconcentrated water samples. ICP-AES analysis of trace-metal preconcentrates for hydrogeochemical surveys is more efficient than GFAAS because a large suite of metals is simultaneously determined with acceptable analytical accuracy and precision. The proposed analytical technique can provide direct evidence of mineralization and is useful in the exploration for unknown ore deposits. ?? 1991.
Minerals and Trace Elements in Milk, Milk Products, Infant Formula, and Adult/Pediatric Nutritional Formula, ICP-MS Method: Collaborative Study, AOAC Final Action 2015.06, ISO/DIS 21424, IDF 243.

PubMed

Pacquette, Lawrence H; Thompson, Joseph J; Malaviole, I; Zywicki, R; Woltjes, F; Ding, Y; Mittal, A; Ikeuchi, Y; Sadipiralla, B; Kimura, S; Veltman, H; Miura, A

2018-03-01

AOAC Final Action Official MethodSM 2015.06 "Minerals and Trace Elements in Milk, Milk Products, Infant Formula and Adult/Pediatric Nutritional Formula, ICP-MS Method" was collaboratively studied. Note that "milk, milk products" has now been added to the title of the Final Action method because whole milk and several dairy ingredients were successfully incorporated into the collaborative study for the purpose of developing an International Organization for Standardization/International Dairy Federation standard (ISO/DIS 21424; in progress). The method determines sodium, magnesium, phosphorus, potassium, calcium, iron, manganese, zinc, copper, chromium, molybdenum, and selenium by inductively coupled plasma (ICP)-MS after microwave digestion. Ten laboratories participated in the study, and data from five different model ICP-MS units were represented. Thirteen products, five placebo products, and six dairy samples were tested as blind duplicates in this study, along with a standard reference material, for a total 50 samples. The overall repeatability and reproducibility for all samples met Standard Method Performance Requirements put forth by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals, with a few exceptions. Comparisons are made to ICP-atomic emission data from a collaborative study of AOAC Official Method 2011.14 carried out concurrently on these same samples.
Rapid Precipitation of Amorphous Silica in Experimental Systems with Nontronite (NAu-1) and Shewanella oneidensis MR-1

DTIC Science & Technology

2007-01-15

law, no person shall be subject to any penalty for failing to comply with a collection of information if it does not display a currently valid OMB...report, we focus on the rapid bio- life because much of our current understanding of early life mineralization of amorphous silica. comes from...matter. The Nanoplast-embedded sample was atomic emission spectroscopy (ICP). After pH analysis ultrathin-sectioned, and examined with JEOL3010 TEM with a
The study on air pollution with nickel and vanadium in Croatia by using moss biomonitoring and ICP-AES.

PubMed

Vučković, Ivana; Špirić, Zdravko; Stafilov, Trajče; Kušan, Vladimir; Bačeva, Katerina

2013-10-01

Moss samples were collected from 121 sampling sites all over Croatia during the summer and autumn of 2010. They were totally digested by using microwave digestion system and analysed by using atomic emission spectrometry with inductively coupled plasma (ICP-AES). Descriptive statistics and maps of distribution were made. The data obtained in this study were compared with those from the study in 2006 and additionally with the data obtained in the similar studies in neighbouring countries and Norway as pristine area. The median value of nickel is 3.16 mg kg(-1) and the content varies from 1.04 to 14.66 mg kg(-1). The content of vanadium ranges between 0.23 and 37.26 mg kg(-1) with the median value of 2.55 mg kg(-1). High contents of these elements are found in the vicinity of Rijeka, Zagreb and Sisak as a result of their emission from oil refinery, thermal power plant and industrial processes.
Invention of the Annular Inductively Coupled Plasma as a Spectroscopic Source

NASA Astrophysics Data System (ADS)

Greenfield, Stanley

2000-05-01

This paper shows how experiments with electrical discharges from the 18th century onward led to their use as sources in atomic spectroscopy and how the invention of the annular inductively coupled plasma (ICP) some 30 years ago arose from the need to solve a problem that necessitated the use of a high-temperature source. The search for such a source followed a fairly logical pattern involving dc plasma jets and an ICP such as had been used by T. B. Reed for crystal growing. The ellipsoidal plasma used by Reed was not entirely suitable as a spectroscopic source, since the analytical sample either mixed with the plasma gases or passed around the plasma, resulting in matrix effects and a diminution in the emission. It is shown how suitable modification of the plasma torch with attention to gas flows made it possible to produce an annular or tunnel plasma through which the sample aerosol could be passed, resulting in an annular ICP with greatly improved spectroscopic properties. The further refinements to the source and ancillary equipment are also discussed.
The Determination of Metals in Sediment Pore Waters and in 1N HCl-Extracted Sediments by ICP-MS

USGS Publications Warehouse

May, T.W.; Wiedmeyer, Ray H.; Brumbaugh, W.G.; Schmitt, C.J.

1997-01-01

Concentrations of metals in sediment interstitial water (pore water) and those extractable from sediment with weak acids can provide important information about the bioavailability and toxicological effects of such contaminants. The highly variable nature of metal concentrations in these matrices requires instrumentation with the detection limit capability of graphite furnace atomic absorption and the wide dynamic linear range capability of ICP-OES. These criteria are satisfied with ICP-MS instrumentation. We investigated the performance of ICP-MS in the determination of certain metals from these matrices. The results for three metals were compared to those determined by graphite furnace atomic absorption spectroscopy. It was concluded that ICP-MS was an excellent instrumental approach for the determination of metals in these matrices.

Forensic analysis of printing inks using tandem Laser Induced Breakdown Spectroscopy and Laser Ablation Inductively Coupled Plasma Mass Spectrometry

NASA Astrophysics Data System (ADS)

Subedi, Kiran; Trejos, Tatiana; Almirall, José

2015-01-01

Elemental analysis, using either LA-ICP-MS or LIBS, can be used for the chemical characterization of materials of forensic interest to discriminate between source materials originating from different sources and also for the association of materials known to originate from the same source. In this study, a tandem LIBS/LA-ICP-MS system that combines the benefits of both LIBS and LA-ICP-MS was evaluated for the characterization of samples of printing inks (toners, inkjets, intaglio and offset.). The performance of both laser sampling methods is presented. A subset of 9 black laser toners, 10 colored (CMYK) inkjet samples, 12 colored (CMYK) offset samples and 12 intaglio inks originating from different manufacturing sources were analyzed to evaluate the discrimination capability of the tandem method. These samples were selected because they presented a very similar elemental profile by LA-ICP-MS. Although typical discrimination between different ink sources is found to be > 99% for a variety of inks when only LA-ICP-MS was used for the analysis, additional discrimination was achieved by combining the elemental results from the LIBS analysis to the LA-ICP-MS analysis in the tandem technique, enhancing the overall discrimination capability of the individual laser ablation methods. The LIBS measurements of the Ca, Fe, K and Si signals, in particular, improved the discrimination for this specific set of different ink samples previously shown to exhibit very similar LA-ICP-MS elemental profiles. The combination of these two techniques in a single setup resulted in better discrimination of the printing inks with two distinct fingerprint spectra, providing information from atomic/ionic emissions and isotopic composition (m/z) for each ink sample.
Evaluation of elemental profiling methods, including laser-induced breakdown spectroscopy (LIBS), for the differentiation of Cannabis plant material grown in different nutrient solutions.

PubMed

El-Deftar, Moteaa M; Robertson, James; Foster, Simon; Lennard, Chris

2015-06-01

Laser-induced breakdown spectroscopy (LIBS) is an emerging atomic emission based solid sampling technique that has many potential forensic applications. In this study, the analytical performance of LIBS, as well as that of inductively coupled plasma mass spectrometry (ICP-MS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and X-ray microfluorescence (μXRF), was evaluated for the ability to conduct elemental analyses on Cannabis plant material, with a specific investigation of the possible links between hydroponic nutrients and elemental profiles from associated plant material. No such study has been previously published in the literature. Good correlation among the four techniques was observed when the concentrations or peak areas of the elements of interest were monitored. For Cannabis samples collected at the same growth time, the elemental profiles could be related to the use of particular commercial nutrients. In addition, the study demonstrated that ICP-MS, LA-ICP-MS and LIBS are suitable techniques for the comparison of Cannabis samples from different sources, with high discriminating powers being achieved. On the other hand, μXRF method was not suitable for the discrimination of Cannabis samples originating from different growth nutrients. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.
[Convertibility of the data determined by ICP-AES and FAAS for soil available K and Na].

PubMed

Zhang, Jian-min; Wang, Meng; Ge, Xiao-ping; Wu, Jian-zhi; Ge, Ying; Li, Shi-peng; Chang, Jie

2009-05-01

In recent years, inductively coupled plasma atomic emission spectrometry (ICP-AES) have been commonly used to determine the soil available K and Na with the extraction solution of HCl-H2SO4, while previous data of soil available K and Na were measured by flame atomic absorption spectrometry (FAAS) with the extraction solution of NH4OAc. In order to utilize previous data, quest for the convertibility of the data determined by ICP-AES and FAAS, and compare the data determined by both methods, the authors chose four types of soil to determine soil available K and Na by ICP-AES and FAAS, respectively. Four types of soil represent grit soil, clay, silt from river and silt from sea, respectively. Soil samples included four types of soil and these samples represent different soil nutrition. The authors analyzed the correlations of two kinds of measured data. The paired samples t-test proves that there was significantly positively correlation between these two methods. The correlation coefficient of the data between these two methods for measuring soil available K is 0.98. The results of soil available K determined by the two methods can be conversed through the formula, y = l.14x + 6.53 (R2 = 0.91, n=24, p < 0.001). As for Na, although there is a significantly positively correlation between these two methods, the slopes of single model of clay and grit soil were different from that of general model. And so the results determined by the two methods can be conversed through different formula according to the types of soil, that is, for clay: y = l.23x + 10.03; for grit soil: y = 3.12x - 23.03; for silt: y = 0.60x. In conclusion, the authors' results showed that previous data of available K and Na measured by FAAS with the extraction solution of NH4OAc were available. And these data were comparable to the data measured by ICP-AES through definite formula The authors' results also suggested that ICP-AES was preferable when many elements were measured at the same time. Under this condition, ICP-AES was economical, efficient and reliable.
Study of the use of axial viewed inductively coupled plasma atomic emission spectrometry with ultrasonic nebulization for the determination of select elemental impurities in oral drug products.

PubMed

Menoutis, James; Parisi, Angela; Verma, Natasha

2018-04-15

In efforts to control the potential presence of heavy metals in pharmaceuticals, the United States Pharmacopeia (USP) and International Conference on Harmonization (ICH) have put forth new requirements and guidelines for their control. The new requirements and guidelines establish specific daily exposures (PDE) for 24 heavy metals/elemental impurities (EI) based upon their toxicological properties. USP General Chapter 〈233〉 provides a general reference procedure for preparing pharmaceutical samples for analysis employing microwave assisted digestion (MWAD). It also provides two Compendial Procedures, Procedure 1 employing ICP-AES, and Procedure 2 employing ICP-MS. Given the extremely low detection limits afforded by ICP-MS, much work has been done in developing and evaluating analytical methods to support the analysis of elemental impurities in finished pharmaceutical products, active pharmaceutical ingredients, and excipients by this analytical technique. In this study, we have evaluated the use of axial ICP-AES. This employs ultrasonic nebulization (UN) for the determination of Class 1 and 2 EI, instead of traditional pneumatic nebulization. The study also employed closed vessel MWAD to prepare samples for analysis. Limits of quantitation were element specific and significantly lower than the PDEs for oral drugs. Spike recoveries for the elements studied ranged between 89.3% and 109.25%, except for Os, which was subject to OsO4 formation during MWAD. The use of axial ICP-AES UN provides an alternative to ICP-MS in the analysis of EI requiring low detection limits. Copyright © 2018 Elsevier B.V. All rights reserved.
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 high concentrations of rubidium chloride by ICP-OES].

PubMed

Zhong, Yuan; Sun, Bai; Li, Hai-jun; Wang, Tao; Li, Wu; Song, Peng-sheng

2015-01-01

The method of ICP-OES for the direct determination of high content of rubidium in rubidium chloride solutions was studied through mass dilution method and optimizing parameters of the instrument in the present paper. It can reduce the times of dilution and the error introduced by the dilution, and improve the accuracy of determination results of rubidium. Through analyzing the sensitivity of the three detection spectral lines for rubidium ion, linearly dependent coefficient and the relative errors of the determination results, the spectral line of Rb 780. 023 nm was chosen as the most suitable wavelength to measure the high content of rubidium in the rubidium chloride solutions. It was found that the instrument parameters of ICP-OES such as the atomizer flow, the pump speed and the high-frequency power are the major factors for the determination of rubidium ion in the rubidium chloride solutions. As we know instrument parameters of ICP-OES have an important influence on the atomization efficiency as well as the emissive power of the spectral lines of rubidium, they are considered as the significant factors for the determination of rubidium. The optimization parameters of the instrument were obtained by orthogonal experiments and further single factor experiment, which are 0. 60 L . min-1 of atomizer flow, 60 r . min-1 of pump speed, and 1 150 W of high-frequency power. The same experiments were repeated a week later with the optimization parameters of the instrument, and the relative errors of the determination results are less than 0. 5% when the concentration of rubidium chloride ranged from 0. 09% to 0. 18%. As the concentration of rubidium chloride is 0. 06%, the relative errors of the determination results are -1. 7%. The determination of lithium chloride and potassium chloride in the high concentration of the aqueous solutions was studied under the condition of similar instrument parameters. It was found by comparison that the determination results of lithium chloride are better than that of potassium chloride and rubidium chloride. The method of ICP-OES used for determination of high content of rubidium is fast and simple for operation, and the results are accurate. It is suitable for studying the equilibrium in the salt-water system containing rubidium and for analysis of products of rubidium with high content.
Removal of Fe3+ and Zn2+ from plasma metalloproteins by iron chelating therapeutics depicted with SEC-ICP-AES.

PubMed

Sooriyaarachchi, Melani; Gailer, Jürgen

2010-08-28

The iron chelation therapy drugs desferrioxamine B (DFO) and deferiprone (DFP) are used to treat iron overload patients, but not much is known about their adverse effects on other essential metals in vivo. After the addition of a clinically relevant dose of DFP or an equimolar dose of DFO to human plasma in vitro, the mixtures were analyzed by size exclusion chromatography (SEC) coupled to an inductively coupled plasma atomic emission spectrometer (ICP-AES). Simultaneous detection of the emission lines of copper, iron and zinc allowed the visualization of changes that these drugs exerted at the metalloprotein level. After the addition of DFP, a <10 kDa novel Fe-peak was detected and identified as (DFP)(3)Fe, whereas DFO resulted in the elution of a much smaller amount of Fe in this elution range. In fact, DFP was approximately 8-times more efficient than DFO regarding the removal of Fe from plasma proteins. The addition of both iron chelators also resulted in the elution of a <10 kDa novel Zn-peak. DFP abstracted twice as much Zn from plasma proteins compared to DFO. The identification of one of these peaks as (DFP)(2)Zn establishes a feasible biomolecular basis for the etiology of Zn-deficiency in patients that undergo long-term treatment with these drugs. Our results demonstrate that the analysis of plasma by SEC-ICP-AES can simultaneously provide insight into the efficacy of chelation therapy drugs and their adverse health effects at the metalloprotein level. Thus, SEC-ICP-AES emerges as a useful analytical tool to visualize health-relevant bioinorganic chemistry-related reactions of medicinal drugs in blood plasma in vitro.
A table of polyatomic interferences in ICP-MS

USGS Publications Warehouse

May, Thomas W.; Wiedmeyer, Ray H.

1998-01-01

Spectroscopic interferences are probably the largest class of interferences in ICP-MS and are caused by atomic or molecular ions that have the same mass-to-charge as analytes of interest. Current ICP-MS instrumental software corrects for all known atomic “isobaric” interferences, or those caused by overlapping isotopes of different elements, but does not correct for most polyatomic interferences. Such interferences are caused by polyatomic ions that are formed from precursors having numerous sources, such as the sample matrix, reagents used for preparation, plasma gases, and entrained atmospheric gases.
Measurement of Trace Metals in Tobacco and Cigarette Ash by Inductively Coupled Plasma-Atomic Emission Spectroscopy

NASA Astrophysics Data System (ADS)

Wang, W.; Finlayson-Pitts, B. J.

2003-01-01

The ICP AES experiment reported here is suitable for use in a junior- or senior-level undergraduate instrumental analysis laboratory. The objective of this experiment is to analyze trace metals present in cigarette tobacco, the cigarette filter, and the ash obtained when the cigarette is burned. Two different brands of cigarettes, one with and one without a filter, were used. The filter was analyzed before and after smoke was drawn through it. The trace metals were extracted using concentrated nitric acid at room temperature and at 100 °C respectively, to test the extraction efficiency. Some tobacco samples were spiked with ZnCl2 and FeCl3 to assess the efficiency of the recovery. Zinc and iron are shown to be present in tobacco, filter, and ash, while chromium was above the detection limit only in the ash. These metals are concentrated in the ash compared to the tobacco by factors of ˜4 (Zn), 12 17 (Fe), and ≥ 2 (Cr). If sufficient laboratory time is available, this experiment could be paired with one using atomic absorption (AA) to demonstrate the advantages and disadvantages of ICP when compared to AA.
Profiling of patterned metal layers by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS)

NASA Astrophysics Data System (ADS)

Bi, Melody; Ruiz, Antonio M.; Gornushkin, Igor; Smith, Ben W.; Winefordner, James D.

2000-02-01

Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was used for profiling patterned thin metal layers on a polymer/silicon substrate. The parameters of the laser and ICP-MS operating conditions have been studied and optimized for this purpose. A new laser ablation chamber was designed and built to achieve the best spatial resolution. The results of the profiling by LA-ICP-MS were compared to those obtained from a laser ablation optical emission spectrometry (LA-OES) instrument, which measured the emission of the plasma at the sample surface, and thus, eliminated the time delay caused by the sample transport into the ICP-MS system. Emission spectra gave better spatial resolution than mass spectra. However, LA-ICP-MS provided much better sensitivity and was able to profile thin metal layers (on the order of a few nanometers) on the silicon surface. A lateral spatial resolution of 45 μm was achieved.
ICP OES and CV AAS in determination of mercury in an unusual fatal case of long-term exposure to elemental mercury in a teenager.

PubMed

Lech, Teresa

2014-04-01

In this work, a case of deliberate self-poisoning is presented. A 14-year-old girl suddenly died during one of the several hospitalizations. Abdominal computer tomography showed a large number of metallic particles in the large intestine. Analysis of blood and internal organs for mercury and other toxic metals carried out by inductively coupled plasma optical emission spectrometry (ICP OES) revealed high concentrations of mercury in kidneys and liver (64,200 and 2470ng/g, respectively), less in stomach (90ng/g), and none in blood. Using cold vapor-atomic absorption spectrometry (CV AAS), high levels of mercury were confirmed in all examined materials, including blood (87ng/g), and additionally in hair. The results of analysis obtained by two techniques revealed that the exposure to mercury was considerable (some time later, it was stated that the mercury originated from thermometers that had been broken over the course of about 1 year, because of Münchausen syndrome). CV AAS is a more sensitive technique, particularly for blood samples (negative results using ICP OES), and tissue samples - with LOQ: 0.63ng/g of Hg (CV AAS) vis-à-vis 70ng/g of Hg (ICP OES). However, ICP OES may be used as a screening technique for autopsy material in acute poisoning by a heavy metal, even one as volatile as mercury. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.
PM2.5 source apportionment in a French urban coastal site under steelworks emission influences using constrained non-negative matrix factorization receptor model.

PubMed

Kfoury, Adib; Ledoux, Frédéric; Roche, Cloé; Delmaire, Gilles; Roussel, Gilles; Courcot, Dominique

2016-02-01

The constrained weighted-non-negative matrix factorization (CW-NMF) hybrid receptor model was applied to study the influence of steelmaking activities on PM2.5 (particulate matter with equivalent aerodynamic diameter less than 2.5 μm) composition in Dunkerque, Northern France. Semi-diurnal PM2.5 samples were collected using a high volume sampler in winter 2010 and spring 2011 and were analyzed for trace metals, water-soluble ions, and total carbon using inductively coupled plasma--atomic emission spectrometry (ICP-AES), ICP--mass spectrometry (ICP-MS), ionic chromatography and micro elemental carbon analyzer. The elemental composition shows that NO3(-), SO4(2-), NH4(+) and total carbon are the main PM2.5 constituents. Trace metals data were interpreted using concentration roses and both influences of integrated steelworks and electric steel plant were evidenced. The distinction between the two sources is made possible by the use Zn/Fe and Zn/Mn diagnostic ratios. Moreover Rb/Cr, Pb/Cr and Cu/Cd combination ratio are proposed to distinguish the ISW-sintering stack from the ISW-fugitive emissions. The a priori knowledge on the influencing source was introduced in the CW-NMF to guide the calculation. Eleven source profiles with various contributions were identified: 8 are characteristics of coastal urban background site profiles and 3 are related to the steelmaking activities. Between them, secondary nitrates, secondary sulfates and combustion profiles give the highest contributions and account for 93% of the PM2.5 concentration. The steelwork facilities contribute in about 2% of the total PM2.5 concentration and appear to be the main source of Cr, Cu, Fe, Mn, Zn. Copyright © 2015. Published by Elsevier B.V.
Applying of Factor Analyses for Determination of Trace Elements Distribution in Water from River Vardar and Its Tributaries, Macedonia/Greece

PubMed Central

Popov, Stanko Ilić; Stafilov, Trajče; Šajn, Robert; Tănăselia, Claudiu; Bačeva, Katerina

2014-01-01

A systematic study was carried out to investigate the distribution of fifty-six elements in the water samples from river Vardar (Republic of Macedonia and Greece) and its major tributaries. The samples were collected from 27 sampling sites. Analyses were performed by mass spectrometry with inductively coupled plasma (ICP-MS) and atomic emission spectrometry with inductively coupled plasma (ICP-AES). Cluster and R mode factor analysis (FA) was used to identify and characterise element associations and four associations of elements were determined by the method of multivariate statistics. Three factors represent the associations of elements that occur in the river water naturally while Factor 3 represents an anthropogenic association of the elements (Cd, Ga, In, Pb, Re, Tl, Cu, and Zn) introduced in the river waters from the waste waters from the mining and metallurgical activities in the country. PMID:24587756
Applying of factor analyses for determination of trace elements distribution in water from Vardar and its tributaries, Macedonia/Greece.

PubMed

Popov, Stanko Ilić; Stafilov, Trajče; Sajn, Robert; Tănăselia, Claudiu; Bačeva, Katerina

2014-01-01

A systematic study was carried out to investigate the distribution of fifty-six elements in the water samples from river Vardar (Republic of Macedonia and Greece) and its major tributaries. The samples were collected from 27 sampling sites. Analyses were performed by mass spectrometry with inductively coupled plasma (ICP-MS) and atomic emission spectrometry with inductively coupled plasma (ICP-AES). Cluster and R mode factor analysis (FA) was used to identify and characterise element associations and four associations of elements were determined by the method of multivariate statistics. Three factors represent the associations of elements that occur in the river water naturally while Factor 3 represents an anthropogenic association of the elements (Cd, Ga, In, Pb, Re, Tl, Cu, and Zn) introduced in the river waters from the waste waters from the mining and metallurgical activities in the country.
Quantification of chemical elements in blood of patients affected by multiple sclerosis.

PubMed

Forte, Giovanni; Visconti, Andrea; Santucci, Simone; Ghazaryan, Anna; Figà-Talamanca, Lorenzo; Cannoni, Stefania; Bocca, Beatrice; Pino, Anna; Violante, Nicola; Alimonti, Alessandro; Salvetti, Marco; Ristori, Giovanni

2005-01-01

Although some studies suggested a link between exposure to trace elements and development of multiple sclerosis (MS), clear information on their role in the aetiology of MS is still lacking. In this study the concentrations of Al, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, Hg, Li, Mg, Mn, Mo, Ni, Pb, Sb, Si, Sn, Sr, Tl, V, W, Zn and Zr were determined in the blood of 60 patients with MS and 60 controls. Quantifications were performed by inductively coupled plasma (ICP) atomic emission spectrometry and sector field ICP mass spectrometry. When the two groups were compared, an increased level of Co, Cu and Ni and a decrement of Be, Fe, Hg, Mg, Mo, Pb and Zn in blood of patients were observed. In addition, the discriminant analysis pointed out that Cu, Be, Hg, Co and Mo were able to discriminate between MS patients and controls (92.5% of cases correctly classified).
Vaporization and atomization of uranium in a graphite tube electrothermal vaporizer: a mechanistic study using electrothermal vaporization inductively coupled plasma mass spectrometry and graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Goltz, D. M.; Grégoire, D. C.; Byrne, J. P.; Chakrabarti, C. L.

1995-07-01

The mechanism of vaporization and atomization of U in a graphite tube electrothermal vaporizer was studied using graphite furnace atomic absorption spectrometry (GFAAS) and electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS). Graphite furnace AAS studies indicate U atoms are formed at temperatures above 2400°C. Using ETV-ICP-MS, an appearance temperature of 1100°C was obtained indicating that some U vaporizes as U oxide. Although U carbides form at temperatures above 2000°C, ETV-ICP-MS studies show that they do not vaporize until 2600°C. In the temperature range between 2200°C and 2600°C, U atoms in GFAAS are likely formed by thermal dissociation of U oxide, whereas at higher temperatures, U atoms are formed via thermal dissociation of U carbide. The origin of U signal suppression in ETV-ICP-MS by NaCl was also investigated. At temperatures above 2000°C, signal suppression may be caused by the accelerated rate of formation of carbide species while at temperatures below 2000°C, the presence of NaCl may cause intercalation of the U in the graphite layers resulting in partial retention of U during the vaporization step. The use of 0.3% freon-23 (CHF 3) mixed with the argon carrier gas was effective in preventing the intercalation of U in graphite and U carbide formation at 2700°C.
Tree ring wood analysis after hydrogen peroxide pressure decomposition with inductively coupled plasma atomic emission spectrometry and electrothermal vaporization

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

Matusiewicz, H.; Barnes, R.M.

1985-02-01

A method utilizing pressure decomposition to minimize sample pretreatment is described for the inductively coupled plasma atomic emission spectrometric analysis of red spruce and sugar maple. Cores collected from trees growing on Camels Hump Mountain, Vermont, were divided into decade increments in order to monitor the temporal changes in concentrations of 21 elements. Dried wood samples were decomposed in a bomb made of Teflon with 50% hydrogen peroxide heated in an oven at 125/sup 0/C for 4 h. The digestion permitted use of aqueous standards and minimized any potential matrix effects. The element concentrations were obtained sequentially by electrothermal vaporizationmore » ICP-AES using 5 ..mu..L sample aliquots. The method precision varied between 3 and 12%. Elements forming oxyanions (Al, As, Fe, Ge, Mn, Si, V) were found at elevated concentrations during the most recent three decades, while other metal (e.g., Mg, Zn) concentrations were unchanged or decreased. 45 references, 6 tables, 1 figure.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)

Gregoire, D.C.; Goltz, D.M.; Chakrabarti, C.L.

Graphite furnace atomic absorption spectrometry (GFAAS) is an insensitive technique for determination of uranium. Experiments were conducted using electrothermal vaporization inductively coupled plasma mass spectrometry to investigate the atomization and vaporization of atomic and molecular uranium species in the graphite furnace. ETV-ICP-MS signals for uranium were observed at temperatures well below the appearance temperature of uranium atoms suggesting the vaporization of molecular uranium oxide at temperatures below 2000{degrees}C. Examination of individual uranium ETV-ICP-MS signals reveals the vaporization of uranium carbide at temperatures above 2600{degrees}C. Chemical modifiers such as 0.2% HF and 0.1% CHF{sub 3} in the argon carrier gas, weremore » ineffective in preventing the formation of uranium carbide at 2700{degrees}C. Vaporization of uranium from a tungsten surface using tungsten foil inserted into the graphite tube prevented the formation of uranium carbide and eliminated the ETV-ICP-MS signal suppression caused by a sodium chloride matrix.« less
Fluorescence quenching and the "ring-mode" to "red-mode" transition in alkali inductively coupled plasmas

NASA Astrophysics Data System (ADS)

Huang, M.; Bazurto, R.; Camparo, J.

2018-01-01

The ring-mode to red-mode transition in alkali metal inductively coupled plasmas (ICPs) (i.e., rf-discharge lamps) is perhaps the most important physical phenomenon affecting these devices as optical pumping light sources for atomic clocks and magnetometers. It sets the limit on useful ICP operating temperature, thereby setting a limit on ICP light output for atomic-clock/magnetometer signal generation, and it is a temperature region of ICP operation associated with discharge instability. Previous work has suggested that the mechanism driving the ring-mode to red-mode transition is associated with radiation trapping, but definitive experimental evidence validating that hypothesis has been lacking. Based on that hypothesis, one would predict that the introduction of an alkali-fluorescence quenching gas (i.e., N2) into the ICP would increase the ring-mode to red-mode transition temperature. Here, we test that prediction, finding direct evidence supporting the radiation-trapping hypothesis.
Matrix effects in inductively coupled plasma mass spectrometry

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

Chen, Xiaoshan

1995-07-07

The inductively coupled plasma is an electrodeless discharge in a gas (usually Ar) at atmospheric pressure. Radio frequency energy generated by a RF power source is inductively coupled to the plasma gas through a water cooled load coil. In ICP-MS the "Fassel" TAX quartz torch commonly used in emission is mounted horizontally. The sample aerosol is introduced into the central flow, where the gas kinetic temperature is about 5000 K. The aerosol is vaporized, atomized, excited and ionized in the plasma, and the ions are subsequently extracted through two metal apertures (sampler and skimmer) into the mass spectrometer. In ICP-MS,more » the matrix effects, or non-spectroscopic interferences, can be defined as the type of interferences caused by dissolved concomitant salt ions in the solution. Matrix effects can be divided into two categories: (1) signal drift due to the deposition of solids on the sampling apertures; and/or (2) signal suppression or enhancement by the presence of the dissolved salts. The first category is now reasonably understood. The dissolved salts, especially refractory oxides, tend to deposit on the cool tip of the sampling cone. The clogging of the orifices reduces the ion flow into the ICP-MS, lowers the pressure in the first stage of ICP-MS, and enhances the level of metal oxide ions. Because the extent of the clogging increases with the time, the signal drifts down. Even at the very early stage of the development of ICP-MS, matrix effects had been observed. Houk et al. found out that the ICP-MS was not tolerant to solutions containing significant amounts of dissolved solids.« less

Separation techniques for the clean-up of radioactive mixed waste for ICP-AES/ICP-MS analysis

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

Swafford, A.M.; Keller, J.M.

1993-03-17

Two separation techniques were investigated for the clean-up of typical radioactive mixed waste samples requiring elemental analysis by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) or Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). These measurements frequently involve regulatory or compliance criteria which include the determination of elements on the EPA Target Analyte List (TAL). These samples usually consist of both an aqueous phase and a solid phase which is mostly an inorganic sludge. Frequently, samples taken from the waste tanks contain high levels of uranium and thorium which can cause spectral interferences in ICP-AES or ICP-MS analysis. The removal of these interferences ismore » necessary to determine the presence of the EPA TAL elements in the sample. Two clean-up methods were studied on simulated aqueous waste samples containing the EPA TAL elements. The first method studied was a classical procedure based upon liquid-liquid extraction using tri-n- octylphosphine oxide (TOPO) dissolved in cyclohexane. The second method investigated was based on more recently developed techniques using extraction chromatography; specifically the use of a commercially available Eichrom TRU[center dot]Spec[trademark] column. Literature on these two methods indicates the efficient removal of uranium and thorium from properly prepared samples and provides considerable qualitative information on the extraction behavior of many other elements. However, there is a lack of quantitative data on the extraction behavior of elements on the EPA Target Analyte List. Experimental studies on these two methods consisted of determining whether any of the analytes were extracted by these methods and the recoveries obtained. Both methods produced similar results; the EPA target analytes were only slightly or not extracted. Advantages and disadvantages of each method were evaluated and found to be comparable.« less
Uncertainty Measurement for Trace Element Analysis of Uranium and Plutonium Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)

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

Gallimore, David L.

2012-06-13

The measurement uncertainty estimatino associated with trace element analysis of impurities in U and Pu was evaluated using the Guide to the Expression of Uncertainty Measurement (GUM). I this evalution the uncertainty sources were identified and standard uncertainties for the components were categorized as either Type A or B. The combined standard uncertainty was calculated and a coverage factor k = 2 was applied to obtain the expanded uncertainty, U. The ICP-AES and ICP-MS methods used were deveoped for the multi-element analysis of U and Pu samples. A typical analytical run consists of standards, process blanks, samples, matrix spiked samples,more » post digestion spiked samples and independent calibration verification standards. The uncertainty estimation was performed on U and Pu samples that have been analyzed previously as part of the U and Pu Sample Exchange Programs. Control chart results and data from the U and Pu metal exchange programs were combined with the GUM into a concentration dependent estimate of the expanded uncertainty. Comparison of trace element uncertainties obtained using this model was compared to those obtained for trace element results as part of the Exchange programs. This process was completed for all trace elements that were determined to be above the detection limit for the U and Pu samples.« less
Synthesis of cellulose functionalized with polyallylamine and its application to on-line collection/concentration and determination of phosphate by ICP/AES.

PubMed

Sumida, Takashi; Yamashita, Minoru; Okazaki, Yuka; Kawakita, Hirohisa; Fukutomi, Takashi

2012-01-01

A novel cellulose-based resin functionalized with polyallylamine was synthesized. It was applied to the collection of phosphate in environmental water samples, followed by concentration determination using an inductively coupled plasma-atomic emission spectrometer (ICP/AES). The synthesized resin, cellulose-glycidylmethacrylate-polyallylamine (CGP), showed good adsorption behavior toward trace amounts of phosphate over a wide pH range. The adsorbed-analyte can be easily eluted using 0.5 M hydrochloric acid; its recoveries was found to be 80 - 100%. The CGP resin synthesized was packed in a mini-column, which was then installed in a computer-controlled auto-pretreatment system for on-line collection/concentration and determination of trace phosphate by ICP/AES. The limit of detection for phosphate was found to be 0.6 µg P l(-1). The sample volumes were only 5 ml and the total analysis time was about 4 min. The developed method with CGP resin was successfully applied to the determination of phosphate in river water and tap water samples with satisfactory results. The recovery test showed that common matrices that may exist in environmental waters did not interfere with the determination of phosphate.
Comparison of MP AES and ICP-MS for analysis of principal and selected trace elements in nitric acid digests of sunflower (Helianthus annuus).

PubMed

Karlsson, Stefan; Sjöberg, Viktor; Ogar, Anna

2015-04-01

The use of nitrogen as plasma gas for microwave plasma atomic emission spectroscopy (MP AES) is an interesting development in analytical science since the running cost can be significantly reduced in comparison to the inductively coupled argon plasma. Here, we evaluate the performance of the Agilent 4100 MP AES instrument for the analysis of principal metals (Ca, K, Mg, and Na), lithogenic metals (Al, Fe, and Mn) and selected trace metals (As, Ba, Cd, Co, Cr, Cu, Mo, Ni, Pb, V, and Zn) in nitric acid plant digests. The digests were prepared by microwave-assisted dissolution of dry plant material from sunflower (Helianthus annuus) in concentrated nitric acid. Comparisons are made with analysis of the same solutions with ICP-MS (Agilent 7500cx) using the octopole reaction system (ORS) in the collision mode for As, Fe, and V. The limits of detection were usually in the low µg L(-1) range and all principal and lithogenic metals were successfully determined with the MP AES and provided almost identical results with the ICP-MS. The same applies for the selected trace metals except for As, Co and Mo where the concentrations were below the detection limit with the MP AES. For successful analysis we recommend that (i) only atom lines are used, (ii) ionization is minimized (e.g. addition of CsNO3) and (iii) the use of internal standards should be considered to resolve spectral interferences. Copyright © 2014 Elsevier B.V. All rights reserved.
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.
Tank 40 Final Sludge Batch 8 Chemical Characterization Results

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

Bannochie, Christopher J.

2013-09-19

A sample of Sludge Batch 8 (SB8) was pulled from Tank 40 in order to obtain radionuclide inventory analyses necessary for compliance with the Waste Acceptance Product Specifications (WAPS). The SB8 WAPS sample was also analyzed for chemical composition, including noble metals, and fissile constituents, and these results are reported here. These analyses along with the WAPS radionuclide analyses will help define the composition of the sludge in Tank 40 that is currently being fed to the Defense Waste Processing Facility (DWPF) as SB8. At SRNL, the 3-L Tank 40 SB8 sample was transferred from the shipping container into amore » 4-L high density polyethylene bottle and solids were allowed to settle. Supernate was then siphoned off and circulated through the shipping container to complete the transfer of the sample. Following thorough mixing of the 3-L sample, a 553 g sub-sample was removed. This sub-sample was then utilized for all subsequent slurry sample preparations. Eight separate aliquots of the slurry were digested, four with HNO{sub 3}/HCl (aqua regia) in sealed Teflon(r) 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 SB8 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-/other base, total inorganic carbon/total organic carbon (TIC/TOC) analyses. 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 developed by SRNL AD and previously described.« less
Tank 40 final sludge batch 9 chemical and fissile radionuclide characterization results

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

Bannochie, C. J.; Kubilius, W. P.; Pareizs, J. M.

A sample of Sludge Batch (SB) 9 was pulled from Tank 40 in order to obtain radionuclide inventory analyses necessary for compliance with the Waste Acceptance Product Specifications (WAPS)i. The SB9 WAPS sample was also analyzed for chemical composition, including noble metals, and fissile constituents, and these results are reported here. These analyses along with the WAPS radionuclide analyses will help define the composition of the sludge in Tank 40 that is fed to the Defense Waste Processing Facility (DWPF) as SB9. At the Savannah River National Laboratory (SRNL), the 3-L Tank 40 SB9 sample was transferred from the shippingmore » container into a 4-L high density polyethylene bottle and solids were allowed to settle. Supernate was then siphoned off and circulated through the shipping container to complete the transfer of the sample. Following thorough mixing of the 3-L sample, a 547 g sub-sample was removed. This sub-sample was then utilized for all subsequent slurry sample preparations. Eight separate aliquots of the slurry were digested, four with HNO3/HCl (aqua regiaii) in sealed Teflon® vessels and four with NaOH/Na2O2 (alkali or peroxide fusioniii) using Zr crucibles. Three Analytical Reference Glass – 1iv (ARG-1) standards were digested along with a blank for each preparation. Each aqua regia digestion and blank was diluted to 1:100 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 SB9 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-/other base, total inorganic carbon/total organic carbon (TIC/TOC) analyses. 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 SB9 WAPS slurry using the specific activity of each isotope. The Pu-241 value was determined from a Pu-238/-241 method developed by SRNL AD and previously described.v« less
Vacuum ultraviolet photon fluxes in argon-containing inductively coupled plasmas

NASA Astrophysics Data System (ADS)

Radovanov, S. B.; Persing, H. M.; Wang, S.; Culver, C. L.; Boffard, J. B.; Lin, C. C.; Wendt, A. E.

2013-09-01

Vacuum ultraviolet (VUV) photons emitted from excited atomic states are ubiquitous in material processing plasmas. Damage of materials is induced by energy transfer from the VUV photons to the surface, causing disorder in the surface region, surface reactions, and affecting bonds in the material bulk. Monitoring of the surface flux of VUV photons from inductively coupled plasmas (ICP) and its dependence on discharge parameters is thus highly desirable. Results of non-invasive, direct windowless VUV detection using a photosensitive diode will be presented. Relative VUV fluxes were also obtained using a sodium salicylate coating on the inside of a vacuum window, converting VUV into visible light detected through the vacuum window. The coating is sensitive to wavelengths in the range 80-300 nm, while the photodiode is only sensitive to wavelengths below 120 nm. In argon the VUV emissions are primarily produced by spontaneous decay from 3p5 4 s resonance levels (1s2,1s4) and may be reabsorbed by ground state atoms. Real-time resonance level concentrations were measured and used to predict the VUV photon flux at the detector for a range of different ICP pressures, powers, and for various admixtures of Ar with N2, and H2. This work was supported in part by NSF grant PHY-1068670.
Stream-sediment samples reanalyzed for major, rare earth, and trace elements from ten 1:250,000-scale quadrangles, south-central Alaska, 2007-08

USGS Publications Warehouse

Bailey, Elizabeth A.; Shew, Nora B.; Labay, Keith A.; Schmidt, Jeanine M.; O'Leary, Richard M.; Detra, David E.

2010-01-01

During the 1960s through the 1980s, the U.S. Geological Survey (USGS) conducted reconnaissance geochemical surveys of the drainage basins throughout most of the Anchorage, Bering Glacier, Big Delta, Gulkana, Healy, McCarthy, Mount Hayes, Nabesna, Talkeetna Mountains, and Valdez 1:250,000-scale quadrangles in Alaska as part of the Alaska Mineral Resource Assessment Program (AMRAP). These geochemical surveys provide data necessary to assess the potential for undiscovered mineral resources on public and other lands, and provide data that may be used to determine regional-scale element baselines. This report provides new data for 366 of the previously collected stream-sediment samples. These samples were selected for reanalysis because recently developed analytical methods can detect additional elements of interest and have lower detection limits than the methods used when these samples were originally analyzed. These samples were all analyzed for arsenic by hydride generation atomic absorption spectrometry (HGAAS), for gold, palladium, and platinum by inductively coupled plasma-mass spectrometry after lead button fire assay separation (FA/ICP-MS), and for a suite of 55 major, rare earth, and trace elements by inductively coupled plasma-atomic emission spectrometry and inductively coupled plasma-mass spectrometry (ICP-AES-MS) after sodium peroxide sinter at 450 degrees Celsius.
Using ICP and micro-PIXE to investigate possible differences in the mineral composition of genetically modified versus wild-type sorghum grain

NASA Astrophysics Data System (ADS)

Ndimba, R.; Cloete, K.; Mehlo, L.; Kossmann, J.; Mtshali, C.; Pineda-Vargas, C.

2017-08-01

In the present study, possible differences in the mineral composition of transgenic versus non-transgenic sorghum grains were investigated using inductively coupled atomic emission spectroscopy (ICP-AES); and, in-tissue elemental mapping by micro Proton-Induced X-ray Emission (micro-PIXE) analysis. ICP AES was used to analyse the bulk mineral content of the wholegrain flour derived from each genotype; whilst micro-PIXE was used to interrogate localised differences in mineral composition specific to certain areas of the grain, such as the bran layer and the central endosperm tissue. According to the results obtained, no significant difference in the average Fe, Zn or Ca content was found to differentiate the transgenic from the wild-type grain using ICP-AES. However, using micro-PIXE, a significant reduction in zinc could be detected in the bran layer of the transgenic grains relative to wild-type. Although it is difficult to draw firm conclusions, as a result of the small sample size used in this study, micro-PIXE has nonetheless proven itself as a useful technique for highlighting the possibility that there may be reduced levels of zinc accumulation in the bran layer of the transgenic grains. Given that the genetic modification targets proteins that are highly concentrated in certain parts of the bran tissue, it seems plausible that the reduced levels of zinc may be an unintended consequence of the silencing of kafirin proteins. Although no immediate health or nutritional concerns emerge from this preliminary finding, it is noted that zinc plays an important biological role within this part of the grain as a structural stabiliser and antioxidant factor. Further study is therefore needed to assess more definitively the extent of the apparent localised reduction in zinc in the transgenic grains and how this may affect other important grain quality characteristics.
Ionomic profiling of Nicotiana langsdorffii wild-type and mutant genotypes exposed to abiotic stresses.

PubMed

Ardini, Francisco; Soggia, Francesco; Abelmoschi, Maria Luisa; Magi, Emanuele; Grotti, Marco

2013-01-01

To provide a new insight into the response of plants to abiotic stresses, the ionomic profiles of Nicotiana langsdorffii specimens have been determined before and after exposure to toxic metals (chromium) or drought conditions. The plants were genetically transformed with the rat glucocorticoid receptor (GR) or the gene for Agrobacterium rhizogenes rolC, because these modifications are known to produce an imbalance in phytohormone equilibria and a significant change in the defence response of the plant. Elemental profiles were obtained by developing and applying analytical procedures based on inductively coupled plasma atomic emission and mass spectrometry (ICP-AES/MS). In particular, the removal of isobaric interferences affecting the determination of Cr and V by ICP-MS was accomplished by use of a dynamic reaction cell, after optimization of the relevant conditions. The combined use of ICP atomic emission and mass spectrometry enabled the determination of 29 major and trace elements (Ba, Bi, Ca, Cd, Co, Cr, Cu, Eu, Fe, Ga, K, Li, Mg, Mn, Mo, Na, P, Pb, Pt, Rb, S, Sb, Sn, Sr, Te, V, W, Y, and Zn) in different parts of the plants (roots, stems, and leaves), with high accuracy and precision. Multivariate data processing and study of element distribution patterns provided new information about the ionomic response of the target organism to chemical treatment or water stress. Genetic modification mainly affected the distribution of Bi, Cr, Mo, Na, and S, indicating that these elements were involved in biochemical processes controlled by the GR or rolC genes. Chemical stress strongly affected accumulation of several elements (Ba, Ca, Fe, Ga, K, Li, Mn, Mo, Na, P, Pb, Rb, S, Sn, Te, V, and Zn) in different ways; for Ca, Fe, K, Mn, Na, and P the effect was quite similar to that observed in other studies after treatment with other transition elements, for example Cu and Cd. The effect of water deficit was less evident, mainly consisting in a decrease of Ba, Cr, Na, and Sr in roots.
Flotation-separation and ICP-AES determination of ultra trace amounts of copper, cadmium, nickel and cobalt using 2-aminocyclopentene-1-dithiocarboxylic acid.

PubMed

Shamsipur, Mojtaba; Hashemi, Omid Reza; Safavi, Afsaneh

2005-09-01

A rapid flotation method for separation and enrichment of ultra trace amounts of copper(II), cadmium(II), nickel(II) and cobalt(II) ions from water samples is established. At pH 6.5 and with sodium dodecylsulfate used as a foaming reagent, Cu2+, Cd2+, Ni2+ and Co2+ were separated simultaneously with 2-aminocyclopentene-1-dithiocarboxylic acid (ACDA) added to 1 l of aqueous solution. The proposed procedure of preconcentration is applied prior to the determination of these four analytes using inductivity coupled plasma-atomic emission spectrometry (ICP-AES). The effects of pH, concentration of ACDA, applicability of different surfactants and foreign ions on the separation efficiency were investigated. The preconcentration factor of the method is 1000 and the detection limits of copper(II), cadmium(II), nickel(II) and cobalt(II) ions are 0.078, 0.075, 0.072 and 0.080 ng ml(-1), respectively.
Migration of components from cork stoppers to food: challenges in determining inorganic elements in food simulants.

PubMed

Corona, T; Iglesias, M; Anticó, E

2014-06-18

The inorganic elements potentially migrating from cork to a food simulant [a hydroalcoholic solution containing 12 and 20% (v/v) ethanol] have been determined by means of inductively coupled plasma (ICP) with atomic emission and mass spectrometric detection. The experimental instrumental conditions were evaluated in depth, taking into account spectroscopic and nonspectroscopic interference caused by the presence of ethanol and other components in the sample. We report concentrations ranging from 4 μg kg(-1) for Cd to 28000 μg kg(-1) for Al in the food simulant (concentrations given in kilograms of cork). The values found for Ba, Mn, Fe, Cu, and Zn have been compared with the guideline values stated in EU Regulation 10/2011. In all cases, cork met the general safety criteria applicable to food contact material. Finally, we have proposed water as an alternative to the hydroalcoholic solution to simplify quantification of the tested elements using ICP techniques.
The deposition of gold nanoparticles in MWCNT forests

NASA Astrophysics Data System (ADS)

de Jong, Franciscus; Buffet, Adeline; Schlueter, Michael

2015-11-01

The deposition, i.e. transport and attachment, of small-sized particles is a basic process, on which many applications are based. The innumerable applications range from biology and medicine to engineering. Due to their promising mechanical properties multi-walled carbon nanotubes (MWCNTs) have gained increasing popularity in the past decade. A large number of dense packed vertically aligned MWCNTs form a so-called MWCNT forest. In our study we functionalized the MWCNT forest to filter gold nanoparticles from a colloidal suspension. An experimental investigation was carried out in which the particle deposition kinetics was locally determined with small-angle X-ray scattering (SAXS). Furthermore, inductively coupled plasma atomic emission spectroscopy (ICP-AES) was used to verify the local observations. It was concluded that both, SAXS and ICP-AES investigations shows very good agreement. Furthermore, an analytical deposition model was developed based on the DLVO-theory. The experimental and theoretical investigation presented here give insight in the deposition kinetics within a MWCNT forest. The results open up pathways to optimize MWCNT forests for filtering purposes.
Determination of Minor and Trace Metals in Aluminum and Aluminum Alloys by ICP-AES; Evaluation of the Uncertainty and Limit of Quantitation from Interlaboratory Testing.

PubMed

Uemoto, Michihisa; Makino, Masanori; Ota, Yuji; Sakaguchi, Hiromi; Shimizu, Yukari; Sato, Kazuhiro

2018-01-01

Minor and trace metals in aluminum and aluminum alloys have been determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) as an interlaboratory testing toward standardization. The trueness of the measured data was successfully investigated to improve the analytical protocols, using certified reference materials of aluminum. Their precision could also be evaluated, feasible to estimate the uncertainties separately. The accuracy (trueness and precision) of the data were finally in good agreement with the certified values and assigned uncertainties. Repeated measurements of aluminum solutions with different concentrations of the analytes revealed the relative standard deviations of the measurements with concentrations, thus enabling their limits of quantitation. They differed separately and also showed slightly higher values with an aluminum matrix than those without one. In addition, the upper limit of the detectable concentration of silicon with simple acid digestion was estimated to be 0.03 % in the mass fraction.
Evaluation of inorganic elements in cat's claw teas using ICP OES and GF AAS.

PubMed

Pereira, João B; Dantas, Kelly G F

2016-04-01

The determination of Ba, Ca, Cu, Fe, Mg, Mn, P, Pb, and Zn by inductively coupled plasma optical emission spectrometry (ICP OES), and Se by graphite furnace atomic absorption spectrometry (GF AAS), has been carried out in dry matter and teas from 11 samples of the cat's claw plant. The accuracy and precision values were verified against GBW 07604 (Poplar leaves) certified reference material and by the recovery test. Results showed a high content of Ca in the medicinal plant studied, followed by Mg and P. The values obtained showed that the elements studied have different concentrations depending on the method of tea preparation. The highest levels were observed in Ca and Mg, and the lowest for Se and Pb, by both infusion and decoction. Teas prepared from this plant were found to be at safe levels for human consumption, and may be suitable as sources of these elements in the human diet. Copyright © 2015 Elsevier Ltd. All rights reserved.
Simplified multi-element analysis of ground and instant coffees by ICP-OES and FAAS.

PubMed

Szymczycha-Madeja, Anna; Welna, Maja; Pohl, Pawel

2015-01-01

A simplified alternative to the wet digestion sample preparation procedure for roasted ground and instant coffees has been developed and validated for the determination of different elements by inductively coupled plasma optical emission spectrometry (ICP-OES) (Al, Ba, Cd, Co, Cr, Cu, Mn, Ni, Pb, Sr, Zn) and flame atomic absorption spectrometry (FAAS) (Ca, Fe, K, Mg, Na). The proposed procedure, i.e. the ultrasound-assisted solubilisation in aqua regia, is quite fast and simple, requires minimal use of reagents, and demonstrated good analytical performance, i.e. accuracy from -4.7% to 1.9%, precision within 0.5-8.6% and recovery in the range 93.5-103%. Detection limits of elements were from 0.086 ng ml(-1) (Sr) to 40 ng ml(-1) (Fe). A preliminary classification of 18 samples of ground and instant coffees was successfully made based on concentrations of selected elements and using principal component analysis and hierarchic cluster analysis.
ICP-AES Determination of Mineral Content in Boletus tomentipes Collected from Different Sites of China.

PubMed

Wang, Xue-mei; Zhang, Ji; Li, Tao; Li, Jie-qing; Wang, Yuan-zhong; Liu, Hong-gao

2015-05-01

P, Na, Ca, Cu, Fe, Mg, Zn, As, Cd, Co, Cr and Ni, contents have been examined in caps and stipes of Boletus tomentipes collected from different sites of Yunnan province, southwest China. The elements were determined using inductively coupled plasma atomic emission spectroscopy (ICP-AES) with microwave digestion. P, Ca, Mg, Fe, Zn and Cu were the most abundant amongst elements determined in Boletus tomentipes. The caps were richer in P, Mg, Zn and Cd, and the stipes in Ca, Co and Ni. Cluster analysis showed a difference between Puer (BT7 and BT8) and other places. The PCA explained about 77% of the total variance, and the minerals differentiating these places were P (PC1) together with Ca, Cu, Fe, Mg, As and Ni, Na (PC2) together with Cd, and Zn (PC3). The results of this study imply that element concentrations of a mushroom are mutative when collected from the different bedrock soil geochemistry.
[Determination of ru, rh and Pd in 30% trialkyl phosphine oxide (TRPO)-kerosene by inductively coupled plasma-atomic emission spectrum (ICP-AES)].

PubMed

Wang, Jian-Chen; Zhang, Lin

2013-07-01

The determination method of Ru, Rh and Pd in 30% TRPO-kerosene ICP-AES was studied by using aqueous calibration reference solution and choosing ethanol as diluent. The effects of the contents of 30% TRPO-kerosene and aqueous solution and the concentration of HNO3 in 30% TRPO-kerosene on the intensities of Ru, Rh and Pd were described. The optimized condition for preparing samples and calibration solutions was chosen as follows: The contents of 30% TRPO-kerosene and aqueous phase were 10% (V/V) and 5% (V/V) respectively and the concentration of HNO3 30% TRPO-kerosene was 0.20 mol x L(-1). The determination method of Au, Ru and Pd was set up according to the above condition. The detection limit, precision and recovery ratio of Ru, Rh and Pd are well. The method is not only used in determination of Au, Ru and Pd in 30% TRPO-kerosene, but also used in other organic phases.
Spatial distribution and historical trends of heavy metals in the sediments of petroleum producing regions of the Beibu Gulf, China.

PubMed

Yang, Jichao; Wang, Weiguo; Zhao, Mengwei; Chen, Bin; Dada, Olusegun A; Chu, Zhihui

2015-02-15

The concentrations of As, Sb, Hg, Pb, Cd, and Ba in the surface and core sediments of the oil and gas producing region of the Beibu Gulf were measured by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), Inductively Coupled Plasma Mass Spectrometry (ICP-MS) and Atomic Fluorescence Spectrometry (AFS), and the spatial distribution and historical trends of these elements are discussed. The results show that the concentrations of these elements are highest near the platforms. The results of Enrichment Factor (EF) and Potential Ecological Risk Index (PERI) also reveal significantly higher enrichment around the platforms, which imply that the offshore petroleum production was the cause of the unusual distribution and severe enrichment of these elements in the study area. The environment around the platforms was highly laden with toxic elements, thereby representing a very high ecological risk to the environment of the study area. Copyright © 2014 Elsevier Ltd. All rights reserved.

40 CFR Table 2 to Subpart Llll of... - Emission Limits and Standards for New Multiple Hearth Sewage Sludge Incineration Units

Code of Federal Regulations, 2013 CFR

2013-07-01

... meters per run) Performance test (Method 29 at 40 CFR part 60, appendix A-8). Use GFAAS or ICP/MS for the...-8. Use GFAAS or ICP/MS for the analytical finish. Fugitive emissions from ash handling Visible...
40 CFR Table 2 to Subpart Llll of... - Emission Limits and Standards for New Multiple Hearth Sewage Sludge Incineration Units

Code of Federal Regulations, 2014 CFR

2014-07-01

... meters per run) Performance test (Method 29 at 40 CFR part 60, appendix A-8). Use GFAAS or ICP/MS for the...-8. Use GFAAS or ICP/MS for the analytical finish. Fugitive emissions from ash handling Visible...
ICP-AES determination of minor- and major elements in apples after microwave assisted digestion.

PubMed

Juranović Cindrić, Iva; Krizman, Ivona; Zeiner, Michaela; Kampić, Štefica; Medunić, Gordana; Stingeder, Gerhard

2012-12-15

The aim of this paper was to determine the content of minor and major elements in apples by inductively coupled plasma atomic emission spectrometry (ICP-AES). Prior to ICP-AES measurement, dried apples were digested in a microwave assisted digestion system. The differences in the measured element concentrations after application of open and closed microwave system as sample preparation procedures are discussed. In whole apples, flesh and peel Ag, Al, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Sr and Zn were analysed after optimisation and validating the analytical method using ICP-AES. The accuracy of the method determined by spiking experiments was very good (recoveries 88-115%) and the limits of detection of elements of interest were from 0.01 up to 14.7 μg g(-1). The reference ranges determined in all apple samples are 39-47 mg g(-1) for K, 9-14 mg g(-1) for Na, 3-7 mg g(-1) for Mg, 3-7 μg g(-1) for Zn, 0.7-2.8 μg g(-1) for Sr. The range of Mn in peel 4-6 μg g(-1) is higher compared to whole apple from 0.7 to 1.7 μg g(-1). Cd is found only in peel, in the concentration range of 0.4-1.1 μg g(-1). Copyright © 2012 Elsevier Ltd. All rights reserved.
Determination of Microelements in Human Milk and Infant Formula Without Digestion by ICP-OES.

PubMed

Đurović, Dijana; Milisavljević, Branka; Nedović-Vuković, Mirjana; Potkonjak, Branislav; Spasić, Snežana; Vrvić, Miroslav

2017-06-01

The concentrations of zinc (Zn), iron (Fe) and copper (Cu) in both human milk and infant formula were determined using a new sample preparation method, by inductively coupled plasma - optical emission spectometry (ICP-OES) and flame atomic absorption spectrometry (FAAS). Human milk samples were diluted in ultrapure water. The infant formula of powder samples (suitable for an infant 1-6 months of age) and standard reference material (SRM-1849) were analyzed in parallel. The results have shown that FAAS method was more sensitive for Fe determination in human milk while ICP-OES was more sensitive for both Zn and Cu detection. The limit of quantification for both Zn and Cu was 5 μg L-1 and 10 μg L-1 for Fe and the recovery for Zn, Fe and Cu was ranged from 90% to 94%, 97% to 103% and 90% to 102%, respectively. Mean concentrations of Zn, Fe, and Cu in human milk samples were 5.35, 0.47 and 0.83 mg L-1, respectively while these values in infant formula were ranged from 3.52-4.75 mg L-1, 3.37-4.56 mg L-1 and 0.28-0.41 mg L-1, respectively. Despite the sample complexity, the proposed method using dilution of milk samples with water was simple, rapid, effective and accurate. ICP-OES was a better method for Zn determination while FAAS was a better method for Fe determination. In the case of Cu both methods were comparable.
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.
Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Elements in Whole-Water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry

USGS Publications Warehouse

Garbarino, John R.; Struzeski, Tedmund M.

1998-01-01

Inductively coupled plasma-optical emission spectrometry (ICP-OES) and inductively coupled plasma-mass spectrometry (ICP-MS) can be used to determine 26 elements in whole-water digests. Both methods have distinct advantages and disadvantages--ICP-OES is capable of analyzing samples with higher elemental concentrations without dilution, however, ICP-MS is more sensitive and capable of determining much lower elemental concentrations. Both techniques gave accurate results for spike recoveries, digested standard reference-water samples, and whole-water digests. Average spike recoveries in whole-water digests were 100 plus/minus 10 percent, although recoveries for digests with high dissolved-solid concentrations were lower for selected elements by ICP-MS. Results for standard reference-water samples were generally within 1 standard deviation of hte most probable values. Statistical analysis of the results from 43 whole-water digest indicated that there was no significant difference among ICP-OES, ICP-MS, and former official methods of analysis for 24 of the 26 elements evaluated.
Biomass burning in Indo-China peninsula and its impacts on regional air quality and global climate change-a review.

PubMed

Yadav, Ishwar Chandra; Linthoingambi Devi, Ningombam; Li, Jun; Syed, Jabir Hussain; Zhang, Gan; Watanabe, Hirozumi

2017-08-01

Although, many biomass burning (BB) emissions products (particulate matter and trace gases) are believed to be trans-boundary pollutants that originates from India and China (the two most populous countries in Asia), the information about BB emission and related contents is limited for Indo-China Peninsula (ICP) region. This motivated us to review this region pertaining to BB emission. The main objective of the review is to document the current status of BB emission in ICP region. In order to highlight the impact of BB on regional air quality and global climate change, the role of BB emission in ICP region is also discussed. Based on the available literature and modeling simulations studies, it is evidenced that ICP is one of the hotspot regional source for aerosols in terms of BB emissions. In addition, regional emissions through BB have significant implications for regional air quality especially in the neighboring countries such as China, Taiwan and India. Our assessment highlight that there is still a general lack of reliable data and research studies addressing BB related issues in context of environmental and human health. There is therefore a critical need to improve the current knowledge base, which should build upon the research experience and further research into these issues is considered vital to help inform future policies/control strategies. Copyright © 2017 Elsevier Ltd. All rights reserved.
Tandem Laser Induced Breakdown Spectroscopy (LIBS), Laser Ablation Inductively Coupled Plasma Mass Spectroscopy (LA-ICP-MS) and/or Laser Ablation Inductively Coupled Plasma Optical Emission Spectroscopy (LA-ICP-OES) for the analysis of samples of geological interest

NASA Astrophysics Data System (ADS)

Oropeza, D.

2016-12-01

A highly innovative laser ablation sampling instrument (J200 Tandem LA - LIBS) that combines the capabilities and analytical benefits of LIBS, LA-ICP-MS and LA-ICP-OES was used for micrometer-scale, spatially-resolved, elemental analysis of a wide variety of samples of geological interest. Data collected using ablation systems consisted of nanosecond (Nd:YAG operated 266nm) and femtosecond lasers (1030 and 343nm). An ICCD LIBS detector and Quadrupole based mass spectrometer were selected for LIBS and ICP-MS detection, respectively. This tandem instrument allows simultaneous determination of major and minor elements (for example, Si, Ca, Na, and Al, and trace elements such as Li, Ce, Cr, Sr, Y, Zn, Zr among others). The research also focused on elemental mapping and calibration strategies, specifically the use of emission and mass spectra for multivariate data analysis. Partial Least Square Regression (PLSR) is shown to minimize and compensate for matrix effects in the emission and mass spectra improving quantitative analysis by LIBS and LA-ICP-MS, respectively. The study provides a benchmark to evaluate analytical results for more complex geological sample matrices.
Determination of Fe, Hg, Mn, and Pb in three-rings of poplar (Populus alba L.) by U-shaped DC arc

NASA Astrophysics Data System (ADS)

Marković, D. M.; Novović, I.; Vilotić, D.; Ignjatović, Lj.

2007-09-01

The U-shaped DC arc with aerosol supply was applied for the determination of Fe, Hg, Mn, and Pb in poplar (Populus alba L.) tree-rings. By optimization of the operating parameters and by selection of the most appropriate signal integration time (20 s for Fe, Mn, and Pb and 30 s for Hg), the obtained limits of detection for Fe, Hg, Mn, and Pb are 5.8, 2.6, 1.6, and 2.0 ng/ml, respectively. The detection limits achieved by this method for Fe, Hg, Mn, and Pb are comparable with the detection limits obtained for these elements by such methods as inductively coupled plasma-atomic emission spectrometry (ICP-AES), direct coupled plasmatomic emission spectrometry (DCP-AES), and microwave-induced plasma-atomic emission spectrometry (MIP-AES). We used the tree-rings of poplar from two different locations. The first one is in the area close to the power plant “Nikola Tesla” TENT A, Obrenovac, while the other one is in the urban area of Novi Sad. In almost all cases, samples from the location at Obrenovac registered elevated average concentrations of Fe, Hg, Mn, and Pb in the tree-rings of poplar.
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.
Converting oil shale to liquid fuels: energy inputs and greenhouse gas emissions of the Shell in situ conversion process.

PubMed

Brandt, Adam R

2008-10-01

Oil shale is a sedimentary rock that contains kerogen, a fossil organic material. Kerogen can be heated to produce oil and gas (retorted). This has traditionally been a CO2-intensive process. In this paper, the Shell in situ conversion process (ICP), which is a novel method of retorting oil shale in place, is analyzed. The ICP utilizes electricity to heat the underground shale over a period of 2 years. Hydrocarbons are produced using conventional oil production techniques, leaving shale oil coke within the formation. The energy inputs and outputs from the ICP, as applied to oil shales of the Green River formation, are modeled. Using these energy inputs, the greenhouse gas (GHG) emissions from the ICP are calculated and are compared to emissions from conventional petroleum. Energy outputs (as refined liquid fuel) are 1.2-1.6 times greater than the total primary energy inputs to the process. In the absence of capturing CO2 generated from electricity produced to fuel the process, well-to-pump GHG emissions are in the range of 30.6-37.1 grams of carbon equivalent per megajoule of liquid fuel produced. These full-fuel-cycle emissions are 21%-47% larger than those from conventionally produced petroleum-based fuels.
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
Essential and toxic elements in meat of wild birds.

PubMed

Roselli, Carla; Desideri, Donatella; Meli, Maria Assunta; Fagiolino, Ivan; Feduzi, Laura

2016-01-01

Essential and toxic elements were determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES), mass spectrometry (MS), and atomic absorption (AS) in meat of 14 migratory birds originating from central and northern Europe to provide baseline data regarding game meat consumed in central Italy. In all samples analyzed, cobalt (Co) and chromium (Cr) (total) levels were <0.326 mg/kg ww . For nonessential or toxic elements, arsenic (As), barium (Ba), cadmium (Cd), stannous (Sn), thallium (Tl), tellurium (Te), titanium (Ti), cerium (Ce), lantanium (La), and uranium (U) concentrations were <0.326 mg/kg ww, thorium (Th) <1.63 mg/kg ww , and mercury (Hg) <0.0163 mg/kg ww . When detectable, lead (Pb) concentrations always exceeded maximal admissible levels for metal (0.1 mg/kg ww ) established by the European Commission for meat. These findings indicate that elevated Pb concentrations in game ingested by humans may be a cause for concern.
Dissolution and precipitation behaviors of silicon-containing ceramic coating on Mg-Zn-Ca alloy in simulated body fluid.

PubMed

Pan, Yaokun; Chen, Chuanzhong; Wang, Diangang; Huang, Danlan

2014-10-01

We prepared Si-containing and Si-free coatings on Mg-1.74Zn-0.55Ca alloy by micro-arc oxidation. The dissolution and precipitation behaviors of Si-containing coating in simulated body fluid (SBF) were discussed. Corrosion products were characterized by scanning electron microscope (SEM), X-ray diffractometer (XRD), fourier transform infrared spectrometer (FT-IR) and X-ray photoelectron spectrometer (XPS). Electrochemical workstation, inductively coupled plasma atomic emission spectrometer (ICP-AES), flame atomic absorption spectrophotometer (AAS) and pH meter were employed to detect variations of electrochemical parameter and ions concentration respectively. Results indicate that the fast formation of calcium phosphates is closely related to the SiOx(n-) groups, which induce the heterogeneous nucleation of amorphous hydroxyapatite (HA) by sorption of calcium and phosphate ions. Copyright © 2014 Elsevier B.V. All rights reserved.
Nanometer-sized ceria-coated silica-iron oxide for the reagentless microextraction/preconcentration of heavy metals in environmental and biological samples followed by slurry introduction to ICP-OES.

PubMed

Dados, A; Paparizou, E; Eleftheriou, P; Papastephanou, C; Stalikas, C D

2014-04-01

A slurry suspension sampling technique is developed and optimized for the rapid microextraction of heavy metals and analysis using nanometer-sized ceria-coated silica-iron oxide particles and inductively coupled plasma optical emission spectrometry (ICP-OES). Magnetic-silica material is synthesized by a co-precipitation and sol-gel method followed by ceria coating through a precipitation. The large particles are removed using a sedimentation-fractionation procedure and a magnetic homogeneous colloidal suspension of ceria-modified iron oxide-silica is produced for microextraction. The nanometer-sized particles are separated from the sample solution magnetically and analyzed with ICP-OES using a slurry suspension sampling approach. The ceria-modified iron oxide-silica does not contain any organic matter and this probably justifies the absence of matrix effect on plasma atomization capacity, when increased concentrations of slurries are aspirated. The As, Be, Mo, Cr, Cu, Pb, Hg, Sb, Se and V can be preconcentrated by the proposed method at pH 6.0 while Mn, Cd, Co and Ni require a pH ≥ 8.0. Satisfactory values are obtained for the relative standard deviations (2-6%), recoveries (88-102%), enrichment factors (14-19) and regression correlation coefficients as well as detectability, at sub-μg L(-1) levels. The applicability of magnetic ceria for the microextraction of metal ions in combination with the slurry introduction technique using ICP is substantiated by the analysis of environmental water and urine samples. Copyright © 2013 Elsevier B.V. All rights reserved.
Inductively Coupled Plasma Optical Emission Spectrometry for Rare Earth Elements Analysis

NASA Astrophysics Data System (ADS)

He, Man; Hu, Bin; Chen, Beibei; Jiang, Zucheng

2017-01-01

Inductively coupled plasma optical emission spectrometry (ICP-OES) merits multielements capability, high sensitivity, good reproducibility, low matrix effect and wide dynamic linear range for rare earth elements (REEs) analysis. But the spectral interference in trace REEs analysis by ICP-OES is a serious problem due to the complicated emission spectra of REEs, which demands some correction technology including interference factor method, derivative spectrum, Kalman filtering algorithm and partial least-squares (PLS) method. Matrix-matching calibration, internal standard, correction factor and sample dilution are usually employed to overcome or decrease the matrix effect. Coupled with various sample introduction techniques, the analytical performance of ICP-OES for REEs analysis would be improved. Compared with conventional pneumatic nebulization (PN), acid effect and matrix effect are decreased to some extent in flow injection ICP-OES, with higher tolerable matrix concentration and better reproducibility. By using electrothermal vaporization as sample introduction system, direct analysis of solid samples by ICP-OES is achieved and the vaporization behavior of refractory REEs with high boiling point, which can easily form involatile carbides in the graphite tube, could be improved by using chemical modifier, such as polytetrafluoroethylene and 1-phenyl-3-methyl-4-benzoyl-5-pyrazone. Laser ablation-ICP-OES is suitable for the analysis of both conductive and nonconductive solid samples, with the absolute detection limit of ng-pg level and extremely low sample consumption (0.2 % of that in conventional PN introduction). ICP-OES has been extensively employed for trace REEs analysis in high-purity materials, and environmental and biological samples.
[Development of ICP-OES, ICP-MS and GF-AAS Methods for Simultaneous Quantification of Lead, Total Arsenic and Cadmium in Soft Drinks].

PubMed

Kataoka, Yohei; Watanabe, Takahiro; Hayashi, Tomoko; Teshima, Reiko; Matsuda, Rieko

2015-01-01

In this study, we developed methods to quantify lead, total arsenic and cadmium contained in various kinds of soft drinks, and we evaluated their performance. The samples were digested by common methods to prepare solutions for measurement by ICP-OES, ICP-MS and graphite furnace atomic absorption spectrometry (GF-AAS). After digestion, internal standard was added to the digestion solutions for measurements by ICP-OES and ICP-MS. For measurement by GF-AAS, additional purification of the digestion solution was conducted by back-extraction of the three metals into nitric acid solution after extraction into an organic solvent with ammonium pyrrolidine dithiocarbamate. Performance of the developed methods were evaluated for eight kinds of soft drinks.
Elemental profiling and geographical differentiation of Ethiopian coffee samples through inductively coupled plasma-optical emission spectroscopy (ICP-OES), ICP-mass spectrometry (ICP-MS) and direct mercury analyzer (DMA).

PubMed

Habte, Girum; Hwang, In Min; Kim, Jae Sung; Hong, Joon Ho; Hong, Young Sin; Choi, Ji Yeon; Nho, Eun Yeong; Jamila, Nargis; Khan, Naeem; Kim, Kyong Su

2016-12-01

This study was aimed to establish the elemental profiling and provenance of coffee samples collected from eleven major coffee producing regions of Ethiopia. A total of 129 samples were analyzed for forty-five elements using inductively coupled plasma (ICP)-optical emission spectroscopy (OES), ICP-mass spectrometry (MS) and direct mercury analyzer (DMA). Among the macro elements, K showed the highest levels whereas Fe was found to have the lowest concentration values. In all the samples, Ca, K, Mg, P and S contents were statistically significant (p<0.05). Micro elements showed the concentrations order of: Mn>Cu>Sr>Zn>Rb>Ni>B. Contents of the trace elements were lower than the permissible standard values. Inter-regions differentiation by cluster analysis (CA), linear discriminant analysis (LDA) and principal component analysis (PCA) showed that micro and trace elements are the best chemical descriptors of the analyzed coffee samples. Copyright © 2016 Elsevier Ltd. All rights reserved.
Application of plasma gas modulation technique for improvement of the measurement of Mn emission intensity in ICP-AES.

PubMed

Kubota, K; Wagatsuma, K

2001-01-02

A phase-sensitive detection technique associated with a digital lock-in amplifier was applied for an improvement of the detection in ICP-AES. The lock-in amplifier works as an extremely narrow band pass filter. It can pick up the modulated signal, which has the same frequency as the reference signal, from any noise and thus it can improve the signal-to-noise ratio. Modulation of the ICP can be performed by mixing small amounts of air to argon as the outer gas cyclically, because the emission intensities of ionic lines are enhanced by using the mixed gas. An electromagnetic valve, which is placed in the outer-gas flow path, causes periodic variation in the air gas in the outer-gas flow, and thus switching the valve on/off can modulate the ICP. By choosing the appropriate conditions, the addition of air gas enhances the emission intensity of ionic lines more than that of the background, thus leading to improved signal-to-background ratios. At the same time the lock-in amplifier further enhances the ionic emissions because it picks up only the modulated part of the signal. By applying the plasma gas flow modulation technique the detection and the determination limits of the Mn II 257.610 nm line are improved in comparison with the conventional method. A change in plasma shape corresponding to the modulation frequency is observed when the ICP is modulated.
A novel methodology for rapid digestion of rare earth element ores and determination by microwave plasma-atomic emission spectrometry and dynamic reaction cell-inductively coupled plasma-mass spectrometry.

PubMed

Helmeczi, Erick; Wang, Yong; Brindle, Ian D

2016-11-01

Short-wavelength infrared radiation has been successfully applied to accelerate the acid digestion of refractory rare-earth ore samples. Determinations were achieved with microwave plasma-atomic emission spectrometry (MP-AES) and dynamic reaction cell - inductively coupled plasma-mass spectrometry (DRC-ICP-MS). The digestion method developed was able to tackle high iron-oxide and silicate matrices using only phosphoric acid in a time frame of only 8min, and did not require perchloric or hydrofluoric acid. Additionally, excellent recoveries and reproducibilities of the rare earth elements, as well as uranium and thorium, were achieved. Digestions of the certified reference materials OREAS-465 and REE-1, with radically different mineralogies, delivered results that mirror those obtained by fusion processes. For the rare-earth CRM OKA-2, whose REE data are provisional, experimental data for the rare-earth elements were generally higher than the provisional values, often exceeding z-values of +2. Determined values for Th and U in this reference material, for which certified values are available, were in excellent agreement. Copyright © 2016 Elsevier B.V. All rights reserved.

Concentrations of mercury and other metals in black bass (Micropterus spp.) from Whiskeytown Lake, Shasta County, California, 2005

USGS Publications Warehouse

May, Jason T.; Hothem, Roger L.; Bauer, Marissa L.; Brown, Larry R.

2012-01-01

This report presents the results of a reconnaissance study conducted by the U.S. Geological Survey (USGS) to determine mercury (Hg) and other selected metal concentrations in Black bass (Micropterus spp.) from Whiskeytown Lake, Shasta County, California. Total mercury concentrations were determined by cold-vapor atomic absorption spectroscopy (CVAAS) in fillets and whole bodies of each sampled fish. Selected metals scans were performed on whole bodies (less the fillets) by inductively coupled plasma–mass spectroscopy (ICP-MS) and inductively coupled plasma–optical emission spectroscopy (ICP-OES). Mercury concentrations in fillet samples ranged from 0.06 to 0.52 micrograms per gram (μg/g) wet weight (ww). Total mercury (HgT) in the same fish whole-body samples ranged from 0.04 to 0.37 (μg/g, ww). Mercury concentrations in 17 percent of "legal catch size" (≥305 millimeters in length) were above the U.S. Environmental Protection Agency water-quality criterion for the protection of human health of 0.30 μg/g (ww). These data will serve as a baseline for future monitoring efforts within Whiskeytown Lake.
Leaching behavior of U, Mn, Sr, and Pb from different particle-size fractions of uranium mill tailings.

PubMed

Liu, Bo; Peng, Tongjiang; Sun, Hongjuan

2017-06-01

Pollution by the release of heavy metals from tailings constitutes a potential threat to the environment. To characterize the processes governing the release of Mn, Sr, Pb, and U from the uranium mill tailings, a dynamic leaching test was applied for different size of uranium mill tailings samples. Inductively coupled plasma atomic emission spectroscopy (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS) were performed to determine the content of Mn, Sr, Pb, and U in the leachates. The release of mobile Mn, Sr, Pb, and U fraction was slow, being faster in the initial stage and then attained a near steady-state condition. The experimental results demonstrate that the release of Mn, Sr, Pb, and U from uranium mill tailings with different size fractions is controlled by a variety of mechanisms. Surface wash-off is the release mechanism for Mn. The main release mechanism of Sr and Pb is the dissolution in the initial leaching stage. For U, a mixed process of wash-off and diffusion is the controlling mechanism.
[Determination and principal component analysis of mineral elements based on ICP-OES in Nitraria roborowskii fruits from different regions].

PubMed

Yuan, Yuan-Yuan; Zhou, Yu-Bi; Sun, Jing; Deng, Juan; Bai, Ying; Wang, Jie; Lu, Xue-Feng

2017-06-01

The content of elements in fifteen different regions of Nitraria roborowskii samples were determined by inductively coupled plasma-atomic emission spectrometry(ICP-OES), and its elemental characteristics were analyzed by principal component analysis. The results indicated that 18 mineral elements were detected in N. roborowskii of which V cannot be detected. In addition, contents of Na, K and Ca showed high concentration. Ti showed maximum content variance, while K is minimum. Four principal components were gained from the original data. The cumulative variance contribution rate is 81.542% and the variance contribution of the first principal component was 44.997%, indicating that Cr, Fe, P and Ca were the characteristic elements of N. roborowskii.Thus, the established method was simple, precise and can be used for determination of mineral elements in N.roborowskii Kom. fruits. The elemental distribution characteristics among N.roborowskii fruits are related to geographical origins which were clearly revealed by PCA. All the results will provide good basis for comprehensive utilization of N.roborowskii. Copyright© by the Chinese Pharmaceutical Association.
Spark ablation-inductively coupled plasma spectrometry for analysis of geologic materials

USGS Publications Warehouse

Golightly, D.W.; Montaser, A.; Smith, B.L.; Dorrzapf, A.F.

1989-01-01

Spark ablation-inductively coupled plasma (SA-ICP) spectrometry is applied to the measurement of hafnium-zirconium ratios in zircons and to the determination of cerium, cobalt, iron, lead, nickel and phosphorus in ferromanganese nodules. Six operating parameters used for the high-voltage spark and argon-ICP combination are established by sequential simplex optimization of both signal-to-background ratio and signal-to-noise ratio. The time-dependences of the atomic emission signals of analytes and matrix elements ablated from a finely pulverized sample embedded in a pressed disk of copper demonstrate selective sampling by the spark. Concentration ratios of hafnium to zirconium in zircons are measured with a precision of 4% (relative standard deviation, RSD). For ferromanganese nodules, spectral measurements based on intensity ratios of analyte line to the Mn(II) 257.610 nm line provide precisions of analysis in the range from 7 to 14% RSD. The accuracy of analysis depends on use of standard additions of the reference material USGS Nod P-1, and an independent measurement of the Mn concentration. ?? 1989.
Anchoring of Cu(II) onto surface of porous metal-organic framework through post-synthesis modification for the synthesis of benzimidazoles and benzothiazoles

NASA Astrophysics Data System (ADS)

Kardanpour, Reihaneh; Tangestaninejad, Shahram; Mirkhani, Valiollah; Moghadam, Majid; Mohammadpoor-Baltork, Iraj; Zadehahmadi, Farnaz

2016-03-01

Efficient synthesis of various benzimidazoles and benzothiazoles under mild conditions catalyzed by Cu(II) anchored onto UiO-66-NH2 metal organic framework is reported. In this manner, first, the aminated UiO-66 was modified with thiophene-2-carbaldehyde and then the prepared Schiff base was reacted with CuCl2. The prepared catalyst was characterized by FT-IR, UV-vis, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), N2 adsorption, inductively coupled plasma atomic emission spectroscopy (ICP-AES) and field emission scanning electron microscopy (FE-SEM). The UiO-66-NH2-TC-Cu was applied as a highly efficient catalyst for synthesis of benzimidazole and benzothiazole derivatives by the reaction of aldehydes with 1,2-diaminobenzene or 2-aminothiophenol. The Cu(II)-containing MOF was reused several times without any appreciable loss of its efficiency.
Efficient alkene epoxidation catalyzed by molybdenyl acetylacetonate supported on aminated UiO-66 metal-organic framework

NASA Astrophysics Data System (ADS)

Kardanpour, Reihaneh; Tangestaninejad, Shahram; Mirkhani, Valiollah; Moghadam, Majid; Mohammadpoor-Baltork, Iraj; Zadehahmadi, Farnaz

2015-03-01

Metal-organic frameworks (MOFs) containing Mo Schiff base complexes were prepared by post-synthesis method and applied as efficient catalysts in the epoxidation of alkenes with tert-BuOOH. In this manner, UiO-66-NH2 (UiO=University of Oslo) MOF was reacted with salicylaldehyde and thiophene-2-carbaldehyde to produce bidentate Schiff bases. Then, the Schiff base ligands were used for immobilization of molybdenyl acetylacetonate. These new catalysts were characterized by FT-IR, UV-vis spectroscopic techniques, X-ray diffraction (XRD), BET, inductively coupled plasma atomic emission spectroscopy (ICP-AES) and field emission scanning electron microscopy (FE-SEM). These catalytic systems showed excellent activity in the epoxidation of alkenes such as cyclic and linear ones with tert-butyl hydroperoxide (TBHP) in 1,2-dichloroethane, and reused several times without any appreciable loss of their activity.
Depleted uranium mobility across a weapons testing site: isotopic investigation of porewater, earthworms, and soils.

PubMed

Oliver, Ian W; Graham, Margaret C; MacKenzie, Angus B; Ellam, Robert M; Farmer, John G

2008-12-15

The mobility and bioavailability of depleted uranium (DU) in soils at a UK Ministry of Defence (UK MoD) weapons testing range were investigated. Soil and vegetation were collected near a test-firing position and at eight points along a transect line extending approximately 200 m down-slope, perpendicular to the firing line, toward a small stream. Earthworms and porewaters were subsequently separated from the soils and both total filtered porewater (<0.2 microm) and discrete size fractions (0.2 microm-100 kDa, 100-30 kDa, 30-3 kDa, and <3 kDa)obtainedvia centrifugal ultrafiltration were examined. Uranium concentrations were determined by inductively coupled plasma optical emission spectrometry (ICP-OES) for soils and ICP-mass spectrometry (MS) for earthworms and porewaters, while 235U:238U atom ratios were determined by multicollector (MC)-ICP-MS. Comparison of the porewater and earthworm isotopic values with those of the soil solids indicated that DU released into the environment during weapons test-firing operations was more labile and more bioavailable than naturally occurring U in the soils at the testing range. Importantly, DU was shown to be present in soil porewater even at a distance of approximately 185 m from the test-firing position and, along the extent of the transect was apparently associated with organic colloids.
[Determination of Fe, Ti and V in vanadium and titanium magnetite by ICP-OES and microwave-assisted digestion].

PubMed

Zhu, Xia-ping; Yin, Ji-xian; Chen, Wei-dong; Hu, Zi-Wen; Liang, Qing-xun; Chen, Tie-yao

2010-08-01

The method of determination of iron, titanium and vanadium in indissolvable vanadium and titanium magnetite has been established by inductively coupled plasma atomic emission spectroscopy through adding the complexant A and using microwave-assisted digestion. The optimal conditions are confirmed by orthogonal experiment: 0.1 g vanadium and titanium magnetite, 0.04 g complexant A, 12 mL concentrated HC1, 10 min digestion time, and 385 W microwave power. The newly-established method has been applied to digest vanadium and titanium magnetite of Panzhihua Iron and Steel Institute (GBW07226). The iron, titanium and vanadium were detected by ICP-OES, and both comparative error (Er%) and comparative standard deviation (RSD%) met the demand of analytical chemistry, and the complexant A can significantly accelerate the dissolution of vanadium and titanium magnetite through the complexation with the dissolved metal ions, and making the surface of sample and hydrochloric acid medium to update constantly. The determination of the main and trace elements of digestion solution at the same time was achieved by ICP-OES. The method has the advantages of less use of reagents, economy, rapidness, and being friendly to environment, and it meets the requirement for rapid and volume determination. So the method has the value of practical application for the entry-exit inspection and quarantine department of the state and other relevant inspection units.
[Performance comparison of material tests for cadmium and lead in food contact plastics].

PubMed

Mutsuga, Motoh; Abe, Tomoyuki; Abe, Yutaka; Ishii, Rie; Itoh, Yuko; Ohno, Hiroyuki; Ohno, Yuichiro; Ozaki, Asako; Kakihara, Yoshiteru; Kaneko, Reiko; Kawamura, Yoko; Shibata, Hiroshi; Sekido, Haruko; Sonobe, Hironori; Takasaka, Noriko; Tajima, Yoshiyasu; Tanaka, Aoi; Nomura, Chie; Hikida, Akinori; Matsuyama, Sigetomo; Murakami, Ryo; Yamaguchi, Miku; Wada, Takenari; Watanabe, Kazunari; Akiyama, Hiroshi

2014-01-01

Based on the Japanese Food Sanitation Law, the performances of official and alternative material test methods for cadmium (Cd) and lead (Pb) in food contact plastics were compared. Nineteen laboratories participated to an interlaboratory study, and quantified Cd and Pb in three PVC pellets. in the official method, a sample is digested with H2SO4, taken up in HCl, and evaporated to dryness on a water bath, then measured by atomic absorption spectrometry (AAS) or inductively coupled plasma-optical emission spectrometry (ICP-OES). Statistical treatment revealed that the trueness, repeatability (RSDr) and reproducibility (RSDr) were 86-95%, 3.1-9.4% and 8.6-22.1%, respectively. The values of the performance parameters fulfilled the requirements , and the performances met the test specifications. The combination of evaporation to dryness on a hot plate and measurement by AAS or ICP-OES is applicable as an alternative method. However, the trueness and RSDr were inferior to those of the official method. The performance parameters obtained by using the microwave digestion method (MW method) to prepare test solution were better than those of the official method. Thus, the MW method is available as an alternative method. Induced coupled plasma-mass spectrometry (ICP-MS) is also available as an alternative method. However, it is necessary to ensure complete digestion of the sample.
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.
Examination Of Sulfur Measurements In DWPF Sludge Slurry And SRAT Product Materials

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

Bannochie, C. J.; Wiedenman, B. J.

2012-11-29

Savannah River National Laboratory (SRNL) was asked to re-sample the received SB7b WAPS material for wt. % solids, perform an aqua regia digestion and analyze the digested material by inductively coupled plasma - atomic emission spectroscopy (ICP-AES), as well as re-examine the supernate by ICP-AES. The new analyses were requested in order to provide confidence that the initial analytical subsample was representative of the Tank 40 sample received and to replicate the S results obtained on the initial subsample collected. The ICP-AES analyses for S were examined with both axial and radial detection of the sulfur ICP-AES spectroscopic emission linesmore » to ascertain if there was any significant difference in the reported results. The outcome of this second subsample of the Tank 40 WAPS material is the first subject of this report. After examination of the data from the new subsample of the SB7b WAPS material, a team of DWPF and SRNL staff looked for ways to address the question of whether there was in fact insoluble S that was not being accounted for by ion chromatography (IC) analysis. The question of how much S is reaching the melter was thought best addressed by examining a DWPF Slurry Mix Evaporator (SME) Product sample, but the significant dilution of sludge material, containing the S species in question, that results from frit addition was believed to add additional uncertainty to the S analysis of SME Product material. At the time of these discussions it was believed that all S present in a Sludge Receipt and Adjustment Tank (SRAT) Receipt sample would be converted to sulfate during the course of the SRAT cycle. A SRAT Product sample would not have the S dilution effect resulting from frit addition, and hence, it was decided that a DWPF SRAT Product sample would be obtained and submitted to SRNL for digestion and sample preparation followed by a round-robin analysis of the prepared samples by the DWPF Laboratory, F/H Laboratories, and SRNL for S and sulfate. The results of this round-robin analytical study are the second subject of this report.« less
[The application of inductively coupled plasma atomic emission spectrometry/mass spectrometry to the analysis of advanced ceramic materials].

PubMed

Wang, Zheng; Wang, Shi-Wei; Qiu, De-Ren; Yang, Peng-Yuan

2009-10-01

Advanced ceramics have been applied to various important fields such as information science, aeronautics and astronautics, and life sciences. However, the optics and electric properties of ceramics are significantly affected by the micro and trace impurities existing in the material even at very low concentration level. Thus, the accurate determination of impurities is important for materials preparation and performance. Methodology of the analysis of advanced ceramic materials using ICP-AES/MS was reviewed in the present paper for the past decade. Various techniques of sample introduction, especially advances in the authors' recent work, are described in detail. The developing trend is also presented. Sixty references are cited.
Synthesis and study of the synthetic hydroxyapatite doped with aluminum

NASA Astrophysics Data System (ADS)

Goldberg, M.; Smirnov, V.; Antonova, O.; Konovalov, A.; Fomina, A.; Komlev, V. S.; Barinov, S.; Rodionov, A.; Gafurov, M.; Orlinskii, S.

2018-05-01

Powders of synthetic hydroxyapatite doped with aluminium (Al) ions in concentrations 0 and 20 mol. % were synthesized by the precipitation method from the nitrate solutions and investigated by atomic emission spectrometry with inductively coupled plasma (AES-ICP), X-ray diffraction (XRD), scanning electron microscopy (SEM), gas absorption and conventional electron paramagnetic resonance (EPR). It is shown that for the chosen synthesis route an introduction of Al provokes formation of highly anisotropic phase, leads to the decrease in the crystallinity while no significant changes in the EPR spectra of the radiation-induced defects is observed. The results could be used for understanding the structural transformations with Al doping of the mineralized materials for geological and biomedical applications.
Quantification of 60Fe atoms by MC-ICP-MS for the redetermination of the half-life.

PubMed

Kivel, Niko; Schumann, Dorothea; Günther-Leopold, Ines

2013-03-01

In many scientific fields, the half-life of radionuclides plays an important role. The accurate knowledge of this parameter has direct impact on, e.g., age determination of archeological artifacts and of the elemental synthesis in the universe. In order to derive the half-life of a long-lived radionuclide, the activity and the absolute number of atoms have to be analyzed. Whereas conventional radiation measurement methods are typically applied for activity determinations, the latter can be determined with high accuracy by mass spectrometric techniques. Over the past years, the half-lives of several radionuclides have been specified by means of multiple-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) complementary to the earlier reported values mainly derived by accelerator mass spectrometry. The present paper discusses all critical aspects (amount of material, radiochemical sample preparation, interference correction, isotope dilution mass spectrometry, calculation of measurement uncertainty) for a precise analysis of the number of atoms by MC-ICP-MS exemplified for the recently published half-life determination of 60Fe (Rugel et al, Phys Rev Lett 103:072502, 2009).
The influence of ns- and fs-LA plume local conditions on the performance of a combined LIBS/LA-ICP-MS sensor

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

LaHaye, Nicole L.; Phillips, Mark C.; Duffin, Andrew M.

2016-01-01

Both laser-induced breakdown spectroscopy (LIBS) and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) are well-established analytical techniques with their own unique advantages and disadvantages. The combination of the two analytical methods is a very promising way to overcome the challenges faced by each method individually. We made a comprehensive comparison of local plasma conditions between nanosecond (ns) and femtosecond (fs) laser ablation (LA) sources in a combined LIBS and LA-ICP-MS system. The optical emission spectra and ICP-MS signal were recorded simultaneously for both ns- and fs-LA and figures of merit of the system were analyzed. Characterization of the plasma was conductedmore » by evaluating temperature and density of the plume under various irradiation conditions using optical emission spectroscopy, and correlations to ns- and fs-LIBS and LA-ICP-MS signal were made. The present study is very useful for providing conditions for a multimodal system as well as giving insight into how laser ablation plume parameters are related to LA-ICP-MS and LIBS results for both ns- and fs-LA.« less
The influence of soil pH and humus content on received by Mehlich 3 method nutrients analysis results

NASA Astrophysics Data System (ADS)

Tonutare, Tonu; Krebstein, Kadri; Rodima, Ako; Kõlli, Raimo; Künnapas, Allan; Rebane, Jaanus; Penu, Priit; Vennik, Kersti; Soobik, Liina

2015-04-01

Soils provide vital ecosystem functions, playing an important role in our economy and in healthy living environment. However, soils are increasingly degrading in Europe and at the global level. Knowledge about the content of major plant available nutrients, i.e. calcium, magnesium, potassium and phosphorus, plays an important role in the sustainable soil management. Mobility of nutrients depends directly on the environmental conditions, two of the most important factors are the pH and organic matter content. Therefore it is essential to have correct information about the content and behaviour of the above named elements in soil, both from the environmental and agronomical viewpoint. During the last decades several extracting solutions which are suitable for the evaluation of nutrient status of soils have been developed for this purpose. One of them is called Mehlich 3 which is widely used in USA, Canada and some European countries (e.g. Estonia, Czech Republic) because of its suitability to extract several major plant nutrients from the soil simultaneously. There are several different instrumental methods used for the analysis of nutrient elements in the soil extract. Potassium, magnesium and calcium are widely analysed by the AAS (atomic absorption spectroscopic) method or by the ICP (inductively coupled plasma) spectroscopic methods. Molecular spectroscopy and ICP spectroscopy were used for the phosphorus determination. In 2011 a new multielemental instrumental method MP-AES (microwave plasma atomic emission spectroscopy) was added to them. Due to its lower detection limits and multielemental character, compared with AAS, and lower exploitation costs, compared with ICP, the MP-AES has a good potential to achieve a leading position in soil nutrient analysis in the future. The objective of this study was to investigate: (i) the impact of soil pH and humus content and (ii) applicability of MP-AES instrumental method for the determination of soil nutrients extracted according to Mehlich 3. For the experiment 100 soil samples with different content of organic matter and pH were used. The determination of Ca, Mg, K and P was analysed by MP and ICP methods and additionally P was analysed molecular spectroscopically. Within the framework of the study the regressions between MP and ICP methods were created for all the analysed elements, i.e. Ca, Mg, K and P. According to MP and ICP, the relationships between the analysed soil major nutrient contents at different soil humus levels and at different pH ranges were determined for the evaluation of their impact. The optimal instrumental settings for calcium, magnesium and potassium analysis, according to Mehlich 3 using MP-AES method, are reported.
[Determination of heavy metals for RoHS compliance by ICP-OES spectrometry coupled with microwave extraction system].

PubMed

Hua, Li; Wu, Yi-Ping; An, Bing; Lai, Xiao-Wei

2008-11-01

The harm of heavy metals contained in electronic and electrical equipment (EEE) on environment is of high concern by human. Aiming to handle the great challenge of RoHS compliance, the determinations of trace or ultratrace chromium (Cr), cadmium (Cd), mercury (Hg) and lead (Pb) by inductively coupled plasma optical emission spectrometry (ICP-OES) was performed in the present paper, wherein, microwave extraction technology was used to prepare the sample solutions. In addition, the precision, recovery, repeatability and interference issues of this method were also discussed. The results exhibited that using the microwave extraction system to prepare samples is more quick, lossless, contamination-free in comparison with the conventional extraction methods such as dry ashing, wet-oven extraction etc. By analyzing the recoveries of these four heavy metals over different working time and wavelengths, the good recovery range between 85% and 115% showed that there was only tiny loss or contamination during the process of microwave extraction, sample introduction and ICP detection. Repeatability experiments proved that ICP plasma had a good stability during the working time and the matrix effect was small. Interference was a problem troublesome for atomic absorption spectrometry (AAS), however, the techniques of standard additions or inter-element correction (IEC) method can effectively eliminated the interferences of Ni, As, Fe etc. with the Cd determination. By employing the multi-wavelengths and two correction point methods, the issues of background curve sloping shift and spectra overlap were successfully overcome. Besides, for the determinations of trace heavy metal elements, the relative standard deviation (RSD) was less than 3% and the detection limits were less than 1 microg x L(-10 (3sigma, n = 5) for samples, standard solutions, and standard additions, which proved that ICP-OES has a good precision and high reliability. This provided a reliable technique support for electronic and electrical (EE) industries to comply with RoHS directive.
INEL BNCT Research Program annual report, 1992

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

Venhuizen, J.R.

1993-05-01

This report is a summary of the progress and research produced for the Idaho National Engineering Laboratory Boron Neutron Capture Therapy (BNCT) Research Program for calendar year 1992. Contributions from all the principal investigators about their individual projects are included, specifically, chemistry (pituitary tumor targeting compounds, boron drug development including liposomes, lipoproteins, and carboranylalanine derivatives), pharmacology (murine screenings, toxicity testing, inductively coupled plasma-atomic emission spectroscopy (ICP-AES) analysis of biological samples), physics (radiation dosimetry software, neutron beam and filter design, neutron beam measurement dosimetry), and radiation biology (small and large animal models tissue studies and efficacy studies). Information on the potentialmore » toxicity of borocaptate sodium and boronophenylalanine is presented, results of 21 spontaneous-tumor-bearing dogs that have been treated with BNCT at the Brookhaven National Laboratory (BNL) Medical Research Reactor (BMRR) are discussed, and predictions for an epithermal-neutron beam at the Georgia Tech Research Reactor (GTRR) are shown. Cellular-level boron detection and localization by secondary ion mass spectrometry, sputter-initiated resonance ionization spectroscopy, low atomization resonance ionization spectroscopy, and alpha track are presented. Boron detection by ICP-AES is discussed in detail. Several boron carrying drugs exhibiting good tumor uptake are described. Significant progress in the potential of treating pituitary tumors with BNCT is presented. Measurement of the epithermal-neutron flux at BNL and comparison to predictions are shown. Calculations comparing the GTRR and BMRR epithermal-neutron beams are also presented. Individual progress reports described herein are separately abstracted and indexed for the database.« less
Heavy metal concentrations in soils as determined by laser-induced breakdown spectroscopy (LIBS), with special emphasis on chromium.

PubMed

Senesi, G S; Dell'Aglio, M; Gaudiuso, R; De Giacomo, A; Zaccone, C; De Pascale, O; Miano, T M; Capitelli, M

2009-05-01

Soil is unanimously considered as one of the most important sink of heavy metals released by human activities. Heavy metal analysis of natural and polluted soils is generally conducted by the use of atomic absorption spectroscopy (AAS) or inductively coupled plasma optical emission spectroscopy (ICP-OES) on adequately obtained soil extracts. Although in recent years the emergent technique of laser-induced breakdown spectroscopy (LIBS) has been applied widely and with increasing success for the qualitative and quantitative analyses of a number of heavy metals in soil matrices with relevant simplification of the conventional methodologies, the technique still requires further confirmation before it can be applied fully successfully in soil analyses. The main objective of this work was to demonstrate that new developments in LIBS technique are able to provide reliable qualitative and quantitative analytical evaluation of several heavy metals in soils, with special focus on the element chromium (Cr), and with reference to the concentrations measured by conventional ICP spectroscopy. The preliminary qualitative LIBS analysis of five soil samples and one sewage sludge sample has allowed the detection of a number of elements including Al, Ca, Cr, Cu, Fe, Mg, Mn, Pb, Si, Ti, V and Zn. Of these, a quantitative analysis was also possible for the elements Cr, Cu, Pb, V and Zn based on the obtained linearity of the calibration curves constructed for each heavy metal, i.e., the proportionality between the intensity of the LIBS emission peaks and the concentration of each heavy metal in the sample measured by ICP. In particular, a triplet of emission lines for Cr could be used for its quantitative measurement. The consistency of experiments made on various samples was supported by the same characteristics of the laser-induced plasma (LIP), i.e., the typical linear distribution confirming the existence of local thermodynamic equilibrium (LTE) condition, and similar excitation temperatures and comparable electron number density measured for all samples. An index of the anthropogenic contribution of Cr in polluted soils was calculated in comparison to a non-polluted reference soil. Thus, the intensity ratios of the emission lines of heavy metal can be used to detect in few minutes the polluted areas for which a more detailed sampling and analysis can be useful.
Assessment of total arsenic and arsenic species stability in alga samples and their aqueous extracts.

PubMed

García Salgado, S; Quijano Nieto, M A; Bonilla Simón, M M

2008-05-30

In order to achieve reliable information on speciation analysis, it is necessary to assess previously the species stability in the sample to analyse. Furthermore, in those cases where the sample treatment for species extraction is time-consuming, an assessment of the species integrity in the extracts is of paramount importance. Thus, the present paper reports total arsenic and arsenic species stability in alga samples (Sargassum fulvellum and Hizikia fusiformis), as well as in their aqueous extracts, which were stored in amber glass and polystyrene containers at different temperatures. Total arsenic determination was carried out by inductively coupled plasma atomic emission spectroscopy (ICP-AES), after sample acid digestion in a microwave oven, while arsenic speciation was conducted by anion exchange high performance liquid chromatography on-line coupled to ICP-AES, with and without sample introduction by hydride generation (HPLC-ICP-AES and HPLC-HG-ICP-AES), after aqueous microwave-assisted extraction. The results obtained for solid alga samples showed that total arsenic (for Hijiki alga) and arsenic species present (As(V) for Hijiki and NIES No. 9 Sargasso) are stable for at least 12 months when samples are stored in polystyrene containers at +20 degrees C. On the other hand, a different behaviour was observed in the stability of total arsenic and As(V) species in aqueous extracts for both samples, being the best storage conditions for Sargasso extracts a temperature of -18 degrees C and polystyrene containers, under which they are stable for at least 15 days, while Hijiki extracts must be stored in polystyrene containers at +4 degrees C in order to ensure the stability for 10 days.

Elemental analyses of modern dust in southern Nevada and California

USGS Publications Warehouse

Reheis, M.C.; Budahn, J.R.; Lamothe, P.J.

1999-01-01

Selected samples of modern dust collected in marble traps at sites in southern Nevada and California (Reheis and Kihl, 1995; Reheis, 1997) have been analyzed for elemental composition using instrumental neutron activation analysis (INAA) and inductively coupled plasma atomic emission spectroscopy (ICP-AES) and inductively coupled plasma mass spectroscopy (ICP-MS). For information on these analytical techniques and their levels of precision and accuracy, refer to Baedecker and McKown (1987) for INAA, to Briggs (1996) for ICP-AES, and to Briggs and Meier (1999) for ICP-MS. This report presents the elemental compositions obtained using these techniques on dust samples collected from 1991 through 1997.The dust-trap sites were established at varying times; some have been maintained since 1984, others since 1991. For details on site location, dust-trap construction, and collection techniques, see Reheis and Kihl (1995) and Reheis (1997). Briefly, the trap consists of a coated angel-food cake pan painted black on the outside and mounted on a post about 2 m above the ground. Glass marbles rest on a circular piece of galvanized hardware cloth (now replaced by stainless-steel mesh), which is fitted into the pan so that it rests 3-4 cm below the rim. The 2-m height eliminates most saltating sand-sized particles. The marbles simulate the effect of a gravelly fan surface and prevent dust that has filtered or washed into the bottom of the pan from being blown back out. The dust traps are fitted with two metal straps looped in an inverted basket shape; the top surfaces of the straps are coated with a sticky material that effectively discourages birds from roosting.
Qualitative and quantitative analysis of human nails to find correlation between nutrients and vitamin D deficiency using LIBS and ICP-AES.

PubMed

Almessiere, M A; Altuwiriqi, R; Gondal, M A; AlDakheel, R K; Alotaibi, H F

2018-08-01

In this work, we analysed human fingernails of people who suffer from vitamin D deficiency using the laser-induced breakdown spectroscopy(LIBS) and inductively coupled plasma atomic emission spectroscopy (ICP-AES)techniques. The measurements have been conducted on 71 nail samples collected randomly from volunteers of different genders and ages ranged between 20 and 50 years. The main aim of this study is to find the correlation between vitamin D deficiency and the intensity of some dominated lines in the LIBS spectra. A LIBS spectrum consists of dominant lines of fifteen elements including calcium, magnesium, sodium, potassium, titanium, iron, chloride, sulphur, copper, chromium, zinc, nitrogen, phosphor, and oxygen. By recording the spectrum in specific ranges and focusing on calcium, magnesium, sodium, and potassium, we found a correlation between the intensity of the potassium (K) lines at (766.5 and 769.9 nm)and vitamin D level in both age groups (20 and 25 years old), with weak correlation for the calcium (Ca), magnesium (Mg), and sodium (Na) lines. To verify the validity of the LIBS results, we analysed the nail samples with ICP, a standard analytical technique. The elements detected with our LIBS technique are in a good agreement with those identified by ICP-AES. From the health and physiological perspectives, the LIBS system, which is used for spectral analysis in this work, is appropriate for diagnostic purposes such as to find the correlation between vitamin D deficiency and potassium content, especially for hypertensive patients who simultaneously take potassium-based medication and vitamin D supplement. Copyright © 2018 Elsevier B.V. All rights reserved.
Application of ICP-OES to the determination of CuIn(1-x)Ga(x)Se2 thin films used as absorber materials in solar cell devices.

PubMed

Fernández-Martínez, Rodolfo; Caballero, Raquel; Guillén, Cecilia; Gutiérrez, María Teresa; Rucandio, María Isabel

2005-05-01

CuIn(1-x)Ga(x)Se2 [CIGS; x=Ga/(In+Ga)] thin films are among of the best candidates as absorber materials for solar cell applications. The material quality and main properties of the polycrystalline absorber layer are critically influenced by deviations in the stoichiometry, particularly in the Cu/(In+Ga) atomic ratio. In this work a simple, sensitive and accurate method has been developed for the quantitative determination of these thin films by inductively coupled plasma optical emission spectrometry (ICP-OES). The proposed method involves an acid digestion of the samples to achieve the complete solubilization of CIGS, followed by the analytical determination by ICP-OES. A digestion procedure with 50% HNO3 alone or in the presence of 10% HCl was performed to dissolve those thin films deposited on glass or Mo-coated glass substrates, respectively. Two analytical lines were selected for each element (Cu 324.754 and 327.396 nm, Ga 294.364 and 417.206 nm, In 303.936 and 325.609 nm, Se 196.090 and 203.985 nm, and Mo 202.030 and 379.825 nm) and a study of spectral interferences was performed which showed them to be suitable, since they offered a high sensitivity and no significant inter-element interferences were detected. Detection limits for all elements at the selected lines were found to be appropriate for this kind of application, and the relative standard deviations were lower than 1.5% for all elements with the exception of Se (about 5%). The Cu/(In+Ga) atomic ratios obtained from the application of this method to CIGS thin films were consistent with the study of the structural and morphological properties by X-ray diffraction (XRD) and scanning electron microscopy (SEM).
Improved approach for routine monitoring of 129I activity and 129I/127I atom ratio in environmental samples using TMAH extraction and ICP-MS/MS.

PubMed

Yang, Guosheng; Tazoe, Hirofumi; Yamada, Masatoshi

2018-05-30

To reconstruct 131 I deposition and identify the source of radioiodine due to the Fukushima Daiichi Nuclear Power Plant (FDNPP) accident, 129 I activity and 129 I/ 127 I atom ratio should be obtained by preparing and analyzing large numbers of samples economically. In this study, great efforts were made to realize mild TMAH (tetramethyl ammonium hydroxide) extraction of environmental samples at 90 °C to obtain solutions suitable for the following triple-quadrupole inductively coupled plasma-mass spectrometry (ICP-QQQ) MS/MS mode analysis. After releasing iodine from organic matter in the TMAH extraction solution via K 2 S 2 O 8 oxidation, organic matter was removed effectively by solvent extraction and back-extraction to avoid a serious matrix effect during ICP-QQQ analysis. At the same time, interfering elements, especially, Mo, Cd, and In were also removed effectively, to avoid their undesirable interferences during mass spectrometric analysis. In addition, 0.01% (NH 4 ) 2 SO 3 was selected to introduce I - into ICP-QQQ to ensure there was no memory effect and a stable signal was gotten. Subsequently, ICP-QQQ MS/MS mode was applied to further eliminate polyatomic interferences ( 127 I(H 2 and D) + , 97 MoO 2 + , 113 InO + , and 113 CdO + ) and isobaric interference from 129 Xe + . Finally, the developed method was successfully applied to measure 129 I/ 127 I atom ratios ((2.61-27.0) × 10 -7 ) and 129 I activities (3.51-11.4 mBq kg -1 ) in soil samples. The developed method allows a greater number of ordinary laboratories to participate in the field of radioiodine analysis. Copyright © 2018 Elsevier B.V. All rights reserved.
Determination of organo-zinc based fungicides in timber treatments employing gas chromatographic analysis with mass selective detection and/or inductively coupled plasma atomic emission spectroscopy.

PubMed

Rimmer, D A; Johnson, P D; Bradley, S D

2001-09-14

A method for the determination of zinc octoate (zinc 2-ethylhexanoate) and acypetacs zinc in occupational hygiene samples and wood treatments formulations is described. The zinc carboxylates are liquid-liquid partitioned between toluene and 1 M HCl, with the liberated acids being extracted into the toluene and zinc (chloride) into the acid. The carboxylic acids are then methylated using trimethylsilyldiazomethane-methanol and the resultant methyl esters are selectively and sensitively analysed by gas chromatography with mass selective detection (GC-MS). Alternatively, the zinc content of the acid extract can be analysed by inductively coupled plasma atomic emission spectroscopy (ICP-AES). GC-MS is the preferred method of analysis for zinc octoate, where a single analyte (methyl-2-ethylhexanoate) is produced for analysis. Because acypetacs zinc contains a complex mixture of carboxylates, quantitative GC-MS analysis of the methyl esters produced is impractical and ICP-AES is the preferred method for quantitation. In this case, GC-MS can be used to confirm the identity of the product used. The analysis of occupational hygiene samples (cotton pads, gloves and socks as well as Tenax tubes and GF/A filters) spiked with metal carboxylates is demonstrated. Recoveries around 70-90% and reproducibilities of 5-23% (n=6-8) were typically achieved for the determination of tin octoate (a surrogate for zinc octoate) at spiking levels ranging from 4 to 190 microg per sampling device. Recoveries around 102-106% and reproducibilities of 10-12% (n=5-6) were typically achieved for acypetacs zinc at spiking levels ranging from 100 mg per sampling device. Reaction yields for the octoate methylation reaction were in the region of 85-87%. The method was used to monitor for occupational exposure to zinc octoate and acypetacs zinc during the application of wood treatments to fences.
High-Resolution Inductively Coupled Plasma Optical Emission Spectrometry for (234)U/(238)Pu Age Dating of Plutonium Materials and Comparison to Sector Field Inductively Coupled Plasma Mass Spectrometry.

PubMed

Krachler, Michael; Alvarez-Sarandes, Rafael; Rasmussen, Gert

2016-09-06

Employing a commercial high-resolution inductively coupled plasma optical emission spectrometry (HR-ICP-OES) instrument, an innovative analytical procedure for the accurate determination of the production age of various Pu materials (Pu powder, cardiac pacemaker battery, (242)Cm heat source, etc.) was developed and validated. This undertaking was based on the fact that the α decay of (238)Pu present in the investigated samples produced (234)U and both mother and daughter could be identified unequivocally using HR-ICP-OES. Benefiting from the high spectral resolution of the instrument (<5 pm) and the isotope shift of the emission lines of both nuclides, (234)U and (238)Pu were selectively and directly determined in the dissolved samples, i.e., without a chemical separation of the two analytes from each other. Exact emission wavelengths as well as emission spectra of (234)U centered around λ = 411.590 nm and λ = 424.408 nm are reported here for the first time. Emission spectra of the isotopic standard reference material IRMM-199, comprising about one-third each of (233)U, (235)U, and (238)U, confirmed the presence of (234)U in the investigated samples. For the assessment of the (234)U/(238)Pu amount ratio, the emission signals of (234)U and (238)Pu were quantified at λ = 424.408 nm and λ = 402.148 nm, respectively. The age of the investigated samples (range: 26.7-44.4 years) was subsequently calculated using the (234)U/(238)Pu chronometer. HR-ICP-OES results were crossed-validated through sector field inductively coupled plasma mass spectrometry (SF-ICPMS) analysis of the (234)U/(238)Pu amount ratio of all samples applying isotope dilution combined with chromatographic separation of U and Pu. Available information on the assumed ages of the analyzed samples was consistent with the ages obtained via the HR-ICP-OES approach. Being based on a different physical detection principle, HR-ICP-OES provides an alternative strategy to the well-established mass spectrometric approach and thus effectively adds to the quality assurance of (234)U/(238)Pu age dates.
Effect of combustion temperature on the emission of trace elements under O2/CO2 atmosphere during coal combustion

NASA Astrophysics Data System (ADS)

Qu, Chengrui; Zhang, Mo; Mann, Michael. D.

2018-03-01

The effect of combustion temperature on the emission of trace elementswas studied under O2/CO2 atmosphere during coal combustion in a laboratory scale fluidized bed combustor. The elemental composition of fine fly ash particles collected with a low pressure impactor(LPI)was quantified by X-Ray F1uorescence Spectrometer (XRF). The elemental composition of coal and bottom ash was quantified byinductively coupled plasma-atomic emission spectroscopy (ICP-AES). The results indicate that the contents of Mn, Zn, Cd and Cr in the fly ash increase with the rise of combustion temperature. It is found that the enrichment of Zn and Cd is greater in the submicrometer particles than the supermicrometer particles, but Mn and Cr do not enrich in the submicrometer particles. Mn, Zn, Cd and Cr display one peak around 0.1 μm. The relative enrichment factor (Rij) of four elements is in the order of Zn, Cd, Mn and Cr. Zn and Cd are mostly retained in fly ashwhileMn and Cr are retained in both the fly ash and bottom ash.
Geographical traceability of wild Boletus edulis based on data fusion of FT-MIR and ICP-AES coupled with data mining methods (SVM)

NASA Astrophysics Data System (ADS)

Li, Yun; Zhang, Ji; Li, Tao; Liu, Honggao; Li, Jieqing; Wang, Yuanzhong

2017-04-01

In this work, the data fusion strategy of Fourier transform mid infrared (FT-MIR) spectroscopy and inductively coupled plasma-atomic emission spectrometry (ICP-AES) was used in combination with Support Vector Machine (SVM) to determine the geographic origin of Boletus edulis collected from nine regions of Yunnan Province in China. Firstly, competitive adaptive reweighted sampling (CARS) was used for selecting an optimal combination of key wavenumbers of second derivative FT-MIR spectra, and thirteen elements were sorted with variable importance in projection (VIP) scores. Secondly, thirteen subsets of multi-elements with the best VIP score were generated and each subset was used to fuse with FT-MIR. Finally, the classification models were established by SVM, and the combination of parameter C and γ (gamma) of SVM models was calculated by the approaches of grid search (GS) and genetic algorithm (GA). The results showed that both GS-SVM and GA-SVM models achieved good performances based on the #9 subset and the prediction accuracy in calibration and validation sets of the two models were 81.40% and 90.91%, correspondingly. In conclusion, it indicated that the data fusion strategy of FT-MIR and ICP-AES coupled with the algorithm of SVM can be used as a reliable tool for accurate identification of B. edulis, and it can provide a useful way of thinking for the quality control of edible mushrooms.
Geographical traceability of wild Boletus edulis based on data fusion of FT-MIR and ICP-AES coupled with data mining methods (SVM).

PubMed

Li, Yun; Zhang, Ji; Li, Tao; Liu, Honggao; Li, Jieqing; Wang, Yuanzhong

2017-04-15

In this work, the data fusion strategy of Fourier transform mid infrared (FT-MIR) spectroscopy and inductively coupled plasma-atomic emission spectrometry (ICP-AES) was used in combination with Support Vector Machine (SVM) to determine the geographic origin of Boletus edulis collected from nine regions of Yunnan Province in China. Firstly, competitive adaptive reweighted sampling (CARS) was used for selecting an optimal combination of key wavenumbers of second derivative FT-MIR spectra, and thirteen elements were sorted with variable importance in projection (VIP) scores. Secondly, thirteen subsets of multi-elements with the best VIP score were generated and each subset was used to fuse with FT-MIR. Finally, the classification models were established by SVM, and the combination of parameter C and γ (gamma) of SVM models was calculated by the approaches of grid search (GS) and genetic algorithm (GA). The results showed that both GS-SVM and GA-SVM models achieved good performances based on the #9 subset and the prediction accuracy in calibration and validation sets of the two models were 81.40% and 90.91%, correspondingly. In conclusion, it indicated that the data fusion strategy of FT-MIR and ICP-AES coupled with the algorithm of SVM can be used as a reliable tool for accurate identification of B. edulis, and it can provide a useful way of thinking for the quality control of edible mushrooms. Copyright © 2017. Published by Elsevier B.V.
Liquid oil and residual characteristics of printed circuit board recycle by pyrolysis.

PubMed

Lin, Kuo-Hsiung; Chiang, Hung-Lung

2014-04-30

Non-metal fractions of waste printed circuit boards (PCBs) were thermally treated (200-500°C) under nitrogen atmosphere. Carbon, hydrogen, and nitrogen were determined by elemental analyzer, bromine by instrumental neutron activation analysis (INAA), phosphorus by energy dispersive X-ray spectrometer (EDX), and 29 trace elements by inductively coupled plasma atomic emission spectrometer (ICP-AES) and mass spectrometry (ICP-MS) for raw material and pyrolysis residues. Organic compositions of liquid oil were identified by GC (gas chromatography)-MS, trace element composition by ICP system, and 12 water-soluble ions by IC (ionic chromatography). Elemental content of carbon was >450 mg/g, oxygen 300 mg/g, bromine and hydrogen 60 mg/g, nitrogen 30 mg/g, and phosphorus 28 mg/g. Sulfur was trace in PCBs. Copper content was 25-28 mg/g, iron 1.3-1.7 mg/g, tin 0.8-1.0mg/g and magnesium 0.4-1.0mg/g; those were the main metals in the raw materials and pyrolytic residues. In the liquid products, carbon content was 68-73%, hydrogen was 10-14%, nitrogen was 4-5%, and sulfur was less than 0.05% at pyrolysis temperatures from 300 to 500°C. Phenol, 3-bromophenol, 2-methylphenol and 4-propan-2-ylphenol were major species in liquid products, accounting for >50% of analyzed organic species. Bromides, ammonium and phosphate were the main species in water sorption samples for PCB pyrolysis exhaust. Copyright © 2014 Elsevier B.V. All rights reserved.
Exploration of robust operating conditions in inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Tromp, John W.; Pomares, Mario; Alvarez-Prieto, Manuel; Cole, Amanda; Ying, Hai; Salin, Eric D.

2003-11-01

'Robust' conditions, as defined by Mermet and co-workers for inductively coupled plasma (ICP)-atomic emission spectrometry, minimize matrix effects on analyte signals, and are obtained by increasing power and reducing nebulizer gas flow. In ICP-mass spectrometry (MS), it is known that reduced nebulizer gas flow usually leads to more robust conditions such that matrix effects are reduced. In this work, robust conditions for ICP-MS have been determined by optimizing for accuracy in the determination of analytes in a multi-element solution with various interferents (Al, Ba, Cs, K, Na), by varying power, nebulizer gas flow, sample introduction rate and ion lens voltage. The goal of the work was to determine which operating parameters were the most important in reducing matrix effects, and whether different interferents yielded the same robust conditions. Reduction in nebulizer gas flow and in sample input rate led to a significantly decreased interference, while an increase in power seemed to have a lesser effect. Once the other parameters had been adjusted to their robust values, there was no additional improvement in accuracy attainable by adjusting the ion lens voltage. The robust conditions were universal, since, for all the interferents and analytes studied, the optimum was found at the same operating conditions. One drawback to the use of robust conditions was the slightly reduced sensitivity; however, in the context of 'intelligent' instruments, the concept of 'robust conditions' is useful in many cases.
Elements and polycyclic aromatic hydrocarbons in exhaust particles emitted by light-duty vehicles.

PubMed

Alves, Célia A; Barbosa, Cátia; Rocha, Sónia; Calvo, Ana; Nunes, Teresa; Cerqueira, Mário; Pio, Casimiro; Karanasiou, Angeliki; Querol, Xavier

2015-08-01

The main purpose of this work was to evaluate the chemical composition of particulate matter (PM) emitted by eight different light-duty vehicles. Exhaust samples from petrol and diesel cars (Euro 3 to Euro 5) were collected in a chassis dynamometer facility. To simulate the real-world driving conditions, three ARTEMIS cycles were followed: road, to simulate a fluid traffic flow and urban with hot and cold starts, to simulate driving conditions in cities. Samples were analysed for the water-soluble ions, for the elemental composition and for polycyclic aromatic hydrocarbons (PAHs), respectively, by ion chromatography, inductively coupled plasma atomic emission spectroscopy (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS) and gas chromatography-mass spectrometry (GC-MS). Nitrate and phosphate were the major water-soluble ions in the exhaust particles emitted from diesel and petrol vehicles, respectively. The amount of material emitted is affected by the vehicle age. For vehicles ≥Euro 4, most elements were below the detection limits. Sodium, with emission factors in the ranges 23.5-62.4 and 78.2-227μg km(-1), for petrol and diesel Euro 3 vehicles, respectively, was the major element. The emission factors of metallic elements indicated that diesel vehicles release three to five times more than petrol automobiles. Element emissions under urban cycles are higher than those found for on-road driving, being three or four times higher, for petrol vehicles, and two or three times, for diesel vehicles. The difference between cycles is mainly due to the high emissions for the urban cycle with hot start-up. As registered for elements, most of the PAH emissions for vehicles ≥Euro 4 were also below the detection limits. Regardless of the vehicle models or driving cycles, the two- to four-ring PAHs were always dominant. Naphthalene, with emission factors up to 925 μg km(-1), was always the most abundant PAH. The relative cancer risk associated with naphthalene was estimated to be up to several orders of magnitude higher than any of the chemical species found in the PM phase. The highest PAH emission factors were registered for diesel-powered vehicles. The condition of the vehicle can exert a decisive influence on both element and PAH emissions.
Physicochemical Analysis of Indicator Lichens as a Component of Conservation Area Baseline Monitoring

NASA Astrophysics Data System (ADS)

Meysurova, A. F.; Notov, A. A.

2016-01-01

The gross and average contents of 15 metals (Al, As, Cd, Co, Cu, Ge, Fe, Mn, Mo, Ni, Pb, Sn, Ti, V, and Zn) in samples of Hypogymnia physodes collected from a reserve area in Tver Region were determined using inductively-coupled plasma atomic emission spectroscopy (ICP-AES). Apparently, most of these elements appeared as a result of transboundary transfer. Their concentration in lichens depended on the atmospheric humidity. An excess of moisture in ecotopes located near rivers and swamps increased the gross concentration of separate elements in the lichens. The average contents of most elements in the specimens were within permissible limits, which allowed possible baseline element concentration ranges for this region to be established.
High resolution mass spectrometric brain proteomics by MALDI-FTICR-MS combined with determination of P, S, Cu, Zn and Fe by LA-ICP-MS

NASA Astrophysics Data System (ADS)

Becker, J. Susanne; Zoriy, Miroslav; Przybylski, Michael; Becker, J. Sabine

2007-03-01

The combination of atomic and molecular mass spectrometric methods was applied for characterization and identification of several human proteins from Alzheimer's diseased brain. A brain protein mixture was separated by two-dimensional (2D) gel electrophoresis and the protein spots were fast screened by microlocal analysis using LA-ICP-MS (laser ablation inductively coupled plasma mass spectrometry) in respect to phosphorus, sulfur, copper, zinc and iron content. Five selected protein spots in 2D gel containing these elements were investigated after tryptic digestion by matrix assisted laser desorption ionization Fourier transform ion cyclotron resonance mass spectrometry (MALDI-FTICR-MS). Than element concentrations (P, Cu, Zn and Fe) were determined in three identified human brain proteins by LA-ICP-MS in the 2D gel. Results of structure analysis of human brain proteins by MALDI-FTICR-MS were combined with those of the direct determination of phosphorus, copper, zinc and iron concentrations in protein spots with LA-ICP-MS. From the results of atomic and molecular mass spectrometric techniques the human brain proteins were characterized in respect to their structure, sequence, phosphorylation state and metal content as well.
RBS, SY-XRF, INAA and ICP-IDMS of antimony implanted in silicon - A multi-method approach to characterize and certify a reference material

NASA Astrophysics Data System (ADS)

Ecker, K. H.; Wätjen, U.; Berger, A.; Persson, L.; Pritzkow, W.; Radtke, M.; Riesemeier, H.

2002-04-01

A layer of Sb atoms, implanted with an energy of 400 keV and a nominal dose of 5×10 16 atoms/cm 2 into a high purity silicon wafer, was certified for its areal density (atoms/cm 2) using Rutherford backscattering spectrometry (RBS), instrumental neutron activation analysis (INAA) and inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) and for its isotope ratio using INAA and ICP-IDMS. Excellent agreement between the results of the different independent methods was found. In the present work, the measurements of the homogeneity of the areal density of Sb, previously determined with RBS in spots having 1 mm diameter, are improved with synchrotron X-ray fluorescence analysis: Higher precision in even smaller sample spots allows to estimate a reduced inhomogeneity of the whole batch of samples of the order of only 0.4%. Thus the uncertainty of the certified value can further be reduced. Down to fractions of a chip with 0.3×0.4 mm 2 area, the areal density is now certified as (4.81±0.06)×10 16 Sb atoms/cm 2, where the expanded uncertainty 0.06 (coverage factor k=2) corresponds to only 1.2%. The relative merits of the different analytical methods are discussed.
Forensic discrimination of three common brands of kitchen knives in China by ICP-AES and infrared absorption.

PubMed

Bai, Ru-feng; Ma, Shu-hua; Zhang, Hai-dong; Chang, Lin; Zhang, Zhong; Liu, Li; Zhang, Feng-qin; Guo, Zhao-ming; Shi, Mei-sen

2014-03-01

A block of an injury instrument will be left in wounds sometimes, and the suspect instrument can be discriminated by comparison with the block that was left through elemental analysis. In this study, three brands (Shibazi, Zhangxiaoquan, Qiaoxifu) of kitchen knives with forged, chop, and slice application series were analyzed by inductively coupled plasma atomic emission spectroscopy (ICP-AES) and Infrared Absorption to investigate the type, number of elements and the reference range used for comparing. The results show that when regarding one or more element as the discriminative threshold, together with 5% relative standard deviation (RSD) as the reference range, all the samples could be distinguished among different series. Furthermore, within the same series, the discriminative capability could reach up to 88.57% for all samples. In addition, elements with high content, such as Cr, Mn, and C, were useful to discriminate among different series, and trace elements, such as Ni, Si, and Cu, were useful within the same series. However, in practice, it is necessary to evaluate the accuracy of the method by Standard Reference Material (SRM) before an examination is performed.
[Spectroscopic methods applied to component determination and species identification for coffee].

PubMed

Chen, Hua-zhou; Xu, Li-li; Qin, Qiang

2014-06-01

Spectroscopic analysis was applied to the determination of the nutrient quality of ground, instant and chicory coffees. By using inductively coupled plasma atomic emission spectrometry (ICP-ES), nine mineral elements were determined in solid coffee samples. Caffeine was determined by ultraviolet (UV) spectrometry and organic matter was investigated by Fourier transform infrared (FTIR) spectroscopy. Oxidation-reduction titration was utilized for measuring the oxalate. The differences between ground coffee and instant coffee was identified on the basis of the contents of caffeine, oxalate and mineral elements. Experimental evidence showed that, caffeine in instant coffee was 2-3 times higher than in ground coffee. Oxalate in instant coffee was significantly higher in ground coffee. Mineral elements of Mg, P and Zn in ground coffee is lower than in instant coffee, while Cu is several times higher. The mineral content in chicory coffee is overall lower than the instant coffee. In addition, we determined the content of Ti for different types of coffees, and simultaneously detected the elements of Cu, Ti and Zn in chicory coffee. As a fast detection technique, FTIR spectroscopy has the potential of detecting the differences between ground coffee and instant coffee, and is able to verify the presence of caffeine and oxalate.
Screening of trace elements in hair of the female population with different types of cancers in Wielkopolska region of Poland.

PubMed

Czerny, Bogusław; Krupka, Krzysztof; Ożarowski, Marcin; Seremak-Mrozikiewicz, Agnieszka

2014-01-01

Cancer constitutes a major health problem worldwide. Thus, search for reliable and practical markers of the disease process remains the key issue of the diagnostic process. The study aims at linking the trace element status of an organism, assessed by hair analysis, with the occurrence of cancer diseases. Hair samples were collected from 299 patients with cancer diseases confirmed by a histopathological test and from 100 controls. Cancer patients were divided into three groups, depending on cancer type: hormone-dependent cancer, cancer of the alimentary tract, and cancer with high glycolytic activity. Mineral element analysis of hair was performed using an atomic emission spectrophotometer with inductively coupled plasma (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). Statistically significantly lower concentrations of selenium, zinc, copper, germanium and boron, iron, and magnesium were observed in the three groups of cancer patients. Disturbance in the axis glucose-insulin and changes in concentrations of heavy metals and toxic elements were also noted. It seems safe to conclude that our results confirmed usefulness of hair element analysis in screening tests for the assessment of the biomarker of various cancer diseases in a female population.
Fundamental and methodological investigations for the improvement of elemental analysis by inductively coupled plasma mass soectrometry

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

Ebert, Christopher Hysjulien

This dissertation describes a variety of studies meant to improve the analytical performance of inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation (LA) ICP-MS. The emission behavior of individual droplets and LA generated particles in an ICP is studied using a high-speed, high frame rate digital camera. Phenomena are observed during the ablation of silicate glass that would cause elemental fractionation during analysis by ICP-MS. Preliminary work for ICP torch developments specifically tailored for the improvement of LA sample introduction are presented. An abnormal scarcity of metal-argon polyatomic ions (MAr{sup +}) is observed during ICP-MS analysis. Evidence shows thatmore » MAr{sup +} ions are dissociated by collisions with background gas in a shockwave near the tip of the skimmer cone. Method development towards the improvement of LA-ICP-MS for environmental monitoring is described. A method is developed to trap small particles in a collodion matrix and analyze each particle individually by LA-ICP-MS.« less
SeO2 adsorption on CaO surface: DFT and experimental study on the adsorption of multiple SeO2 molecules

NASA Astrophysics Data System (ADS)

Fan, Yaming; Zhuo, Yuqun; Li, Liangliang

2017-10-01

SeO2 adsorption mechanisms on CaO surface were firstly investigated by both density functional theory (DFT) calculations and adsorption experiments. Adsorption of multiple SeO2 on the CaO (001) surface was investigated using slab model. Based on the results of adsorption energy and surface property, a double-layer adsorption mechanisms were proposed. In experiments, the SeO2 adsorption products were prepared in a U-shaped quartz reactor at 200 °C. The surface morphology was investigated by field emission scanning electron microscopy (FE-SEM). The superficial and total SeO2 mass fractions were measured by X-ray photoelectron spectroscopy (XPS) and inductively coupled plasma atomic emission spectroscopy (ICP-AES), respectively. The surface valence state and bulk structure are determined by XPS and X-Ray Diffraction (XRD). The experimental results are in good agreement with the DFT results. In conclusion, the fundamental SeO2 chemisorption mechanisms on CaO surface were suggested.

Method validation for simultaneous determination of chromium, molybdenum and selenium in infant formulas by ICP-OES and ICP-MS.

PubMed

Khan, Naeem; Jeong, In Seon; Hwang, In Min; Kim, Jae Sung; Choi, Sung Hwa; Nho, Eun Yeong; Choi, Ji Yeon; Kwak, Byung-Man; Ahn, Jang-Hyuk; Yoon, Taehyung; Kim, Kyong Su

2013-12-15

This study aimed to validate the analytical method for simultaneous determination of chromium (Cr), molybdenum (Mo), and selenium (Se) in infant formulas available in South Korea. Various digestion methods of dry-ashing, wet-digestion and microwave were evaluated for samples preparation and both inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) were compared for analysis. The analytical techniques were validated by detection limits, precision, accuracy and recovery experiments. Results showed that wet-digestion and microwave methods were giving satisfactory results for sample preparation, while ICP-MS was found more sensitive and effective technique than ICP-OES. The recovery (%) of Se, Mo and Cr by ICP-OES were 40.9, 109.4 and 0, compared to 99.1, 98.7 and 98.4, respectively by ICP-MS. The contents of Cr, Mo and Se in infant formulas by ICP-MS were found in good nutritional values in accordance to nutrient standards for infant formulas CODEX values. Copyright © 2013 Elsevier Ltd. All rights reserved.
99Tc atom counting by quadrupole ICP-MS. Optimisation of the instrumental response

NASA Astrophysics Data System (ADS)

Más, José L.; Garcia-León, Manuel; Bolívar, Juan P.

2002-05-01

In this paper, an extensive work is done on the specific tune of a conventional ICP-MS for 99Tc atom counting. For this, two methods have been used and compared: the partial variable control method and the 5D Simplex method. Instrumental limits of detection of 0.2 and 0.8 ppt, respectively, were obtained. They are noticeably lower than that found with the automatic tune method of the spectrometer, 47 ppt, which shows the need of a specific tune when very low levels of 99Tc have to be determined. A study is presented on the mass interferences for 99Tc. Our experiments show that the formation of polyatomic atoms or refractory oxides as well as 98Mo hydrides seem to be irrelevant for 99Tc atom counting. The opposite occurs with the presence of isobaric interferences, i.e. 99Ru, and the effect of abundance sensitivity, or low-mass resolution, which can modify the response at m/ z=99 to a non-negligible extent.
Isolation and characterization of Bacillus cereus IST105 from electroplating effluent for detoxification of hexavalent chromium.

PubMed

Naik, Umesh Chandra; Srivastava, Shaili; Thakur, Indu Shekhar

2011-08-01

Electroplating industries are the main sources of heavy metals, chromium, nickel, lead, zinc, cadmium and copper. The highest concentrations of chromium (VI) in the effluent cause a direct hazards to human and animals. Therefore, there is a need of an effective and affordable biotechnological solution for removal of chromium from electroplating effluent. Bacterial strains were isolated from electroplating effluent to find out higher tolerant isolate against chromate. The isolate was identified by 16S rDNA sequence analysis. Absorbed chromium level of bacterium was determined by inductively coupled plasma-atomic emission spectrometer (ICP-AES), atomic absorption spectrophotometer (AAS), scanning electron microscope (SEM), transmission electron microscope (TEM) and energy dispersive X-ray analysis (EDX). Removal of metals by bacterium from the electroplating effluent eventually led to the detoxification of effluent confirmed by MTT assay. Conformational changes of functional groups of bacterial cell surface were studied through Fourier transform infrared spectroscopy. The chromate tolerant isolate was identified as Bacillus cereus. Bacterium has potency to remove more than 75% of chromium as measured by ICP-AES and AAS. The study indicated the accumulation of chromium (VI) on bacterial cell surface which was confirmed by the SEM-EDX and TEM analysis. The biosorption of metals from the electroplating effluent eventually led to the detoxification of effluent. The increased survivability of Huh7 cells cultured with treated effluent also confirmed the detoxification as examined by MTT assay. Isolated strain B. cereus was able to remove and detoxify chromium (VI). It would be an efficient tool of the biotechnological approach in mitigating the heavy metal pollutants.
Low gas flow inductively coupled plasma optical emission spectrometry for the analysis of food samples after microwave digestion.

PubMed

Nowak, Sascha; Gesell, Monika; Holtkamp, Michael; Scheffer, Andy; Sperling, Michael; Karst, Uwe; Buscher, Wolfgang

2014-11-01

In this work, the recently introduced low flow inductively coupled plasma optical emission spectrometry (ICP-OES) with a total argon consumption below 0.7 L/min is applied for the first time to the field of food analysis. One goal is the investigation of the performance of this low flow plasma compared to a conventional ICP-OES system when non-aqueous samples with a certain matrix are introduced into the system. For this purpose, arsenic is determined in three different kinds of fish samples. In addition several nutrients (K, Na, Mg, Ca) and trace metals (Co, Cu, Mn, Cd, Pb, Zn, Fe, and Ni) are determined in honey samples (acacia) after microwave digestion. The precision of the measurements is characterized by relative standard deviations (RSD) and compared to the corresponding precision values achieved using the conventional Fassel-type torch of the ICP. To prove the accuracy of the low flow ICP-OES method, the obtained data from honey samples are validated by a conventional ICP-OES. For the measurements concerning arsenic in fish, the low flow ICP-OES values are validated by conventional Fassel-type ICP-OES. Furthermore, a certified reference material was investigated with the low gas flow setup. Limits of detection (LOD), according to the 3σ criterion, were determined to be in the low microgram per liter range for all analytes. Recovery rates in the range of 96-106% were observed for the determined trace metal elements. It was proven that the low gas flow ICP-OES leads to results that are comparable with those obtained with the Fassel-type torch for the analysis of food samples. Copyright © 2014 Elsevier B.V. All rights reserved.
Selected problems with boron determination in water treatment processes. Part I: comparison of the reference methods for ICP-MS and ICP-OES determinations.

PubMed

Kmiecik, Ewa; Tomaszewska, Barbara; Wątor, Katarzyna; Bodzek, Michał

2016-06-01

The aim of the study was to compare the two reference methods for the determination of boron in water samples and further assess the impact of the method of preparation of samples for analysis on the results obtained. Samples were collected during different desalination processes, ultrafiltration and the double reverse osmosis system, connected in series. From each point, samples were prepared in four different ways: the first was filtered (through a membrane filter of 0.45 μm) and acidified (using 1 mL ultrapure nitric acid for each 100 mL of samples) (FA), the second was unfiltered and not acidified (UFNA), the third was filtered but not acidified (FNA), and finally, the fourth was unfiltered but acidified (UFA). All samples were analysed using two analytical methods: inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES). The results obtained were compared and correlated, and the differences between them were studied. The results show that there are statistically significant differences between the concentrations obtained using the ICP-MS and ICP-OES techniques regardless of the methods of sampling preparation (sample filtration and preservation). Finally, both the ICP-MS and ICP-OES methods can be used for determination of the boron concentration in water. The differences in the boron concentrations obtained using these two methods can be caused by several high-level concentrations in selected whole-water digestates and some matrix effects. Higher concentrations of iron (from 1 to 20 mg/L) than chromium (0.02-1 mg/L) in the samples analysed can influence boron determination. When iron concentrations are high, we can observe the emission spectrum as a double joined and overlapping peak.
Application of ICP-OES for Evaluating Energy Extraction and Production Wastewater Discharge Impacts on Surface Waters in Western Pennsylvania

EPA Science Inventory

Oil and gas extraction and coal-fired electrical power generating stations produce wastewaters that are treated and discharged to rivers in Western Pennsylvania with public drinking water system (PDWS) intakes. Inductively coupled plasma optical emission spectroscopy (ICP-OES) w...
Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: a tutorial review. Part II. Practical considerations.

PubMed

Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

2015-07-23

Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review, Electrothermal Vaporization and Laser Ablation will also be shortly described. The second issue is devoted to the analytical strategies for elemental quantification in such matrices, with particular insight into the isotope dilution technique, particularly used in speciation analysis by ICP-coupled separation techniques. Copyright © 2015 Elsevier B.V. All rights reserved.
Removal of uranium from soil samples for ICP-OES analysis of RCRA metals

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

Wero, M.; Lederer-Cano, A.; Billy, C.

1995-12-01

Soil samples containing high levels of uranium present unique analytical problems when analyzed for toxic metals (Ag, As, Ba, Cd, Cr, Cu, Ni, Pb, Se and Tl) because of the spectral interference of uranium in the ICP-OES emission spectrometer. Methods to remove uranium from the digestates of soil samples, known to be high in uranium, have been developed that reduce the initial uranium concentration (1-3%) to less than 500 ppm. UTEVA ion exchange columns, used as an ICP-OES analytical pre-treatment, reduces uranium to acceptable levels, permitting good analytical results of the RCRA metals by ICP-OES.
A critical review of inductively coupled plasma-mass spectrometry for geoanalysis, geochemistry and hydrology, Part 1. Analytical performance

USGS Publications Warehouse

Brenner, I.B.; Taylor, Howard E.

1992-01-01

Present-day inductively coupled plasma-mass spectrometry (ICP-MS) instrumentation is described briefly. Emphasis is placed on performance characteristics for geoanalysis, geochemistry, and hydrology. Applications where ICP-MS would be indispensable are indicated. Determination of geochemically diagnostic trace elements (such as the rare earth elements [REE], U and Th), of isotope ratios for fingerprinting, tracer and other geo-isotope applications, and benchmark isotope dilution determinations are considered to be typical priority applications for ICP-MS. It is concluded that ICP-MS furnishes unique geoanalytical and environmental data that are not readily provided by conventional spectroscopic (emission and absorption) techniques.
Multi-elemental analysis of aqueous geological samples by inductively coupled plasma-optical emission spectrometry

USGS Publications Warehouse

Todorov, Todor I.; Wolf, Ruth E.; Adams, Monique

2014-01-01

Typically, 27 major, minor, and trace elements are determined in natural waters, acid mine drainage, extraction fluids, and leachates of geological and environmental samples by inductively coupled plasma-optical emission spectrometry (ICP-OES). At the discretion of the analyst, additional elements may be determined after suitable method modifications and performance data are established. Samples are preserved in 1–2 percent nitric acid (HNO3) at sample collection or as soon as possible after collection. The aqueous samples are aspirated into the ICP-OES discharge, where the elemental emission signals are measured simultaneously for 27 elements. Calibration is performed with a series of matrix-matched, multi-element solution standards.
Ion Chromatography as an Alternative to Standard Methods for Analysis of Macro-nutrients in Mehlich 1 Extracts of Unfertilized Forest Soils

Treesearch

Joseph B. Fischer; James H. Miller

2004-01-01

This study evaluates ion chromatography (IC) as an alternative to atomic absorption (AA) and inductively-coupled plasma spectromctry (ICP) for analysis of potassium (K), magnesium (Mg), and calcium (Ca), and and as an alternative to antimonylmolybdate colorimetry and ICP for analysis of phosphorus (P) macro-nutrients in Mehlich 1 extracts. Soils typical of pine forests...
Concentration and distribution of sixty-one elements in coals from DPR Korea

USGS Publications Warehouse

Hu, Jiawen; Zheng, B.; Finkelman, R.B.; Wang, B.; Wang, M.; Li, S.; Wu, D.

2006-01-01

Fifty coal samples (28 anthracite and 22 lignites) were collected from both main and small coal mines in DPR Korea prioritized by resource distribution and coal production. The concentrations of 61 elements in 50 coal samples were determined by several multielement and element-specific techniques, including inductively coupled plasma atomic emission spectrometry (ICP-AES), and inductively coupled plasma mass spectrometry (ICP-MS), ion chromatogram (IC), cold-vapor atomic absorption spectrometry (CV-AAS), and hydride generation atomic absorption spectrometry (HGAAS). The ranges, arithmetic means and geometric means of concentrations of these elements are presented. A comparison with crustal abundances (Clarke values) shows that some potentially hazardous elements in the coals of DPR Korea are highly enriched Li, B, S, Cl, Zn, As, Se, Cd, Sn, Sb, W, Te, Hg, Ag, Pb, and La, Ce, Dy, Tm, Ge, Mo, Cs, Tl, Bi, Th and U are moderately enriched. A comparison of ranges and means of elemental concentrations in DPR Korea, Chinese, and world coals shows the ranges of most elements in DPR Korea coals are very close to the ranges of world coals. Arithmetic means of most elements in DPR Korea coals are close to that of American coals. Most elements arithmetic means are higher in Jurassic and Paleogene coals than coals of other ages. In DPR Korea coals, only seven elements in early Permian coals are higher than other periods: Li, Zn, Se, Cd, Hg, Pb, and Bi. Only five elements B, As, Sr, Mo, W in Neogene coals have arithmetic means higher than others. SiO2 and Al2O 3 in ashes are more than 70% except six samples. The correlation between ash yields and major elements from high to low is in the order of Si>Al>Ti>K>Mg>Fe>Na>Ca>P>S. Most elements have high positive correlation with ash (r>0.5) and show high inorganic affinity. ?? 2005 Elsevier Ltd. All rights reserved.
Dopant occupancy and UV-VIS-NIR spectroscopy of Mg (0, 4, 5 and 6 mol.%):Dy:LiNbO3 crystal

NASA Astrophysics Data System (ADS)

Dai, Li; Liu, Chunrui; Han, Xianbo; Wang, Luping; Tan, Chao; Yan, Zhehua; Xu, Yuheng

2017-09-01

A series of Dy:LiNbO3 crystals with x mol.% Mg2+ ions (x =0, 4, 5 and 6 mol.%) were grown by the Czochralski method. The effective segregation coefficient of Mg2+ and Dy3+ ions was studied by the inductively coupled plasma-atomic emission spectrometry (ICP-AES). UV-VIS-NIR absorption spectra and Judd-Ofelt theory were used to investigate their spectroscopic properties. J-O intensity parameters (Ω2 = 7.53 × 10-20cm2, Ω4 = 6.98 × 10-20cm2, and Ω6 = 3.09 × 10-20cm2) and larger spectroscopic quality factor (X = 2.26) for Mg:(6 mol.%)Dy:LiNbO3 crystals were obtained.
Distinguishing Astragalus mongholicus and Its Planting Soil Samples from Different Regions by ICP-AES.

PubMed

Li, Lin; Zheng, Sihao; Yang, Qingzhen; Chen, Shilin; Huang, Linfang

2016-04-12

"Daodi herb" enjoys a good reputation for its quality and clinical effects. As one of the most popular daodi herbs, Astragalus membranaceus (Fisch.) Bge var. mongholicus (Bge.) Hsiao (A. membranaceus) is popularly used for its anti-oxidant, anti-inflammatory and immune-enhancing properties. In this study, we used inductively coupled plasma atomic emission spectrometry (ICP-AES) technique to investigate the inorganic elements contents in A. mongholicu and its soil samples from daodi area (Shanxi) and non-daodi areas (Inner Mongolia and Gansu). A total of 21 inorganic elements (Pb, Cd, As, Hg, Cu, P, K, Zn, Mn, Ca, Mg, Fe, Se, B, Al, Na, Cr, Ni, Ba, Ti and Sr) were simultaneously determined. Principal component analysis (PCA) was performed to differentiate A. mongholicu and soil samples from the three main producing areas. It was found that the inorganic element characteristics as well as the uptake and accumulation behavior of the three kinds of samples were significantly different. The high contents of Fe, B, Al, Na, Cr and Ni could be used as a standard in the elements fingerprint to identify daodi and non-daodi A. Mongholicus. As the main effective compounds were closely related to the pharmacodynamics activities, the inter-relationships between selected elements and components could reflect that the quality of A. Mongholicus from Shanxi were superior to others to a certain degree. This finding highlighted the usefulness of ICP-AES elemental analysis and evidenced that the inorganic element profile can be employed to evaluate the genuineness of A. mongholicus.
Metabolite profiling with HPLC-ICP-MS as a tool for in vivo characterization of imaging probes.

PubMed

Boros, Eszter; Pinkhasov, Omar R; Caravan, Peter

2018-01-01

Current analytical methods for characterizing pharmacokinetic and metabolic properties of positron emission tomography (PET) and single photon emission computed tomography (SPECT) probes are limited. Alternative methods to study tracer metabolism are needed. The study objective was to assess the potential of high performance liquid chromatography - inductively coupled plasma - mass spectrometry (HPLC-ICP-MS) for quantification of molecular probe metabolism and pharmacokinetics using stable isotopes. Two known peptide-DOTA conjugates were chelated with nat Ga and nat In. Limit of detection of HPLC-ICP-MS for 69 Ga and 115 In was determined. Rats were administered 50-150 nmol of Ga- and/or In-labeled probes, blood was serially sampled, and plasma analyzed by HPLC-ICP-MS using both reverse phase and size exclusion chromatography. The limits of detection were 0.16 pmol for 115 In and 0.53 pmol for 69 Ga. Metabolites as low as 0.001 %ID/g could be detected and transchelation products identified. Simultaneous administration of Ga- and In-labeled probes allowed the determination of pharmacokinetics and metabolism of both probes in a single animal. HPLC-ICP-MS is a robust, sensitive and radiation-free technique to characterize the pharmacokinetics and metabolism of imaging probes.
40 CFR Table 1 to Subpart Llll of... - Emission Limits and Standards for New Fluidized Bed Sewage Sludge Incineration Units

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 CFR part 60, appendix A-8). Use GFAAS or ICP/MS for the analytical finish. Lead 0.00062 milligrams... per run) Performance test (Method 29 at 40 CFR part 60, appendix A-8. Use GFAAS or ICP/MS for the...
40 CFR Table 1 to Subpart Llll of... - Emission Limits and Standards for New Fluidized Bed Sewage Sludge Incineration Units

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 CFR part 60, appendix A-8). Use GFAAS or ICP/MS for the analytical finish. Lead 0.00062 milligrams... per run) Performance test (Method 29 at 40 CFR part 60, appendix A-8. Use GFAAS or ICP/MS for the...
Inductively coupled plasma mass spectrometry (ICP MS): a versatile tool.

PubMed

Ammann, Adrian A

2007-04-01

Inductively coupled plasma (ICP) mass spectrometry (MS) is routinely used in many diverse research fields such as earth, environmental, life and forensic sciences and in food, material, chemical, semiconductor and nuclear industries. The high ion density and the high temperature in a plasma provide an ideal atomizer and element ionizer for all types of samples and matrices introduced by a variety of specialized devices. Outstanding properties such as high sensitivity (ppt-ppq), relative salt tolerance, compound-independent element response and highest quantitation accuracy lead to the unchallenged performance of ICP MS in efficiently detecting, identifying and reliably quantifying trace elements. The increasing availability of relevant reference compounds and high separation selectivity extend the molecular identification capability of ICP MS hyphenated to species-specific separation techniques. While molecular ion source MS is specialized in determining the structure of unknown molecules, ICP MS is an efficient and highly sensitive tool for target-element orientated discoveries of relevant and unknown compounds. This special-feature, tutorial article presents the principle and advantages of ICP MS, highlighting these using examples from recently published investigations. Copyright 2007 John Wiley & Sons, Ltd.
Spectral interferences in the determination of rhenium in molybdenum and copper concentrates by inductively coupled plasma optical emission spectrometry (ICP-OES)

NASA Astrophysics Data System (ADS)

Karadjov, Metody; Velitchkova, Nikolaya; Veleva, Olga; Velichkov, Serafim; Markov, Pavel; Daskalova, Nonka

2016-05-01

This paper deals with spectral interferences of complex matrix containing Mo, Al, Ti, Fe, Mg, Ca and Cu in the determination of rhenium in molybdenum and copper concentrates by inductively coupled plasma optical emission spectrometry (ICP-OES). By radial viewing 40.68 MHz ICP equipped with a high resolution spectrometer (spectral bandwidth = 5 pm) the hyperfine structure (HFS) of the most prominent lines of rhenium (Re II 197.248 nm, Re II 221.426 nm and Re II 227.525 nm) was registered. The HFS components under high resolution conditions were used as separate prominent line in order to circumvent spectral interferences. The Q-concept was applied for quantification of spectral interferences. The quantitative databases for the type and the magnitude of the spectral interferences in the presence of above mentioned matrix constituents were obtained by using a radial viewing 40.68 MHz ICP with high resolution and an axial viewing 27.12 MHz ICP with middle resolution. The data for the both ICP-OES systems were collected chiefly with a view to spectrochemical analysis for comparing the magnitude of line and wing (background) spectral interference and the true detection limits with spectroscopic apparatus with different spectral resolution. The sample pretreatment methods by sintering with magnesium oxide and oxidizing agents as well as a microwave acid digestion were applied. The feasibility, accuracy and precision of the analytical results were experimentally demonstrated by certified reference materials.
Elemental assessment of vegetation via portable X-ray fluorescence (PXRF) spectrometry.

PubMed

McGladdery, Candice; Weindorf, David C; Chakraborty, Somsubhra; Li, Bin; Paulette, Laura; Podar, Dorina; Pearson, Delaina; Kusi, Nana Yaw O; Duda, Bogdan

2018-03-15

Elemental concentrations in vegetation are of critical importance, whether establishing plant essential element concentrations (toxicity vs. deficiency) or investigating deleterious elements (e.g., heavy metals) differentially extracted from the soil by plants. Traditionally, elemental analysis of vegetation has been facilitated by acid digestion followed by quantification via inductively coupled plasma (ICP) or atomic absorption (AA) spectroscopy. Previous studies have utilized portable X-ray fluorescence (PXRF) spectroscopy to quantify elements in soils, but few have evaluated the vegetation. In this study, a PXRF spectrometer was employed to scan 228 organic material samples (thatch, deciduous leaves, grasses, tree bark, and herbaceous plants) from smelter-impacted areas of Romania, as well as National Institute of Standards and Technology (NIST) certified reference materials, to demonstrate the application of PXRF for elemental determination in vegetation. Samples were scanned in three conditions: as received from the field (moist), oven dry (70 °C), and dried and powdered to pass a 2 mm sieve. Performance metrics of PXRF models relative to ICP atomic emission spectroscopy were developed to asses optimal scanning conditions. Thatch and bark samples showed the highest mean PXRF and ICP concentrations (e.g., Zn, Pb, Cd, Fe), with the exceptions of K and Cl. Validation statistics indicate that the stable validation predictive capacity of PXRF increased in the following order: oven dry intact < field moist < oven dried and powdered. Even under field moist conditions, PXRF could reasonably be used for the determination of Zn (coefficient of determination, R 2 val 0.86; residual prediction deviation, RPD 2.72) and Cu (R 2 val 0.77; RPD 2.12), while dried and powdered samples allowed for stable validation prediction of Pb (R 2 val 0.90; RPD 3.29), Fe (R 2 val 0.80; RPD 2.29), Cd (R 2 val 0.75; RPD 2.07) and Cu (R 2 val 0.98; RPD of 8.53). Summarily, PXRF was shown to be a useful approach for quickly assessing the elemental concentration in vegetation. Future PXRF/vegetation research should explore additional elements and investigate its usefulness in evaluating phytoremediation effectiveness. Copyright © 2018 Elsevier Ltd. All rights reserved.

Pyrolysis characteristics of integrated circuit boards at various particle sizes and temperatures.

PubMed

Chiang, Hung-Lung; Lin, Kuo-Hsiung; Lai, Mei-Hsiu; Chen, Ting-Chien; Ma, Sen-Yi

2007-10-01

A pyrolysis method was employed to recycle the metals and brominated compounds blended into printed circuit boards. This research investigated the effect of particle size and process temperature on the element composition of IC boards and pyrolytic residues, liquid products, and water-soluble ionic species in the exhaust, with the overall goal being to identify the pyrolysis conditions that will have the least impact on the environment. Integrated circuit (IC) boards were crushed into 5-40 mesh (0.71-4.4mm), and the crushed particles were pyrolyzed at temperatures ranging from 200 to 500 degrees C. The thermal decomposition kinetics were measured by a thermogravimetric (TG) analyzer. The composition of pyrolytic residues was analyzed by Energy Dispersive X-ray Spectrometer (EDS), Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). In addition, the element compositions of liquid products were analyzed by ICP-AES and ICP-MS. Pyrolytic exhaust was collected by a water-absorption system in an ice-bath cooler, and IC analysis showed that the absorbed solution comprised 11 ionic species. Based on the pyrolytic kinetic parameters of TG analysis and pyrolytic residues at various temperatures for 30 min, the effect of particle size was insignificant in this study, and temperature was the key factor for the IC board pyrolysis. Two stages of decomposition were found for IC board pyrolysis under nitrogen atmosphere. The activation energy was 38-47 kcal/mol for the first-stage reaction and 5.2-9.4 kcal/mol for the second-stage reaction. Metal content was low in the liquid by-product of the IC board pyrolysis process, which is an advantage in that the liquid product could be used as a fuel. Brominate and ammonium were the main water-soluble ionic species of the pyrolytic exhaust. A plan for their safe and effective disposal must be developed if the pyrolytic recycling process is to be applied to IC boards.
DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Wei; Zhao, Shu-Xia; Liu, Yong-Xin

The F-atom kinetics in SF{sub 6} and SF{sub 6}/Ar inductively coupled plasmas (ICPs) were investigated using a global model. This report particularly focuses on the effects of ICP power and Ar fraction on F-atom density and its main production and loss mechanisms. The results are presented for a relatively wide pressure range of 1–100 mTorr. Very different behaviors were observed for Ar fractions in the low- and high-pressure limits, which can be attributed to different electron kinetics. In addition, the authors found that increasing the Ar fraction in the SF{sub 6}/Ar plasma has almost the same effects on the F-atommore » kinetics as increasing the power in the SF{sub 6} plasma. This is because a high electron density occurs in both cases. Moreover, it was confirmed that, for both sample types, a cycle of F atoms formed in the bulk plasma. The source of these is F{sub 2} molecules that are first formed on the chamber wall and then emitted. Finally, the simulations of F-atom kinetics are validated by quantitatively comparing the calculated electron and F-atom densities with identical experimental discharge conditions.« less
Evaluation of analytical performance for the simultaneous detection of trace Cu, Co and Ni by using liquid cathode glow discharge-atomic emission spectrometry

NASA Astrophysics Data System (ADS)

Yu, Jie; Zhang, Xiaomin; Lu, Quanfang; Sun, Duixiong; Wang, Xing; Zhu, Shuwen; Zhang, Zhichao; Yang, Wu

2018-07-01

In this paper, a novel liquid cathode glow discharge (LCGD) was established as a micro-plasma excitation source of atomic emission spectrometry (AES) for simultaneous detection of trace Cu, Co and Ni in aqueous solution. In order to evaluate the analytical performance, the operating parameters such as discharge voltage, supporting electrolyte, solution pH and flow rate were thoroughly investigated. The results showed that the optimal conditions are 640 V discharge voltage, pH = 1 HNO3 as supporting electrolyte and 4.5 mL min-1 flow rate. The R2 of Cu, Co and Ni are 0.9977, 0.9991 and 0.9977, respectively. The relative standard deviation (RSD) is 1.4% for Cu, 3.2% for Co and 0.8% for Ni. Under this condition, the power of LCGD is below 55 W and the plasma is quite stable. The limits of detections (LODs) for Cu, Co and Ni are 0.380, 0.080, and 0.740 mg L-1, respectively, which are basically consistent with the closed-type electrolyte cathode atmospheric glow discharge (ELCAD). Compared with ICP-AES, the LCGD-AES has small size, low power consumption, no inert gas requirement and low cost in set-up. It may be developed as a portable instrument for in-site and real-time monitoring of metals in solution samples with further improvement.
Studies on transport phenomena in electrothermal vaporization sample introduction applied to inductively coupled plasma for optical emission and mass spectrometry

NASA Astrophysics Data System (ADS)

Kántor, T.; Maestre, S.; de Loos-Vollebregt, M. T. C.

2005-10-01

In the present work electrothermal vaporization (ETV) was used in both inductively coupled plasma mass spectrometry (ICP-MS) and optical emission spectrometry (OES) for sample introduction of solution samples. The effect of (Pd + Mg)-nitrate modifier and CaCl 2 matrix/modifier of variable amounts were studied on ETV-ICP-MS signals of Cr, Cu, Fe, Mn and Pb and on ETV-ICP-OES signals of Ag, Cd, Co, Cu, Fe, Ga, Mn and Zn. With the use of matrix-free standard solutions the analytical curves were bent to the signal axes (as expected from earlier studies), which was observed in the 20-800 pg mass range by ICP-MS and in the 1-50 ng mass range by ICP-OES detection. The degree of curvature was, however, different with the use of single element and multi-element standards. When applying the noted chemical modifiers (aerosol carriers) in microgram amounts, linear analytical curves were found in the nearly two orders of magnitude mass ranges. Changes of the CaCl 2 matrix concentration (loaded amount of 2-10 μg Ca) resulted in less than 5% changes in MS signals of 5 elements (each below 1 ng) and OES signals of 22 analytes (each below 15 ng). Exceptions were Pb (ICP-MS) and Cd (ICP-OES), where the sensitivity increase by Pd + Mg modifier was much larger compared to other elements studied. The general conclusions suggest that quantitative analysis with the use of ETV sample introduction requires matrix matching or matrix replacement by appropriate chemical modifier to the specific concentration ranges of analytes. This is a similar requirement to that claimed also by the most commonly used pneumatic nebulization of solutions, if samples with high matrix concentration are concerned.
Metallic elements (Ca, Hg, Fe, K, Mg, Mn, Na, Zn) in the fruiting bodies of Boletus badius.

PubMed

Kojta, Anna K; Falandysz, Jerzy

2016-06-01

The aim of this study was to investigate and compare the levels of eight metallic elements in the fruiting bodies of Bay Bolete (Boletus badius; current name Imleria badia) collected from ten sites in Poland to understand better the value of this popular mushroom as an organic food. Bay Bolete fruiting bodies were collected from the forest area near the towns and villages of Kętrzyn, Poniatowa, Bydgoszcz, Pelplin, Włocławek, Żuromin, Chełmno, Ełk and Wilków communities, as well as in the Augustów Primeval Forest. Elements such as Ca, Fe, K, Mg, Mn, Na and Zn were analyzed by inductively coupled plasma atomic emission spectroscopy (ICP-OES), and mercury by cold vapor atomic absorption spectrometry (CV-AAS). This made it possible to assess the nutritional value of the mushroom, as well as possible toxicological risks associated with its consumption. The results were subjected to statistical analysis (Kruskal-Wallis test, cluster analysis, principal component analysis). Copyright © 2016 Elsevier Ltd. All rights reserved.
Characterization of brines and evaporites of Lake Katwe, Uganda

NASA Astrophysics Data System (ADS)

Kasedde, Hillary; Kirabira, John Baptist; Bäbler, Matthäus U.; Tilliander, Anders; Jonsson, Stefan

2014-03-01

Lake Katwe brines and evaporites were investigated to determine their chemical, mineralogical and morphological composition. 30 brine samples and 3 solid salt samples (evaporites) were collected from different locations of the lake deposit. Several analytical techniques were used to determine the chemical composition of the samples including Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES), Inductively Coupled Plasma-Sector Field Mass Spectrometry (ICP-SFMS), ion chromatography, and potentiometric titration. The mineralogical composition and morphology of the evaporites was determined using X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. Physical parameters of the lake brines such as density, electrical conductivity, pH, and salinity were also studied. The results show that the lake brines are highly alkaline and rich in Na+, Cl-, CO32-, SO42-, and HCO3- with lesser amounts of K+, Mg2+, Ca2+, Br-, and F- ions. The brines show an intermediate transition between Na-Cl and Na-HCO3 water types. Among the trace metals, the lake brines were found to be enriched in B, I, Sr, Fe, Mo, Ba, and Mn. The solid salts are composed of halite mixed with other salts such as hanksite, burkeite and trona. It was also observed that the composition of the salts varies considerably even within the same grades.
Influence of soil composition on the major, minor and trace metal content of Velebit biomedical plants.

PubMed

Zeiner, Michaela; Juranović Cindrić, Iva; Požgaj, Martina; Pirkl, Raimund; Šilić, Tea; Stingeder, Gerhard

2015-03-15

The use of medical herbs for the treatment of many human diseases is increasing nowadays due to their mild features and low side effects. Not only for their healing properties, but also for their nutritive value supplementation of diet with various herbs is recommended. Thus also their analysis is of rising importance. While total elemental compositions are published for many common herbs, the origin of toxic as well as beneficial elements is not yet well investigated. Thus different indigenous medicinal plants, namely Croatian spruce (Picea abies), savory (Satureja montana L.), mountain yarrow (Achillea clavennae), showy calamint (Calamintha grandiflora), micromeria (Micromeria croatica), yellow gentian (Gentiana lutea) and fir (Abies alba) together with soil samples were collected in the National Park Northern Velebit. The macro- and trace elements content, after microwave digestion, was determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and inductively coupled plasma mass spectroscopy (ICP-MS). The study focuses on the one hand on essential elements and on the other hand on non-essential elements which are considered as toxic for humans, covering in total Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Sr and Zn. Copyright © 2014 Elsevier B.V. All rights reserved.
Feature Fusion of ICP-AES, UV-Vis and FT-MIR for Origin Traceability of Boletus edulis Mushrooms in Combination with Chemometrics.

PubMed

Qi, Luming; Liu, Honggao; Li, Jieqing; Li, Tao; Wang, Yuanzhong

2018-01-15

Origin traceability is an important step to control the nutritional and pharmacological quality of food products. Boletus edulis mushroom is a well-known food resource in the world. Its nutritional and medicinal properties are drastically varied depending on geographical origins. In this study, three sensor systems (inductively coupled plasma atomic emission spectrophotometer (ICP-AES), ultraviolet-visible (UV-Vis) and Fourier transform mid-infrared spectroscopy (FT-MIR)) were applied for the origin traceability of 192 mushroom samples (caps and stipes) in combination with chemometrics. The difference between cap and stipe was clearly illustrated based on a single sensor technique, respectively. Feature variables from three instruments were used for origin traceability. Two supervised classification methods, partial least square discriminant analysis (FLS-DA) and grid search support vector machine (GS-SVM), were applied to develop mathematical models. Two steps (internal cross-validation and external prediction for unknown samples) were used to evaluate the performance of a classification model. The result is satisfactory with high accuracies ranging from 90.625% to 100%. These models also have an excellent generalization ability with the optimal parameters. Based on the combination of three sensory systems, our study provides a multi-sensory and comprehensive origin traceability of B. edulis mushrooms.
Feature Fusion of ICP-AES, UV-Vis and FT-MIR for Origin Traceability of Boletus edulis Mushrooms in Combination with Chemometrics

PubMed Central

Qi, Luming; Liu, Honggao; Li, Jieqing; Li, Tao

2018-01-01

Origin traceability is an important step to control the nutritional and pharmacological quality of food products. Boletus edulis mushroom is a well-known food resource in the world. Its nutritional and medicinal properties are drastically varied depending on geographical origins. In this study, three sensor systems (inductively coupled plasma atomic emission spectrophotometer (ICP-AES), ultraviolet-visible (UV-Vis) and Fourier transform mid-infrared spectroscopy (FT-MIR)) were applied for the origin traceability of 184 mushroom samples (caps and stipes) in combination with chemometrics. The difference between cap and stipe was clearly illustrated based on a single sensor technique, respectively. Feature variables from three instruments were used for origin traceability. Two supervised classification methods, partial least square discriminant analysis (FLS-DA) and grid search support vector machine (GS-SVM), were applied to develop mathematical models. Two steps (internal cross-validation and external prediction for unknown samples) were used to evaluate the performance of a classification model. The result is satisfactory with high accuracies ranging from 90.625% to 100%. These models also have an excellent generalization ability with the optimal parameters. Based on the combination of three sensory systems, our study provides a multi-sensory and comprehensive origin traceability of B. edulis mushrooms. PMID:29342969
Exposure assessment of heavy metals in an e-waste processing area in northern Vietnam.

PubMed

Oguri, Tomoko; Suzuki, Go; Matsukami, Hidenori; Uchida, Natsuyo; Tue, Nguyen Minh; Tuyen, Le Huu; Viet, Pham Hung; Takahashi, Shin; Tanabe, Shinsuke; Takigami, Hidetaka

2018-04-15

In developing countries, inappropriate recycling of e-waste has resulted in the environmental release of toxicants, including heavy metals, that may have deleterious health effects. In this study, we estimated daily metal intakes in five households in a Vietnamese village located in an e-waste processing area and assessed the health risk posed by exposure to the metals. Garden soil, floor dust, 24-h duplicate diet, and ambient air samples were collected from five households in northern Vietnam in January 2014. All samples were acid-digested, and contents of Cd, Cu, Mn, Pb, Sb, and Zn were measured by using ICP mass spectrometry and ICP atomic emission spectroscopy. In addition, the soil, dust, and diet samples were subjected to an bioaccessibility extraction test to determine bioaccessible metal concentrations. Hazard quotients were estimated from bioaccessible metal concentrations, provisional tolerable weekly intakes, and reference doses. Garden soil and floor dust were estimated to be mainly contributors to daily Pb intake, as indicated by calculations using bioaccessible metal concentrations and the U.S. Environmental Protection Agency soil plus dust ingestion rate. Diet was suggested to contribute significantly to daily Cd, Cu, Mn, Sb, and Zn intake. Estimated metal exposures via inhalation were negligible, as indicated by calculations using International Atomic Energy Agency reference inhalation rates. The maximum hazard quotients were calculated as 0.2 (Cd), 0.09 (Cu), 0.3 (Mn), 0.6 (Pb), 0.2 (Sb), and 0.5 (Zn), on the basis of bioaccessible metal concentrations. The contributions of Cd, Cu, Mn, Sb, and Zn except Pb to potential noncancer risk for adult residents of the five households in the e-waste processing area may be low. Copyright © 2017 Elsevier B.V. All rights reserved.
Elemental analysis of glass by laser ablation inductively coupled plasma optical emission spectrometry (LA-ICP-OES).

PubMed

Schenk, Emily R; Almirall, José R

2012-04-10

The elemental analysis of glass evidence has been established as a powerful discrimination tool for forensic analysts. Laser ablation inductively coupled plasma optical emission spectrometry (LA-ICP-OES) has been compared to laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and energy dispersive micro X-ray fluorescence spectroscopy (μXRF/EDS) as competing instrumentation for the elemental analysis of glass. The development of a method for the forensic analysis of glass coupling laser ablation to ICP-OES is presented for the first time. LA-ICP-OES has demonstrated comparable analytical performance to LA-ICP-MS based on the use of the element menu, Al (Al I 396.15 nm), Ba (Ba II 455.40 nm), Ca (Ca II 315.88 nm), Fe (Fe II 238.20 nm), Li (Li I 670.78 nm), Mg (Mg I 285.21 nm), Sr (Sr II 407.77 nm), Ti (Ti II 368.51 nm), and Zr (Zr II 343.82 nm). The relevant figures of merit, such as precision, accuracy and sensitivity, are presented and compared to LA-ICP-MS. A set of 41 glass samples was used to assess the discrimination power of the LA-ICP-OES method in comparison to other elemental analysis techniques. This sample set consisted of several vehicle glass samples that originated from the same source (inside and outside windshield panes) and several glass samples that originated from different vehicles. Different match criteria were used and compared to determine the potential for Type I and Type II errors. It was determined that broader match criteria is more applicable to the forensic comparison of glass analysis because it can reduce the affect that micro-heterogeneity inherent in the glass fragments and a less than ideal sampling strategy can have on the interpretation of the results. Based on the test set reported here, a plus or minus four standard deviation (± 4s) match criterion yielded the lowest possibility of Type I and Type II errors. The developed LA-ICP-OES method has been shown to perform similarly to LA-ICP-MS in the discrimination among different sources of glass while offering the advantages of a lower cost of acquisition and operation of analytical instrumentation making ICP-OES a possible alternative elemental analysis method for the forensic laboratory. Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.
A matrix effect and accuracy evaluation for the determination of elements in milk powder LIBS and laser ablation/ICP-OES spectrometry.

PubMed

Gilon, N; El-Haddad, J; Stankova, A; Lei, W; Ma, Q; Motto-Ros, V; Yu, J

2011-11-01

Laser ablation coupled to inductively coupled plasma optical emission spectrometry (LA-ICP-OES) and laser-induced breakdown spectroscopy (LIBS) were investigated for the determination of Ca, Mg, Zn and Na in milk samples. The accuracy of both methods was evaluated by comparison of the concentration found using LA-ICP-OES and LIBS with classical wet digestion associated with ICP-OES determination. The results were not fully acceptable, with biases from less than 1% to more than 60%. Matrix effects were also investigated. The sample matrix can influence the temperature, electron number density (n (e)) and other excitation characteristics in the ICP. These ICP characteristics were studied and evaluated during ablation of eight milk samples. Differences in n (e) (from 8.9 to 13.8 × 10(14) cm(-3)) and rotational temperature (ranging from 3,400 to 4,400 K) occurred with no correlation with trueness. LIBS results obtained after classical external calibration procedure gave degraded accuracy, indicating a strong matrix effect. The LIBS measurements clearly showed that the major problem in LA-ICP was related to the ablation process and that LIBS spectroscopy is an excellent diagnostic tool for LA-ICP techniques.
Elemental bioimaging by means of LA-ICP-OES: investigation of the calcium, sodium and potassium distribution in tobacco plant stems and leaf petioles.

PubMed

Thyssen, G M; Holtkamp, M; Kaulfürst-Soboll, H; Wehe, C A; Sperling, M; von Schaewen, A; Karst, U

2017-06-21

Laser ablation-inductively coupled plasma-optical emission spectroscopy (LA-ICP-OES) is presented as a valuable tool for elemental bioimaging of alkali and earth alkali elements in plants. Whereas LA-ICP-OES is commonly used for micro analysis of solid samples, laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) has advanced to the gold standard for bioimaging. However, especially for easily excitable and ubiquitous elements such as alkali and earth alkali elements, LA-ICP-OES holds some advantages regarding simultaneous detection, costs, contamination, and user-friendliness. This is demonstrated by determining the calcium, sodium and potassium distribution in tobacco plant stem and leaf petiole tissues. A quantification of the calcium contents in a concentration range up to 1000 μg g -1 using matrix-matched standards is presented as well. The method is directly compared to a LA-ICP-MS approach by analyzing parallel slices of the same samples.
[Study on the determination of 28 inorganic elements in sunflower seeds by ICP-OES/ICP-MS].

PubMed

Liu, Hong-Wei; Qin, Zong-Hui; Xie, Hua-Lin; Cao, Shu

2013-01-01

The present paper describes a simple method for the determination of trace elements in sunflower seeds by using inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma spectrometry (ICP-MS). HNO3 + H2O2 were used to achieve the complete decomposition of the organic matrix in a closed-vessel microwave oven. The contents of 10 trace elements (Al, B, Ca, Fe, K, Mg, Na, Si, P and S) in sunflower seeds were determined by ICP-OES while 18 trace elements (As, Ba, Cd, Co, Cr, Cu, Li, Mn, Mo, Ni, Pb, Rb, Sr, Sn, Sb, Ti, V and Zn) were determined by ICP-MS. The rice reference material (GBW10045) was used as standard reference materials. The results showed a good agreement between measured and certified values for all analytes. The concentrations of necessary micro elements Ca, K, Mg, P and S were higher. This method was simple, sensitive and precise and can perform simultaneous multi-elements determination of sunflower seeds.
[Simultaneous Determination of Sn and S in Methyltin Mercaptide by Microwave-Assisted Acid Digestion and ICP-OES].

PubMed

Chen, Qian; Wu, Xi; Hou, Xian-deng; Xu, Kai-lai

2015-09-01

Methyltin mercaptide is widely used as one of the best heat stabilizer in the polyvinylchloride (PVC) thermal processing due to its excellent stability, good transparency, high compatibility and weather resistance. The content of sulfur and tin significantly affects its quality and performance, so it is of great significance to develop an analytical method for the simultaneous determination of sulfur and tin. Inductively coupled plasma atomic emission spectrometry (ICP-OES) has been a powerful analytical tool for a myriad of complex samples owing to its advantages of the low detection limits, rapid and precise determinations over wide dynamic ranges, freedom from chemical inter-element interferences, the high sample throughput and above all, simultaneous multi-elements analysis. Microwave technique as a well-developed method for sample preparation can dramatically reduce the digestion time and the loss of volatile elements compared with the traditional open digestion. Hereby, a microwave-assisted acid digestion (MW-AAD) procedure followed by inductively coupled plasma optical emission spectroscopy (ICP-OES) analysis was developed for the simultaneous determination of Sn and S in methyltin mercaptide. This method has the advantages of simplicity, rapidness, good accuracy, green and less use of samples. Parameters affecting the MW-AAD such as the digestion solution and digestion time were optimized by using a chemical analyzed reference sample (DX-181) to attain tin and sulfur quantitative recoveries. HNO3-HCl-HClO4 (v/v/v=9:3:1) and 10 min were the optimum digestion solution and digestion time, respectively. Under optimum conditions, the standard addition method and the standard calibration curve method were both been used to detect Sn and S in DX-181. There was no significant difference between two methods and the relative deviations to the chemical analysis values were both less than 2%. Additionally, the accuracy of the MW-AAD method was examined by analyzing three methyltin mercaptide samples (DX-181, DX-990, DX-960). The results were satisfactory with the relative deviations (<3%) and the recoveries of standard addition (99%~102%).
H-bonding scheme and cation partitioning in axinite: a single-crystal neutron diffraction and Mössbauer spectroscopic study

NASA Astrophysics Data System (ADS)

Gatta, G. Diego; Redhammer, Günther J.; Guastoni, Alessandro; Guastella, Giorgio; Meven, Martin; Pavese, Alessandro

2016-05-01

The crystal chemistry of a ferroaxinite from Colebrook Hill, Rosebery district, Tasmania, Australia, was investigated by electron microprobe analysis in wavelength-dispersive mode, inductively coupled plasma-atomic emission spectroscopy (ICP-AES), 57Fe Mössbauer spectroscopy and single-crystal neutron diffraction at 293 K. The chemical formula obtained on the basis of the ICP-AES data is the following: ^{X1,X2} {{Ca}}_{4.03} Y ( {{{Mn}}_{0.42} {{Mg}}_{0.23} {{Fe}}^{2 + }_{1.39} } )_{Σ 2.04} ^{Z1,Z2} ( {{{Fe}}^{3 + }_{0.15} {{Al}}_{3.55} {{Ti}}_{0.12} } )_{Σ 3.82} ^{T1,T2,T3,T4} ( {{{Ti}}_{0.03} {{Si}}_{7.97} } )_{Σ 8} ^{T5} {{B}}_{1.96} {{O}}_{30} ( {{OH}} )_{2.18} . The 57Fe Mössbauer spectrum shows unambiguously the occurrence of Fe2+ and Fe3+ in octahedral coordination only, with Fe2+/Fe3+ = 9:1. The neutron structure refinement provides a structure model in general agreement with the previous experimental findings: the tetrahedral T1, T2, T3 and T4 sites are fully occupied by Si, whereas the T5 site is fully occupied by B, with no evidence of Si at the T5, or Al or Fe3+ at the T1- T5 sites. The structural and chemical data of this study suggest that the amount of B in ferroaxinite is that expected from the ideal stoichiometry: 2 a.p.f.u. (for 32 O). The atomic distribution among the X1, X2, Y, Z1 and Z2 sites obtained by neutron structure refinement is in good agreement with that based on the ICP-AES data. For the first time, an unambiguous localization of the H site is obtained, which forms a hydroxyl group with the oxygen atom at the O16 site as donor. The H-bonding scheme in axinite structure is now fully described: the O16- H distance (corrected for riding motion effect) is 0.991(1) Å and an asymmetric bifurcated bonding configuration occurs, with O5 and O13 as acceptors [i.e. with O16··· O5 = 3.096(1) Å, H··· O5 = 2.450(1) Å and O16- H··· O5 = 123.9(1)°; O16··· O13 = 2.777(1) Å, H··· O13 = 1.914(1) Å and O16- H··· O13 = 146.9(1)°].
Rapid screening of heavy metals and trace elements in environmental samples using portable X-ray fluorescence spectrometer, A comparative study

PubMed Central

McComb, Jacqueline Q.; Rogers, Christian; Han, Fengxiang X.; Tchounwou, Paul B.

2014-01-01

With industrialization, great amounts of trace elements and heavy metals have been excavated and released on the surface of the earth and dissipated into the environments. Rapid screening technology for detecting major and trace elements as well as heavy metals in variety of environmental samples is most desired. The objectives of this study were to determine the detection limits, accuracy, repeatability and efficiency of a X-ray fluorescence spectrometer (Niton XRF analyzer) in comparison with the traditional analytical methods, inductively coupled plasma optical emission spectrometer (ICP-OES) and inductively coupled plasma optical emission spectrometer (ICP-MS) in screening of major and trace elements of environmental samples including estuary soils and sediments, contaminated soils, and biological samples. XRF is a fast and non-destructive method in measuring the total concentration of multi--elements simultaneously. Contrary to ICP-OES and ICP-MS, XRF analyzer is characterized by the limited preparation required for solid samples, non-destructive analysis, increased total speed and high throughout, the decreased production of hazardous waste and the low running costs as well as multi-elemental determination and portability in the fields. The current comparative study demonstrates that XRF is a good rapid non-destructive method for contaminated soils, sediments and biological samples containing higher concentrations of major and trace elements. Unfortunately, XRF does not have sensitive detection limits of most major and trace elements as ICP-OES or ICP-MS but it may serve as a rapid screening tool for locating hot spots of uncontaminated field soils and sediments. PMID:25861136
Hydraulic Evolution of Karst Microfracture

NASA Astrophysics Data System (ADS)

Windom, L. M.; Dragila, M. I.; Weisbrod, N.

2017-12-01

Karst terrain comprises an astounding 25% of our planet's potable water resources, yet the evolution of these systems from micro-fracture to open channel is poorly understood. Focusing on the unsaturated portion of an evolving karst system, we present a conceptual model for the hydraulic evolution of micro-fractures into larger conduits. Tensional micro-fractures (< 1mm thick) under unsaturated conditions may be eroded by water flowing either as seepage films or as capillary rivulets. In addition to general erosion, the narrow width of capillary rivulets may etch the beginning of preferential paths within the tensional micro-fractures that will lead to tubular channels. Both fluid mechanisms, seepage and rivulets, were tested in the laboratory, and data of the resulting geochemical erosion rates are presented in the form of calcium dissolution rates measured by inductively coupled plasma atomic emission spectroscopy (ICP-OES).
Determination of platinum in waste platinum-loaded carbon catalyst samples using microwave-assisted sample digestion and ICP-OES

NASA Astrophysics Data System (ADS)

Ma, Yinbiao; Wei, Xiaojuan

2017-04-01

A novel method for the determination of platinum in waste platinum-loaded carbon catalyst samples was established by inductively coupled plasma optical emission spectrometry after samples digested by microwave oven with aqua regia. Such experiment conditions were investigated as the influence of sample digestion methods, digestion time, digestion temperature and interfering ions on the determination. Under the optimized conditions, the linear range of calibration graph for Pt was 0 ˜ 200.00 mg L-1, and the recovery was 95.67% ˜ 104.29%. The relative standard deviation (RSDs) for Pt was 1.78 %. The proposed method was applied to determine the same samples with atomic absorption spectrometry with the results consistently, which is suitable for the determination of platinum in waste platinum-loaded carbon catalyst samples.
Monitoring the growth of polyoxomolybdate nanoparticles in suspension by flow field-flow fractionation.

PubMed

Chen, Bailin; Jiang, Huijian; Zhu, Yan; Cammers, Arthur; Selegue, John P

2005-03-30

We follow the evolution of polyoxomolybdate nanoparticles in suspensions derived from the keplerate (NH4)42[MoVI72MoV60O372(CH3CO2)30(H2O)72].ca..300H2O.ca..10CH3CO2NH4 ({Mo132}) by flow field-flow fractionation (FlFFF) to monitor the particle-size distribution in situ, atomic force and high-resolution transmission electron microscopy (AFM, SEM, and HRTEM) to confirm particle sizes, inductively coupled plasma-optical emission spectrometry (ICP-OES) to determine the Mo content of the FlFFF-separated fractions, and UV/visible spectroscopy to confirm the identity of the species in suspension. We observe the formation of 3-75-nm polyoxomolybdate particles in suspension and the dynamic growth of {Mo132} crystals.

Fluid Shifts: Otoacoustical Emission Changes in Response to Posture and Lower Body Negative Pressure

NASA Technical Reports Server (NTRS)

Melgoza, R.; Kemp, D.; Ebert, D.; Danielson, R.; Stenger, M.; Hargens, A.; Dulchavsky, S.

2016-01-01

INTRODUCTION: The purpose of the NASA Fluid Shifts Study is to characterize fluid distribution and compartmentalization associated with long-duration spaceflight and to correlate these findings with vision changes and other elements of the visual impairment and intracranial pressure (VIIP) syndrome. VIIP signs and symptoms, as well as postflight lumbar puncture data, suggest that elevated intracranial pressure (ICP) may be associated with spaceflight-induced cephalad fluid shifts, but this hypothesis has not been tested. Due to the invasive nature of direct measures of ICP, a noninvasive technique of monitoring ICP is desired for use during spaceflight. The phase angle and amplitude of otoacoustic emissions (OAEs) have been shown to be sensitive to posture change and ICP (1, 2), therefore use of OAEs is an attractive option. OAEs are low-level sounds produced by the sensory cells of the cochlea in response to auditory stimulation. These sounds travel peripherally from the cochlea, through the oval window, to the ear canal where they can be recorded. OAE transmission is sensitive to changes in the stiffness of the oval window, occurring as a result of changes in cochlear pressure. Increased stiffness of the oval window largely affects the transmission of sound from the cochlea at frequencies between 800 Hz and 1600 Hz. OAEs can be self-recorded in the laboratory or on the ISS using a handheld device. Our primary objectives regarding OAE measures in this experiment were to 1) validate this method during preflight testing of each crewmember (while sitting, supine and in head-down tilt position), and 2) determine if OAE measures (and presumably ICP) are responsive to lower body negative pressure and to spaceflight. METHODS: Distortion-product otoacoustic emissions (DPOAEs) and transient evoked otoacoustic emissions (TEOAEs) were recorded preflight using the Otoport Advance OAE system (Otodynamics Ltd., Hatfield, UK). Data were collected in four conditions (seated, supine, 15 degrees head down tilt (HDT), and 15 degrees HDT with lower body negative pressure (LBNP)) to produce a range of ICP in each subject and test the susceptibility of OAEs to LBNP. LBNP was induced using the Russian Chibis suit to produce the same fit and pressures that would be experienced inflight during Chibis LBNP trials. Similar trials have occurred inflight on the ISS. A comparative analysis of preflight and inflight phase measurements and magnitudes was completed in both broad and narrow band frequency ranges. RESULTS: TEOAE data demonstrated notable phase shifts from 859-1640 Hz when the seated baseline condition is compared to supine, HDT, and HDT plus Chibis conditions. Changes were particularly pronounced at low frequencies and were consistent with the expected ICP changes. Preflight DPOAE magnitude data revealed changes consistent with increased ICP in two conditions at 1414 Hz, where a magnitude change (relative to the seated condition) was seen in the HDT position and in HDT plus Chibis. DISCUSSION: OAEs revealed systematic changes in phase and magnitude throughout all test conditions (including use of Chibis LBNP) that were consistent with ICP changes. Results indicate that OAEs may provide a rapid noninvasive means of monitoring ICP changes. The first two subjects are projected to complete inflight testing on the ISS in early 2016, with the full complement of 10 subjects scheduled to be complete in 2018.
Aerosol detection efficiency in inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Hubbard, Joshua A.; Zigmond, Joseph A.

2016-05-01

An electrostatic size classification technique was used to segregate particles of known composition prior to being injected into an inductively coupled plasma mass spectrometer (ICP-MS). Size-segregated particles were counted with a condensation nuclei counter as well as sampled with an ICP-MS. By injecting particles of known size, composition, and aerosol concentration into the ICP-MS, efficiencies of the order of magnitude aerosol detection were calculated, and the particle size dependencies for volatile and refractory species were quantified. Similar to laser ablation ICP-MS, aerosol detection efficiency was defined as the rate at which atoms were detected in the ICP-MS normalized by the rate at which atoms were injected in the form of particles. This method adds valuable insight into the development of technologies like laser ablation ICP-MS where aerosol particles (of relatively unknown size and gas concentration) are generated during ablation and then transported into the plasma of an ICP-MS. In this study, we characterized aerosol detection efficiencies of volatile species gold and silver along with refractory species aluminum oxide, cerium oxide, and yttrium oxide. Aerosols were generated with electrical mobility diameters ranging from 100 to 1000 nm. In general, it was observed that refractory species had lower aerosol detection efficiencies than volatile species, and there were strong dependencies on particle size and plasma torch residence time. Volatile species showed a distinct transition point at which aerosol detection efficiency began decreasing with increasing particle size. This critical diameter indicated the largest particle size for which complete particle detection should be expected and agreed with theories published in other works. Aerosol detection efficiencies also displayed power law dependencies on particle size. Aerosol detection efficiencies ranged from 10- 5 to 10- 11. Free molecular heat and mass transfer theory was applied, but evaporative phenomena were not sufficient to explain the dependence of aerosol detection on particle diameter. Additional work is needed to correlate experimental data with theory for metal-oxides where thermodynamic property data are sparse relative to pure elements. Lastly, when matrix effects and the diffusion of ions inside the plasma were considered, mass loading was concluded to have had an effect on the dependence of detection efficiency on particle diameter.
Determination of trace metals in TSP and PM2.5 materials collected in the Metropolitan Area of Monterrey, Mexico: A characterization study by XPS, ICP-AES and SEM-EDS

NASA Astrophysics Data System (ADS)

González, Lucy T.; Longoria Rodríguez, F. E.; Sánchez-Domínguez, M.; Cavazos, Aleyda; Leyva-Porras, C.; Silva-Vidaurri, L. G.; Askar, Karim Acuña; Kharissov, B. I.; Villarreal Chiu, J. F.; Alfaro Barbosa, J. M.

2017-11-01

The concentration levels of trace metals of toxicological importance were evaluated in the total suspended particles (TSP) and particulate matter smaller than 2.5 μm (PM2.5) collected in the Metropolitan Area of Monterrey (MAM) in Mexico. Samples were characterized by inductively coupled plasma atomic emission spectroscopy (ICP-AES), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy with an energy-dispersive spectroscopy system (SEM-EDS). In addition, the data were statistically treated by the methodology of Pearson Correlation (PC) and Principal Components Analysis (PCA) to identify the possible emitting sources. Surface analysis of the particulate matter (PM) by XPS revealed that the most abundant elements were Ca, Al, Na, Zn, Cu and Mg. The deconvolution of the Ca2p, Zn2p and Cu2p signals showed that the main contributors were CaCO3, ZnO and Cu/Cu2O, respectively. The bulk analysis of the PM by ICP-AES showed Fe, Cu and Zn as the most abundant elements. Fe-rich particles presented two different morphologies: the prismatic particles were associated with a natural origin, while the spherical particles with anthropogenic sources. The Zn and Cu were predominantly observed in the sampling stations with high vehicular traffic, and the emitting sources were associated with the burning of fuels from automobiles and the wear of the tires and brakes. The highest concentration of Pb was detected in the sampling station located near the industrial zones, and its cause was associated with the ceramic and glass industries, the burning of fuel oil in power plants and the production of lead-based batteries for automobiles.
Heavy-metal contamination on training ranges at the Grafenwoehr Training Area, Germany

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

Zellmer, S.D.; Schneider, J.F.

1993-05-01

Large quantities of lead and other heavy metals are deposited in the environment of weapons ranges during training exercises. This study was conducted to determine the type, degree, and extent of heavy-metal contamination on selected handgun, rifle, and hand-grenade ranges at Grafenwoehr Training Area, Germany. Soil, vegetation, and surface-water samples were collected and analyzed using the inductively-coupled plasma atomic-emission spectroscopy (ICP-AES) method and the toxic characterization leaching procedure (TCLP). The ICP-AES results show that above-normal levels of lead and copper are in the surface soil at the handgun range, high concentrations of lead and copper are in the berm andmore » soil surface at the rifle range, and elevated levels of cadmium and above-normal concentrations of arsenic, copper, and zinc are present in the surface soil at the hand-grenade range. The TCLP results show that surface soils can be considered hazardous waste because of lead content at the rifle range and because of cadmium concentration at the hand-grenade range. Vegetation at the handgun and rifle ranges has above-normal concentrations of lead. At the hand-grenade range, both vegetation and surface water have high levels of cadmium. A hand-held X-ray fluorescence (XRF) spectrum analyzer was used to measure lead concentrations in soils in a field test of the method. Comparison of XRF readings with ICP-AES results for lead indicate that the accuracy and precision of the hand-held XRF unit must improve before the unit can be used as more than a screening tool. Results of this study show that heavy-metal contamination at all three ranges is limited to the surface soil; heavy metals are not being leached into the soil profile or transported into adjacent areas.« less
Discrimination of wine from grape cultivated in Japan, imported wine, and others by multi-elemental analysis.

PubMed

Shimizu, Hideaki; Akamatsu, Fumikazu; Kamada, Aya; Koyama, Kazuya; Okuda, Masaki; Fukuda, Hisashi; Iwashita, Kazuhiro; Goto-Yamamoto, Nami

2018-04-01

Differences in mineral concentrations were examined among three types of wine in the Japanese market place: Japan wine, imported wine, and domestically produced wine mainly from foreign ingredients (DWF), where Japan wine has been recently defined by the National Tax Agency as domestically produced wine from grapes cultivated in Japan. The main objective of this study was to examine the possibility of controlling the authenticity of Japan wine. The concentrations of 18 minerals (Li, B, Na, Mg, Si, P, S, K, Ca, Mn, Co, Ni, Ga, Rb, Sr, Mo, Ba, and Pb) in 214 wine samples were determined by inductively coupled-plasma mass spectrometry (ICP-MS) and ICP-atomic emission spectrometry (ICP-AES). In general, Japan wine had a higher concentration of potassium and lower concentrations of eight elements (Li, B, Na, Si, S, Co, Sr, and Pb) as compared with the other two groups of wine. Linear discriminant analysis (LDA) models based on concentrations of the 18 minerals facilitated the identification of three wine groups: Japan wine, imported wine, and DWF with a 91.1% classification score and 87.9% prediction score. In addition, an LDA model for discrimination of wine from four domestic geographic origins (Yamanashi, Nagano, Hokkaido, and Yamagata Prefectures) using 18 elements gave a classification score of 93.1% and a prediction score of 76.4%. In summary, we have shown that an LDA model based on mineral concentrations is useful for distinguishing Japan wine from other wine groups, and can contribute to classification of the four main domestic wine-producing regions of Japan. Copyright © 2017 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.
Gd-DTPA T1 relaxivity in brain tissue obtained by convection-enhanced delivery, magnetic resonance imaging and emission spectroscopy

NASA Astrophysics Data System (ADS)

Haar, Peter J.; Broaddus, William C.; Chen, Zhi-jian; Fatouros, Panos P.; Gillies, George T.; Corwin, Frank D.

2010-06-01

A common approach to quantify gadolinium (Gd) contrast agents involves measuring the post-contrast change in T1 rate and then using the constant T1 relaxivity R to determine the contrast agent concentration. Because this method is fast and non-invasive, it could be potentially valuable in many areas of brain research. However, to accurately measure contrast agent concentrations in the brain, the T1 relaxivity R of the specific agent must be accurately known. Furthermore, the macromolecular content and compartmentalization of the brain extracellular space (ECS) are expected to significantly alter R from values measured in aqueous solutions. In this study, the T1 relaxivity R of gadolinium-diethylene-triamine penta-acetic acid (Gd-DTPA) was measured following direct interstitial infusions of three different contrast agent concentrations to the parenchyma of rat brains. Changes in magnetic resonance (MR) T1 values were compared to brain slice concentrations determined with inductively coupled plasma atomic emission spectroscopy (ICP-AES) to determine R in 15 rats. Additionally, samples of cerebrospinal fluid, blood and urine were analyzed to evaluate possible Gd-DTPA clearance from the brain. The T1 relaxivity R of Gd-DTPA in the brain ECS was measured to be 5.35 (mM s)-1 in a 2.4 T field. This value is considerably higher than estimations used in studies by other groups. Measurements of brain Gd-DTPA tissue concentrations using MRI and ICP-AES demonstrated a high degree of coincidence. Clearance of Gd-DTPA was minimal at the time point immediately after infusion. These results suggest that the environment of the brain does in fact significantly affect Gd T1 relaxivity, and that MRI can accurately measure contrast agent concentrations when this relaxivity is well characterized.
Daily and hourly chemical impact of springtime transboundary aerosols on Japanese air quality

NASA Astrophysics Data System (ADS)

Moreno, T.; Kojima, T.; Amato, F.; Lucarelli, F.; de la Rosa, J.; Calzolai, G.; Nava, S.; Chiari, M.; Alastuey, A.; Querol, X.; Gibbons, W.

2013-02-01

The regular eastward drift of transboundary aerosol intrusions from the Asian mainland into the NW Pacific region has a pervasive impact on air quality in Japan, especially during springtime. Analysis of 24-h filter samples with Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) and Mass Spectrometry (ICP-MS), and hourly Streaker with Particle Induced X-ray Emission (PIXE) samples collected continuously for six weeks reveal the chemistry of successive waves of natural mineral desert dust ("Kosa") and metalliferous sulphatic pollutants arriving in western Japan during spring 2011. The main aerosol sources recognised by Positive Matrix Factorization (PMF) analysis of Streaker data are mineral dust and fresh sea salt (both mostly in the coarser fraction PM2.5-10), As-bearing sulphatic aerosol (PM0.1-2.5), metalliferous sodic particulate matter (PM) interpreted as aged, industrially contaminated marine aerosol, and ZnCu-bearing aerosols. Whereas mineral dust arrivals are typically highly transient, peaking over a few hours, sulphatic intrusions build up and decline more slowly, and are accompanied by notable rises in ambient concentrations of metallic trace elements such as Pb, As, Zn, Sn and Cd. The magnitude of the loss in regional air quality due to the spread and persistence of pollution from mainland Asia is especially clear when cleansing oceanic air advects westward across Japan, removing the continental influence and reducing concentrations of the undesirable metalliferous pollutants by over 90%. Our new chemical database, especially the Streaker data, demonstrates the rapidly changing complexity of ambient air inhaled during these transboundary events, and implicates Chinese coal combustion as the main source of the anthropogenic aerosol component.
Multi-elemental analysis of aqueous geochemical samples by quadrupole inductively coupled plasma-mass spectrometry (ICP-MS)

USGS Publications Warehouse

Wolf, Ruth E.; Adams, Monique

2015-01-01

Typically, quadrupole inductively coupled plasma-mass spectrometry (ICP-MS) is used to determine as many as 57 major, minor, and trace elements in aqueous geochemical samples, including natural surface water and groundwater, acid mine drainage water, and extracts or leachates from geological samples. The sample solution is aspirated into the inductively coupled plasma (ICP) which is an electrodeless discharge of ionized argon gas at a temperature of approximately 6,000 degrees Celsius. The elements in the sample solution are subsequently volatilized, atomized, and ionized by the ICP. The ions generated are then focused and introduced into a quadrupole mass filter which only allows one mass to reach the detector at a given moment in time. As the settings of the mass analyzer change, subsequent masses are allowed to impact the detector. Although the typical quadrupole ICP-MS system is a sequential scanning instrument (determining each mass separately), the scan speed of modern instruments is on the order of several thousand masses per second. Consequently, typical total sample analysis times of 2–3 minutes are readily achievable for up to 57 elements.
Challenges in the quality assurance of elemental and isotopic analyses in the nuclear domain benefitting from high resolution ICP-OES and sector field ICP-MS.

PubMed

Krachler, Michael; Alvarez-Sarandes, Rafael; Van Winckel, Stefaan

Accurate analytical data reinforces fundamentally the meaningfulness of nuclear fuel performance assessments and nuclear waste characterization. Regularly lacking matrix-matched certified reference materials, quality assurance of elemental and isotopic analysis of nuclear materials remains a challenging endeavour. In this context, this review highlights various dedicated experimental approaches envisaged at the European Commission-Joint Research Centre-Institute for Transuranium Elements to overcome this limitation, mainly focussing on the use of high resolution-inductively coupled plasma-optical emission spectrometry (HR-ICP-OES) and sector field-inductively coupled plasma-mass spectrometry (SF-ICP-MS). However, also α- and γ-spectrometry are included here to help characterise extensively the investigated actinide solutions for their actual concentration, potential impurities and isotopic purity.
[Pretreatment of Aluminum-Lithium Alloy Sample and Determination of Argentum and Lithium by Spectral Analysis].

PubMed

Zhou, Hui; Tan, Qian; Gao, Ya-ling; Sang, Shi-hua; Chen, Wen

2015-10-01

Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), Flame Atomic Absorption Spectrometry (FAAS) and Visible Spectrometry (VS) was applied for determination of Ag and Li in lithium-aluminium alloy standard sample and test sample, their respective advantages and disadvantages were compared, the excellent selectivity of ICP-OES was confirmed by analyses of certified standard sample. Three different sample digestion methods were compared and discussed in this study. It was found that the better accuracy would be obtained by digesting sample with chloroazotic acid while the content of Li was measured by FAAS, and it was better to digest sample with hydrochloric acid and hydrogen peroxide while determining Ag and Li by ICP-OES simultaneously and determining Ag by FAAS and VS. The interference of co-existing elements and elimination methods was detailedly discussed. Ammonium hydroxide was added to adjust the sample solution into alkalescent and Al, Ti, Zr was precipitated by forming hydroxide precipitation, Mg and Cu was formed complex precipitation with 8-hydroxyquinoline in this condition, then the interference from matrix element to determinate Ag by FAAS was eliminated. In addition, phosphate was used to precipitate Ti to eliminate its interference for determination of Li by FAAS. The same treatment of determination for Ag by FAAS was used to eliminate the interference of matrix element for determination of Ag by VS, the excess of nitrate was added into sample and heated to release Ag+ from silver chloride complex, and the color of 8-hydroxyquinoline was eliminated because of decomposed by heating. The accuracy of analysis result for standard sample was conspicuously improved which confirms the efficient of the method to eliminate interference in this study. The optimal digestion method and eliminate interference method was applied to lithium-aluminium alloy samples. The recovery of samples was from 100.39% to 103.01% by ICP-OES determination for Ag, and from 100.42% to 103.01% by ICP-OES determination for Li. The recovery ranged from 95.91% to 99.98% by FAAS determination for Ag, and ranged from 98.04% to 99.98% for FAAS determination of Li. The recovery was from 98.00% to 101.00 by VS determination for Ag, the analysis results all meet the analysis requirement.
Collection of trace evidence of explosive residues from the skin in a death due to a disguised letter bomb. The synergy between confocal laser scanning microscope and inductively coupled plasma atomic emission spectrometer analyses.

PubMed

Turillazzi, Emanuela; Monaci, Fabrizio; Neri, Margherita; Pomara, Cristoforo; Riezzo, Irene; Baroni, Davide; Fineschi, Vittorio

2010-04-15

In most deaths caused by explosive, the victim's body becomes a depot for fragments of explosive materials, so contributing to the collection of trace evidence which may provide clues about the specific type of device used with explosion. Improvised explosive devices are used which contain "homemade" explosives rather than high explosives because of the relative ease with which such components can be procured. Many methods such as chromatography-mass spectrometry, scanning electron microscopy, stereomicroscopy, capillary electrophoresis are available for use in the identification of explosive residues on objects and bomb fragments. Identification and reconstruction of the distribution of explosive residues on the decedent's body may give additional hints in assessing the position of the victim in relation to the device. Traditionally these residues are retrieved by swabbing the body and clothing during the early phase, at autopsy. Gas chromatography-mass spectrometry and other analytical methods may be used to analyze the material swabbed from the victim body. The histological examination of explosive residues on skin samples collected during the autopsy may reveal significant details. The information about type, quantity and particularly about anatomical distribution of explosive residues obtained utilizing confocal laser scanning microscope (CLSM) together with inductively coupled plasma atomic emission spectrometer (ICP-AES), may provide very significant evidence in the clarification and reconstruction of the explosive-related events. Copyright 2009 Elsevier Ireland Ltd. All rights reserved.
In vitro biocompatibility of magnesium-incorporated submicro-porous titanium oxide surface produced by hydrothermal treatment

NASA Astrophysics Data System (ADS)

Park, Jin-Woo; Kim, Youn-Jeong; Jang, Je-Hee; An, Chang-Hyeon

2010-11-01

This study investigated the surface characteristics and in vitro biocompatibility of titanium (Ti) oxide surface incorporating magnesium ions (Mg), produced by hydrothermal treatment using an alkaline Mg-containing solution, for future biomedical applications. The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy, inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and optical profilometry. Mouse calvaria-derived osteoblastic cell (MC3T3-E1) attachment, spreading, proliferation, alkaline phosphatase (ALP) activity, and osteoblastic gene expression on Mg-containing surfaces were compared with untreated Ti surfaces. Hydrothermal treatment resulted in Mg-incorporated Ti oxide layer with submicro-porous surface structures approximately 2 μm in thickness. ICP-AES analysis revealed Mg ions release from treated surfaces into the solution. The Mg-incorporated surface displayed significantly increased cellular attachment and ALP activity compared with untreated surface ( p < 0.05), and supported better cell spreading. Real-time polymerase chain reaction analysis showed notably higher mRNA expression of the osteoblast transcription factor genes (Dlx5, Runx2) and the osteoblast phenotype genes (ALP, bone sialoprotein and osteocalcin) in cells grown on the Mg-incorporated surfaces than untreated surfaces. These results demonstrate that the Mg-incorporated submicro-porous Ti oxide surface produced by hydrothermal treatment may improve implant osseointegration by enhancing the attachment, spreading and differentiation of osteoblastic cells.
Mineralogical basis for the interpretation of multi-element (ICP-AES), oxalic acid, and aqua regia partial digestions of stream sediments for reconnaissance exploration geochemistry

USGS Publications Warehouse

Church, S.E.; Mosier, E.L.; Motooka, J.M.

1987-01-01

We have applied partial digestion procedures, primarily oxalic acid and aqua regia leaches, to several regional geochemical reconnaissance studies carried out using Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) analytical methods. We have chosen to use these two acids because the oxalic acid primarily attacks those compounds formed during secondary geochemical processes, whereas aqua regia will digest the primary sulfide phases as well as secondary phases. Application of the partial digestion technique has proven superior to total digestion because the concentration of metals in hydromorphic compounds and the sulfides is enhanced relative to the metals bound in the unattacked silicate phases. The aqua regia digestion attacks and leaches metals from the mafic chain silicates and the phyllosilicates (coordination number of VI or more), yielding a characteristic geochemical signature, but does not leach appreciable metal from many other silicates. In order to interpret the results from these leach studies, we have initiated an investigation of a large suite of hand-picked mineral separates. The study includes analyses of about two hundred minerals representing the common rock-forming minerals as well as end-member compositions of various silicates, oxides, sulfides, carbonates, sulfates, and some vanadates, molybdates, tungstates, and phosphates. The objective of this study is to evaluate the effect of leaching by acids of particular lattice sites in specific mineral structures. ?? 1987.
Vanadium Recovery from Oil Fly Ash by Carbon Removal and Roast-Leach Process

NASA Astrophysics Data System (ADS)

Jung, Myungwon; Mishra, Brajendra

2018-02-01

This research mainly focuses on the recovery of vanadium from oil fly ash by carbon removal and the roast-leach process. The oil fly ash contained about 85% unburned carbon and 2.2% vanadium by weight. A vanadium-enriched product was obtained after carbon removal, and the vanadium content of this product was 19% by weight. Next, the vanadium-enriched product was roasted with sodium carbonate to convert vanadium oxides to water-soluble sodium metavanadate. The roasted sample was leached with water at 60°C, and the extraction percentage of vanadium was about 92% by weight. Several analytical techniques, such as inductively coupled plasma atomic emission spectroscopy (ICP-AES), x-ray fluorescence (XRF), and thermogravimetric and differential thermal analysis (TG-DTA), were utilized for sample analyses. Thermodynamic modeling was also conducted with HSC chemistry software to explain the experimental results.
Mineral and heavy metal levels of some fruits grown at the roadsides.

PubMed

Hamurcu, Mehmet; Ozcan, Mehmet Musa; Dursun, Nesim; Gezgin, Sait

2010-06-01

The rate of heavy metal pollution of some minor fruit samples growing at the roadsides in Turkey were determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). Pb, Zn and Cu were found at the high levels in the fruit samples. The results showed that the average level of Cu changed between 0.27 mg/kg (Sample 11) and 0.05 mg/kg (Sample 15), Cr 0.32 mg/kg (Sample 14) and 0.18 mg/kg (Sample 13), Ni 0.68 mg/kg (Sample 12) and 0.26 g/kg (Sample 15), Pb 2.86 mg/kg (Sample 12) and 1.54 mg/kg (Sample 4) and Se 12.96 mg/kg (Sample 14) and 5.42 mg/kg (Sample 7). The levels of Cu, Cd and Cr in samples do not appear to reach pollution levels. Copyright 2010 Elsevier Ltd. All rights reserved.
Release of titanium after insertion of dental implants with different surface characteristics – an ex vivo animal study

PubMed Central

Pettersson, Mattias; Pettersson, Jean; Molin Thorén, Margareta; Johansson, Anders

2017-01-01

Abstract In the present study, amount of titanium (Ti) released into the surrounding bone during placement of implants with different surface structure was investigated. Quantification of Ti released during insertion from three different implants was performed in this ex vivo study. Jaw bone from pigs was used as model for installation of the implants and Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) was used for analysis of the released Ti. Implant surface were examined with scanning electron microscopy (SEM), before and after the placement into the bone. Ti was abraded to the surrounding bone upon insertion of a dental implant and the surface roughness of the implant increased the amount of Ti found. Diameter and total area of the implant were of less importance for the Ti released to the bone. No visible damages to the implant surfaces could be identified in SEM after placement. PMID:29242814
Differences in the element contents between gunshot entry wounds with full-jacketed bullet and lead bullet.

PubMed

Wunnapuk, Klintean; Durongkadech, Piya; Minami, Takeshi; Ruangyuttikarn, Werawan; Tohno, Setsuko; Vichairat, Karnda; Azuma, Cho; Sribanditmongkol, Pongruk; Tohno, Yoshiyuki

2007-01-01

To elucidate characteristics of gunshot residues in gunshot entry wounds with full-jacketed and lead bullets, element contents in entry gunshot wounds and control skins were analyzed by inductively coupled plasma-atomic emission spectrometry (ICP-AES). It was found that a high content of Fe and Zn was deposited in the gunshot entry wounds with full-jacketed bullet, whereas a high content of Pb was deposited in the gunshot entry wounds with lead (unjacked) bullet. It should be noted that the content of Pb was significantly higher in the gunshot entry wounds with lead bullet than in those with full-jacketed bullet. Regarding the relationships among elements, it was found that there were significant direct correlations between Pb and either Sb or Ba contents in both gunshot entry wounds with full-jacketed and lead bullets. As Pb increased in both gunshot entry wounds, Sb and Ba also increased in the wounds.
X-ray fluorescence analysis of K, Al and trace elements in chloroaluminate melts

NASA Astrophysics Data System (ADS)

Shibitko, A. O.; Abramov, A. V.; Denisov, E. I.; Lisienko, D. G.; Rebrin, O. I.; Bunkov, G. M.; Rychkov, V. N.

2017-09-01

Energy dispersive x-ray fluorescence spectrometry was applied to quantitative determination of K, Al, Cr, Fe and Ni in chloroaluminate melts. To implement the external standard calibration method, an unconventional way of samples preparation was suggested. A mixture of metal chlorides was melted in a quartz cell at 350-450 °C under a slightly excessive pressure of purified argon (99.999 %). The composition of the calibration samples (CSs) prepared was controlled by means of the inductively coupled plasma atomic emission spectrometry (ICP-AES). The optimal conditions for analytical lines excitation were determined, the analytes calibration curves were obtained. There was some influence of matrix effects in synthesized samples on the analytical signal of some elements. The CSs are to be stored in inert gas atmosphere. The precision, accuracy, and reproducibility factors of the quantitative chemical analysis were computed.
[Determination and correlation analysis of trace elements in Boletus tomentipes].

PubMed

Li, Tao; Wang, Yuan-zhong; Zhang, Ji; Zhao, Yan-li; Liu, Hong-gao

2011-07-01

The contents of eleven trace elements in Boletus tomentipes were determined by inductively coupled plasma atomic emission spectroscopy (ICP-AES). The results showed that the fruiting bodies of B. tomentipes were very rich in Mg and Fe (>100 mg x kg(-1)) and rich in Mn, Zn and Cu (>10 mg x kg(-1)). Cr, Pb, Ni, Cd, and As were relatively minor contents (0.1-10.0 mg x kg(-1)) of this species, while Hg occurred at the smallest content (< 0.1 mg x kg(-1)). Among the determined 11 trace elements, Zn-Cu had significantly positive correlation (r = 0.659, P < 0.05), whereas, Hg-As, Ni-Fe, and Zn-Mg had significantly negative correlation (r = -0.672, -0.610, -0.617, P < 0.05). This paper presented the trace elements properties of B. tomentipes, and is expected to be useful for exploitation and quality evaluation of this species.
Rapid Catalyst Capture Enables Metal-Free para-Hydrogen-Based Hyperpolarized Contrast Agents.

PubMed

Barskiy, Danila A; Ke, Lucia A; Li, Xingyang; Stevenson, Vincent; Widarman, Nevin; Zhang, Hao; Truxal, Ashley; Pines, Alexander

2018-05-10

Hyperpolarization techniques based on the use of para-hydrogen provide orders of magnitude signal enhancement for magnetic resonance spectroscopy and imaging. The main drawback limiting widespread applicability of para-hydrogen-based techniques in biomedicine is the presence of organometallic compounds (the polarization transfer catalysts) in solution with hyperpolarized contrast agents. These catalysts are typically complexes of platinum-group metals, and their administration in vivo should be avoided. Herein, we show how extraction of a hyperpolarized compound from an organic phase to an aqueous phase combined with a rapid (less than 10 s) Ir-based catalyst capture by metal scavenging agents can produce pure para-hydrogen-based hyperpolarized contrast agents, as demonstrated by high-resolution nuclear magnetic resonance (NMR) spectroscopy and inductively coupled plasma atomic emission spectroscopy (ICP-AES). The presented methodology enables fast and efficient means of producing pure hyperpolarized aqueous solutions for biomedical and other uses.

Biological monitoring of glazers exposed to lead in the ceramics industry in Iran.

PubMed

Shouroki, Fatemeh Kargar; Shahtaheri, Seyed Jamaleddin; Golbabaei, Farideh; Barkhordari, Abolfazle; Rahimi-Froushani, Abbas

2015-01-01

Exposure to heavy metals, particularly lead, takes place in the ceramics industry. Lead is used in glaze to produce smooth and brilliant surfaces; thus, there is a likelihood of occupational adverse effects on humans. Urine samples were collected from 49 glazers at the start and end of the work shifts (98 samples). Solid phase extraction was used for separation and pre-concentration of the analyte. Samples were analysed by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Lung function tests were performed on both control and lead exposed subjects. Statistical analysis of covariance (ANCOVA) was used to evaluate the data obtained. The concentration of lead in glazers was 6.37 times higher than in the control group. Lung functions were significantly lower in the glazers compared to the control group (p < 0.001). Results showed that poor ventilation systems, overtime work and work history are effective determinants of high exposure levels.
Field analyses of (238)U and (226)Ra in two uranium mill tailings piles from Niger using portable HPGe detector.

PubMed

Déjeant, Adrien; Bourva, Ludovic; Sia, Radia; Galoisy, Laurence; Calas, Georges; Phrommavanh, Vannapha; Descostes, Michael

2014-11-01

The radioactivities of (238)U and (226)Ra in mill tailings from the U mines of COMINAK and SOMAÏR in Niger were measured and quantified using a portable High-Purity Germanium (HPGe) detector. The (238)U and (226)Ra activities were measured under field conditions on drilling cores with 600s measurements and without any sample preparation. Field results were compared with those obtained by Inductive Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) and emanometry techniques. This comparison indicates that gamma-ray absorption by such geological samples does not cause significant deviations. This work shows the feasibility of using portable HPGe detector in the field as a preliminary method to observe variations of radionuclides concentration with the aim of identifying samples of interest. The HPGe is particularly useful for samples with strong secular disequilibrium such as mill tailings. Copyright © 2014 Elsevier Ltd. All rights reserved.
Rapid and simple determination of selenium in blood serum by inductively coupled plasma-mass spectrometry (ICP-MS).

PubMed

Labat, L; Dehon, B; Lhermitte, M

2003-05-01

An inductively coupled plasma mass spectrometer (ICP-MS) with a rapid sample-preparative procedure was used for the determination of selenium in blood serum. Blood serum was prepared by dilution in an acidic solution consisting of nitric acid (1%), X-triton (0.1%) and 1-butanol (0.8%). A calibration curve was established for 1-40 microg mL(-1) (r(2)>0.99). The limit of detection was 0.5 microg mL(-1). Repeatability and intermediate precision were satisfactory with relative standard deviations (RSD) of 2.0% and 3.2%, respectively. This method was easily applied to reference materials with satisfactory accuracy. Good correlation (r(2)=0.96) was observed between ICP-MS and atomic absorption spectrometry (AAS) for the determination of (82)Se in blood serum from 23 patients. These results suggest that the sample preparative procedure coupled with ICP-MS can be used for the routine determination of (82)Se in human blood serum.
Surface functionalisation of polypropylene hernia-repair meshes by RF-activated plasma polymerisation of acrylic acid and silver nanoparticles

NASA Astrophysics Data System (ADS)

Nisticò, Roberto; Rosellini, Andrea; Rivolo, Paola; Faga, Maria Giulia; Lamberti, Roberta; Martorana, Selanna; Castellino, Micaela; Virga, Alessandro; Mandracci, Pietro; Malandrino, Mery; Magnacca, Giuliana

2015-02-01

Hernia diseases are among the most common and diffuse causes of surgical interventions. Unfortunately, still nowadays there are different phenomena which can cause the hernioplasty failure, for instance post-operative prostheses displacements and proliferation of bacteria in the surgical site. In order to limit these problems, commercial polypropylene (PP) and polypropylene/Teflon (PP/PTFE) bi-material meshes were surface functionalised to confer adhesive properties (and therefore reduce undesired displacements) using polyacrylic acid synthesized by plasma polymerisation (PPAA). A broad physico-chemical and morphological characterisation was carried out and adhesion properties were investigated by means of atomic force microscopy (AFM) used in force/distance (F/D) mode. Once biomedical devices surface was functionalised by PPAA coating, metallic silver nanoparticles (AgNPs) with antimicrobial properties were synthesised and loaded onto the polymeric prostheses. The effect of the PPAA, containing carboxylic functionalities, adhesive coating towards AgNPs loading capacity was verified by means of X-ray photoelectron spectroscopy (XPS). Preliminary measurement of the Ag loaded amount and release in water were also investigated via inductively coupled plasma atomic emission spectroscopy (ICP-AES). Promising results were obtained for the functionalised biomaterials, encouraging future in vitro and in vivo tests.
Determination of metallo-organic and particulate wear metals in lubricating oils associated with hybrid ceramic bearings by inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Russell, Robin Ann

It is possible to increase both the performance and operating environment of jet engines by using hybrid ceramic bearings. Our laboratory is concerned with investigating lubricating fluids for wear metals associated with silicon nitride ball bearings and steel raceways. Silicon nitride is characterized by low weight, low thermal expansion, high strength, and corrosion resistance. These attributes result in longer engine lifetimes than when metallic ball bearings are used. Before the routine use of ceramic ball bearings can be realized, the wear mechanisms of the materials should be thoroughly understood. One important variable in determining wear degradation is the concentration of metal present in the lubricating oils used with the bearings. A complete method for analyzing used lubricating oils for wear metal content must accurately determine all metal forms present. Oil samples pose problems for routine analysis due to complex organic matrices. Nebulizing these types of samples into an Inductively Coupled Plasma - Mass Spectrometer introduces many problems including clogging of the sample cone with carbon and increasing interferences. In addition, other techniques such as Atomic Absorption Spectrometry and Atomic Emission Spectrometry are particle size dependent. They are unable to analyze particles greater than 10 mum in size. This dissertation describes a method of analyzing lubricating oils for both metallo-organic and particulate species by ICP-MS. Microwave digestion of the oil samples eliminates the need for elaborate sample introduction schemes as well as the use of a modified carrier gas. Al, Cr, Fe, Mg, Mo, Ni, Ti, and Y have been determined in both aqueous and organic media. Metallo-organic solutions of these metals were successfully digested, nebulized into the ICP, and the singly charged ions measured by mass spectrometry. Metal particulates in oil matrices have also been quantitatively determined by the above method. Linear analytical curves were obtained for these elements from the detection limits (˜1 ppb) to greater than 1 ppm. Used lubricating oil samples were also analyzed by microwave digestion ICP-MS. Oil samples were collected from a Rolling Contact Fatigue tester. Two bearing systems were evaluated: M50 steel balls on an M50 steel rod, and Sisb3Nsb4 balls on an M50 steel rod. Improved operating conditions were obtained when the Sisb3Nsb4 balls were used, which corresponds to longer engine lifetimes.
Optoelectronic properties of Black-Silicon generated through inductively coupled plasma (ICP) processing for crystalline silicon solar cells

NASA Astrophysics Data System (ADS)

Hirsch, Jens; Gaudig, Maria; Bernhard, Norbert; Lausch, Dominik

2016-06-01

The optoelectronic properties of maskless inductively coupled plasma (ICP) generated black silicon through SF6 and O2 are analyzed by using reflection measurements, scanning electron microscopy (SEM) and quasi steady state photoconductivity (QSSPC). The results are discussed and compared to capacitively coupled plasma (CCP) and industrial standard wet chemical textures. The ICP process forms parabolic like surface structures in a scale of 500 nm. This surface structure reduces the average hemispherical reflection between 300 and 1120 nm up to 8%. Additionally, the ICP texture shows a weak increase of the hemispherical reflection under tilted angles of incidence up to 60°. Furthermore, we report that the ICP process is independent of the crystal orientation and the surface roughness. This allows the texturing of monocrystalline, multicrystalline and kerf-less wafers using the same parameter set. The ICP generation of black silicon does not apply a self-bias on the silicon sample. Therefore, the silicon sample is exposed to a reduced ion bombardment, which reduces the plasma induced surface damage. This leads to an enhancement of the effective charge carrier lifetime up to 2.5 ms at 1015 cm-3 minority carrier density (MCD) after an atomic layer deposition (ALD) with Al2O3. Since excellent etch results were obtained already after 4 min process time, we conclude that the ICP generation of black silicon is a promising technique to substitute the industrial state of the art wet chemical textures in the solar cell mass production.
Aerosol detection efficiency in inductively coupled plasma mass spectrometry

DOE PAGES

Hubbard, Joshua A.; Zigmond, Joseph A.

2016-03-02

We used an electrostatic size classification technique to segregate particles of known composition prior to being injected into an inductively coupled plasma mass spectrometer (ICP-MS). Moreover, we counted size-segregated particles with a condensation nuclei counter as well as sampled with an ICP-MS. By injecting particles of known size, composition, and aerosol concentration into the ICP-MS, efficiencies of the order of magnitude aerosol detection were calculated, and the particle size dependencies for volatile and refractory species were quantified. Similar to laser ablation ICP-MS, aerosol detection efficiency was defined as the rate at which atoms were detected in the ICP-MS normalized bymore » the rate at which atoms were injected in the form of particles. This method adds valuable insight into the development of technologies like laser ablation ICP-MS where aerosol particles (of relatively unknown size and gas concentration) are generated during ablation and then transported into the plasma of an ICP-MS. In this study, we characterized aerosol detection efficiencies of volatile species gold and silver along with refractory species aluminum oxide, cerium oxide, and yttrium oxide. Aerosols were generated with electrical mobility diameters ranging from 100 to 1000 nm. In general, it was observed that refractory species had lower aerosol detection efficiencies than volatile species, and there were strong dependencies on particle size and plasma torch residence time. Volatile species showed a distinct transition point at which aerosol detection efficiency began decreasing with increasing particle size. This critical diameter indicated the largest particle size for which complete particle detection should be expected and agreed with theories published in other works. Aerosol detection efficiencies also displayed power law dependencies on particle size. Aerosol detection efficiencies ranged from 10 -5 to 10 -11. Free molecular heat and mass transfer theory was applied, but evaporative phenomena were not sufficient to explain the dependence of aerosol detection on particle diameter. Additional work is needed to correlate experimental data with theory for metal-oxides where thermodynamic property data are sparse relative to pure elements. Finally, when matrix effects and the diffusion of ions inside the plasma were considered, mass loading was concluded to have had an effect on the dependence of detection efficiency on particle diameter.« less
Mechanisms and Permanence of Sequestered Pb and As in Soils: Impact on Human Bioavailability

DTIC Science & Technology

2016-12-01

Human health risk assessment ICP-MS Inductively coupled plasma - mass spectrometry ICP-OES Inductively coupled plasma – optical emission spectrometry...the most common contaminants of concern exceeding risk criteria because soil ingestion is the primary human health risk driver at many DoD sites...development activities must address to realize the use of bioavailability in human health risk assessment (HHRA). Our proposal addressed three of the
Comparative study of atomic fluorescence spectroscopy and inductively coupled plasma mass spectrometry for mercury and arsenic multispeciation.

PubMed

Gómez-Ariza, José Luis; Lorenzo, Fernando; García-Barrera, Tamara

2005-05-01

Mercury and arsenic are two elements of undoubted importance owing to their toxic character. Although speciation of these elements has been developed separately, in this work for the first time the speciation of As and Hg using two atomic fluorescence detectors in a sequential ensemble is presented. A coupling based on the combination of high-performance liquid chromatography (where mercury and arsenic species are separated) and two atomic fluorescence detectors in series, with several online treatments, including photooxidation (UV) and hydride generation, has allowed the determination of mercury and arsenic compounds simultaneously. The detection limits for this device were 16, 3, 17, 12 and 8 ng mL(-1) for As(III), monomethylarsinic acid, As(V), Hg2+ and methylmercury, respectively. This coupling was compared with an analogous one based on inductively coupled plasma-mass spectrometry (ICP-MS) detection, with detection limits of 0.7, 0.5, 0.8, 0.9 and 1.1 ng mL(-1), respectively. Multispeciation based on ICP-MS exhibits better sensitivity than the coupling based on tandem atomic fluorescence, but this second device is a very robust system and exhibits obvious advantages related to the low cost of acquisition and maintenance, as well as easy handling, which makes it a suitable system for routine laboratories.
Intracranial pressure increases during weightlessness: A parabolic flights study

NASA Astrophysics Data System (ADS)

Denise, P.; Normand, H.; Buzer, L.; Duretete, A.; Avan, P.

2005-08-01

The fluid shift induced by weightlessness likely induces an elevated intracranial pressure (ICP). This factor may contribute to space adaptation syndrome (SAS). Recently, it has been shown that ICP can be monitored every few seconds non invasively by otoacoustic emissions (OAE). The OAE of 6 subjects were measured along the course of parabolic flights aboard the zero-gravity A300 Airbus. Built-in noise rejection and signal processing techniques enabled valid OAE signals to be collected and analyzed online in 4 of 6 subjects. On average, the phase of 1 kHz- OAE rotated by -41° from 1 to 1.8 g, and by +78.7° at 0 g relative to 1 g. From reference invasive ICP measurements in a control group of neurosurgery patients, it is possible to infer that ICP increased by about 34 mmHg in transient weightlessness.
Provenance establishment of coffee using solution ICP-MS and ICP-AES.

PubMed

Valentin, Jenna L; Watling, R John

2013-11-01

Statistical interpretation of the concentrations of 59 elements, determined using solution based inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma emission spectroscopy (ICP-AES), was used to establish the provenance of coffee samples from 15 countries across five continents. Data confirmed that the harvest year, degree of ripeness and whether the coffees were green or roasted had little effect on the elemental composition of the coffees. The application of linear discriminant analysis and principal component analysis of the elemental concentrations permitted up to 96.9% correct classification of the coffee samples according to their continent of origin. When samples from each continent were considered separately, up to 100% correct classification of coffee samples into their countries, and plantations of origin was achieved. This research demonstrates the potential of using elemental composition, in combination with statistical classification methods, for accurate provenance establishment of coffee. Copyright © 2013 Elsevier Ltd. All rights reserved.
Hydrothermal synthesis of 4ZnO·B2O3·H2O:Ln3 + (Ln = Eu, Tb) phosphors: Morphology-tunable and luminescence properties

NASA Astrophysics Data System (ADS)

Cao, Shiwei; Jiao, Yang; Han, Weifang; Ge, Chunhua; Song, Bo; Wang, Jie; Zhang, Xiangdong

2018-02-01

4ZnO·B2O3·H2O:Ln3 + (Ln = Eu, Tb) phosphors with different morphologies have been successfully synthesized via one-step hydrothermal method through regulating the molar amount of Eu3 + and Tb3 +. Comprehensive scanning electron microscopy (SEM), X-ray diffraction (XRD) Fourier transform infrared spectrum (FT-IR) and inductively coupled plasma atomic emission spectrometer (ICP-AES) characterizations all confirm that obtained products are 4ZnO·B2O3·H2O:Ln3 + (Ln = Eu, Tb). The experimental results displayed that the morphology and photoluminescence of compounds is regularly changed with increased the molar amount of rare earth ions. For the Eu3 +-doped, Tb3 +-doped and Eu3 +/Tb3 + co-doped 4ZnO·B2O3·H2O phosphors of morphologies, the rod-like structures gradually changed to flower-like structures, fine wire-like structure and hybrid structure, respectively. To their photoluminescence, the Eu3 + shows a red emission (615 nm); the Tb3 + shows a green emission (545 nm); for the Eu3 +/Tb3 + co-doped 4ZnO·B2O3·H2O phosphors, a combination of blue (5d-4f of Eu2 +), green (5D4-7F5 of Tb3 +) and red (5D0-7F2 of Eu3 +) emissions emerges to achieve white emission. In addition, the energy transfer among Eu3 +, Eu2 + and Tb3 + ions was also discussed.
Method of low tantalum amounts determination in niobium and its compounds by ICP-OES technique.

PubMed

Smolik, Marek; Turkowska, Magdalena

2013-10-15

A method of determination of low amounts of tantalum in niobium and niobium compounds without its prior separation by means of inductively coupled plasma optical emission spectrometry (ICP-OES) has been worked out. The method involves dissolution of the analyzed samples of niobium as well as its various compounds (oxides, fluorides, chlorides, niobates(V)) in fluoride environments, precipitation of sparingly soluble niobic(tantalic) acid (Nb2O5(Ta2O5) · xH2O), converting them into soluble complex compounds by means of oxalic acid with addition of hydrogen peroxide and finally analyzing directly obtained solutions by ICP-OES. This method permits determination of Ta in niobium at the level of 10(-3)% with relatively good precision (≤ 8% RSD) and accuracy (recovery factor: 0.9-1.1). Relative differences in the results obtained by two independent methods (ICP-OES and ICP-MS) do not exceed 14%, and other elements present in niobium compounds (Ti, W, Zr, Hf, V, Mo, Fe, Cr) at the level of 10(-2)% do not affect determination. © 2013 Elsevier B.V. All rights reserved.
Mn-oxidizing Bacteria in Oak Ridge, TN and the Potential for Mercury Remediation

NASA Astrophysics Data System (ADS)

Wright, K. L.; McNeal, K. S.; Han, F. X.

2012-12-01

East Fork Poplar Creek (EFPC) in Oak Ridge, TN was highly contaminated with elemental mercury in the 1950 and 1960. The area is still experiencing the effects of mercury contamination, and researchers are searching for ways to remediate the EFPC. One possible mechanism for bioremediation is the use of biogenic Mn oxides to remove heavy metals from water systems. Six native Pseudomonas bacteria species were isolated from the EFPC in order to examine biogenic Mn oxides production and bioremediation of Oak Ridge slurries. To investigate the biochemical interactions of Pseudomonas and the native microbial communities with Hg, Mn, Fe, S, six different slurry treatment groups were compared using inductively coupled plasma-atomic emission spectrometry (ICP-AES) and cold vapor atomic absorption spectrometry (CVAAS). Oak Ridge slurries were autoclaved to inhibit microbial growth (group 1), autoclaved and amended with HgS (group 2), autoclaved and amended with Pseudomonas isolates and additional HgS (group 3), untreated slurry (group 4), normal slurry amended with HgS (group 5), and normal slurry amended with Pseudomonas isolates and additional HgS (group 6). The comparison of the autoclaved groups with the counterpart untreated and normal Oak Ridge slurries highlighted important microbial interactions. Also, the Pseudomonas isolates were grown separately in a MnSO4 media, and the individual bacteria were monitored for Mn-oxidization using ICP-AES and transmission electron microscopy (TEM). In the slurry sediments, the Pseudomonas isolates did produce Mn oxides which bound to mercury, and mercury bound to organic matter significantly decreased. However, after a significant decrease of dissolved mercury in the water, dissolved mercury was cycled back into the water system on day 10 of the study. Additionally, two individual native Oak Ridge Pseudomonas isolates demonstrated Mn-oxidization. Biogenic Mn oxides have the potential to decrease mercury cycling, however there is need for more in depth and long-term studies to confirm their sustained use as Hg bioremediators.
Noninvasive Intracranial Pressure Monitoring for Severe Traumatic Brain Injury in Children: A Concise Update on Current Methods.

PubMed

Narayan, Vinayak; Mohammed, Nasser; Savardekar, Amey R; Patra, Devi Prasad; Notarianni, Christina; Nanda, Anil

2018-06-01

Traumatic brain injury (TBI) is a leading cause of pediatric morbidity and mortality worldwide and intracranial pressure (ICP) monitoring plays a crucial role in its management. Based on existing literature, we review the current practicing noninvasive ICP monitoring devices and their accuracy in predicting increased ICP in pediatric TBI. A thorough literature search was conducted on PubMed, Medline, and the Cochrane database, articles were selected systematically and reviewed completely, and relevant data were summarized and discussed. A total of 27 articles pertaining to pediatric TBI were included and reviewed. We found various modalities of noninvasive ICP monitoring devices used over the last few years. The noninvasive modalities so far attempted in pediatric TBI and so reviewed here are transcranial Doppler, optic nerve sheath diameter, otoacoustic emission, near-infrared spectroscopy, contrast-enhanced ultrasonography, and quantitative pupillometry. Invasive monitoring methods are the current gold standard for monitoring ICP; however, complications caused by their invasive nature are of concern. Of all the noninvasive methods based on the literature, we found transcranial Doppler and optic nerve sheath diameter assessment to be the best tools to monitor ICP in pediatric TBI. The promising results and developments of noninvasive ICP monitoring modalities with its ideal features of high sensitivity, diagnostic accuracy, and simple acquisition technique may make it the future of neurointensive monitoring in pediatric TBI. Copyright © 2018 Elsevier Inc. All rights reserved.
Atmospheric lead deposition to Okefenokee Swamp, Georgia, USA

USGS Publications Warehouse

Jackson, B.P.; Winger, P.V.; Lasier, P.J.

2004-01-01

'Capsule:' Coal combustion emissions appear to be a major source of Pb in the Okefenokee wetland. Contamination of the environment from atmospheric deposition during the twentieth century is pervasive even in areas ostensibly considered pristine or remote from point sources. In this study, Pb concentrations in a Pb-210-dated peat core collected from the Okefenokee Swamp, GA were used to assess historical contaminant input via atmospheric deposition. Lead isotope ratios were determined by dynamic reaction cell ICP-MS (DRC-ICP-MS). Increases in Pb concentration occurred in the late nineteenth century and a marked rise in Pb concentrations pre-dated the widespread use of leaded gasoline within the US. The Pb-206/Pb-207 ratios of 1.19 during this period were consistent with coal combustion emissions. A later increase in Pb concentration, concurrent with a trend toward more radiogenic Pb-206/Pb-207 ratios in gasoline is consistent with an increased input of Pb from leaded gasoline emissions. However, it appears that coal combustion emissions remain a major source of Pb to the Okefenokee.
Application of infrared thermography for online monitoring of wall temperatures in inductively coupled plasma torches with conventional and low-flow gas consumption

NASA Astrophysics Data System (ADS)

Engelhard, Carsten; Scheffer, Andy; Maue, Thomas; Hieftje, Gary M.; Buscher, Wolfgang

2007-10-01

Inductively coupled plasma (ICP) sources typically used for trace elemental determination and speciation were investigated with infrared (IR) thermography to obtain spatially resolved torch temperature distributions. Infrared thermographic imaging is an excellent tool for the monitoring of temperatures in a fast and non-destructive way. This paper presents the first application of IR thermography to inductively coupled plasma torches and the possibility to investigate temperatures and thermal patterns while the ICP is operating and despite background emission from the plasma itself. A fast and easy method is presented for the determination of temperature distributions and stress features within ICP torches. Two different ICP operating torches were studied: a commercially available Fassel-type ICP unit with 14 L min - 1 total Ar consumption and a SHIP torch with the unusually low Ar flow of 0.6 L min - 1 . Spatially resolved infrared images of both torches were obtained and laterally resolved temperature profiles were extracted. After temperature-resolved calibration of the emissivity (between 0.5 and 0.35 at 873-1323 K) and transmission (20% between 3.75 and 4.02 μm) of the fused quartz used in the torch construction, an image correction was applied. Inhomogeneous temperature distributions with locally defined stress areas in the conventional Fassel-type torch were revealed. As a general trend, it was found that the SHIP torch exhibited higher temperatures ( Tmax = 1580 K) than the conventional torch ( Tmax = 730 K). In the former case, torch sites with efficient and inefficient cooling were discovered and the external flow of cooling air (24-48 m s - 1 ) was identified as the limiting factor.
Application of isotope-dilution laser ablation ICP-MS for direct determination of Pu concentrations in soils at pg g(-1) levels.

PubMed

Boulyga, Sergei F; Tibi, Markus; Heumann, Klaus G

2004-01-01

The methods available for determination of environmental contamination by plutonium at ultra-trace levels require labor-consuming sample preparation including matrix removal and plutonium extraction in both nuclear spectroscopy and mass spectrometry. In this work, laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for direct analysis of Pu in soil and sediment samples. Application of a LINA-Spark-Atomizer system (a modified laser ablation system providing high ablation rates) coupled with a sector-field ICP-MS resulted in detection limits as low as 3x10(-13) g g(-1) for Pu isotopes in soil samples containing uranium at a concentration of a few microg g(-1). The isotope dilution (ID) technique was used for quantification, which compensated for matrix effects in LA-ICP-MS. Interferences by UH+ and PbO2+ ions and by the peak tail of 238U+ ions were reduced or separated by use of dry plasma conditions and a mass resolution of 4000, respectively. No other effects affecting measurement accuracy, except sample inhomogeneity, were revealed. Comparison of results obtained for three contaminated soil samples by use of alpha-spectrometry, ICP-MS with sample decomposition, and LA-ICP-IDMS showed, in general, satisfactory agreement of the different methods. The specific activity of (239+240)Pu (9.8 +/- 3.0 mBq g(-1)) calculated from LA-ICP-IDMS analysis of SRM NIST 4357 coincided well with the certified value of 10.4 +/- 0.2 mBq g(-1). However, the precision of LA-ICP-MS for determination of plutonium in inhomogeneous samples, i.e. if "hot" particles are present, is limited. As far as we are aware this paper reports the lowest detection limits and element concentrations yet measured in direct LA-ICP-MS analysis of environmental samples.
Gas-phase reactions of carbon dioxide with atomic transition-metal and main-group cations: room-temperature kinetics and periodicities in reactivity.

PubMed

Koyanagi, Gregory K; Bohme, Diethard K

2006-02-02

The chemistry of carbon dioxide has been surveyed systematically with 46 atomic cations at room temperature using an inductively-coupled plasma/selected-ion flow tube (ICP/SIFT) tandem mass spectrometer. The atomic cations were produced at ca. 5500 K in an ICP source and allowed to cool radiatively and to thermalize by collisions with Ar and He atoms prior to reaction downstream in a flow tube in helium buffer gas at 0.35 +/- 0.01 Torr and 295 +/- 2 K. Rate coefficients and products were measured for the reactions of first-row atomic ions from K(+) to Se(+), of second-row atomic ions from Rb(+) to Te(+) (excluding Tc(+)), and of third-row atomic ions from Cs(+) to Bi(+). CO(2) was found to react in a bimolecular fashion by O atom transfer only with 9 early transition-metal cations: the group 3 cations Sc(+), Y(+), and La(+), the group 4 cations Ti(+), Zr(+), and Hf(+), the group 5 cations Nb(+) and Ta(+), and the group 6 cation W(+). Electron spin conservation was observed to control the kinetics of O atom transfer. Addition of CO(2) was observed for the remaining 37 cations. While the rate of addition was not measurable some insight was obtained into the standard free energy change, DeltaG(o), for CO(2) ligation from equilibrium constant measurements. A periodic variation in DeltaG(o) was observed for first row cations that is consistent with previous calculations of bond energies D(0)(M(+)-CO(2)). The observed trends in D(0) and DeltaG(o) are expected from the variation in electrostatic attraction between M(+) and CO(2) which follows the trend in atomic-ion size and the trend in repulsion between the orbitals of the atomic cations and the occupied orbitals of CO(2). Higher-order CO(2) cluster ions with up to four CO(2) ligands also were observed for 24 of the atomic cations while MO(2)(+) dioxide formation by sequential O atom transfer was seen only with Hf(+), Nb(+), Ta(+), and W(+).
DOE Office of Scientific and Technical Information (OSTI.GOV)

Mourey, Odile; Petit-Etienne, Camille; Cunge, Gilles, E-mail: gilles.cunge@cea.fr

Pulsed plasmas are promising candidates to go beyond limitations of continuous waves' plasma. However, their interaction with surfaces remains poorly understood. The authors investigated the silicon etching mechanism in inductively coupled plasma (ICP) Cl{sub 2} operated either in an ICP-pulsed mode or in a bias-pulsed mode (in which only the bias power is pulsed). The authors observed systematically the development of an important surface roughness at a low duty cycle. By using plasma diagnostics, they show that the roughness is correlated to an anomalously large (Cl atoms flux)/(energetic ion flux) ratio in the pulsed mode. The rational is that themore » Cl atom flux is not modulated on the timescale of the plasma pulses although the ion fluxes and energy are modulated. As a result, a very strong surface chlorination occurs during the OFF period when the surface is not exposed to energetic ions. Therefore, each energetic ion in the ON period will bombard a heavily chlorinated silicon surface, leading to anomalously high etching yield. In the ICP pulsed mode (in which the ion energy is high), the authors report yields as high as 40, which mean that each individual ion impacts will generate a “crater” of about 2 nm depth at the surface. Since the ion flux is very small in the pulsed ICP mode, this process is stochastic and is responsible for the roughness initiation. The roughness expansion can then be attributed partly to the ion channeling effect and is probably enhanced by the formation of a SiClx reactive layer with nonhomogeneous thickness over the topography of the surface. This phenomenon could be a serious limitation of pulsed plasma processes.« less

Geochemistry of environmentally sensitive trace elements in Permian coals from the Huainan coalfield, Anhui, China

USGS Publications Warehouse

Chen, J.; Liu, Gaisheng; Jiang, M.; Chou, C.-L.; Li, H.; Wu, B.; Zheng, Lingyun; Jiang, D.

2011-01-01

To study the geochemical characteristics of 11 environmentally sensitive trace elements in the coals of the Permian Period from the Huainan coalfield, Anhui province, China, borehole samples of 336 coals, two partings, and four roof and floor mudstones were collected from mineable coal seams. Major elements and selected trace elements were determined by inductively coupled plasma optical emission spectrometry (ICP-OES), inductively coupled plasma mass spectrometry (ICP-MS), and hydride generation atomic absorption spectrometry (HAAS). The depositional environment, abundances, distribution, and modes of occurrence of trace elements were investigated. Results show that clay and carbonate minerals are the principal inorganic constituents in the coals. A lower deltaic plain, where fluvial channel systems developed successively, was the likely depositional environment of the Permian coals in the Huainan coalfield. All major elements have wider variation ranges than those of Chinese coals except for Mg and Fe. The contents of Cr, Co, Ni, and Se are higher than their averages for Chinese coals and world coals. Vertical variations of trace elements in different formations are not significant except for B and Ba. Certain roof and partings are distinctly higher in trace elements than underlying coal bench samples. The modes of occurrence of trace elements vary in different coal seams as a result of different coal-forming environments. Vanadium, Cr, and Th are associated with aluminosilicate minerals, Ba with carbonate minerals, and Cu, Zn, As, Se, and Pb mainly with sulfide minerals. ?? 2011 Elsevier B.V.
Characterization of edible seaweed harvested on the Galician coast (northwestern Spain) using pattern recognition techniques and major and trace element data.

PubMed

Romarís-Hortas, Vanessa; García-Sartal, Cristina; Barciela-Alonso, María Carmen; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Pilar

2010-02-10

Major and trace elements in North Atlantic seaweed originating from Galicia (northwestern Spain) were determined by using inductively coupled plasma-optical emission spectrometry (ICP-OES) (Ba, Ca, Cu, K, Mg, Mn, Na, Sr, and Zn), inductively coupled plasma-mass spectrometry (ICP-MS) (Br and I) and hydride generation-atomic fluorescence spectrometry (HG-AFS) (As). Pattern recognition techniques were then used to classify the edible seaweed according to their type (red, brown, and green seaweed) and also their variety (Wakame, Fucus, Sea Spaghetti, Kombu, Dulse, Nori, and Sea Lettuce). Principal component analysis (PCA) and cluster analysis (CA) were used as exploratory techniques, and linear discriminant analysis (LDA) and soft independent modeling of class analogy (SIMCA) were used as classification procedures. In total, t12 elements were determined in a range of 35 edible seaweed samples (20 brown seaweed, 10 red seaweed, 4 green seaweed, and 1 canned seaweed). Natural groupings of the samples (brown, red, and green types) were observed using PCA and CA (squared Euclidean distance between objects and Ward method as clustering procedure). The application of LDA gave correct assignation percentages of 100% for brown, red, and green types at a significance level of 5%. However, a satisfactory classification (recognition and prediction) using SIMCA was obtained only for red seaweed (100% of cases correctly classified), whereas percentages of 89 and 80% were obtained for brown seaweed for recognition (training set) and prediction (testing set), respectively.
Inter-laboratory validation of an inexpensive streamlined method to measure inorganic arsenic in rice grain.

PubMed

Chaney, Rufus L; Green, Carrie E; Lehotay, Steven J

2018-05-04

With the establishment by CODEX of a 200 ng/g limit of inorganic arsenic (iAs) in polished rice grain, more analyses of iAs will be necessary to ensure compliance in regulatory and trade applications, to assess quality control in commercial rice production, and to conduct research involving iAs in rice crops. Although analytical methods using high-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) have been demonstrated for full speciation of As, this expensive and time-consuming approach is excessive when regulations are based only on iAs. We report a streamlined sample preparation and analysis of iAs in powdered rice based on heated extraction with 0.28 M HNO 3 followed by hydride generation (HG) under control of acidity and other simple conditions. Analysis of iAs is then conducted using flow-injection HG and inexpensive ICP-atomic emission spectroscopy (AES) or other detection means. A key innovation compared with previous methods was to increase the acidity of the reagent solution with 4 M HCl (prior to reduction of As 5+ to As 3+ ), which minimized interferences from dimethylarsinic acid. An inter-laboratory method validation was conducted among 12 laboratories worldwide in the analysis of six shared blind duplicates and a NIST Standard Reference Material involving different types of rice and iAs levels. Also, four laboratories used the standard HPLC-ICP-MS method to analyze the samples. The results between the methods were not significantly different, and the Horwitz ratio averaged 0.52 for the new method, which meets official method validation criteria. Thus, the simpler, more versatile, and less expensive method may be used by laboratories for several purposes to accurately determine iAs in rice grain. Graphical abstract Comparison of iAs results from new and FDA methods.
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.
Comparison method for uranium determination in ore sample by inductively coupled plasma optical emission spectrometry (ICP-OES).

PubMed

Sert, Şenol

2013-07-01

A comparison method for the determination (without sample pre-concentration) of uranium in ore by inductively coupled plasma optical emission spectrometry (ICP-OES) has been performed. The experiments were conducted using three procedures: matrix matching, plasma optimization, and internal standardization for three emission lines of uranium. Three wavelengths of Sm were tested as internal standard for the internal standardization method. The robust conditions were evaluated using applied radiofrequency power, nebulizer argon gas flow rate, and sample uptake flow rate by considering the intensity ratio of the Mg(II) 280.270 nm and Mg(I) 285.213 nm lines. Analytical characterization of method was assessed by limit of detection and relative standard deviation values. The certificated reference soil sample IAEA S-8 was analyzed, and the uranium determination at 367.007 nm with internal standardization using Sm at 359.260 nm has been shown to improve accuracy compared with other methods. The developed method was used for real uranium ore sample analysis.
Trace element determination using static high-sensitivity inductively coupled plasma optical emission spectrometry (SHIP-OES).

PubMed

Engelhard, Carsten; Scheffer, Andy; Nowak, Sascha; Vielhaber, Torsten; Buscher, Wolfgang

2007-02-05

A low-flow air-cooled inductively coupled plasma (ICP) design for optical emission spectrometry (OES) with axial plasma viewing is described and an evaluation of its analytical capabilities in trace element determinations is presented. Main advantage is a total argon consumption of 0.6 L min(-1) in contrast to 15 L min(-1) using conventional ICP sources. The torch was evaluated in trace element determinations and studied in direct comparison with a conventional torch under the same conditions with the same OES system, ultrasonic nebulization (USN) and single-element optimization. A variety of parameters (x-y-position of the torch, rf power, external air cooling, gas flow rates and USN operation parameters) was optimized to achieve limits of detection (LOD) which are competitive to those of a conventional plasma source. Ionic to atomic line intensity ratios for magnesium were studied at different radio frequency (rf) power conditions and different sample carrier gas flows to characterize the robustness of the excitation source. A linear dynamic range of three to five orders of magnitude was determined under compromise conditions in multi-element mode. The accuracy of the system was investigated by the determination of Co, Cr, Mn, Zn in two certified reference materials (CRM): CRM 075c (Copper with added impurities), and CRM 281 (Trace elements in rye grass). With standard addition values of 2.44+/-0.04 and 3.19+/-0.21 microg g(-1) for Co and Mn in the CRM 075c and 2.32+/-0.09, 81.8+/-0.4, 32.2+/-3.9 for Cr, Mn and Zn, respectively, were determined in the samples and found to be in good agreement with the reported values; recovery rates in the 98-108% range were obtained. No influence on the analysis by the matrix load in the sample was observed.
Titanium (III) cation selective electrode based on synthesized tris(2pyridyl) methylamine ionophore and its application in water samples

NASA Astrophysics Data System (ADS)

Rezayi, Majid; Karazhian, Reza; Abdollahi, Yadollah; Narimani, Leila; Sany, Seyedeh Belin Tavakoly; Ahmadzadeh, Saeid; Alias, Yatimah

2014-04-01

The introduction of low detection limit ion selective electrodes (ISEs) may well pave the way for the determination of trace targets of cationic compounds. This research focuses on the detection of titanium (III) cation using a new PVC-membrane sensor based on synthesized tris(2pyridyl) methylamine (tpm) ionophore. The application and validation of the proposed sensor was done using potentiometric titration, inductively coupled plasma atomic emission spectrometry (ICP-AES), and atomic absorption spectrometry (AAS). The membrane sensor exhibited a Nernstian response to the titanium (III) cation over a concentration range of 1.0 × 10-6-1.0 × 10-2 M and pH range from 1-2.5. The Nernstian slope, the lower of detection (LOD), and the response time (t95%) of the proposed sensor were 29.17 +/- 0.24 mV/dec, 7.9 × 10-7 M, and 20 s, respectively. The direct determination of 4-39 μg/ml of titanium (III) standard solution showed an average recovery of 94.60 and a mean relative standard deviation of 1.8 at 100.0 μg/ml. Finally, the utilization of the electrodes as end-point indicators for potentiometric titration with EDTA solutions for titanium (III) sensor was successfully carried out.
Influence of natural organic matter on the adsorption of metal ion onto clay particles

USGS Publications Warehouse

Schmitt, D.; Taylor, Howard E.; Aiken, G.R.; Roth, D.A.; Frimmel, F.H.

2002-01-01

The influence of natural organic matter (NOM) on the adsorption of Al, Fe, Zn, and Pb onto clay minerals was investigated. Adsorption experiments were carried out at pH = 5 and pH = 7 in the presence and absence of NOM. In general, the presence of NOM decreased the adsorption of metal ions onto the clay particles. Al and Fe were strongly influenced by NOM, whereas Zn and Pb adsorption was only slightly altered. The interaction of the metal ions with the minerals and the influence of NOM on this interaction was investigated by coupling SdFFF with an inductively coupled plasma mass spectrometer (ICPMS) or an inductively coupled plasma atomic emission spectrometer (ICPAES). Quantitative atomization of the clay particles in the ICP was confirmed by comparing elemental content determined by direct injection of the clay into the ICPMS with values from acid digestion. Particle sizes of the clays were found to be between 0.1 and 1 μm by sedimentation field-flow fractionation (SdFFF) with UV detection. Aggregation of particles due to metal adsorption was observed using SdFFF-ICPMS measurements. This aggregation was dependent on the specific metal ion and decreased in the presence of NOM and at higher pH value.
Wheat flour confectionery products as a source of inorganic nutrients: zinc and copper contents in hard biscuits.

PubMed

Sebecić, Blazenka; Vedrina-Dragojević, Irena

2004-04-01

Cereal-based confectionery products being consumed through whole human life are considered mainly to be a source of carbohydrates, that is energy, although cereals are a rich source of minerals as well. To evaluate some hard biscuits produced in Croatia as a source of different trace elements in nutrition, in this study Zn and Cu contents were determined in classic wheat flour biscuits and in dietetic biscuits enriched with whole wheat grain flour or whole wheat grain grits, soya flour and skimmed milk. Zn was determined by flame atomic absorption spectrometry (AAS); Cu was determined by inductively coupled plasma atomic emission spectroscopy (ICP-AES). The results show that the Zn content in different kinds of biscuits ranges from 5.89 up to 17.64 mg/kg and the Cu content ranges from 1.15 up to 2.79 mg/kg depending on the type of wheat milling products and mineral content of other ingredients used. Enriched dietetic biscuits produced from wheat flour type 850 and whole wheat grain flour and/or soya flour and skimmed milk were almost 200% and 150% higher in Zn and Cu, respectively, in comparison to classic white wheat flour biscuits and can be considered as good sources of Zn and Cu in nutrition.
Several methods to determine heavy metals in the human brain

NASA Astrophysics Data System (ADS)

Andrási, Erzsébet; Igaz, Sarolta; Szoboszlai, Norbert; Farkas, Éva; Ajtony, Zsolt

1999-05-01

The determination of naturally occurring heavy metals in various parts of the human brain is discussed. The patients had no diseases in their central nervous systems (five individuals, mean age 70 years). Twenty brain parts were selected from both hemispheres. The analysis was carried out by graphite furnace atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry and instrumental neutron activation analysis methods. Accuracy and precision of the applied techniques were tested by using standard reference materials. Two digestion methods were used to dissolve the brain samples for ICP-AES and GF-AAS. One was performed in a Parr-bomb and the second in a microwave oven. The present results show a non-homogeneous distribution of the essential elements (Cu, Fe, Mn, Zn) in normal human brain. Corresponding regions in both hemispheres showed an almost identical concentration of these elements. In the case of toxic elements (Pb, Cd) an average value in different brain regions can not be established because of the high variability of individual data. This study indicates that beside differences in Pb and Cd intake with foods or cigarette smoke inhalation, the main factors of the high inter-individual variability of these element concentrations in human brain parts may be a marked difference in individual elimination or accumulation capabilities.
Polonium (²¹⁰Po), uranium (²³⁴U, ²³⁸U) isotopes and trace metals in mosses from Sobieszewo Island, northern Poland.

PubMed

Boryło, Alicja; Nowicki, Waldemar; Olszewski, Grzegorz; Skwarzec, Bogdan

2012-01-01

The activity of polonium (210)Po and uranium (234)U, (238)U radionuclides, as well as trace metals in mosses, collected from Sobieszewo Island area (northern Poland), were determined using the alpha spectrometry, AAS (atomic absorption spectrometry) and OES-ICP (atomic emission spectrometry with inductively coupled plasma). The concentrations of mercury (directly from the solid sample) were determined by the cold vapor technique of CV AAS. The obtained results revealed that the concentrations of (210)Po, (234)U, and (238)U in the two analyzed kinds of mosses: schrebers big red stem moss (Pleurozium schreberi) and broom moss (Dicranum scoparium) were similar. The higher polonium concentrations were found in broom moss (Dicranum scoparium), but uranium concentrations were relatively low for both species of analyzed mosses. Among the analyzed trace metals the highest concentration in mosses was recorded for iron, while the lowest for nickel, cadmium and mercury. The obtained studies showed that the sources of polonium and uranium isotopes, as well as trace metals in analyzed mosses are air city contaminations transported from Gdańsk and from existing in the vicinity the phosphogypsum waste heap in Wiślinka (near Gdańsk).
Evaluation of calcium alginate beads for Ce, La and Nd preconcentration from groundwater prior to ICP OES analysis.

PubMed

Arantes de Carvalho, Gabriel G; Kondaveeti, Stalin; Petri, Denise F S; Fioroto, Alexandre M; Albuquerque, Luiza G R; Oliveira, Pedro V

2016-12-01

Analytical methods for the determination of rare earth elements (REE) in natural waters by plasma spectrochemical techniques often require sample preparation procedures for analytes preconcentration as well as for removing matrix constituents, that may interfere on the analytical measurements. In the present work, calcium alginate (CA) beads were used for the first time aiming at Ce, La and Nd preconcentration from groundwater samples for further determination by inductively coupled plasma optical emission spectrometry (ICP OES). Test samples were analyzed in batch mode by transferring a 40mL test portion (pH=5±0.2) into a 50mL polyethylene flask containing 125mg CA beads. After 15min contact, the analytes were quantitatively extracted from the loaded CA beads with 2.0mL of 1.0molL -1 HCl solution for further determination by ICP OES, using Ce (II) 456.236, La (II) 379.478 and Nd (II) 430.358nm emission lines. The proposed approach is a reliable alternative for REE single-stage preconcentration from aqueous samples, as it provided accurate results based on the addition and recovery analysis of groundwater. The results obtained by the proposed method were also compared with those from reference method based on inductively coupled plasma mass spectrometry (ICP-MS) and no significant differences were observed after applying the Student's t-test at 95% confidence level. Copyright © 2016 Elsevier B.V. All rights reserved.
Preliminary magnetotelluric results across Dalma Volcanics, Eastern India: Inferences on metallogeny

NASA Astrophysics Data System (ADS)

Maurya, Ved P.; Shalivahan; Bhattacharya, B. B.; Adhikari, P. K.; Das, L. K.

2015-04-01

The regional magnetotelluric (MT) survey across Dalma Volcanics (DVs) in North Singhbhum Mobile Belt (NSMB) was carried out to obtain the conductivity model and to understand the metallogeny. The structure in general is 2-D and the average strike is N60°W. 2-D inversions using TE + TM and TE + TM + Tzy were carried out. Both inversions derived models with similar features but with modified shape. The TE + TM + Tzy inversion brings up two conducting zones enveloping three anomalous conducting bodies. Inductively coupled plasma atomic emission spectroscopy (ICP-AES) analysis of the samples collected from 8 to 10 m pit from different stratigraphic units of Dalma volcano-sedimentary belt indicates the presence of gold, silver, uranium and copper. The study area is a felsic dominated rifted margin and shows high conductivity contrast along with high gravity, magnetic and significant radiometric anomaly. Thus, the conducting zones indicate the presence of volcanogenic massive sulfide (VMS) or volcano hosted gold deposit (Au-VMS) in NSMB.
Syntheses, structures and properties of three new two-dimensional Cu(I)-Ln(III) heterometallic coordination polymers based on 2,2'-dipyridyl-5,5'-dicarboxylate ligands.

PubMed

Zhao, Junwei; Cheng, Yamin; Shang, Sensen; Zhang, Fang; Chen, Li; Chen, Lijuan

2013-12-01

Three new two-dimensional Cu(I)-Ln(III) heterometallic coordination polymers [Ln(III)Cu2(I)(Hbpdc)4] · Cl · xH2O [Ln(III) = La(III), x = 8 (1); Ln(III) = Pr(III), x=9 (2); Ln(III) = Eu(III), x = 8 (3)] (H2bpdc = 2,2'-bipyridyl-5,5'-dicarboxylic acid) have been prepared under hydrothermal conditions and structurally characterized by elemental analyses, inductively coupled plasma atomic emission spectrometry (ICP-AES) analyses, IR spectra, X-ray photoelectron spectroscopy (XPS) and single-crystal X-ray diffraction. X-ray diffraction indicates that the isomorphic 1-3 display the two-dimensional sheet structure constructed from [Cu(I)(Hbpdc)2](-) fragments through Ln(3+) connectors. Moreover, the solid-state photoluminescence measurements of 3 indicate that the Eu(III) ions, Hbpdc(-) ligands and Cu(I) cations make contributions to its luminescent properties simultaneously. Copyright © 2013 Elsevier B.V. All rights reserved.
Gold and gold-iron oxide magnetic glyconanoparticles: synthesis, characterization and magnetic properties.

PubMed

de la Fuente, Jesús M; Alcántara, David; Eaton, Peter; Crespo, Patricia; Rojas, Teresa C; Fernandez, Asunción; Hernando, Antonio; Penadés, Soledad

2006-07-06

The preparation, characterization and the magnetic properties of gold and gold-iron oxide glyconanoparticles (GNPs) are described. Glyconanoparticles were prepared in a single step procedure in the presence of aqueous solution of thiol functionalized neoglycoconjugates and either gold salts or both gold and iron salts. Neoglycoconjugates of lactose and maltose disaccharides with different linkers were used. Iron-free gold or gold-iron oxide GNPs with controlled gold-iron ratios were obtained. The average core-size diameters are in the range of 1.5-2.5 nm. The GNPs are fully characterized by (1)H NMR spectrometry, transmission electron microscopy (TEM), and UV-vis and X-ray absorption (XAS) spectroscopies. Inductive plasma-atomic emission spectrometry (ICP) and elemental analysis gave the average number of neoglycoconjugates per cluster. The magnetic properties were measured in a SQUID magnetometer. The most remarkable results was the observation of a permanent magnetism up to room temperature in the iron-free gold GNPs, that was not present in the corresponding gold-iron oxide GNPs.
Quantitative analysis of gallstones using laser-induced breakdown spectroscopy

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

Singh, Vivek K.; Singh, Vinita; Rai, Awadhesh K.

2008-11-01

The utility of laser-induced breakdown spectroscopy (LIBS) for categorizing different types of gallbladder stone has been demonstrated by analyzing their major and minor constituents. LIBS spectra of three types of gallstone have been recorded in the 200-900 nm spectral region. Calcium is found to be the major element in all types of gallbladder stone. The spectrophotometric method has been used to classify the stones. A calibration-free LIBS method has been used for the quantitative analysis of metal elements, and the results have been compared with those obtained from inductively coupled plasma atomic emission spectroscopy (ICP-AES) measurements. The single-shot LIBS spectramore » from different points on the cross section (in steps of 0.5 mm from one end to the other) of gallstones have also been recorded to study the variation of constituents from the center to the surface. The presence of different metal elements and their possible role in gallstone formation is discussed.« less
Chemical Analysis of Suspected Unrecorded Alcoholic Beverages from the States of São Paulo and Minas Gerais, Brazil

PubMed Central

Soares Neto, Julino Assunção Rodrigues

2015-01-01

Our study analyzed 152 samples of alcoholic beverages collected from the states of São Paulo and Minas Gerais, Brazil, using gas chromatography with flame ionization detection (GC-FID) and mass spectrometry (GC-MS), Fourier transform infrared spectroscopy (FT-IR), and inductively coupled plasma atomic emission spectrometry (ICP-AES). The methanol content varied from 20 to 180 ppm in 28 samples, and the limit of the accepted level of 200 ppm was exceeded in only one sample. High content of cyanide derivatives and ethyl carbamate, above the accepted level of 150 ppb, was observed in 109 samples. Carbonyl compounds were also observed in 111 samples, showing hydroxy 2-propanone, 4-methyl-4-hepten-3-one, furfural, and 2-hydroxyethylcarbamate as main constituents. Copper was found at concentrations above 5 ppm in 26 samples; the maximum value observed was 28 ppm. This work evaluated the human health risk associated with the poor quality of suspected unrecorded alcohols beverages. PMID:26495155
Heavy Metal Detoxification by Different Bacillus Species Isolated from Solar Salterns

PubMed Central

Syed, Shameer; Chinthala, Paramageetham

2015-01-01

The biosorption mechanism is an alternative for chemical precipitation and ultrafiltration which have been employed to treat heavy metal contamination with a limited success. In the present study, three species of Bacillus which were isolated from solar salterns were screened for their detoxification potential of the heavy metals, lead, chromium, and copper, by biosorption. Biosorption potential of each isolate was determined by Atomic Absorption Spectroscopy (AAS), Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES), and Energy Dispersive Spectroscopy (EDS) as the amount of metal present in the medium after the treatment with the isolates. Bacterial isolates, Bacillus licheniformis NSPA5, Bacillus cereus NSPA8, and Bacillus subtilis NSPA13, showed significant level of lead biosorption with maximum of 87–90% by Bacillus cereus NSPA8. The biosorption of copper and chromium was relatively low in comparison with lead. With the obtained results, we have concluded that the bacterial isolates are potential agents to treat metal contamination in more efficient and ecofriendly manner. PMID:26525498
Characterization of Santa Catarina (Brazil) coal with respect to human health and environmental concerns

USGS Publications Warehouse

Silva, L.F.O.; Oliveira, M.L.S.; Boit, K.M.; Finkelman, R.B.

2009-01-01

The current paper presents the concentration, distribution, and modes of occurrence of trace elements of 13 coals from south Brazil. The samples were collected in the state of Santa Catarina. Chemical analyses and the high ash yields indicate that all studied coals are rich in mineral matter, with SiO2 and Al2O3 dominating as determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). Quartz is the main mineral species and is associated with minor levels of feldspars, kaolinite, hematite, and iron-rich carbonates. The contents of trace elements, including As, Pb, Cd, Ni, Cr, Mn, Be, V, U, Zn, Li, Cu, Tl, and Ni, in coals were determined. A comparison of ranges and means of elemental concentrations in Santa Catarina, Brazil, and world coals shows that the ranges of most elements in Santa Catarina coal are very close to the usual worldwide concentration ranges in coal. ?? Springer Science+Business Media B.V. 2008.
Leaching and toxicity behavior of coal-biomass waste cocombustion ashes.

PubMed

Skodras, G; Prokopidou, M; Sakellaropoulos, G P

2006-08-01

Land disposal of ash residues, obtained from the cocombustion of Greek lignite with biomass wastes, is known to create problems due to the harmful constituents present. In this regard, the leachability of trace elements from lignite, biomass, and blends cocombustion ashes was investigated by using the Toxicity Characteristic Leaching Procedure (TCLP) of the US Environmental Protection Agency (US EPA). In this work, the toxicity of the aqueous leachates and the concentrations of the metals obtained from the leaching procedure were measured using the Microtox test (Vibrio fischeri) and inductive coupled plasma-atomic emission spectrometer (ICP-AES), respectively. The toxic effects of most leachates on Vibrio fischeri were found to be significantly low in both 45% and 82% screening test protocols. However, the liquid sample originating from olive kernels fly ash (FA4) caused the highest toxic effect in both protocols, which can be attributed to its relatively high concentrations of As, Cd, Co, Cu, Mn, Ni, and Zn. Copyright 2006 Wiley Periodicals, Inc.

Mineral contents and proximate composition of Pistacia vera kernels.

PubMed

Harmankaya, Mustafa; Ozcan, Mehmet Musa; Al Juhaimi, Fahad

2014-07-01

The mineral contents of Pistacia vera kernels were determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The minimum and maximum values of K, P, Ca, Mg, and S elements ranged from 6,333 to 8,064 mg/kg, 3,630 to 5,228 mg/kg, 1,614 to 3,226 mg/kg, 1,716 to 2,402 mg/kg, and 1,417 to 1,825 mg/kg, respectively. In addition, the mean values of Fe, Zn, Cu, Mn, B, Mo, Cr and Ni elements were determined as 42.48, 20.52, 12.81, 7.48, 11.31, 0.106, 0.511 and 1.67 mg/kg, respectively. Ash levels of kernels were found between 2.28 % (Urfa) and 2.79 % (Halebi). In addition, crude oil and protein contents were determined between 48.8 % (Halebi) to 55.3 % (Siirt) and 23.33 % (Uzun) to 27.16 % (Halebi), respectively.
Natural fluoride levels in some springs and streams from the late Maastrichtian Ajali formation in Ohafia-Arochukwu area of south eastern Nigeria.

PubMed

Ibe, K K; Adlegbembo, A O; Mafeni, J O; Danfillo, I S

1999-09-01

The aim of this study was to provide baseline data on the fluoride levels in waters associated with the late Maastrichtian Ajali formation in Ohafia-Arochukwu area of South Eastern Nigeria. Water samples from 14 artesian, perched springs and eight streams from the formation were collected with plastic containers. Fluoride analysis was carried out with inductively coupled plasma Atomic Emission Spectrometry (ICP-AES) equipment at the laboratories of the Department of Earth Science, University of Leeds, United Kingdom. The results showed that fluoride occurred in only one of the 14 spring water samples. Fluoride level in the sample was 0.03 ppm. The spring water, which contained some fluoride, was possibly associated with another rock formation: namely, the limestone bearing Nsukka formation, which overlies the Ajali formation. No fluoride was observed in all the stream water samples. This study reported the absence of fluoride in spring and stream waters associated with the late Maastrichtian formations in Nigeria.
Synthesis, purification, and structural characterization of the dimethyldiselenoarsinate anion.

PubMed

Gailer, Jürgen; George, Graham N; Harris, Hugh H; Pickering, Ingrid J; Prince, Roger C; Somogyi, Arpad; Buttigieg, Gavin A; Glass, Richard S; Denton, M Bonner

2002-10-21

A novel arsenic-selenium solution species was synthesized by reacting equimolar sodium selenite and sodium dimethylarsinate with 10 mol equiv of glutathione (pH 7.5) in aqueous solution. The solution species showed a single (77)Se NMR resonance at 112.8 ppm. Size-exclusion chromatography (SEC) using an inductively coupled plasma atomic emission spectrometer (ICP-AES) as the simultaneous arsenic-, selenium-, sulfur-, and carbon-specific detector revealed an arsenic-selenium moiety with an As:Se molar ratio of 1:2. Electrospray ionization mass spectrometry (ESI-MS) of the chromatographically purified compound showed a molecular mass peak at m/z 263 in the negative ion mode. Fragmentation of the parent ion (ESI-MS-MS) produced (CH(3))(2)As(-) and Se(2)(-) fragments. Arsenic and selenium extended X-ray absorption fine structure spectroscopy (EXAFS) of the purified species revealed two As-C interactions at 1.943 A and two As-Se interactions at 2.279 A. On the basis of these results this novel solution species is identified as the dimethyldiselenoarsinate anion.
Enhancing effect of Fe2+ on the formaldehyde production from trimethylamine N-oxide decomposition catalyzed by the extract of Harpadon nehereus kidney

NASA Astrophysics Data System (ADS)

Sun, Yong; Zhou, Deqing; Zhao, Feng

2011-03-01

The effects of Fe2+ on the trimethylamine N-oxide (TMAO) demethylating activity of the Harpadon nehereus kidney extract were studied in this research. The activity of the kidney extract was presumably inhibited by ethylene diamine tetra-acetic acid (EDTA), which indicates that the kidney extract contains an enzyme or enzyme system with metal cations as activator. Activity of the kidney extract was enhanced significantly when Fe2+ was added into the model system in vitro. As the concentration of Fe2+ increased, the decomposing rate of TMAO increased rapidly until TMAO decomposed completely. The activity of the kidney extract was also enhanced by reductant such as ascorbic acid. Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) was employed to determine the content of total iron in a number of fishery products. Significant positive correlation between the contents of total iron and endogenous formaldehyde (FA) was found, especially in marine products.
Problems of Determining the Content of Cr(VI) in Raw Materials and Materials Containing Chromite Ore.

PubMed

Stec, Katarzyna

2017-11-02

Materials made with chromite ore are widely applied in the industry metallurgy as well as in the foundry industry. The oxidation number of chromium in these materials is both (III) and (VI). Currently there are no procedures allowing proper determination of chrome in chromite ores and ore-containing materials. The analytical methods applied, which are dedicated to a very narrow range of materials, e.g., cement, and cannot be applied in the case of materials which, apart from trace amounts of Cr(VI), contain mainly compounds of Cr(III), Fe(III) as well as trace compounds of Cu(II), Ni(II) and V(V). In the work particular attention has been paid to the preparation of test samples and creating measurement conditions in which interferences from Cr(III) and Fe(III) spectral lines could be minimized. Two separate instrumental measurement techniques have been applied: Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP AES) and the spectrophotometric method using diphenylcarbazide.
Characterization of metals emitted from motor vehicles.

PubMed

Schauer, James J; Lough, Glynis C; Shafer, Martin M; Christensen, William F; Arndt, Michael F; DeMinter, Jeffrey T; Park, June-Soo

2006-03-01

A systematic approach was used to quantify the metals present in particulate matter emissions associated with on-road motor vehicles. Consistent sampling and chemical analysis techniques were used to determine the chemical composition of particulate matter less than 10 microm in aerodynamic diameter (PM10*) and particulate matter less than 2.5 microm in aerodynamic diameter (PM2.5), including analysis of trace metals by inductively coupled plasma mass spectrometry (ICP-MS). Four sources of metals were analyzed in emissions associated with motor vehicles: tailpipe emissions from gasoline- and diesel-powered vehicles, brake wear, tire wear, and resuspended road dust. Profiles for these sources were used in a chemical mass balance (CMB) model to quantify their relative contributions to the metal emissions measured in roadway tunnel tests in Milwaukee, Wisconsin. Roadway tunnel measurements were supplemented by parallel measurements of atmospheric particulate matter and associated metals at three urban locations: Milwaukee and Waukesha, Wisconsin, and Denver, Colorado. Ambient aerosol samples were collected every sixth day for one year and analyzed by the same chemical analysis techniques used for the source samples. The two Wisconsin sites were studied to assess the spatial differences, within one urban airshed, of trace metals present in atmospheric particulate matter. The measurements were evaluated to help understand source and seasonal trends in atmospheric concentrations of trace metals. ICP-MS methods have not been widely used in analyses of ambient aerosols for metals despite demonstrated advantages over traditional techniques. In a preliminary study, ICP-MS techniques were used to assess the leachability of trace metals present in atmospheric particulate matter samples and motor vehicle source samples in a synthetic lung fluid.
Initial evaluation and comparison of plasma damage to atomic layer carbon materials using conventional and low T{sub e} plasma sources

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

Jagtiani, Ashish V.; Miyazoe, Hiroyuki; Chang, Josephine

2016-01-15

The ability to achieve atomic layer precision is the utmost goal in the implementation of atomic layer etch technology. Carbon-based materials such as carbon nanotubes (CNTs) and graphene are single atomic layers of carbon with unique properties and, as such, represent the ultimate candidates to study the ability to process with atomic layer precision and assess impact of plasma damage to atomic layer materials. In this work, the authors use these materials to evaluate the atomic layer processing capabilities of electron beam generated plasmas. First, the authors evaluate damage to semiconducting CNTs when exposed to beam-generated plasmas and compare thesemore » results against the results using typical plasma used in semiconductor processing. The authors find that the beam generated plasma resulted in significantly lower current degradation in comparison to typical plasmas. Next, the authors evaluated the use of electron beam generated plasmas to process graphene-based devices by functionalizing graphene with fluorine, nitrogen, or oxygen to facilitate atomic layer deposition (ALD). The authors found that all adsorbed species resulted in successful ALD with varying impact on the transconductance of the graphene. Furthermore, the authors compare the ability of both beam generated plasma as well as a conventional low ion energy inductively coupled plasma (ICP) to remove silicon nitride (SiN) deposited on top of the graphene films. Our results indicate that, while both systems can remove SiN, an increase in the D/G ratio from 0.08 for unprocessed graphene to 0.22 to 0.26 for the beam generated plasma, while the ICP yielded values from 0.52 to 1.78. Generally, while some plasma-induced damage was seen for both plasma sources, a much wider process window as well as far less damage to CNTs and graphene was observed when using electron beam generated plasmas.« less
Hydrothermal synthesis of 4ZnO·B2O3·H2O:Ln3+ (Ln=Eu, Tb) phosphors: Morphology-tunable and luminescence properties.

PubMed

Cao, Shiwei; Jiao, Yang; Han, Weifang; Ge, Chunhua; Song, Bo; Wang, Jie; Zhang, Xiangdong

2018-02-05

4ZnO·B 2 O 3 ·H 2 O:Ln 3+ (Ln=Eu, Tb) phosphors with different morphologies have been successfully synthesized via one-step hydrothermal method through regulating the molar amount of Eu 3+ and Tb 3+ . Comprehensive scanning electron microscopy (SEM), X-ray diffraction (XRD) Fourier transform infrared spectrum (FT-IR) and inductively coupled plasma atomic emission spectrometer (ICP-AES) characterizations all confirm that obtained products are 4ZnO·B 2 O 3 ·H 2 O:Ln 3+ (Ln=Eu, Tb). The experimental results displayed that the morphology and photoluminescence of compounds is regularly changed with increased the molar amount of rare earth ions. For the Eu 3+ -doped, Tb 3+ -doped and Eu 3+ /Tb 3+ co-doped 4ZnO·B 2 O 3 ·H 2 O phosphors of morphologies, the rod-like structures gradually changed to flower-like structures, fine wire-like structure and hybrid structure, respectively. To their photoluminescence, the Eu 3+ shows a red emission (615nm); the Tb 3+ shows a green emission (545nm); for the Eu 3+ /Tb 3+ co-doped 4ZnO·B 2 O 3 ·H 2 O phosphors, a combination of blue (5d-4f of Eu 2+ ), green ( 5 D 4 - 7 F 5 of Tb 3+ ) and red ( 5 D 0 - 7 F 2 of Eu 3+ ) emissions emerges to achieve white emission. In addition, the energy transfer among Eu 3+ , Eu 2+ and Tb 3+ ions was also discussed. Copyright © 2017. Published by Elsevier B.V.
Uncertainty estimation in the determination of metals in superficial water by ICP-OES

NASA Astrophysics Data System (ADS)

Faustino, Mainara G.; Marques, Joyce R.; Monteiro, Lucilena R.; Stellato, Thamiris B.; Soares, Sabrina M. V.; Silva, Tatiane B. S. C.; da Silva, Douglas B.; Pires, Maria Aparecida F.; Cotrim, Marycel E. B.

2016-07-01

From validation studies, it was possible to estimate a measurement uncertainty of several elements such as Al, Ba, Ca, Cu, Cr, Cd, Fe, Mg, Mn, Ni and K in water samples from Guarapiranga Dam. These elements were analyzed by optical emission spectrometry with inductively coupled plasma (ICP-OES). The value of relative estimated uncertainties were between 3% and 15%. The greatest uncertainty contributions were analytical curve, and the recovery method, which were related with elements concentrations and the equipment response. Water samples analyzed were compared with CONAMA Resolution #357/2005.
Biomonitoring of boron: Development and characterization of a simple, reliable and quality controlled biomonitoring method.

PubMed

Michalke, Bernhard

2017-03-01

Boron exposure is of interest and concern from an occupational point of view. Usual daily boron intake is related to boron blood plasma concentration <1mg/L and to <3mg/L in urine, but after exposure urine concentrations are quickly elevated. Reliable boron biomonitoring, typically in urine, thus is mandatory for occupational health control institutions. This paper reports on the development of a simple, fast and reliable boron determination procedure based on inductively coupled plasma - optical emission spectrometry (ICP-OES). Major aims for this method were simplicity in sample preparation, low risk for artifacts and interferences, high precision and accuracy, possibly low costs, including lower costs for element selective detection, short total analysis time and suitability for occupational health laboratories. Precision data (serial or day-to-day) from urine and doped urine were very good: <1.5 or <2%. Accuracy was calculated from analysis of a certified reference material (ERM-CD 281), as 99% or according to recoveries of doped concentrations ranging from 102 to 109% recovery. For cross-checking ICP-OES determinations, samples were analyzed also by quadrupole ICP-qMS and by sectorfield ICP-sf-MS at low and medium resolution. Both systems confirmed ICP-OES measurements when using 11 B for quantification. Determinations based on 10 B however showed some bias, except with ICP-sf-MS at medium resolution. The observed elevated signals are discussed with respect to the known Ne ++ interference (as an impurity in Ar), which is not separated in low resolving quadrupole ICP-MS systems or ICP-sf-MS at low resolution. Copyright © 2016 Elsevier GmbH. All rights reserved.
Characterization of the Etna volcanic emissions through an active biomonitoring technique (moss-bags): part 1--major and trace element composition.

PubMed

Calabrese, S; D'Alessandro, W; Bellomo, S; Brusca, L; Martin, R S; Saiano, F; Parello, F

2015-01-01

Active biomonitoring using moss-bags was applied to an active volcanic environment for the first time. Bioaccumulation originating from atmospheric deposition was evaluated by exposing mixtures of washed and air-dried mosses (Sphagnum species) at 24 sites on Mt. Etna volcano (Italy). Concentrations of major and a large suite of trace elements were analysed by inductively coupled mass and optical spectrometry (ICP-MS and ICP-OES) after total acid digestion. Of the 49 elements analysed those which closely reflect summit volcanic emissions were S, Tl, Bi, Se, Cd, As, Cu, B, Na, Fe, Al. Enrichment factors and cluster analysis allowed clear distinction between volcanogenic, geogenic and anthropogenic inputs that affect the local atmospheric deposition. This study demonstrates that active biomonitoring with moss-bags is a suitable and robust technique for implementing inexpensive monitoring in scarcely accessible and harsh volcanic environments, giving time-averaged quantitative results of the local exposure to volcanic emissions. This task is especially important in the study area because the summit area of Mt. Etna is visited by nearly one hundred thousand tourists each year who are exposed to potentially harmful volcanic emissions. Copyright © 2014 Elsevier Ltd. All rights reserved.
DPASV analytical technique for ppb level uranium analysis

NASA Astrophysics Data System (ADS)

Pal, Sangita; Singha, Mousumi; Meena, Sher Singh

2018-04-01

Determining uranium in ppb level is considered to be most crucial for reuse of water originated in nuclear industries at the time of decontamination of plant effluents generated during uranium (fuel) production, fuel rod fabrication, application in nuclear reactors and comparatively small amount of effluents obtained during laboratory research and developmental work. Higher level of uranium in percentage level can be analyzed through gravimetry, titration etc, whereas inductively coupled plasma-atomic energy spectroscopy (ICP-AES), fluorimeter are well suited for ppm level. For ppb level of uranium, inductively coupled plasma - mass spectroscopy (ICP-MS) or Differential Pulse Anodic Stripping Voltammetry (DPASV) serve the purpose. High precision, accuracy and sensitivity are the crucial for uranium analysis in trace (ppb) level, which are satisfied by ICP-MS and stripping voltammeter. Voltammeter has been found to be less expensive, requires low maintenance and is convenient for measuring uranium in presence of large number of other ions in the waste effluent. In this paper, necessity of uranium concentration quantification for recovery as well as safe disposal of plant effluent, working mechanism of voltammeter w.r.t. uranium analysis in ppb level with its standard deviation and a data comparison with ICP-MS has been represented.
Study of the chemical composition of particulate matter from the Rio de Janeiro metropolitan region, Brazil, by inductively coupled plasma-mass spectrometry and optical emission spectrometry

NASA Astrophysics Data System (ADS)

Mateus, Vinícius Lionel; Monteiro, Isabela Luizi Gonçalves; Rocha, Rafael Christian Chávez; Saint'Pierre, Tatiana Dillenburg; Gioda, Adriana

2013-08-01

Air quality in the metropolitan region of Rio de Janeiro was evaluated by analysis of particulate matter (PM) in industrial (Santa Cruz) and rural (Seropédica) areas. Total suspended particles (TSP) and fine particulate matter (PM2.5) collected in filters over 24 h were quantified and their chemical composition determined. TSP exceeded Brazilian guidelines (80 μg m- 3) in Santa Cruz, while PM2.5 levels exceeded the World Health Organization guidelines (10 μg m- 3) in both locations. Filters were extracted with water and/or HNO3, and the concentrations of 20 elements, mostly metals, were determined by inductively coupled plasma mass spectrometry (ICP-MS) and optical emission spectrometry (ICP OES). Water soluble inorganic anions were determined by ion chromatography (IC). To estimate the proportion of these elements extracted, a certified reference material (NIST SRM 1648a, Urban Dust) was subjected to the same extraction process. Concordant results were obtained by ICP-MS and ICP OES for most elements. Some elements could not be quantified by both techniques; the most appropriate technique was chosen in each case. The urban dust was also analyzed by the United States Environmental Protection Agency (US EPA) method, which employs a combination of hydrochloric and nitric acids for the extraction, but higher extraction efficiency was obtained when only nitric acid was employed. The US EPA method gave better results only for Sb. In the PM samples, the elements found in the highest average concentrations by ICP were Zn and Al (3-6 μg m- 3). The anions found in the highest average concentrations were SO42 - in PM2.5 (2-4 μg m- 3) and Cl- in TSP (2-6 μg m- 3). Principal component analysis (PCA) in combination with enrichment factors (EF) indicated industrial sources in PM2.5. Analysis of TSP suggested both anthropogenic and natural sources. In conclusion, this work contributes data on air quality, as well as a method for the analysis of PM samples by ICP-MS.
Comparative evaluation of GFAAS and ICP-MS for analyses of cadmium in blood.

PubMed

Fukui, Yoshinari; Ohashi, Fumiko; Sakuragi, Sonoko; Moriguchi, Jiro; Ikeda, Masayuki

2011-01-01

Cadmium in blood (Cd-B) is an important indicator, next to Cd in urine, in biological monitoring of exposure to Cd. The present study was initiated to examine compatibility in results of analysis for Cd-B between graphite furnace atomic absorption spectrophotometry (GFAAS) and inductively-coupled plasma mass-spectrometry (ICP-MS). For this purpose, 1,159 blood samples were collected from adult women (with no occupational exposure to Cd) in eight prefectures nation-widely in Japan. The samples were analyzed by the two methods; geometric mean (the maximum) concentrations were 1.22 (6.90) μg/l by ICP-MS, and 1.47 (7.40) μg/l by GFAAS. Statistical analyses showed that there was a close correlation between the results by the two methods. The regression line (with ICP-MS and GFAAS results as an independent variable and a dependent variable, respectively) had a slope close to one and an intercept next to zero to suggest that ICP-MS gave values compatible with that of GFAAS. Further analysis with the ratio of Cd-B by GFAAS over that by ICP-MS revealed that the two results were close to each other, and that the agreement was even closer when Cd-B was >2 μg/l. Thus, the two methods can be employed inter-convertibly when Cd-B is relatively high, e.g. >2 μg/l. Care may need to be practiced, however, for possible 'between methods' difference when Cd-B is low, e.g., ≤2 μg/l.
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.
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 U isotope ratios in sediments using ICP-QMS after sample cleanup with anion-exchange and extraction chromatography.

PubMed

Zheng, Jian; Yamada, Masatoshi

2006-01-15

The determination of uranium is important for environmental radioactivity monitoring, which investigates the releases of uranium from nuclear facilities and of naturally occurring radioactive materials by the coal, oil, natural gas, mineral, ore refining and phosphate fertilizer industries, and it is also important for studies on the biogeochemical behavior of uranium in the environment. In this paper, we describe a quadrupole ICP-MS (ICP-QMS)-based analytical procedure for the accurate determination of U isotope ratios ((235)U/(238)U atom ratio and (234)U/(238)U activity ratio) in sediment samples. A two-stage sample cleanup using anion-exchange and TEVA extraction chromatography was employed in order to obtain accurate and precise (234)U/(238)U activity ratios. The factors that affect the accuracy and precision of U isotope ratio analysis, such as detector dead time, abundance sensitivity, dwell time and mass bias were carefully evaluated and corrected. With natural U, a precision lower than 0.5% R.S.D. for (235)U/(238)U atom ratio and lower than 2.0% R.S.D. for (234)U/(238)U activity ratio was obtained with less than 90 ng uranium. The developed analytical method was validated using an ocean sediment reference material and applied to an investigation into the uranium isotopic compositions in a sediment core in a brackish lake in the vicinity of U-related nuclear facilities in Japan.
Analysis of trace metals in water by inductively coupled plasma emission spectrometry using sodium dibenzyldithiocarbamate for preconcentration

USGS Publications Warehouse

Smith, C.L.; Motooka, J.M.; Willson, W.R.

1984-01-01

Since concentrations of trace elements in most natural waters seldom exceed the ??g/L level, analysis of trace elements in natural waters by inductively coupled plasma emission spectrometry (ICP) requires a preconcentration procedure. The elements Ag, Bi, Cd, Co, Cu, Fe, Mo, Ni, Pb, Sn, V, W, and Zn were separated and concentrated from 500 mL of water by coprecipitating them with sodium dibenzyldithiocarbamate (NaDBDTC) using nickel or silver as a carrier. The precipitated trace elements were collected on a membrane filter, redissolved from the filter with hot nitric and hydrochloric acids, and analyzed using ICP. Recoveries for all the trace elements except tungsten exceeded 80%. Coprecipitation of trace elements with NaDBDTC eliminated the use of difficult-to-inject organic solvents, and NaDBDTC coprecipitated a wider array of trace elements than ammoniumpyrrolidinedithiocarbamate (APDC), another commonly used coprecipitate.
Trace elemental composition of curry by inductively coupled plasma optical emission spectrometry (ICP-OES).

PubMed

Gonzálvez, A; Armenta, S; De La Guardia, M

2008-01-01

A methodology based on inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave-assisted acid digestion was developed to determine the content of traces elements in curry samples from the Spanish market. The methodology was validated in terms of accuracy by the analysis of citrus and tomato leaf reference materials achieving comparable results with the certified values. The trace metal content of curry samples was compared with data available from previously published reports concerning Indian samples, especially in terms of heavy metal composition, in order to guarantee the quality of the commercially available spices in the European countries. Values found for the analysis of arsenic, lead and cadmium were significantly lower than the maximum limit allowed by European Union statutory limits for heavy metals and lower than those obtained for Indian curry leaves reported by Indian research teams by using neutron activation and γ-ray analysis.
A rapid and practical strategy for the determination of platinum, palladium, ruthenium, rhodium, iridium and gold in large amounts of ultrabasic rock by inductively coupled plasma optical emission spectrometry combined with ultrasound extraction

NASA Astrophysics Data System (ADS)

Zhang, Gai; Tian, Min

2015-04-01

This proposed method regulated the determination of platinum, palladium, ruthenium, rhodium, iridium and gold in platinum-group ores by nickel sulfide fire assay—inductively coupled plasma optical emission spectrometry (ICP-OES) combined with ultrasound extraction for the first time. The quantitative limits were 0.013-0.023μg/g. The samples were fused to separate the platinum-group elements from matrix. The nickel sulfide button was then dissolved with hydrochloric acid and the insoluble platinum-group sulfide residue was dissolved with aqua regia by ultrasound bath and finally determined by ICP-OES. The proposed method has been applied into the determination of platinum-group element and gold in large amounts of ultrabasic rocks from the Great Dyke of Zimbabwe.

Trace-Level Automated Mercury Speciation Analysis

PubMed Central

Taylor, Vivien F.; Carter, Annie; Davies, Colin; Jackson, Brian P.

2011-01-01

An automated system for methyl Hg analysis by purge and trap gas chromatography (GC) was evaluated, with comparison of several different instrument configurations including chromatography columns (packed column or capillary), detector (atomic fluorescence, AFS, or inductively coupled plasma mass spectrometry, ICP-MS, using quadrupole and sector field ICP- MS instruments). Method detection limits (MDL) of 0.042 pg and 0.030 pg for CH3Hg+ were achieved with the automated Hg analysis system configured with AFS and ICPMS detection, respectively. Capillary GC with temperature programming was effective in improving resolution and decreasing retention times of heavier Hg species (in this case C3H7Hg+) although carryover between samples was increased. With capillary GC, the MDL for CH3Hg+ was 0.25 pg for AFS detection and 0.060 pg for ICP-MS detection. The automated system was demonstrated to have high throughput (72 samples analyzed in 8 hours) requiring considerably less analyst time than the manual method for methyl mercury analysis described in EPA 1630. PMID:21572543
High-Temperature Isothermal Capacitance Transient Spectroscopy Study on Inductively Coupled Plasma Etching Damage for p-GaN Surfaces

NASA Astrophysics Data System (ADS)

Aoki, Toshichika; Wakayama, Hisashi; Kaneda, Naoki; Mishima, Tomoyoshi; Nomoto, Kazuki; Shiojima, Kenji

2013-11-01

The effects of the inductively coupled plasma (ICP) etching damage on the electrical characteristics of low-Mg-doped p-GaN Schottky contacts were evaluated by high-temperature isothermal capacitance transient spectroscopy. A large single peak for an acceptor-type surface state was dominantly detected for as-grown samples. The energy level and state density were obtained to be 1.18 eV above the valence band, which is close to a Ga vacancy (VGa), and 1.5×1013 cm-2, respectively. It was speculated that a small portion of Ga atoms were missing from the surface, and a high VGa density was observed in a few surface layers. The peak intensity decreased by 60% upon annealing at 800 °C, and further decrease was found by ICP etching. This decrease is consistent with the suppression of the memory effect in current-voltage characteristics. Upon annealing and ICP etching, since the VGa structure might be disordered, the peak intensity decreased.
Metal(loid) levels in biological matrices from human populations exposed to mining contamination--Panasqueira Mine (Portugal).

PubMed

Coelho, Patrícia; Costa, Solange; Silva, Susana; Walter, Alan; Ranville, James; Sousa, Ana C A; Costa, Carla; Coelho, Marta; García-Lestón, Julia; Pastorinho, M Ramiro; Laffon, Blanca; Pásaro, Eduardo; Harrington, Chris; Taylor, Andrew; Teixeira, João Paulo

2012-01-01

Mining activities may affect the health of miners and communities living near mining sites, and these health effects may persist even when the mine is abandoned. During mining processes various toxic wastes are produced and released into the surrounding environment, resulting in contamination of air, drinking water, rivers, plants, and soils. In a geochemical sampling campaign undertaken in the Panasqueira Mine area of central Portugal, an anomalous distribution of several metals and arsenic (As) was identified in various environmental media. Several potentially harmful elements, including As, cadmium (Cd), chromium (Cr), manganese (Mn), nickel (Ni), lead (Pb), and selenium (Se), were quantified in blood, urine, hair, and nails (toe and finger) from a group of individuals living near the Panasqueira Mine who were environmentally and occupationally exposed. A group with similar demographic characteristics without known exposure to mining activities was also compared. Genotoxicity was evaluated by means of T-cell receptor (TCR) mutation assay, and percentages of different lymphocyte subsets were selected as immunotoxicity biomarkers. Inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) analysis showed elevated levels of As, Cd, Cr, Mn, and Pb in all biological samples taken from populations living close to the mine compared to controls. Genotoxic and immunotoxic differences were also observed. The results provide evidence of an elevated potential risk to the health of populations, with environmental and occupational exposures resulting from mining activities. Further, the results emphasize the need to implement preventive measures, remediation, and rehabilitation plans for the region.
Development of certified reference materials for electrolytes in human serum (GBW09124-09126).

PubMed

Feng, Liuxing; Wang, Jun; Cui, Yanjie; Shi, Naijie; Li, Haifeng; Li, Hongmei

2017-05-01

Three reference materials, at relatively low, middle, and high concentrations, were developed for analysis of the mass fractions of electrolytes (K, Ca, Na, Mg, Cl, and Li) in human serum. The reference materials were prepared by adding high purity chloride salts to normal human serum. The concentration range of the three levels is within ±20% of normal human serum. It was shown that 14 units with duplicate analysis is enough to demonstrate the homogeneity of these candidate reference materials. The statistical results also showed no significant trends in both short-term stability test for 1 week at 40 °C and long-term stability test for 14 months. The certification methods of the six elements include isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS), inductively coupled plasma optical emission spectroscopy (ICP-OES), atomic absorption spectroscopy (AAS), ion chromatography (IC), and ion-selective electrode (ISE). The certification methods were validated by international comparisons among a number of national metrology institutes (NMIs). The combined relative standard uncertainties of the property values were estimated by considering the uncertainties of the analytical methods, homogeneity, and stability. The range of the expanded uncertainties of all the elements is from 2.2% to 3.9%. The certified reference materials (CRMs) are primarily intended for use in the calibration and validation of procedures in clinical analysis for the determination of electrolytes in human serum or plasma. Graphical Abstract Certified reference materials for K, Ca, Mg, Na, Cl and Li in human serum (GBW09124-09126).
Distribution of chemical elements in soils and stream sediments in the area of abandoned Sb-As-Tl Allchar mine, Republic of Macedonia.

PubMed

Bačeva, Katerina; Stafilov, Trajče; Šajn, Robert; Tănăselia, Claudiu; Makreski, Petre

2014-08-01

The aim of this study was to investigate the distribution of some toxic elements in topsoil and subsoil, focusing on the identification of natural and anthropogenic element sources in the small region of rare As-Sb-Tl mineralization outcrop and abandoned mine Allchar known for the highest natural concentration of Tl in soil worldwide. The samples of soil and sediments after total digestion were analyzed by inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES). Factor analysis (FA) was used to identify and characterize element associations. Six associations of elements were determined by the method of multivariate statistics: Rb-Ta-K-Nb-Ga-Sn-Ba-Bi-Li-Be-(La-Eu)-Hf-Zr-Zn-In-Pd-Ag-Pt-Mg; Tl-As-Sb-Hg; Te-S-Ag-Pt-Al-Sc-(Gd-Lu)-Y; Fe-Cu-V-Ge-Co-In; Pd-Zr-Hf-W-Be and Ni-Mn-Co-Cr-Mg. The purpose of the assessment was to determine the nature and extent of potential contamination as well as to broadly assess possible impacts to human health and the environment. The results from the analysis of the collected samples in the vicinity of the mine revealed that As and Tl elements have the highest median values. Higher median values for Sb are obviously as a result of the past mining activities and as a result of area surface phenomena in the past. Copyright © 2014 Elsevier Inc. All rights reserved.
[Standard addition determination of impurities in Na2CrO4 by ICP-AES].

PubMed

Wang, Li-ping; Feng, Hai-tao; Dong, Ya-ping; Peng, Jiao-yu; Li, Wu; Shi, Hai-qin; Wang, Yong

2015-02-01

Coupled plasma atomic emission spectrometry (ICP-AES) was used to determine the trace impurities of Ca, Mg, Al, Fe and Si in industrial sodium chromate. Wavelengths of 167.079, 393.366, 259.940, 279.533 and 251.611 nm were selected as analytical lines for the determination of Al, Ca, Fe, Mg and Si, respectively. The analytical errors can be eliminated by adjusting the determined solution with high pure hydrochloric acid. Standard addition method was used to eliminate matrix effects. The linear correlation, detection limit, precision and recovery for the concerned trace impurities have been examined. The effect of standard addition method on the accuracy for the determination under the selected analytical lines has been studied in detail. The results show that the linear correlations of standard curves were very good (R2 = 0.9988 to 0.9996) under the determined conditions. Detection limits of these trace impurities were in the range of 0.0134 to 0.0280 mg x L(-1). Sample recoveries were within 97.30% to 107.50%, and relative standard deviations were lower than 5.86% for eleven repeated determinations. The detection limits and accuracies established by the experiment can meet the analytical requirements and the analytic procedure was used to determine trace impurities in sodium chromate by ion membrane electrolysis technique successfully. Due to sodium chromate can be changed into sodium dichromate and chromic acid by adding acids, the established method can be further used to monitor trace impurities in these compounds or other hexavalent chromium compounds.
Divalent cations in tears, and their influence on tear film stability in humans and rabbits.

PubMed

Wei, Xiaojia Eric; Markoulli, Maria; Millar, Thomas J; Willcox, Mark D P; Zhao, Zhenjun

2012-06-05

Reduced tear film stability is reported to contribute to dry eye. Rabbits are known to have a more stable tear film than humans. Thus, we sought to examine the tears of rabbits and humans for metal cations, and to test how they influence tear film stability. Tears were collected from 10 healthy humans and 6 rabbits. Tear osmolality was measured by vapor pressure osmometer, and metals analyzed using inductively coupled plasma (ICP) mass spectrometry or ICP atomic emission spectroscopy. The influence of divalent cations on tears was analyzed by measuring surface tension using the Langmuir trough in vitro, using different concentrations of cations in the subphase, and grading the tear break-up in rabbits in vivo after instillation of chelating agents. Rabbit tears had a higher osmolality compared to humans. Major metals did not differ between species; however, rabbits had higher levels of Mg(2+) (1.13 vs. 0.39 mM) and Ca(2+) (0.75 vs. 0.36 mM). In rabbit tears in vitro, diminishing divalent cations resulted in a decrease in the maximum surface pressure from 37 to 30 mN/m. In vivo, an increase in the amount of tear film that was broken-up was found. In contrast, when changing divalent cation concentrations in human tears, the maximum surface pressure remained at 26 mN/m. The normal osmolality of rabbit tears is significantly higher than that in humans. While divalent cations had little influence on human tears, they appear to have an important role in maintaining tear film stability in rabbits.
Vivianite formation and distribution in Lake Baikal sediments

NASA Astrophysics Data System (ADS)

Fagel, N.; Alleman, L. Y.; Granina, L.; Hatert, F.; Thamo-Bozso, E.; Cloots, R.; André, L.

2005-04-01

In an effort to better understand vivianite formation processes, four Lake Baikal sediment cores spanning two to four interglacial stages in the northern, central and southern basins and under various biogeochemical environments are scrutinized. The vivianite-rich layers were detected by anomalous P-enrichments in bulk geochemistry and visually by observations on X-radiographs. The millimetric concretions of vivianite were isolated by sieving and analysed by X-ray diffraction, scanning electron microscope (SEM), microprobe, infrared spectroscopy, inductively coupled plasma atomic emission spectrometry and mass spectrometry (ICP-AES, ICP-MS). All the vivianites display similar morphological, mineralogical and geochemical signature, suggesting a common diagenetic origin. Their geochemical signature is sensitive to secondary alteration where vivianite concretions are gradually transformed from the rim to the center into an amorphous santabarbaraite phase with a decreasing Mn content. We analysed the spatial and temporal distribution of the concretions in order to determine the primary parameters controlling the vivianite formation, e.g., lithology, sedimentation rates, and porewater chemistry. We conclude that vivianite formation in Lake Baikal is mainly controlled by porewater chemistry and sedimentation rates, and it is not a proxy for lacustrine paleoproductivity. Vivianite accumulation is not restricted to areas of slow sedimentation rates (e.g., Academician and Continent ridges). At the site of relatively fast sedimentation rate, i.e., the Posolsky Bank near the Selenga Delta, vivianite production may be more or less related to the Selenga River inputs. It could be also indirectly related to the past intensive methane escapes from the sediments. While reflecting an early diagenetic signal, the source of P and Fe porewater for vivianites genesis is still unclear.
Monitoring of Cr, Cu, Pb, V and Zn in polluted soils by laser induced breakdown spectroscopy (LIBS).

PubMed

Dell'Aglio, Marcella; Gaudiuso, Rosalba; Senesi, Giorgio S; De Giacomo, Alessandro; Zaccone, Claudio; Miano, Teodoro M; De Pascale, Olga

2011-05-01

Laser Induced Breakdown Spectroscopy (LIBS) is a fast and multi-elemental analytical technique particularly suitable for the qualitative and quantitative analysis of heavy metals in solid samples, including environmental ones. Although LIBS is often recognised in the literature as a well-established analytical technique, results about quantitative analysis of elements in chemically complex matrices such as soils are quite contrasting. In this work, soil samples of various origins have been analyzed by LIBS and data compared to those obtained by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). The emission intensities of one selected line for each of the five analytes (i.e., Cr, Cu, Pb, V, and Zn) were normalized to the background signal, and plotted as a function of the concentration values previously determined by ICP-OES. Data showed a good linearity for all calibration lines drawn, and the correlation between ICP-OES and LIBS was confirmed by the satisfactory agreement obtained between the corresponding values. Consequently, LIBS method can be used at least for metal monitoring in soils. In this respect, a simple method for the estimation of the soil pollution degree by heavy metals, based on the determination of an anthropogenic index, was proposed and determined for Cr and Zn.
[Study on microwave digestion of gypsum for the determination of multielement by ICP-OES and ICP-MS].

PubMed

Wang, Hui; Song, Qiang; Yang, Rui-ming; Yao, Qiang; Chen, Chang-he

2010-09-01

Three acids (HNO3, HNO3/HF and HNO3 /HF+ H3BO3) were used to decompose gypsum with microwave digestion system. The contents of 10 mineral elements (Al, Ca, Mg, Fe, K, Na, S, Ti, Si and Sr) in gypsum were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES) while 6 heavy metals (V, Cr, Mn, Zn, Se and Ce) were determined by inductively coupled plasma-mass spectrometry (ICP-MS). GBW03109a, GBW03110 and FGD-2 were used as gypsum standard reference materials. The results showed that two-step microwave digestion with HNO3/HF at 210 degrees C and then adding H3BO3 for the removal of HF and fluorides completely decomposed the gypsums, while this method achieved good recoveries for all elements in the three gypsum standard reference materials. The recovery was from 88% to 112% and the RSD of tests was below 3%. The method was applied to the elemental analysis for flue gas desulfurization gypsums from three coal-fired power plants.
Environmental impact of heavy metals on the soils and plants around a coke-making factory of Jiyuan city, China

NASA Astrophysics Data System (ADS)

Lun Leung, Kwun

2010-05-01

The combustion of coal usually leads to many different kinds of pollution around coke-making factories. Among these pollutions, the heavy metal contamination in the soil and plants is one of the major concerns by people living around. Heavy metals are highly attracted to the biological tissue, and can stay in bodies of organisms for long period of time, causing a lot of hazardous diseases to human beings, animal and plants. In the developing regions of China, developing of industries has been based on the sacrifices of environments and human health. In order to evaluate the danger of heavy metal contamination from a coke factory to citizens of close inhabitants, a survey on soil and plants was conducted in the region around a coke-making factory in Jiyuan city, which is a major electricity supplying city for the Henan Province in China. In this study, 8 surface soil samples and 11 plant samples were collected from 8 different places around the coke-making factory in Jiyuan city. The collected samples are then treated in the laboratory, and 8 types of heavy metals, which include arsenic, cadmium, chromium, cobalt, copper, lead, nickel and zinc, are analyzed by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) and Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES). The concentration data of heavy metals that collected from the analysis are then used to evaluate their toxicity towards living organisms and ecology by applying several biological effect standards, such as effect-range low (ERL), effect-range median (ERM) and several maximum allowances standards of heavy metal concentrations in soils and plants that established by different countries. Moreover, the relationship between the distance from the factory and the concentration of heavy metals in soils and plants are also evaluated in order to find out the contamination ranges of those heavy metals from the source. The result shows that the concentration of these 8 types of heavy metals in the site exceeds the ERL, with lead being the heavy metals that exceeds the biological effect standards the most. This study suggests some remediate measures that must be made in order to decrease the emission of these elements to meet the national standards. The local government is now realized the problems and begins to limit the emissions and offers medical treatments to kids detected with high blood lead.
High Resolution Studies of the Origins of Polyatomic Ions in Inductively Coupled Plasma-Mass Spectrometry

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

Ferguson, Jill Wisnewski

2006-01-01

The inductively coupled plasma (ICP) is an atmospheric pressure ionization source. Traditionally, the plasma is sampled via a sampler cone. A supersonic jet develops behind the sampler, and this region is pumped down to a pressure of approximately one Torr. A skimmer cone is located inside this zone of silence to transmit ions into the mass spectrometer. The position of the sampler and skimmer cones relative to the initial radiation and normal analytical zones of the plasma is key to optimizing the useful analytical signal [1]. The ICP both atomizes and ionizes the sample. Polyatomic ions form through ion-molecule interactionsmore » either in the ICP or during ion extraction [l]. Common polyatomic ions that inhibit analysis include metal oxides (MO +), adducts with argon, the gas most commonly used to make up the plasma, and hydride species. While high resolution devices can separate many analytes from common interferences, this is done at great cost in ion transmission efficiency--a loss of 99% when using high versus low resolution on the same instrument [2]. Simple quadrupole devices, which make up the bulk of ICP-MS instruments in existence, do not present this option. Therefore, if the source of polyatomic interferences can be determined and then manipulated, this could potentially improve the figures of merit on all ICP-MS devices, not just the high resolution devices often utilized to study polyatomic interferences.« less
Practical utilization of spICP-MS to study sucrose density gradient centrifugation for the separation of nanoparticles.

PubMed

Johnson, Monique E; Montoro Bustos, Antonio R; Winchester, Michael R

2016-11-01

Single particle inductively coupled plasma mass spectrometry (spICP-MS) is shown to be a practical technique to study the efficacy of rate-zonal sucrose density gradient centrifugation (SDGC) separations of mixtures of gold nanoparticles (AuNPs) in liquid suspension. spICP-MS enabled measurements of AuNP size distributions and particle number concentrations along the gradient, allowing unambiguous evaluations of the effectiveness of the separation. Importantly, these studies were conducted using AuNP concentrations that are directly relevant to environmental studies (sub ng mL -1 ). At such low concentrations, other techniques [e.g., dynamic light scattering (DLS), transmission and scanning electron microscopies (TEM and SEM), UV-vis spectroscopy, atomic force microscopy (AFM)] do not have adequate sensitivity, highlighting the inherent value of spICP-MS for this and similar applications. In terms of the SDGC separations, a mixture containing three populations of AuNPs, having mean diameters of 30, 80, and 150 nm, was fully separated, while separations of two other mixtures (30, 60, 100 nm; and 20, 50, 100 nm) were less successful. Finally, it is shown that the separation capacity of SDGC can be overwhelmed when particle number concentrations are excessive, an especially relevant finding in view of common methodologies taken in nanotechnology research. Graphical Abstract Characterization of the separation of a gold nanoparticle mixture by sucrose density gradient centrifugation by conventional and single particle ICP-MS analysis.
Investigating Pu and U isotopic compositions in sediments: a case study in Lake Obuchi, Rokkasho Village, Japan using sector-field ICP-MS and ICP-QMS.

PubMed

Zheng, Jian; Yamada, Masatoshi

2005-08-01

The objectives of the present work were to study isotope ratios and the inventory of plutonium and uranium isotope compositions in sediments from Lake Obuchi, which is in the vicinity of several nuclear fuel facilities in Rokkasho, Japan. Pu and its isotopes were determined using sector-field ICP-MS and U and its isotopes were determined with ICP-QMS after separation and purification with a combination of ion-exchange and extraction chromatography. The observed (240)Pu/(239)Pu atom ratio (0.186 +/- 0.016) was similar to that of global fallout, indicating that the possible early tropospheric fallout Pu did not deliver Pu from the Pacific Proving Ground to areas above 40 degrees N. The previously reported higher Pu inventory in the deep water area of Lake Obuchi could be attributed to the lateral transportation of Pu deposited in the shallow area which resulted from the migration of deposited global fallout Pu from the land into the lake by river runoff and from the Pacific Ocean by tide movement and sea water scavenging, as well as from direct soil input by winds. The (235)U/(238)U atom ratios ranged from 0.00723 to 0.00732, indicating the natural origin of U in the sediments. The average (234)U/(238)U activity ratio of 1.11 in a sediment core indicated a significant sea water U contribution. No evidence was found for the release of U containing wastes from the nearby nuclear facilities. These results will serve as a reference baseline on the levels of Pu and U in the studied site so that any further contamination from the spent nuclear fuel reprocessing plants, the radioactive waste disposal and storage facilities, and the uranium enrichment plant can be identified, and the impact of future release can be rapidly assessed.
The ac stark shift and space-borne rubidium atomic clocks

NASA Astrophysics Data System (ADS)

Formichella, V.; Camparo, J.; Sesia, I.; Signorile, G.; Galleani, L.; Huang, M.; Tavella, P.

2016-11-01

Due to its small size, low weight, and low power consumption, the Rb atomic frequency standard (RAFS) is routinely the first choice for atomic timekeeping in space. Consequently, though the device has very good frequency stability (rivaling passive hydrogen masers), there is interest in uncovering the fundamental processes limiting its long-term performance, with the goal of improving the device for future space systems and missions. The ac Stark shift (i.e., light shift) is one of the more likely processes limiting the RAFS' long-term timekeeping ability, yet its manifestation in the RAFS remains poorly understood. In part, this comes from the fact that light-shift induced frequency fluctuations must be quantified in terms of the RAFS' light-shift coefficient and the output variations in the RAFS' rf-discharge lamp, which is a nonlinear inductively-couple plasma (ICP). Here, we analyze the light-shift effect for a family of 10 on-orbit Block-IIR GPS RAFS, examining decade-long records of their on-orbit frequency and rf-discharge lamp fluctuations. We find that the ICP's light intensity variations can take several forms: deterministic aging, jumps, ramps, and non-stationary noise, each of which affects the RAFS' frequency via the light shift. Correlating these light intensity changes with RAFS frequency changes, we estimate the light-shift coefficient, κLS, for the family of RAFS: κLS = -(1.9 ± 0.3) × 10-12/%. The 16% family-wide variation in κLS indicates that while each RAFS may have its own individual κLS, the variance of κLS among similarly designed RAFS can be relatively small. Combining κLS with our estimate of the ICP light intensity's non-stationary noise, we find evidence that random-walk frequency noise in high-quality space-borne RAFS is strongly influenced by the RAFS' rf-discharge lamp via the light shift effect.
Titanium (III) cation selective electrode based on synthesized tris(2pyridyl) methylamine ionophore and its application in water samples

PubMed Central

Rezayi, Majid; Karazhian, Reza; Abdollahi, Yadollah; Narimani, Leila; Sany, Seyedeh Belin Tavakoly; Ahmadzadeh, Saeid; Alias, Yatimah

2014-01-01

The introduction of low detection limit ion selective electrodes (ISEs) may well pave the way for the determination of trace targets of cationic compounds. This research focuses on the detection of titanium (III) cation using a new PVC-membrane sensor based on synthesized tris(2pyridyl) methylamine (tpm) ionophore. The application and validation of the proposed sensor was done using potentiometric titration, inductively coupled plasma atomic emission spectrometry (ICP-AES), and atomic absorption spectrometry (AAS). The membrane sensor exhibited a Nernstian response to the titanium (III) cation over a concentration range of 1.0 × 10−6–1.0 × 10−2 M and pH range from 1–2.5. The Nernstian slope, the lower of detection (LOD), and the response time (t95%) of the proposed sensor were 29.17 ± 0.24 mV/dec, 7.9 × 10−7 M, and 20 s, respectively. The direct determination of 4–39 μg/ml of titanium (III) standard solution showed an average recovery of 94.60 and a mean relative standard deviation of 1.8 at 100.0 μg/ml. Finally, the utilization of the electrodes as end-point indicators for potentiometric titration with EDTA solutions for titanium (III) sensor was successfully carried out. PMID:24722576
Induced Phytoextraction of Lead Through Chemical Manipulation of Switchgrass and Corn; Role of Iron Supplement.

PubMed

Johnson, Deayne M; Deocampo, Daniel M; El-Mayas, Hanan; Greipsson, Sigurdur

2015-01-01

The effects of combined chemical application of benomyl, ethylenedianinetetraacetate (EDTA), and iron (Fe) (foliar and root) on lead (Pb) phytoextraction by switchgrass (Panicum virgatum) and corn (Zea mays) was examined. Switchgrass was grown in Pb-contaminated urban topsoil with the following treatments: (C) Control, (B) benomyl, (E) EDTA, (F) foliar-Fe, (BE) benomyl + EDTA, (BF) benomyl + foliar-Fe, (FE) foliar-Fe + EDTA, (BFE) benomyl + foliar-Fe + EDTA. Corn was grown in sand-culture supplemented with Pb (500 mg kg(-1)) with the following treatments: (C) control, (B) benomyl, (E) EDTA, (F) root-Fe, (BE) benomyl + EDTA, (BF) benomyl + root-Fe, (FE) root-iron + EDTA, and, (BFE) benomyl + root-Fe + EDTA. All treatments were replicated three times and pots were arranged in a completely randomized design. Plants were analyzed for element concentration (Fe, Zn, P, and Pb) using either inductively coupled plasma (argon) atomic emission spectroscopy (ICP-AES) or graphite furnace atomic absorption spectrometer. Iron supplementation (foliar and root) affected Pb-translocation in plants. Foliar-Fe treatment increased translocation ratio of Pb (TF-Pb) significantly compared to other treatments with the exception of plants treated with benomyl and BF. Root-Fe treatment in combination with EDTA (FE) increased TF-Pb significantly compared to other treatments. Phytoextraction was improved by the combined chemical application; plants treated with BFE treatment increased Pb-total-phytoextraction by 424% compared to Control plants.
Photocatalytic oxidation of aqueous ammonia over microwave-induced titanate nanotubes.

PubMed

Ou, Hsin-Hung; Liao, Ching-Hui; Liou, Ya-Hsuan; Hong, Jian-Hao; Lo, Shang-Lien

2008-06-15

Characterizations of microwave-induced titanate nanotubes (NaxH(2-x)Ti3O7, TNTs) were conducted by the determinations of specific surface area (S(BET)), X-ray diffraction (XRD), X-ray photoelectron spectroscopic (XPS), ionic coupled plasma-atomic emission spectrometry(ICP-AES), scanning electron microscopy/ energy dispersive X-ray (SEM/EDX), and high-resolution transmission electron microscopy (HR-TEM). The applied level of microwave irradiation during the fabrication process is responsible for both the intercalation intensity of Na atoms into TNTs and the type of crystallization phase within TNTs, which dominate the efficiency of photocatalytic NH3/NH4+. A pure TNT phase presents no powerful ability toward photocatalytic NH3/ NH4+, while the photocatalytic efficiency can be enhanced with the presence of a rutile phase within TNTs. In addition, the mixture of anatase and rutile phase within P25 TiO2 prefers forming NO3-, whereas TNTs yield higher NO2- amount Regarding the effect of acid-washing treatment on TNTs, the acid-treated TNTs with enhanced ion exchangeability considerably improve the NH3/NH4+ degradation and NO2-/NO3- yields. This result is likely ascribed to the easy intercalation of NH3/ NH4+ into the structure of acid-washing TNTs so that the photocatalytic oxidation of intercalated NH3/NH4+ is not limited to the shielding effect resulting from the overload of TNTs.
Mapping of lead, magnesium and copper accumulation in plant tissues by laser-induced breakdown spectroscopy and laser-ablation inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Kaiser, J.; Galiová, M.; Novotný, K.; Červenka, R.; Reale, L.; Novotný, J.; Liška, M.; Samek, O.; Kanický, V.; Hrdlička, A.; Stejskal, K.; Adam, V.; Kizek, R.

2009-01-01

Laser-Induced Breakdown Spectroscopy (LIBS) and Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) were utilized for mapping the accumulation of Pb, Mg and Cu with a resolution up to 200 μm in a up to cm × cm area of sunflower ( Helianthus annuus L.) leaves. The results obtained by LIBS and LA-ICP-MS are compared with the outcomes from Atomic Absorption Spectrometry (AAS) and Thin-Layer Chromatography (TLC). It is shown that laser-ablation based analytical methods can substitute or supplement these techniques mainly in the cases when a fast multi-elemental mapping of a large sample area is needed.
Evaluation of a new optic-enabled portable X-ray fluorescence spectrometry instrument for measuring toxic metals/metalloids in consumer goods and cultural products

NASA Astrophysics Data System (ADS)

Guimarães, Diana; Praamsma, Meredith L.; Parsons, Patrick J.

2016-08-01

X-ray fluorescence spectrometry (XRF) is a rapid, non-destructive multi-elemental analytical technique used for determining elemental contents ranging from percent down to the μg/g level. Although detection limits are much higher for XRF compared to other laboratory-based methods, such as inductively coupled plasma mass spectrometry (ICP-MS), ICP-optical emission spectrometry (OES) and atomic absorption spectrometry (AAS), its portability and ease of use make it a valuable tool, especially for field-based studies. A growing necessity to monitor human exposure to toxic metals and metalloids in consumer goods, cultural products, foods and other sample types while performing the analysis in situ has led to several important developments in portable XRF technology. In this study, a new portable XRF analyzer based on the use of doubly curved crystal optics (HD Mobile®) was evaluated for detecting toxic elements in foods, medicines, cosmetics and spices used in many Asian communities. Two models of the HD Mobile® (a pre-production and a final production unit) were investigated. Performance parameters including accuracy, precision and detection limits were characterized in a laboratory setting using certified reference materials (CRMs) and standard solutions. Bias estimates for key elements of public health significance such as As, Cd, Hg and Pb ranged from - 10% to 11% for the pre-production, and - 14% to 16% for the final production model. Five archived public health samples including herbal medicine products, ethnic spices and cosmetic products were analyzed using both XRF instruments. There was good agreement between the pre-production and final production models for the four key elements, such that the data were judged to be fit-for-purpose for the majority of samples analyzed. Detection of the four key elements of interest using the HD Mobile® was confirmed using archived samples for which ICP-OES data were available based on digested sample materials. The HD Mobile® XRF units were shown to be suitable for rapid screening of samples likely to be encountered in field based studies.

Passive degassing at Nyiragongo (D.R. Congo) and Etna (Italy) volcanoes: the chemical characterization of the emissions and assessment of their uptake of trace elements emissions on the local environment

NASA Astrophysics Data System (ADS)

Calabrese, Sergio; Scaglione, Sarah; Milazzo, Silvia; D'Alessandro, Walter; Bobrowski, Nicole; Giuffrida, Giovanni; Tedesco, Dario; Parello, Francesco

2014-05-01

Volcanoes are well known as an impressive large natural source of trace elements into the troposphere. Among others, Etna (Italy) and Nyiragongo (D.R. Congo), two noteworthy emitters on Earth, are two stratovolcanoes located in different geological settings, both characterized by persistent passive degassing from their summit craters. Here, we present some results on trace element composition in volcanic plume emissions, atmospheric bulk deposition (rainwater) and their uptake of the surrounding vegetation, with the aim to compare and identify differences and similarities between this these two volcanoes. Volcanic emissions were sampled by using active filter-pack for acid gases (sulfur and halogens) and specific teflon filters for particulates (major and trace elements). The impact of the volcanogenic deposition in the surrounding of the crater rims was investigated by using different sampling techniques: bulk rain collectors gauges were used to collect atmospheric bulk deposition, and biomonitoring technique was carried out to collect gases and particulates by using endemic plant species. Concentrations of major and trace elements of volcanic plume emissions (gases and particulates) were obtained by elution and microwave digestion of the collected filters: sulfur and halogens were determined by ion chromatography and ICP-MS, and untreated filters for particulate were acid digested and analysed by ICP-OES and ICP-MS. Rain water and plant samples were also analysed for major and trace elements by using ICP-OES and ICP-MS. In total 55 elements were determined. The estimates of the trace element fluxes confirm that Etna and Nyiragongo are large sources of metals to the atmosphere, especially considering their persistent state of passive degassing. In general, chemical composition of the volcanic aerosol particles of both volcanoes is characterized by two main components: one is related to the silicic component produced by magma bursting and fragmentation, enriching the plume in Si, Al, Fe, Ti, Mg, Ca, Na, K and other trace elements like Ni, Cr, Co, Th and U; another one components, is dominated by volatile trace elements (As, Bi, Cd, Cu, Hg, Se, Te, Tl) related to the gas volatile phase (H2O, CO2, SO2, HCl, HF) and transported to the atmosphere mainly as hydro-soluble salts and/or in gaseous form in some cases. The large amount of emitted trace elements have a strong impact on the close surrounding of both volcanoes. This is clearly reflected by in the chemical composition of rain water collected at the summit areas both for Etna and Nyiragongo. In fact, rain water samples have low pH values (<2) and high concentrations of dissolved toxic metals. Moreover, the biomonitoring results highlight that bioaccumulation of trace elements is extremely high in the proximity of the crater rim and decreases with the distance from the active craters. In particular, we found a good correlation between volatile elements (Tl, As, Bi, Cd, Se, Cu) concentrations in the leaves of Senecio species collected in on both volcanoes, showing a clear influence of volcanic deposition.
TANK 40 FINAL SB7B CHEMICAL CHARACTERIZATION RESULTS

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

Bannochie, C.

2012-03-15

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, and these results are reported here. These analyses along with the WAPS radionuclide analyses will help define the composition of the sludge in Tank 40 that is currently being fed to the Defense Waste Processing Facility (DWPF) as SB7b. At the Savannah River National Laboratory (SRNL) the 3-L Tank 40 SB7b sample was transferred frommore » 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 thorough 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{reg_sign} 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{sup -}/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 developed by SRNL AD and previously described. The following conclusions were drawn from the analytical results reported here: (1) The ratios of the major elements for the SB7b WAPS sample are different from those measured for the SB7a WAPS sample. There is less Al and Mn relative to Fe than the previous sludge batch. (2) The elemental composition of this sample and the analyses conducted here are reasonable and consistent with DWPF batch data measurements in light of DWPF pre-sample concentration and SRAT product heel contributions to the DWPF SRAT receipt analyses. The element ratios for Al/Fe, Ca/Fe, Mn/Fe, and U/Fe agree within 10% between this work and the DWPF Sludge Receipt and Adjustment Tank (SRAT) receipt analyses. (3) Sulfur in the SB7b WAPS sample is 82% soluble, slightly less than results reported for SB3, SB4, and SB6 samples but unlike the 50% insoluble sulfur observed in the SB5 WAPS sample. In addition, 23% of the soluble sulfur is not present as sulfate in SB7b. (4) The average activities of the fissile isotopes of interest in the SB7b WAPS sample are (in {mu}Ci/g of total dried solids): 4.22E-02 U-233, 6.12E-04 U-235, 1.08E+01 Pu-239, and 5.09E+01 Pu-241. The full radionuclide composition will be reported in a future document. (5) The fission product noble metal and Ag concentrations appear to have largely peaked in previous DWPF sludge batches, with the exception of Ru, which still shows a slight increase in SB7b.« less
Determination of As, Cd, Hg and Pb in continuous use drugs and excipients by plasma-based techniques in compliance with the United States Pharmacopeia requirements

NASA Astrophysics Data System (ADS)

da Silva, Caroline Santos; Pinheiro, Fernanda Costa; do Amaral, Clarice Dias Britto; Nóbrega, Joaquim Araújo

2017-12-01

Some inorganic impurities are toxic to human health even when present at low concentrations and therefore must be carefully monitored in products as continuous use drugs. This work aimed the development of a simple microwave-assisted digestion procedure for different types of drugs and excipients and the analytical determination of elemental impurities according to the new regulations of the United States Pharmacopeia (USP) 232 and 233 using inductively coupled plasma optical emission spectrometry (ICP-OES) or inductively coupled plasma mass spectrometry (ICP-MS). Eight drugs samples and two excipients of different brands were microwave-assisted digested with inverse aqua regia. Addition and recovery experiments were performed according to J values, once permissible daily exposure value is specific for each element and estimated according to the maximum daily dose of drug indicated by the label. Samples were spiked with values of 1.5J in order to check accuracies for As, Cd, Hg, and Pb. Recoveries obtained by ICP-OES ranged from 75 to 148% and for ICP-MS ranged from 74 to 120%. The limits of detection for ICP-OES ranged from 0.4 to 17 mg kg- 1 and for ICP-MS from 7.4 to 41.6 μg kg- 1. Both analytical methods were adequate in terms of accuracies and sensitivities. Considering the maximum daily dose, all drugs samples and excipients contained As, Cd, Hg and Pb below the maximum limits stipulated by USP since all of them presented contents below respective limits of detection.
[Determination of tungsten and cobalt in the air of workplace by ICP-OES].

PubMed

Zhang, J; Ding, C G; Li, H B; Song, S; Yan, H F

2017-08-20

Objective: To establish the inductively coupled plasma optical emission spectrometry (ICP-OES) method for determination of cobalt and tungsten in the air of workplace. Methods: The cobalt and tungsten were collected by filter membrane and then digested by nitric acid, inductively coupled plasma optical emission spectrometry (ICP-OES) was used for the detection of cobalt and tungsten. Results: The linearity of tungsten was good at the range of 0.01-1 000 μg/ml with a correlation coefficient of 0.999 9, the LOD and LOQ were 0.006 7 μg/ml and 0.022 μg/ml, respectively. The recovery was ranged from 98%-101%, the RSD of intra-and inter-batch precision were 1.1%-3.0% and 2.1%-3.8%, respectively. The linearity of cobalt was good at the range of 0.01-100 μg/ml with a correlation coefficient of 0.999 9, the LOD and LOQ were 0.001 2 μg/ml and 0.044 μg/ml, respectively. The recovery was ranged from 95%-97%, the RSD of intra-and inter-batch precision were 1.1%-2.4% and 1.1%-2.9%, respectively. The sampling efficiency of tungsten and cobalt were higher than 94%. Conclusion: The linear range, sensitivity and precision of the method was suitable for the detection of tungsten and cobalt in the air of workplace.
Using Gamma ray and Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) to Evaluate Elemental Sequences in Cap-carbonates and Cap-like Carbonates of the Death Valley Region

NASA Astrophysics Data System (ADS)

Holter, S. A.; Theissen, K. M.; Hickson, T. A.; Bostick, B.

2004-12-01

The Snowball Earth theory of Hoffman et al. (1998) proposes dramatic post-glacial chemical weathering as large concentrations of carbon were removed from the atmosphere. This would result in a large input of terrigenous material into the oceans; hence, we might expect that carbonates formed under these conditions would demonstrate elevated K, U, Th levels in comparison to carbonates formed under more typical conditions. In January of 2004 we collected spectral gamma data (K, U, Th) and hand samples from cap carbonates (Noonday Dolomite) and cap-like carbonates (Beck Spring Dolomite) of the Death Valley region in order to explore elemental changes in post-snowball Earth oceans. Based on our spectral gamma results, Th/U ratio trends suggested variations in the oxidation state of the Precambrian ocean. We pursued further investigations of trace elements to ascertain the reliability of these results by using ICP-OES. A suite of 25 trace elements was measured, most notably including U and Th. The ICP-OES data not only allow us to compare elemental changes between cap-carbonates and cap-like carbonates, but they also allow for a comparison of optical emission spectrometry and hand held gamma spectrometry methods. Both methods show similar trends in U and Th values for both the cap-carbonates and cap-like carbonates.
Glassy carbon/multi walled carbon nanotube/cadmium sulphide photoanode for light energy storage in vanadium photoelectrochemical cell

NASA Astrophysics Data System (ADS)

Peimanifard, Zahra; Rashid-Nadimi, Sahar

2015-12-01

The aim of this study is utilizing the artificial photosynthesis, which is an attractive and challenging theme in the photoelectrocatalytic water splitting, to charge the vanadium redox flow battery (VRFB). In this work multi walled carbon nanotube/cadmium sulphide hybrid is employed as a photoanode material to oxidize VO2+ toVO2+ for charging the positive vanadium redox flow battery's half-cell. Characterization studies are also described using the scanning electron microscopic-energy-dispersive X-ray spectroscopy (SEM-EDS), inductively coupled plasma atomic emission spectroscopy (ICP-AES) and UV-Visible methods. The phtoelectrochemical performance is characterized by cyclic voltammetry and chronoamperometry. Applied bias photon-to-current efficiency (ABPE) is achieved for both two and three-electrode configurations. The glassy carbon/multi walled carbon nanotube/cadmium sulphide yields high maximum ABPE of 2.6% and 2.12% in three and two-electrode setups, respectively. These results provide a useful guideline in designing photoelectrochemical cells for charging the vanadium redox flow batteries by sunlight as a low cost, free and abundant energy source, which does not rely on an external power input.
Water analysis via portable X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Pearson, Delaina; Chakraborty, Somsubhra; Duda, Bogdan; Li, Bin; Weindorf, David C.; Deb, Shovik; Brevik, Eric; Ray, D. P.

2017-01-01

Rapid, in-situ elemental water analysis would be an invaluable tool in studying polluted and/or salt-impacted waters. Analysis of water salinity has commonly used electrical conductance (EC); however, the identity of the elements responsible for the salinity are not revealed using EC. Several studies have established the viability of using portable X-ray fluorescence (PXRF) spectrometry for elemental data 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 used PXRF elemental data in water samples to predict water EC. A total of 256 water samples, from 10 different countries were collected and analyzed via PXRF, inductively coupled plasma atomic emission spectroscopy (ICP-AES), and a digital salinity bridge. The PXRF detected some elements more effectively than others, but overall results indicated that PXRF can successfully predict water EC via quantifying Cl in water samples (validation R2 and RMSE of 0.77 and 0.95 log μS cm-1, respectively). The findings of this study elucidated the potential of PXRF for future analysis of pollutant and/or metal contaminated waters.
Effect of [Li]/[Nb] ratio on composition and defect structure of Zr:Yb:Tm:LiNbO3 crystals

NASA Astrophysics Data System (ADS)

Liu, Chunrui; Dai, Li; Wang, Luping; Shao, Yu; Yan, Zhehua; Xu, Yuheng

2018-04-01

Zr:Yb:Tm:LiNbO3 crystals with various [Li]/[Nb] ratios (0.946, 1.05, 1.20 and 1.38) were grown by the Czochralski technique. Distribution coefficients of Zr4+, Yb3+ and Tm3+ ions were analyzed by the inductively coupled plasma-atomic emission spectrometer (ICP-AES). The influence of [Li]/[Nb] ratio on the composition and defect structure of Zr:Yb:Tm:LiNbO3 crystals was investigated by X-ray diffraction and IR transmission spectrum. The results show that as the [Li]/[Nb] ratio increases in the melt, the distribution coefficients of Yb3+ and Tm3+ ions both increase while that of Zr4+ ion deceases. When the [Li]/[Nb] ratio increases to 1.20 in the melt, Zr:Yb:Tm:LiNbO3 crystal is nearly stoichiometric. In addition, when the [Li]/[Nb] ratio reaches up to 1.38, NbLi4+ are completely replaced and Li+ starts to impel the Zr4+, Yb3+ and Tm3+ into the normal Li sites.
Application of solid phase extraction on multiwalled carbon nanotubes of some heavy metal ions to analysis of skin whitening cosmetics using ICP-AES.

PubMed

Alqadami, Ayoub A; Abdalla, Mohammad Abulhassan; AlOthman, Zeid A; Omer, Kamal

2013-01-14

A novel and highly sensitive method for the determination of some heavy metals in skin whitening cosmetics creams using multiwalled carbon nanotubes MWCNTs as solid phase extraction sorbent for the preconcentration of these heavy metals prior to their determination by inductively coupled plasma atomic emission spectrometry is described. Different practical parameters have been thoroughly investigated and the optimum experimental conditions were employed. The developed method was then applied for the determination of arsenic, bismuth, cadmium, mercury, lead and titanium in samples of skin whitening cosmetics. The detection limits under these conditions for As, Bi, Cd, Pb, Hg and Ti were 2.4, 4.08, 0.3, 2.1, 1.8, and 1.8 ng·mL-1, respectively. The relative standard deviations (RSDs) were found to be less than 2.0%. For validation, a certified reference material of NIST SRM 1570a spinach leaves was analyzed and the determined values were in good agreement with the certified values. The recoveries for spiked samples were found to be in the range of 89.6-104.4%.
Multifunctional Fe3O4/ZnO nanocomposites with magnetic and optical properties.

PubMed

Zou, Peng; Hong, Xia; Chu, Xueying; Li, Yajun; Liu, Yichun

2010-03-01

Multifunctional Fe3O4/ZnO nanocomposites were successfully synthesized through two-step solution-based methods. Fe3O4 nanoparticles were used as seeds for the deposit and growth of ZnO nanocrystals. Transmission electron microscopy (TEM) images, X-ray diffraction (XRD) patterns, and inductively coupled plasma-atomic emission spectroscopy (ICP-AES) were employed to observe the morphology, size, structure, and crystalline phase of the nanocomposites and confirm their chemical composition. The results of magnetization curves, resonant Raman scattering, and photoluminescence spectra revealed that the nanocomposites simultaneously possessed the super-paramagnetism of Fe3O4 and the multiphonon resonant Raman scattering and photoluminescence (PL) properties of ZnO. Compared with that of pure Fe3O4, the saturation magnetization of the Fe3O4 component within the nanocomposites was enhanced. The Raman spectroscopic fingerprint of ZnO component was preserved, and the fluorescent background was efficiently reduced. The interfacial effect was found to play an important role in modulating or improving the properties of the nanocomposites.
Estimation of daily aluminum intake in Japan based on food consumption inspection results: impact of food additives

PubMed Central

Sato, Kyoko; Suzuki, Ippei; Kubota, Hiroki; Furusho, Noriko; Inoue, Tomoyuki; Yasukouchi, Yoshikazu; Akiyama, Hiroshi

2014-01-01

Dietary aluminum (Al) intake by young children, children, youths, and adults in Japan was estimated using the market basket method. The Al content of food category (I–VII) samples for each age group was determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The Al content in processed foods and unprocessed foods ranged from 0.40 to 21.7 mg/kg and from 0.32 to 0.54 mg/kg, respectively. For processed foods in all age groups, the Al content in food category VI samples, sugar and confections/savories, was the highest, followed by those in category II, cereals. The daily dietary Al intake from processed foods was much larger than that from unprocessed foods. The mean weekly percentages of the provisional tolerable weekly intake (PTWI, established by the joint FAO/WHO Expert Committee on Food Additives in 2011) from processed foods for all age groups are 43.1, 22.4, 17.6 and 15.1%, respectively. Only the highest consumer Al exposure value (>P95) of the young children group exceeded the PTWI. PMID:25473496
Profile of Trace Elements in Selected Medicinal Plants Used for the Treatment of Diabetes in Eritrea

PubMed Central

Kareru, Patrick; Keriko, Joseph; Girmay, Berhane; Medhanie, Ghebrehiwet; Debretsion, Semere

2016-01-01

This study was designed to investigate the profile of certain trace elements having therapeutic properties related to diabetes mellitus. The investigated plants were Aloe camperi, Meriandra dianthera, Lepidium sativum, Brassica nigra, and Nigella sativa. These plants are traditionally used in the management of diabetes in Eritrea. The elemental analysis was conducted using inductively coupled plasma optical emission spectrometry (ICP-OES) and flame atomic absorption spectroscopy (FAAS) techniques. The accuracy of the methods was verified using in-house reference materials (CRMs) and no significant differences were observed between the measured and certified values. The analysis displayed variable concentrations of the different trace elements including Zn, Cr, V, Mn, and Se in the plants. Moreover, the levels of major elements, such as Mg, Ca, K, Na, and Ba, and heavy metals, such as Fe, Cu, Ni, Co, As, and Pb, were determined and found to be in the permissible limit defined by WHO. Among the plants, Meriandra dianthera showed the highest levels of Mn, Cr, V, and other elements and the values were significantly different (P < 0.05). PMID:27795982
Profile of Trace Elements in Selected Medicinal Plants Used for the Treatment of Diabetes in Eritrea.

PubMed

Sium, Mussie; Kareru, Patrick; Keriko, Joseph; Girmay, Berhane; Medhanie, Ghebrehiwet; Debretsion, Semere

This study was designed to investigate the profile of certain trace elements having therapeutic properties related to diabetes mellitus. The investigated plants were Aloe camperi , Meriandra dianthera , Lepidium sativum , Brassica nigra, and Nigella sativa . These plants are traditionally used in the management of diabetes in Eritrea. The elemental analysis was conducted using inductively coupled plasma optical emission spectrometry (ICP-OES) and flame atomic absorption spectroscopy (FAAS) techniques. The accuracy of the methods was verified using in-house reference materials (CRMs) and no significant differences were observed between the measured and certified values. The analysis displayed variable concentrations of the different trace elements including Zn, Cr, V, Mn, and Se in the plants. Moreover, the levels of major elements, such as Mg, Ca, K, Na, and Ba, and heavy metals, such as Fe, Cu, Ni, Co, As, and Pb, were determined and found to be in the permissible limit defined by WHO. Among the plants, Meriandra dianthera showed the highest levels of Mn, Cr, V, and other elements and the values were significantly different ( P < 0.05).
DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

The methods cover: C in solutions, F (electrode), elements by atomic emission spectrometry, inorganic anions by ion chromatography, Hg in water/solids/sludges, As, Se, Bi, Pb, data calculations for SST (single shell tank?) samples, Sb, Tl, Ag, Pu, O/M ratio, ignition weight loss, pH value, ammonia (N), Cr(VI), alkalinity, U, C sepn. from soil/sediment/sludge, Pu purif., total N, water, C and S, surface Cl/F, leachable Cl/F, outgassing of Ge detector dewars, gas mixing, gas isotopic analysis, XRF of metals/alloys/compounds, H in Zircaloy, H/O in metals, inpurity extraction, reduced/total Fe in glass, free acid in U/Pu solns, density of solns, Kr/Xe isotopesmore » in FFTF cover gas, H by combustion, MS of Li and Cs isotopes, MS of lanthanide isotopes, GC operation, total Na on filters, XRF spectroscopy QC, multichannel analyzer operation, total cyanide in water/solid/sludge, free cyanide in water/leachate, hydrazine conc., ICP-MS, {sup 99}Tc, U conc./isotopes, microprobe analysis of solids, gas analysis, total cyanide, H/N{sub 2}O in air, and pH in soil.« less
Baseline study on essential and trace elements in polished rice from South Korea.

PubMed

Jung, Myung Chae; Yun, Seong-Taek; Lee, Jin-Soo; Lee, Jong-Un

2005-09-01

In 2000, 63 (polished) white rice samples were collected in eight administrative areas all over South Korea and analyzed for 16 elements by inductively coupled plasma atomic emission spectrometry (ICP-AES). Potassium had the highest content, next to Mg, Ca, Si, Zn, Na, Al and Fe. Most of the samples contained worldwide average concentrations of essential and trace elements in rice grains reported by various researches. For inter-area differences in those elements in the rice, the statistical analysis showed no significant differences (p > 0.05) among the eight administrative areas, suggesting that inter-area differences were not substantial in most cases. Thus, the present data can be used as national background levels of elements in rice produced in South Korea. Using the published data on daily consumption of rice in South Korea, it was possible to estimate the daily intake of As, Cd, Cu, Pb and Zn via rice. The results showed that a regular consumption of rice produced in Korea plays an important role in accumulation of essential and trace elements in Korean, especially for farm-households consuming relatively large amounts of rice.
[Analysis of biological material originating from the body of general Władysław Sikorski for inorganic poisons and diatoms presence].

PubMed

Sadlik, Józefa Krystyna; Brozek-Mucha, Zuzanna

2009-01-01

Results of the analysis of biological materials originating from the body of general Sikorski are presented in the paper. Samples of the liver, kidney, intestine and lung were analysed for metals and As content, and samples of the lung, liver, kidney, stomach, intestine and bone marrow--for diatoms presence. The analysis for metals and As was performed by atomic absorption spectrometry (AAS) and inductively coupled plasma optical emission spectrometry (ICP-OES). Before the analysis, the samples were wet digested by the classic and microwave assisted method. The analysis did not result in detecting the presence of As, Co, Ni, and Tl in any of the studied materials, while Hg was not revealed in the liver, intestines and lung and Pb in the intestines and lung. The content of Ba, Cd, Cr, Cu, Fe, Mn, Sr and Zn in all the studied materials, Hg in the kidney, and Pb in the liver and kidney did not indicate poisoning by the above-mentioned metals or arsenic. No diatoms were found in the studied materials.
Selective precipitation of potassium in seawater samples for improving the sensitivity of plain γ-ray spectrometry

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

Ferrante, Marco, E-mail: marco.ferrante@lngs.infn.it; De Angelis, Francesco, E-mail: francesco.deangelis@univaq.it; Nisi, Stefano, E-mail: stefano.nisi@lngs.infn.it

2015-08-17

An analytical method is presented to reduce the amount of {sup 40}K in sea water samples, in order to lower its interference in γ-ray analysis below 1.4 MeV due to the Compton continuum. Sodium tetraphenylborate was used to successfully precipitate {sup 40}K in the samples. A custom procedure for precipitation of potassium was developed and it was evaluated for its selectivity, reproducibility and efficiency, using conventional analytical techniques such as atomic absorption spectrophotometry and inductively coupled plasma mass spectrometry (ICP-MS). This work has shown that the selective precipitation of potassium with sodium tetraphenylborate has led to a decrease of detectionmore » limit of radio nuclides such as {sup 238}U, {sup 226}Ra, {sup 228}Ra, {sup 137}Cs, {sup 134}Cs, {sup 133}I, {sup 134}I, {sup 60}Co in γ-analysis. In particular, the detection limit for nuclides with emissions in the energy window energy below 1400 keV is improved by almost one order of magnitude.« less
Cobalt-cadmium bimetallic porphyrin coordination polymers for electrochemistry application

NASA Astrophysics Data System (ADS)

Wang, C. Y.; Cui, G. Y.; Ding, D.; Zhou, B.

2018-01-01

In this paper, we used tetra (4-carboxyphenyl) porphyrin (H2TCPP) and metal cadmium, cobalt as reactants to synthesize metal porphyrin coordination polymers that they had different metal ratio. They were expressed as Co1Cd3TCPP, Co1Cd1TCPP, Co3Cd1TCPP, respectively. The results were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and inductively coupled plasma atomic emission spectrometer (ICP). Herein, a series of metal porphyrin coordination polymers has multiple metal active centers and constructs electrochemistry sensors. In order to increase the conductivity, multi-walled carbon nanotubes (MWCNTs) can be used to modify the electrodes. The polymer/MWCNTs/GCE electrode was studied by cyclic voltammetry and chronoamperometry as sensor for sodium nitrite. The performance of Co1Cd1TCPP/MWCNTs/GCE electrode is best, the sensitivity for sodium nitrite is 350.95 mA M-1 cm-2 and the. The results indicate that metal porphyrin coordination polymers have excellent performance. It also enriches the application of metal porphyrin coordination polymer in electrochemistry sensor.
Bioimaging of metallothioneins in ocular tissue sections by laser ablation-ICP-MS using bioconjugated gold nanoclusters as specific tags.

PubMed

Cruz-Alonso, María; Fernandez, Beatriz; Álvarez, Lydia; González-Iglesias, Héctor; Traub, Heike; Jakubowski, Norbert; Pereiro, Rosario

2017-12-18

An immunohistochemical method is described to visualize the distribution of metallothioneins 1/2 (MT 1/2) and metallothionein 3 (MT 3) in human ocular tissue. It is making use of (a) antibodies conjugated to gold nanoclusters (AuNCs) acting as labels, and (b) laser ablation (LA) coupled to inductively coupled plasma - mass spectrometry (ICP-MS). Water-soluble fluorescent AuNCs (with an average size of 2.7 nm) were synthesized and then conjugated to antibody by carbodiimide coupling. The surface of the modified AuNCs was then blocked with hydroxylamine to avoid nonspecific interactions with biological tissue. Immunoassays for MT 1/2 and MT 3 in ocular tissue sections (5 μm thick) from two post mortem human donors were performed. Imaging studies were then performed by fluorescence using confocal microscopy, and LA-ICP-MS was performed in the retina to measure the signal for gold. Signal amplification by the >500 gold atoms in each nanocluster allowed the antigens (MT 1/2 and MT 3) to be imaged by LA-ICP-MS using a laser spot size as small as 4 μm. The image patterns found in retina are in good agreement with those obtained by conventional fluorescence immunohistochemistry which was used as an established reference method. Graphical abstract Gold nanoclusters (AuNCs) conjugated to a primary specific antibody serve as a label for amplified bioimaging of metallothioneins (MTs) by laser ablation coupled to inductively coupled plasma - mass spectrometry (ICP-MS) in human ocular tissue sections.
The astrophysics of the intracluster plasma

NASA Astrophysics Data System (ADS)

Cavaliere, Alfonso; Lapi, Andrea

2013-12-01

Since 1971 observations in X rays of several thousands of galaxy clusters have uncovered huge amounts of hot baryons filling up the deep gravitational potential wells provided by dark matter (DM) halos with masses of some 1015 M⊙ and sizes of millions of light-years. At temperatures T˜108 K and with average densities of n˜1 particle per liter, such baryons add up to some 1014 M⊙. With the neutralizing electrons, they constitute the best proton-electron plasma in the Universe (whence the apt name Intra Cluster Plasma, ICP), one where the thermal energy per particle overwhelms the electron-proton Coulomb interaction by extralarge factors of order 1012. The ICP shines in X rays by thermal bremsstrahlung radiation, with powers up to several 1045erg s-1 equivalent to some 1011 solar luminosities. The first observations were soon confirmed in X rays by the detection of high excitation emission lines, and in the radio band by studies of streamlined radiogalaxies moving through the ICP. Later on they were nailed down by the first measurements in microwaves of the Sunyaev-Zel’dovich effect, i.e., the inverse Compton upscattering of cold cosmic background photons at T≈2.73 K off the hot ICP electrons at kBT˜5 keV. A key physical feature of the ICP is constituted by its good local thermal equilibrium, and by its overall hydrostatic condition in the DM wells, modulated by entropy. The latter is set up in the cluster center by the initial halo collapse, and is progressively added at the outgrowing cluster boundary by standing shocks in the supersonic flow of intergalactic gas into the DM potential wells. Such physical conditions are amenable to detailed modeling. We review here these entropy-based models and discuss their outcomes and predictions concerning the ICP observables in X rays and in microwaves, as well as the underlying DM parameters. These quantitative outcomes highlight the tight relationship between the detailed ICP profiles and the cosmological evolution of the containing DM potential wells. The results also provide the simplest baseline for disentangling a number of additional and intriguing physical processes superposed to the general equilibrium. The present Report is focused on the ICP physics as driven by the two-stage evolution of the containing DM halos. We extensively discuss the basic entropy pattern established by the cluster formation and development, and cover: the central entropy erosion produced by radiative cooling that competes with the intermittent energy inputs due to active galactic nuclei and mergers; outer turbulent support linked with weakening shocks and decreasing inflow through the virial boundary, causing reduced entropy production during the late stage of DM halo evolution; the development from high to low entropy levels throughout a typical cluster; perturbations of the equilibrium up to outright disruption due to deep impacts of infalling galaxy groups or collisions with comparable companion clusters; relativistic energy distributions of electrons accelerated during such events, producing extended radio emission by synchrotron radiation and contributing non thermal pressure support for the ICP. We conclude with discussing selected contributions from cluster astrophysics to cosmology at large, and by addressing how the ICP features and processes will constitute enticing targets for observations with the ongoing Planck mission, for upcoming instrumentation like ALMA and other ground-based radio observatories, and for the next-generation of X-ray satellites from ASTRO-H to eROSITA.

Uniformity studies of inductively coupled plasma etching in fabrication of HgCdTe detector arrays

NASA Astrophysics Data System (ADS)

Bommena, R.; Velicu, S.; Boieriu, P.; Lee, T. S.; Grein, C. H.; Tedjojuwono, K. K.

2007-04-01

Inductively coupled plasma (ICP) chemistry based on a mixture of CH 4, Ar, and H II was investigated for the purpose of delineating HgCdTe mesa structures and vias typically used in the fabrication of second and third generation infrared photo detector arrays. We report on ICP etching uniformity results and correlate them with plasma controlling parameters (gas flow rates, total chamber pressure, ICP power and RF power). The etching rate and surface morphology of In-doped MWIR and LWIR HgCdTe showed distinct dependences on the plasma chemistry, total pressure and RF power. Contact stylus profilometry and cross-section scanning electron microscopy (SEM) were used to characterize the anisotropy of the etched profiles obtained after various processes and a standard deviation of 0.06 μm was obtained for etch depth on 128 x 128 format array vias. The surface morphology and the uniformity of the etched surfaces were studied by plan view SEM. Atomic force microscopy was used to make precise assessments of surface roughness.
The determination of trace elements in crude oil and its heavy fractions by atomic spectrometry

NASA Astrophysics Data System (ADS)

Duyck, Christiane; Miekeley, Norbert; Porto da Silveira, Carmem L.; Aucélio, Ricardo Q.; Campos, Reinaldo C.; Grinberg, Patrícia; Brandão, Geisamanda P.

2007-09-01

A literature review on the determination of trace elements in crude oil and heavy molecular mass fractions (saturates, aromatics, resins and asphaltenes) by ICP-MS, ICP OES and AAS is presented. Metal occurrences, forms and distributions are examined as well as their implications in terms of reservoir geochemistry, oil refining and environment. The particular analytical challenges for the determination of metals in these complex matrices by spectrochemical techniques are discussed. Sample preparation based on ashing, microwave-assisted digestion and combustion decomposition procedures is noted as robust and long used. However, the introduction of non-aqueous solvents and micro-emulsions into inductively coupled plasmas is cited as a new trend for achieving rapid and accurate analysis. Separation procedures for operationally defined fractions in crude oil are more systematically applied for the observation of metal distributions and their implications. Chemical speciation is of growing interest, achieved by the coupling of high efficiency separation techniques (e.g., HPLC and GC) to ICP-MS instrumentation, which allows the simultaneous determination of multiple organometallic species of geochemical and environmental importance.
Comparison of ultrasonic and thermospray systems for high performance sample introduction to inductively coupled plasma atomic emission spectrometry

NASA Astrophysics Data System (ADS)

Conver, Timothy S.; Koropchak, John A.

1995-06-01

This paper describes detailed work done in our lab to compare analytical figures of merit for pneumatic, ultrasonic and thermospray sample introduction (SI) systems with three different inductively coupled plasma-atomic emission spectrometry (ICP-AES) instruments. One instrument from Leeman Labs, Inc. has an air path echelle spectrometer and a 27 MHz ICP. For low dissolved solid samples with this instrument, we observed that the ultrasonic nebulizer (USN) and fused silica aperture thermospray (FSApT) both offered similar LOD improvements as compared to pneumatic nebulization (PN), 14 and 16 times, respectively. Average sensitivities compared to PN were better for the USN, by 58 times, compared to 39 times for the FSApT. For solutions containing high dissolved solids we observed that FSApT optimized at the same conditions as for low dissolved solids, whereas USN required changes in power and gas flows to maintain a stable discharge. These changes degraded the LODs for USN substantially as compared to those utilized for low dissolved solid solutions, limiting improvement compared to PN to an average factor of 4. In general, sensitivities for USN were degraded at these new conditions. When solutions with 3000 μg/g Ca were analyzed, LOD improvements were smaller for FSApT and USN, but FSApT showed an improvement over USN of 6.5 times. Sensitivities compared to solutions without high dissolved solids were degraded by 19% on average for FSApT, while those for USN were degraded by 26%. The SI systems were also tested with a Varian Instruments Liberty 220 having a vacuum path Czerny-Turner monochromator and a 40 MHz generator. The sensitivities with low dissolved solids solutions compared to PN were 20 times better for the USN and 39 times better for FSApT, and LODs for every element were better for FSApT. Better correlation between relative sensitivities and anticipated relative analyte mass fluxes for FSApT and USN was observed with the Varian instrument. LOD improvements averaged 18 times lower than PN with FSApT while with USN values averaged 8 times lower. When solutions with high dissolved solids were studied it was found that FSApT still offered 5.5 times better LODs than PN and USN offered 4.6 times better LODs than PN. Sensitivities for FSApT averaged 20 times better, while those for USN were 13 times better compared to PN. Finally, background RSDs on the Varian system were generally higher for FSApT than for the USN for similar sample types. A third instrument used for a small set of elements was a Perkin-Elmer model 5500 ICP-AES. This system has a 27 MHz generator with a N 2 purged Czerny-Turner monochromator. LOD trends, background RSDs, and sensitivities were similar to those with the Leeman instrument. However, matrix effects more closely resembled those seen with the Varian instrument for both SI systems. To compare performance and recoveries on a real sample, a National Institute of Standards and Technology, Standard Reference Material 1643c trace elements in water, was analyzed using the Varian system and it was found that both SI systems offered similar recoveries.
Development of routines for simultaneous in situ chemical composition and stable Si isotope ratio analysis by femtosecond laser ablation inductively coupled plasma mass spectrometry.

PubMed

Frick, Daniel A; Schuessler, Jan A; von Blanckenburg, Friedhelm

2016-09-28

Stable metal (e.g. Li, Mg, Ca, Fe, Cu, Zn, and Mo) and metalloid (B, Si, Ge) isotope ratio systems have emerged as geochemical tracers to fingerprint distinct physicochemical reactions. These systems are relevant to many Earth Science questions. The benefit of in situ microscale analysis using laser ablation (LA) over bulk sample analysis is to use the spatial context of different phases in the solid sample to disclose the processes that govern their chemical and isotopic compositions. However, there is a lack of in situ analytical routines to obtain a samples' stable isotope ratio together with its chemical composition. Here, we evaluate two novel analytical routines for the simultaneous determination of the chemical and Si stable isotope composition (δ(30)Si) on the micrometre scale in geological samples. In both routines, multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) is combined with femtosecond-LA, where stable isotope ratios are corrected for mass bias using standard-sample-bracketing with matrix-independent calibration. The first method is based on laser ablation split stream (LASS), where the laser aerosol is split and introduced simultaneously into both the MC-ICP-MS and a quadrupole ICP-MS. The second method is based on optical emission spectroscopy using direct observation of the MC-ICP-MS plasma (LA-MC-ICP-MS|OES). Both methods are evaluated using international geological reference materials. Accurate and precise Si isotope ratios were obtained with an uncertainty typically better than 0.23‰, 2SD, δ(30)Si. With both methods major element concentrations (e.g., Na, Al, Si, Mg, Ca) can be simultaneously determined. However, LASS-ICP-MS is superior over LA-MC-ICP-MS|OES, which is limited by its lower sensitivity. Moreover, LASS-ICP-MS offers trace element analysis down to the μg g(-1)-range for more than 28 elements due to lower limits of detection, and with typical uncertainties better than 15%. For in situ simultaneous stable isotope measurement and chemical composition analysis LASS-ICP-MS in combination with MC-ICP-MS is the method of choice. Copyright © 2016 Elsevier B.V. All rights reserved.
LIBS coupled with ICP/OES for the spectral analysis of betel leaves

NASA Astrophysics Data System (ADS)

Rehan, I.; Rehan, K.; Sultana, S.; Khan, M. Z.; Muhammad, R.

2018-05-01

Laser-induced breakdown spectroscopy (LIBS) system was optimized and was applied for the elemental analysis and exposure of the heavy metals in betel leaves in air. Pulsed Nd:YAG (1064 nm) in conjunction with a suitable detector (LIBS 2000+, Ocean Optics, Inc) having the optical resolution of 0.06 nm was used to record the emission spectra from 200 to 720 nm. Elements like Al, Ba, Ca, Cr, Cu, P, Fe, K, Mg, Mn, Na, P, S, Sr, and Zn were found to be present in the samples. The abundances of observed elements were calculated through normalized calibration curve method, integrated intensity ratio method, and calibration free-LIBS approach. Quantitative analyses were accomplished under the assumption of local thermodynamic equilibrium (LTE) and optically thin plasma. LIBS findings were validated by comparing its results with the results obtained using a typical analytical technique of inductively coupled plasma-optical emission spectroscopy (ICP/OES). Limit of detection (LOD) of the LIBS system was also estimated for heavy metals.
Newly Developed Biocompatible Material: Dispersible Titanium-Doped Hydroxyapatite Nanoparticles Suitable for Antibacterial Coating on Intravascular Catheters.

PubMed

Furuzono, Tsutomu; Okazaki, Masatoshi; Azuma, Yoshinao; Iwasaki, Mitsunobu; Kogai, Yasumichi; Sawa, Yoshiki

2017-01-01

Thirteen patients with chlorhexidine-silver sulfadiazine-impregnated catheters have experienced serious anaphylactic shock in Japan. These adverse reactions highlight the lack of commercially available catheters impregnated with strong antibacterial chemical agents. A system should be developed that can control both biocompatibility and antibacterial activity. Hydroxyapatite (HAp) is biocompatible with bone and skin tissues. To provide antibacterial activity by using an external physical stimulus, titanium (Ti) ions were doped into the HAp structure. Highly dispersible, Ti-doped HAp (Ti-HAp) nanoparticles suitable as a coating material were developed. In 3 kinds of Ti-HAp [Ti/(Ca + Ti) = 0.05, 0.1, 0.2], the Ti content in the HAp was approximately 70% of that used in the Ti-HAp preparation, as determined by inductively coupled plasma atomic emission spectroscopy (ICP-AES). ICP-AES and X-ray diffraction showed Ti ions were well substituted into the HAp lattice. The nanoparticles were almost uniformly coated on a polyethylene (PE) sheet in a near-monolayer with a surface coverage ratio >95%. The antibacterial activity of the Ti-HAp nanoparticles containing 7.3% Ti ions and coating the sheet was evaluated by calculating the survival ratio of Pseudomonas aeruginosa on the coated sheet after ultraviolet (UV) irradiation. The Ti-HAp-coated sheet showed a 50% decrease in the number of P. aeruginosa compared with that on an uncoated control PE sheet after UV irradiation for 30 s. Key Messages: A system of biocompatibility and antibacterial activity with an on/off switch controlled by external UV stimulation was developed. The system is expected to be applicable in long-term implanted intravascular catheters. © 2017 S. Karger AG, Basel.
Sepsis does not alter red blood cell glucose metabolism or Na+ concentration: A 2H-, 23Na-NMR study

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

Hotchkiss, R.S.; Song, S.K.; Ling, C.S.

The effects of sepsis on intracellular Na+ concentration ((Na+)i) and glucose metabolism were examined in rat red blood cells (RBCs) by using 23Na- and 2H-nuclear magnetic resonance (NMR) spectroscopy. Sepsis was induced in 15 halothane-anesthetized female Sprague-Dawley rats by using the cecal ligation and perforation technique; 14 control rats underwent cecal manipulation without ligation. The animals were fasted for 36 h, but allowed free access to water. At 36 h postsurgery, RBCs were examined by 23Na-NMR by using dysprosium tripolyphosphate as a chemical shift reagent. Human RBCs from 17 critically ill nonseptic patients and from 7 patients who were diagnosedmore » as septic were also examined for (Na+)i. Five rat RBC specimens had (Na+)i determined by both 23Na-NMR and inductively coupled plasma-atomic emission spectroscopy (ICP-AES). For glucose metabolism studies, RBCs from septic and control rats were suspended in modified Krebs-Henseleit buffer containing (6,6-2H2)glucose and examined by 2H-NMR. No significant differences in (Na+)i or glucose utilization were found in RBCs from control or septic rats. There were no differences in (Na+)i in the two groups of patients. The (Na+)i determined by NMR spectroscopy agreed closely with measurements using ICP-AES and establish that 100% of the (Na+)i of the RBC is visible by NMR. Glucose measurements determined by 2H-NMR correlated closely (correlation coefficient = 0.93) with enzymatic analysis. These studies showed no evidence that sepsis disturbed RBC membrane function or metabolism.« less
[Determination of Mineral Elements in Choerospondias Axillaris and Its Extractives by ICP-AES].

PubMed

Zhai, Yu-xin; Chen, Jun; Li, Ti; Liu, Ji-yan; Wang, Xie-yi; Cheng, Chao; Liu, Cheng-mei

2015-04-01

Nine elements in Choerospondias axillaris flesh, peels, aqueous extractives and gastric digesta were determined by the inductively coupled plasma atomic emission spectrometry (ICP-AES) in the present study. The results showed that the contents of Fe, Ca, Zn, Mn, Al, Mg, Cu, K and P in the flesh were 27.37, 269.88, 1.51, 2.45, 1.95, 195.30, 2.45, 2,970.11, and 133.94 µg · g(-1), respectively. They are lower than that in the peels, about 40.31%, 11.70%, 21.68%, 4.27%, 10.58%, 15.76%, 68.72%, 42.04%, and 22.59%, respectively. For microwave assistant extraction, the release rate of Mn was highest (81.68%), while Fe was lowest (4.42%) in the flesh. The release rate of Zn was the highest (79.00%), while that of A1 was the lowest (4.94%) in the peels. Except Fe, Cu and Zn, the release rates of the other elements in flesh were higher than those in the peels. After gastric digestion, the release rates of nine elements were 3.25%-87.51% in the flesh and 7.11%-50.69% in the peels. The release rates of minerals in the flesh were found to be higher than those in the peels except Fe and Cu. Microwave assistant extraction can more efficiently release Fe, Ca, Mn, Mg and K from the flesh than the gastric digestion do. While gastric digestion had a significant effect on the peels, the release rates of elements, except Zn, were higher than those in microwave assistant extraction. Therefore, the difference of distribution and release of mineral elements between peels and flesh of Choerospondias axillaris was understood, which will provide a positive guide for further study of bioavailability of minerals for human body.
[Mineral elements analysis of Momordica charantiap seeds by ICP-AES and fatty acid profile identification of seed oil by GC-MS].

PubMed

Liu, Xiao-ru; Deng, Ze-yuan; Fan, Ya-wei; Li, Jing; Liu, Zhi-han

2010-08-01

In the present study, a special kind of Momordica charantia seeds produced in Hai Nan was selected and analyzed. Firstly, inductively coupled plasma-atomic emission spectrophotometry (ICP-AES) was used to determine the mineral elements. It was clear that the contents of K, Mg and P are the highest in the seeds; Cr and Zn takes up to 5.65% and 45.45% high, especially, which are rare in plant foods. These minerals, especially Cr and Zn might have a complex effect on those proteins or polysaccharides and form a stronger anticipation of hyperlipidemia, hyperglycemia and cholesterol. Secondly, seed oil was extracted by supercritical CO2 extraction with a yield ratio of 36.89, and the fatty acids were treated by methylation in alkaline process and purified by thin-layer chromatography, then analyzed by gas chromatography-mass spectrometer (GC-MS) identification. The saturated fatty acids (SFA) take up 36.712, and mainly are stearic acid; monounsaturated fatty acid (MUFA) is only 3.33% which is dominantly linoleic acid (LA); Polyunsaturated fatty acid (PUFA) accounted for 59.96%, and the alpha-eleostearic acid takes up 54.26% as the main fatty acids in all. The plentiful alpha-eleostearic acid leads to strong effects of inhibiting tumor cell proliferation, lowering blood fat, anti-cancer, anti-inflammatory and preventing cardiovascular diseases, and so on. Knowing clearly the mineral elements distribution and identifying the composition of fatty acid, especially the main fatty acids in the oil, are both of great guiding importance to further exploit the clinical and edible value in Momordica charantiap seeds.
Phenolics and essential mineral profile of organic acid pretreated unripe banana flour.

PubMed

Anyasi, Tonna A; Jideani, Afam I O; Mchau, Godwin R A

2018-02-01

Banana fruit (Musa spp) though rich in essential minerals, has also been implicated for the presence of phytochemicals which nonetheless beneficial, can also act as mineral inhibitors when in forms such as phenolic compounds, phytates and tannins. This study assayed the essential macro and trace minerals as well as phenolic compounds present in unripe banana flour (UBF) obtained from the pulp of four different cultivars. Unripe banana flour was processed by oven drying in a forced air oven dryer at 70°C upon pretreatment with ascorbic, citric and lactic acid. Organic acid pretreatment was done separately on each unripe banana cultivar at concentrations of 10, 15 and 20g/L. Phenolic compounds were profiled using liquid chromatography mass spectrometry electrospray ion (LC-MS-ESI) while essential minerals were determined using inductively coupled plasma atomic emission spectroscopy (ICP-AES) and mass spectroscopy (ICP-MS) respectively. Results of LC-MS-ESI assay of phenolics revealed the presence of flavonoids: epicatechin and myricetin 3-O-rhamnosyl-glucoside in varying concentrations in UBF. Essential mineral profile indicated that Zinc had the least occurrence of 3.55mg/kg (p<0.05), while potassium was the most abundant mineral at 14746.73mg/kg in UBF of all four banana cultivars. Correlation between phenolic compounds and essential minerals using Pearson's Correlation Coefficient test revealed weak and inverse association between flavonoids and most macro and trace minerals present in UBF samples. Organic acid pretreatment thus exhibited little effect on phenolics and essential minerals of UBF samples, though, inhibitory influence of phenolic compounds was recorded on essential minerals. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.
Determination of 18 kinds of trace impurities in the vanadium battery grade vanadyl sulfate by ICP-OES

NASA Astrophysics Data System (ADS)

Yong, Cheng

2018-03-01

The method that direct determination of 18 kinds of trace impurities in the vanadium battery grade vanadyl sulfate by inductively coupled plasma atomic emission spectrometry (ICP-OES) was established, and the detection range includes 0.001% ∼ 0.100% of Fe, Cr, Ni, Cu, Mn, Mo, Pb, As, Co, P, Ti, Zn and 0.005% ∼ 0.100% of K, Na, Ca, Mg, Si, Al. That the influence of the matrix effects, spectral interferences and background continuum superposition in the high concentrations of vanadium ions and sulfate coexistence system had been studied, and then the following conclusions were obtained: the sulfate at this concentration had no effect on the determination, but the matrix effects or continuous background superposition which were generated by high concentration of vanadium ions had negative interference on the determination of potassium and sodium, and it produced a positive interference on the determination of the iron and other impurity elements, so that the impacts of high vanadium matrix were eliminated by the matrix matching and combining synchronous background correction measures. Through the spectral interference test, the paper classification summarized the spectral interferences of vanadium matrix and between the impurity elements, and the analytical lines, the background correction regions and working parameters of the spectrometer were all optimized. The technical performance index of the analysis method is that the background equivalent concentration -0.0003%(Na)~0.0004%(Cu), the detection limit of the element is 0.0001%∼ 0.0003%, RSD<10% when the element content is in the range from 0.001% to 0.007%, RSD< 20% even if the element content is in the range from 0.0001% to 0.001% that is beyond the scope of the method of detection, recoveries is 91.0% ∼ 110.0%.
Analytical Results for 42 Fluvial Tailings Cores and 7 Stream Sediment Samples from High Ore Creek, Northern Jefferson County, Montana

USGS Publications Warehouse

Fey, David L.; Church, Stan E.

1998-01-01

Metal-mining related wastes in the Boulder River basin study area in northern Jefferson County, Montana have been implicated in their detrimental effects on water quality with regard to acid-generation and toxic-metal solubility. Sediments, fluvial tailings and water from High Ore Creek have been identified as significant contributors to water quality degradation of the Boulder River below Basin, Montana. A study of 42 fluvial tailings cores and 7 stream sediments from High Ore Creek was undertaken to determine the concentrations of environmentally sensitive elements (i.e. Ag, As, Cd, Cu, Pb, Zn) present in these materials, and the mineral phases containing those elements. Two sites of fluvial deposition of mine-waste contaminated sediment on upper High Ore Creek were sampled using a one-inch soil probe. Forty-two core samples were taken producing 247 subsamples. The samples were analyzed by ICP-AES (inductively coupled-plasma atomic emission spectroscopy) using a total mixed-acid digestion. Results of the core analyses show that the elements described above are present at very high concentrations (to 22,000 ppm As, to 460 ppm Ag, to 900 ppm Cd, 4,300 ppm Cu, 46,000ppm Pb, and 50,000 ppm Zn). Seven stream-sediment samples were also analyzed by ICP-AES for total element content and for leachable element content. Results show that the sediment of High Ore Creek has elevated levels of ore-related metals throughout its length, down to the confluence with the Boulder River, and that the metals are, to a significant degree, contained in the leachable phase, namely the hydrous amorphous iron- and manganese-hydroxide coatings on detrital sediment particles.
Geochemistry of rare earth elements in Permian coals from the Huaibei Coalfield, China

USGS Publications Warehouse

Zheng, Lingyun; Liu, Gaisheng; Chou, C.-L.; Qi, C.; Zhang, Y.

2007-01-01

The rare earth elements (REEs) in coals are important because of: (a) REE patterns can be an indicator of the nature of source rocks of the mineral matter as well as sedimentary environments; (b) REEs abundance in coal may have industrial-significance. In this study, a total of thirty-four samples of Permian coal, partings, roof, and floor were collected from the Huaibei Coalfield, Anhui Province, China. Abundances of rare earth elements (REEs) and other elements in the samples were determined by inductively coupled-plasma mass spectrometry (ICP-MS) and inductively coupled-plasma atomic emission spectrometry (ICP-AES). The results show that the REEs are enriched in coals in the Huaibei Coalfield as compared with Chinese and U.S. coals and the world coal average. Coals in the Lower Shihezi Formation (No. 7, 5, and 4 Coals) and Upper Shihezi Formation (No. 3) have higher REE abundances than the coals in Shanxi Formation (No. 10). Magmatic intrusion resulted in high enrichment of REEs concentrations in No. 5 and 7 Coals. The REE abundances are positively correlated with the ash content. The mineral matter in these coals is mainly made up of clay minerals and carbonates. The REEs are positively correlated with lithophile elements including Si, Al, Ti, Fe, and Na, which are mainly distributed in clay minerals, indicating that REEs are contained mainly in clay minerals. The REE abundances in coals normalized by the ash are higher than that in partings. REEs abundances of coals cannot be accounted for by the REE content in the mineral matter, and some REEs associated with organic matter in coals. ?? 2007 Elsevier Ltd. All rights reserved.
Atomic spectrometry update - atomic mass spectrometry.

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

Bacon, J.; Crain, J. S.; McMahon, A. W.

The MS and XRF updates have been published together since their introduction in 1988. In the last few years, however, the two sections have been prepared independently of each other and it therefore seemed appropriate to publish the two sections separately. With effect from this issue, the MS Update will appear in the October issue of JAAS and the XRF Update in the November issue. The format used for the MS section is broadly similar to that used last year, with some additional sub-headings. This Update is intended to cover all atomic and stable isotopic MS techniques, but not thosemore » used in studies of fundamental nuclear physics and exotic nuclei far from stability. Also excluded are those reports in which MS is used as a tool in the study of molecular processes and of gaseous components. the review is based on critical selection of developments in instrumentation and methodology, notable for their innovation, originality or achievement of significant advances, and is not intended to be comprehensive in its coverage. Conference papers are only included if they contain enough information to show they meet these criteria, and our policy in general remains one of waiting for a development to appear in a full paper before inclusion in the review. a similar policy applies to foreign language papers unlikely to reach a wide audience. Routine applications of atomic MS are not included in this Update and the reader is referred to the Updates on Industrial Analysis: Metals, Chemicals and Advanced Materials (96/416), Environmental Analysis (96/1444) and Clinical and Biological Materials, Food and Beverages (96/2479). Also excluded are those applications, even if not routine, which use atomic spectroscopy as a tool for the study of a non-atomic property, for example, the use of stable isotope labeling of carbon or nitrogen in biomolecules in metabolic studies. There have been few general reviews on atomic MS of note in the period covered by this update. That of Colodner et al.(95/3890) gave a general review of ion sources, in particular GDMS, ICP-MS, SIMS and TIMS, and that of Blades (95/2568 and 95/3077) was a very general overview of some of the techniques covered in this Update. The review of the literature in the period covered by this Update reveals strong advances in all areas, with a continuing push to achieve better analyses on smaller samples and in less time. Most advances generally require more sophisticated instrumentation, improved sample preparation methods or new methods of sample introduction. This is typified by advances in ICP-MS, which see considerable emphasis on sample introduction techniques and a move towards magnetic sector instruments. Most applications of ICP-MS are now highly routine. There is still, however, a desire to achieve affordable analysis with simplified and cost-effective instruments, as illustrated by the development of mobile, in-situ isotope MS for environmental studies.« less
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.
Results from the (U-Th)/He dating systems in Japan Atomic Energy Agency

NASA Astrophysics Data System (ADS)

Yamada, K.; Hanamuro, T.; Tagami, T.; Yamada, R.; Umeda, K.

2007-12-01

Japan Atomic Energy Agency (JAEA) has jointly set up the lab of the (U-Th)/He dating in cooperation with Kyoto University and National Research Institute for Earth Science and Disaster Prevention. We use the MM5400 rare gas mass spectrometer and the SPQ9000 ICP quadrupole mass spectrometer, belonging to JAEA, and built a new vacuum heater using infrared laser to extract helium. HF decomposes zircon after the alkali-fusion method using XRF bead sampler and LiBO3 in the preparation of ICP solution. Helium is quantified using sensitivity method. Uranium and thorium are using standard addition method. Quantifications of uranium-238 and thorium-232 are only need for parent isotopes to date samples because they are expected that the state of secular equilibrium becomes established and samarium does not compose the samples. At the present stage, we calibrate our systems by dating some standards, such as zircon from the Fish Canyon Tuff and apatite from the Durango, those are the international age standard, and apatite and zircon from the Tanzawa Tonalite Complex, that was dated in Yamada's PhD thesis, as a working standard. We report the results and detailed views of the dating systems.
Contribution of ICP-IDMS to the certification of antimony implanted in a silicon wafer--comparison with RBS and INAA results.

PubMed

Pritzkow, W; Vogl, J; Berger, A; Ecker, K; Grötzschel, R; Klingbeil, P; Persson, L; Riebe, G; Wätjen, U

2001-11-01

A thin-layer reference material for surface and near-surface analytical methods was produced and certified. The surface density of the implanted Sb layer was determined by Rutherford backscattering spectrometry (RBS), instrumental neutron activation analysis (INAA), and inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) equipped with a multi-collector. The isotopic abundances of Sb (121Sb and 123Sb) were determined by multi-collector ICP-MS and INAA. ICP-IDMS measurements are discussed in detail in this paper. All methods produced values traceable to the SI and are accompanied by a complete uncertainty budget. The homogeneity of the material was measured with RBS. From these measurements the standard uncertainty due to possible inhomogeneities was estimated to be less than 0.78% for fractions of the area increments down to 0.75 mm2 in size. Excellent agreement between the results of the three different methods was found. For the surface density of implanted Sb atoms the unweighted mean value of the means of four data sets is 4.81 x 10(16) cm(-2) with an expanded uncertainty (coverage factor k = 2) of 0.09 x 10(16) cm(-2). For the isotope amount ratio R (121Sb/123Sb) the unweighted mean value of the means of two data sets is 1.435 with an expanded uncertainty (coverage factor k = 2) of 0.006.
Volatile Organic Silicon Compounds in Biogases: Development of Sampling and Analytical Methods for Total Silicon Quantification by ICP-OES

PubMed Central

Julien, Jennifer; Dumont, Nathalie; Lebouil, David; Germain, Patrick

2014-01-01

Current waste management policies favor biogases (digester gases (DGs) and landfill gases (LFGs)) valorization as it becomes a way for energy politics. However, volatile organic silicon compounds (VOSiCs) contained into DGs/LFGs severely damage combustion engines and endanger the conversion into electricity by power plants, resulting in a high purification level requirement. Assessing treatment efficiency is still difficult. No consensus has been reached to provide a standardized sampling and quantification of VOSiCs into gases because of their diversity, their physicochemical properties, and the omnipresence of silicon in analytical chains. Usually, samplings are done by adsorption or absorption and quantification made by gas chromatography-mass spectrometry (GC-MS) or inductively coupled plasma-optical emission spectrometry (ICP-OES). In this objective, this paper presents and discusses the optimization of a patented method consisting in VOSiCs sampling by absorption of 100% ethanol and quantification of total Si by ICP-OES. PMID:25379538
Volatile organic silicon compounds in biogases: development of sampling and analytical methods for total silicon quantification by ICP-OES.

PubMed

Chottier, Claire; Chatain, Vincent; Julien, Jennifer; Dumont, Nathalie; Lebouil, David; Germain, Patrick

2014-01-01

Current waste management policies favor biogases (digester gases (DGs) and landfill gases (LFGs)) valorization as it becomes a way for energy politics. However, volatile organic silicon compounds (VOSiCs) contained into DGs/LFGs severely damage combustion engines and endanger the conversion into electricity by power plants, resulting in a high purification level requirement. Assessing treatment efficiency is still difficult. No consensus has been reached to provide a standardized sampling and quantification of VOSiCs into gases because of their diversity, their physicochemical properties, and the omnipresence of silicon in analytical chains. Usually, samplings are done by adsorption or absorption and quantification made by gas chromatography-mass spectrometry (GC-MS) or inductively coupled plasma-optical emission spectrometry (ICP-OES). In this objective, this paper presents and discusses the optimization of a patented method consisting in VOSiCs sampling by absorption of 100% ethanol and quantification of total Si by ICP-OES.
Characteristics of n-GaN After Cl2/Ar and Cl2/N2 Inductively Coupled Plasma Etching

NASA Astrophysics Data System (ADS)

Han, Yan-Jun; Xue, Song; Guo, Wen-Ping; Sun, Chang-Zheng; Hao, Zhi-Biao; Luo, Yi

2003-10-01

A systematic study on the effect of inductively coupled plasma (ICP) etching on n-type GaN is presented. The optical and electrical properties and surface stoichiometry of n-type GaN are evaluated using room-temperature photoluminescence (PL) and current-voltage (I-V) characteristic measurements, and X-ray photoelectron spectroscopy (XPS), respectively. Investigation of the effect of additive gas (N2 and Ar) and RF power on these characteristics has also been carried out. It is shown that the decrease in the O/Ga ratio after ICP etching can suppress the deterioration of the near-band-edge emission intensity. Furthermore, N vacancy (VN) with a shallow donor nature and Ga vacancy (VGa) with a deep acceptor nature are generated after ICP etching upon the addition of Ar and N2 to Cl2 plasma, respectively. Lower ohmic contact resistance could be obtained when VN or ion-bombardment-induced defect is dominant at the surface. Improved etching conditions have been obtained based on these results.

Superradiators created atom by atom

NASA Astrophysics Data System (ADS)

Meschede, Dieter

2018-02-01

High radiation rates are usually associated with macroscopic lasers. Laser radiation is “coherent”—its amplitude and phase are well-defined—but its generation requires energy inputs to overcome loss. Excited atoms spontaneously emit in a random and incoherent fashion, and for N such atoms, the emission rate simply increases as N. However, if these atoms are in close proximity and coherently coupled by a radiation field, this microscopic ensemble acts as a single emitter whose emission rate increases as N2 and becomes “superradiant,” to use Dicke's terminology (1). On page 662 of this issue, Kim et al. (2) show the buildup of coherent light fields through collective emission from atomic radiators injected one by one into a resonator field. There is only one atom ever in the cavity, but the emission is still collective and superradiant. These results suggest another route toward thresholdless lasing.
Microwave-assisted wet digestion with H2O2 at high temperature and pressure using single reaction chamber for elemental determination in milk powder by ICP-OES and ICP-MS.

PubMed

Muller, Edson I; Souza, Juliana P; Muller, Cristiano C; Muller, Aline L H; Mello, Paola A; Bizzi, Cezar A

2016-08-15

In this work a green digestion method which only used H2O2 as an oxidant and high temperature and pressure in the single reaction chamber system (SRC-UltraWave™) was applied for subsequent elemental determination by inductively coupled plasma-based techniques. Milk powder was chosen to demonstrate the feasibility and advantages of the proposed method. Samples masses up to 500mg were efficiently digested, and the determination of Ca, Fe, K, Mg and Na was performed by inductively coupled plasma optical emission spectrometry (ICP-OES), while trace elements (B, Ba, Cd, Cu, Mn, Mo, Pb, Sr and Zn) were determined by inductively coupled plasma mass spectrometry (ICP-MS). Residual carbon (RC) lower than 918mgL(-1) of C was obtained for digests which contributed to minimizing interferences in determination by ICP-OES and ICP-MS. Accuracy was evaluated using certified reference materials NIST 1549 (non-fat milk powder certified reference material) and NIST 8435 (whole milk powder reference material). The results obtained by the proposed method were in agreement with the certified reference values (t-test, 95% confidence level). In addition, no significant difference was observed between results obtained by the proposed method and conventional wet digestion using concentrated HNO3. As digestion was performed without using any kind of acid, the characteristics of final digests were in agreement with green chemistry principles when compared to digests obtained using conventional wet digestion method with concentrated HNO3. Additionally, H2O2 digests were more suitable for subsequent analysis by ICP-based techniques due to of water being the main product of organic matrix oxidation. The proposed method was suitable for quality control of major components and trace elements present in milk powder in consonance with green sample preparation. Copyright © 2016 Elsevier B.V. All rights reserved.
Development of the Flame Test Concept Inventory: Measuring Student Thinking about Atomic Emission

ERIC Educational Resources Information Center

Bretz, Stacey Lowery; Murata Mayo, Ana Vasquez

2018-01-01

This study reports the development of a 19-item Flame Test Concept Inventory, an assessment tool to measure students' understanding of atomic emission. Fifty-two students enrolled in secondary and postsecondary chemistry courses were interviewed about atomic emission and explicitly asked to explain flame test demonstrations and energy level…
In vivo testing for gold nanoparticle toxicity.

PubMed

Simpson, Carrie A; Huffman, Brian J; Cliffel, David E

2013-01-01

A technique for measuring the toxicity of nanomaterials using a murine model is described. Blood samples are collected via submandibular bleeding while urine samples are collected on cellophane sheets. Both biosamples are then analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES) for nanotoxicity. Blood samples are further tested for immunological response using a standard Coulter counter. The major organs of interest for filtration are also digested and analyzed via ICP-OES, producing useful information regarding target specificity of the nanomaterial of interest. Collection of the biosamples and analysis afterward is detailed, and the operation of the technique is described and illustrated by analysis of the nanotoxicity of an injection of a modified tiopronin monolayer-protected cluster.
TRENDS IN SURFACE WATER ACIDIFICATION IN EUROPE AND NORTH AMERICA (1989-1998)

EPA Science Inventory

During the last 20 years, emission reductions in Europe and North America have resulted in decreased atmospheric Sulfur-deposition of up to 50%, while Nitrogen-deposition has stayed almost constant. Data from 98 ICP Waters sites were tested for trends in concentrations of major c...
PREDICTION OF FORBIDDEN ULTRAVIOLET AND VISIBLE EMISSIONS IN COMET 67P/CHURYUMOV–GERASIMENKO

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

Raghuram, Susarla; Galand, Marina; Bhardwaj, Anil, E-mail: raghuramsusarla@gmail.com

Remote observation of spectroscopic emissions is a potential tool for the identification and quantification of various species in comets. The CO Cameron band (to trace CO{sub 2}) and atomic oxygen emissions (to trace H{sub 2}O and/or CO{sub 2}, CO) have been used to probe neutral composition in the cometary coma. Using a coupled-chemistry-emission model, various excitation processes controlling the CO Cameron band and different atomic oxygen and atomic carbon emissions have been modeled in comet 67P/Churyumov–Gerasimenko at 1.29 AU (perihelion) and at 3 AU heliocentric distances, which is being explored by ESA's Rosetta mission. The intensities of the CO Cameronmore » band, atomic oxygen, and atomic carbon emission lines as a function of projected distance are calculated for different CO and CO{sub 2} volume mixing ratios relative to water. Contributions of different excitation processes controlling these emissions are quantified. We assess how CO{sub 2} and/or CO volume mixing ratios with respect to H{sub 2}O can be derived based on the observed intensities of the CO Cameron band, atomic oxygen, and atomic carbon emission lines. The results presented in this work serve as baseline calculations to understand the behavior of low out-gassing cometary coma and compare them with the higher gas production rate cases (e.g., comet Halley). Quantitative analysis of different excitation processes governing the spectroscopic emissions is essential to study the chemistry of inner coma and to derive neutral gas composition.« less
Rocket and spacecraft studies of ultraviolet emissions from astrophysical targets

NASA Technical Reports Server (NTRS)

Fastie, W. G.; Moos, H. W.; Feldman, P. D.; Henry, R. C.

1975-01-01

Rocket and spacecraft far-UV spectral measurements of several astrophysical targets are reviewed. These include observations of Ly-alpha emissions from Arcturus, Apollo-17 far-UV spectrometry of eta UMa and five other stars, Apollo-17 observations of the lunar atmosphere and the diffuse UV background, and far-UV spectral studies of Venus, Jupiter, and Comet Kohoutek. The Arcturus observations indicated a chromosphere with neutral atomic-hydrogen and atomic-oxygen emissions as well as a very weak atomic-carbon line. The planetary studies revealed O I and C I emissions in the Venusian spectrum as well as large Ly-alpha emissions and possible molecular-hydrogen emissions in that of Jupiter. The lunar observations demonstrated that solar protons do not produce an atomic-hydrogen atmosphere on the moon.
Oxidation kinetics of the combustible fraction of construction and demolition wastes.

PubMed

Chang, N B; Lin, K S; Sun, Y P; Wang, H P

2001-01-01

Proper disposal of construction and demolition wastes (CDW) has received wide attention recently due to significantly large quantities of waste streams collected from razed or retrofitted buildings in many metropolitan regions. Burning the combustible fractions of CDW (CCDW) and possibly recovering part of the heat content for economic uses could be valuable for energy conservation. This paper explores the oxidation kinetics of CCDW associated with its ash characterization. Kinetic parameters for the oxidation of CCDW were numerically calculated using thermal gravimetric analysis (TGA) and the resultant rate equations were therefore developed for illustrating the oxidation processes of CCDW simultaneously. Based on three designated heating rates, each of the oxidation processes can be featured distinctively with five different stages according to the rate of weight change at the temperature between 300 K and 923 K. In addition, Fourier transform infrared (FTIR) spectroscopy was employed, associated with a lab-scale fixed-bed incinerator for monitoring the composition of flue gas. Carbon dioxide (CO2) was found as a major component in the flue gas. The fuel analysis also included an ash composition analysis via the use of X-ray powder diffraction (XRD), atomic absorption (AA) spectroscopy, inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and scanning electron microscopy-energy dispersive spectroscopy (SEM-EDX). The ash streams were identified as nonhazardous materials based on the toxicity characteristic leaching procedure (TCLP). Overall, the scientific findings gained in this study will be helpful for supporting a sound engineering design of real-world CCDW incineration systems.
Radiation of partially ionized atomic hydrogen

NASA Technical Reports Server (NTRS)

Soon, W. H.; Kunc, J. A.

1990-01-01

A nonlinear collisional-radiative model for determination of production of electrons, positive and negative ions, excited atoms, and spectral and continuum line intensities in stationary partially ionized atomic hydrogen is presented. Transport of radiation is included by coupling the rate equations for production of the electrons, ions, and excited atoms with the radiation escape factors, which are not constant but depend on plasma conditions. It is found that the contribution of the negative ion emission to the total continuum emission can be important. Comparison of the calculated total continuum emission coefficient, including the negative ion emission, is in good agreement with experimental results.
[Atomic/ionic fluorescence in microwave plasma torch discharge excited by high current microsecond pulsed hollow cathode lamp-europium atomic/ionic fluorescence spectrometry].

PubMed

Gong, Z; Liang, F; Yang, P; Jin, Q; Huang, B

1999-06-01

Eu atomic and ionic fluorescence spectrometry in microwave plasma torch discharge excited by high current microsecond pulsed hollow cathode lamp (HCMP HCL-MPT AFS/IFS) was studied. Operating conditions were optimized. The best detection limits for AFS and IFS obtained with a desolvated ultrasonic nebulization system were 42.0 ng/mL for Eu I 462.7 nm and 21.8 ng/mL for Eu II 381.97 nm, respectively, both were better than those given by the instruction manual of a Baird ICP AFS-2000 spectrometer using pneumatic concentric nebulizer with desolvation for AFS, but were significantly higher than those obtained by using the Baird spectrometer with a mini-monochromator and a ultrasonic nebulzer system.
Continuous Liquid-Sample Introduction for Bunsen Burner Atomic Emission Spectrometry.

ERIC Educational Resources Information Center

Smith, Gregory D.; And Others

1995-01-01

Describes a laboratory-constructed atomic emission spectrometer with modular instrumentation components and a simple Bunsen burner atomizer with continuous sample introduction. A schematic diagram and sample data are provided. (DDR)
Accurate quantitation standards of glutathione via traceable sulfur measurement by inductively coupled plasma optical emission spectrometry and ion chromatography

PubMed Central

Rastogi, L.; Dash, K.; Arunachalam, J.

2013-01-01

The quantitative analysis of glutathione (GSH) is important in different fields like medicine, biology, and biotechnology. Accurate quantitative measurements of this analyte have been hampered by the lack of well characterized reference standards. The proposed procedure is intended to provide an accurate and definitive method for the quantitation of GSH for reference measurements. Measurement of the stoichiometrically existing sulfur content in purified GSH offers an approach for its quantitation and calibration through an appropriate characterized reference material (CRM) for sulfur would provide a methodology for the certification of GSH quantity, that is traceable to SI (International system of units). The inductively coupled plasma optical emission spectrometry (ICP-OES) approach negates the need for any sample digestion. The sulfur content of the purified GSH is quantitatively converted into sulfate ions by microwave-assisted UV digestion in the presence of hydrogen peroxide prior to ion chromatography (IC) measurements. The measurement of sulfur by ICP-OES and IC (as sulfate) using the “high performance” methodology could be useful for characterizing primary calibration standards and certified reference materials with low uncertainties. The relative expanded uncertainties (% U) expressed at 95% confidence interval for ICP-OES analyses varied from 0.1% to 0.3%, while in the case of IC, they were between 0.2% and 1.2%. The described methods are more suitable for characterizing primary calibration standards and certifying reference materials of GSH, than for routine measurements. PMID:29403814
Spatial and temporal variations in infrared emissions of the upper atmosphere. 1. Atomic oxygen (λ 63 μm) emission

NASA Astrophysics Data System (ADS)

Semenov, A. I.; Medvedeva, I. V.; Perminov, V. I.; Khomich, V. Yu.

2016-09-01

Rocket and balloon measurement data on atomic-oxygen (λ 63 µm) emission in the upper atmosphere are presented. The data from the longest (1989-2003) period of measurements of the atomic-oxygen (λ 63 µm) emission intensity obtained by spectral instruments on sounding balloons at an altitude of 38 km at midlatitudes have been systematized and analyzed. Regularities in diurnal and seasonal variations in the intensity of this emission, as well as in its relation with solar activity, have been revealed.
[Study on microwave digestion of coal for the determination of multi-element by ICP-OES and ICP-MS].

PubMed

Wang, Hui; Song, Qiang; Yao, Qiang; Chen, Chang-He; Yu, Fei-Lu

2012-06-01

Effects of temperature and four acids (HNO3, HNO3/H2O2, HNO3/HF and HNO3/HF+H3BO3) on the coal decomposition by microwave digestion and the multi-element analysis were studied. SARM20 was used as a coal standard reference material. The contents of 10 mineral elements (Al, Ca, Fe, Mg, K, Na, S, Si, Sr and Ti) in the coal SARM20 were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES). And the contents of 20 heavy metals (Li, Be, Sc, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, As, Se, Zr, Sn, Cs, Ba, Ce, Eu and Pb) were determined by inductively coupled plasma-mass spectrometry (ICP-MS). The results showed that the coal was completely decomposed by microwave digestion with HNO3/HF+ H3BO3 at 210 degrees C. Good recoveries for all elements in the coal SARM20 were obtained by this two-step microwave digestion method. The recoveries of the 10 mineral elements were from 87.5% to 98.8%, and the recoveries of the 20 heavy metals were from 85% to 112.5%. All RSDs of tests were below 3%.
LA-ICP-MS-derived U-concentrations and microstructural domains within biogenic aragonite of Arctica islandica shell.

PubMed

Helama, Samuli; Heikkilä, Pasi; Rinne, Katja; Nielsen, Jan Kresten; Nielsen, Jesper Kresten

2015-05-01

Understanding of the uranium uptake processes (both in vivo and post-mortem) into the skeletal structures of marine calcifiers is a subject of multi-disciplinary interest. U-concentration changes within the molluscan shell may serve as a paleoceanographic proxy of the pH history. A proxy of this type is needed to track the effects of fossil fuel emissions to ocean acidification. Moreover, attaining reliable U-series dates using shell materials would be a geochronological breakthrough. Picturing the high-resolution changes of U-concentrations in shell profiles is now possible by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS). Here, we analyzed in situ U-concentration variations in sub-fossilized shells of ocean quahog (Arctica islandica), a commonly studied bivalve species in Quaternary geoscience, using LA-ICP-MS. Microstructural details of the shell profiles were achieved by the scanning electron microscopy (SEM). Comparison of the shell aragonite microstructure with the changes in U-concentration revealed that uranium of possibly secondary origin is concentrated into the porous granular layers of the shell. Our results reinforce the hypothesis that U-concentration variations can be linked with microstructural differences within the shell. A combination of LA-ICP-MS and SEM analyses is recommended as an interesting approach for understanding the U-concentration variations in similar materials.
Study of atomic and molecular emission spectra of Sr by laser induced breakdown spectroscopy (LIBS).

PubMed

Bhatt, Chet R; Alfarraj, Bader; Ayyalasomayajula, Krishna K; Ghany, Charles; Yueh, Fang Y; Singh, Jagdish P

2015-12-01

Laser Induced Breakdown Spectroscopy (LIBS) is an ideal analytical technique for in situ analysis of elemental composition. We have performed a comparative study of the quantitative and qualitative analysis of atomic and molecular emission from LIBS spectra. In our experiments, a mixture of SrCl2 and Al2O3 in powder form was used as a sample. The atomic emission from Sr and molecular emission from SrCl and SrO observed in LIBS spectra were analyzed. The optimum laser energies, gate delays, and gate widths for selected atomic lines and molecular bands were determined from spectra recorded at various experimental parameters. These optimum experimental conditions were used to collect calibration data, and the calibration curves were used to predict the Sr concentration. Limits of detection (LODs) for selected atomic and molecular emission spectra were determined.
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...
Carbon-, sulfur-, and phosphorus-based charge transfer reactions in inductively coupled plasma-atomic emission spectrometry

NASA Astrophysics Data System (ADS)

Grindlay, Guillermo; Gras, Luis; Mora, Juan; de Loos-Vollebregt, Margaretha T. C.

2016-01-01

In this work, the influence of carbon-, sulfur-, and phosphorus-based charge transfer reactions on the emission signal of 34 elements (Ag, Al, As, Au, B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe, Ga, Hg, I, In, Ir, K, Li, Mg, Mn, Na, Ni, P, Pb, Pd, Pt, S, Sb, Se, Sr, Te, and Zn) in axially viewed inductively coupled plasma-atomic emission spectrometry has been investigated. To this end, atomic and ionic emission signals for diluted glycerol, sulfuric acid, and phosphoric acid solutions were registered and results were compared to those obtained for a 1% w w- 1 nitric acid solution. Experimental results show that the emission intensities of As, Se, and Te atomic lines are enhanced by charge transfer from carbon, sulfur, and phosphorus ions. Iodine and P atomic emission is enhanced by carbon- and sulfur-based charge transfer whereas the Hg atomic emission signal is enhanced only by carbon. Though signal enhancement due to charge transfer reactions is also expected for ionic emission lines of the above-mentioned elements, no experimental evidence has been found with the exception of Hg ionic lines operating carbon solutions. The effect of carbon, sulfur, and phosphorus charge transfer reactions on atomic emission depends on (i) wavelength characteristics. In general, signal enhancement is more pronounced for electronic transitions involving the highest upper energy levels; (ii) plasma experimental conditions. The use of robust conditions (i.e. high r.f. power and lower nebulizer gas flow rates) improves carbon, sulfur, and phosphorus ionization in the plasma and, hence, signal enhancement; and (iii) the presence of other concomitants (e.g. K or Ca). Easily ionizable elements reduce ionization in the plasma and consequently reduce signal enhancement due to charge transfer reactions.
Studies for the Loss of Atomic and Molecular Species from Io

NASA Technical Reports Server (NTRS)

Smyth, William H.

1998-01-01

Continued effort is reported to improve the emission rates of various emission lines for atomic oxygen and sulfur. Atomic hydrogen has been included as a new species in the neutral cloud model. The pertinent lifetime processes for hydrogen in the plasma torus and the relevant excitation processes for H Lyman-alpha emission in Io's atmosphere are discussed.

Geometry dependent suppression of collective quantum jumps in Rydberg atoms

NASA Astrophysics Data System (ADS)

Lees, Eitan; Clemens, James

2015-05-01

We consider N driven, damped Rydberg atoms in different spatial arrangements. Treating the atoms as two-level systems we model the coupling to the environment via the Lehmberg-Agarwal master equation which interpolates between fully independent and fully collective spontaneous emission depending on the specific locations of the atoms. We also include a collective dipole-dipole energy shift in the excited Rydberg state which leads to collective quantum jumps in the atomic excitation when the system is driven off resonance. We show that the quantum jumps are suppressed as the system makes a transition from independent to collective emission as the spacing of a linear array of atoms is decreased below the emission wavelength.
PILOT STUDY: CCQM-P39.1: As, Hg, Pb, Se and methylmercury in salmon

NASA Astrophysics Data System (ADS)

Aregbe, Y.; Taylor, P. D. P.

2006-01-01

CCQM-P39.1 was organized as a follow-up pilot study in parallel to the key comparison CCQM-K43 after the previous pilot study on tuna fish. CCQM-P39.1 was an activity of the Inorganic Analysis Working Group (IAWG) of CCQM and was coordinated by the Joint Research Centre-Institute for Reference Materials and Measurements (IRMM, Geel, Belgium) of the European Commission (EC). In CCQM-P39.1 the amount contents of As, Hg, Pb, Se and methylmercury (CH3Hg) in salmon (muscle and skin) were the measurands under investigation. Besides the national metrology institutes (NMIs) also non-IAWG members, expert laboratories for mercury and methylmercury measurements, were invited to participate in this pilot study. Results were reported by six IAWG members and six expert laboratories. During the CCQM-IAWG autumn meeting in Berlin, October 2005, it was agreed that in CCQM-K43 the KCRV is calculated as the mixture model median (MM-median) of all reported results. Therefore in CCQM-P39.1 the reported results are presented graphically with the KCRV from CCQM-K43. The reported results of the IAWG members fall within a range of +/-4% for arsenic and lead relative to the CCQM-K43 KCRV. For mercury, the spread was +/-2%, but one IAWG member reported a very large uncertainty on the measurement result. For selenium the spread of IAGW members is +/-2% deviation from the CCQM-K43 KCRV. Including the reported results from the invited expert laboratories, the spread of results increased for arsenic, lead and mercury to +/-8%. The reported results including the experts fall within a range of +/-20% for selenium and +/-30% for methylmercury. The methods applied were isotope dilution mass spectrometry (IDMS) using sector field or quadrupole inductively coupled plasma-mass spectrometry (ICP-MS), external calibration or standard addition using ICP-MS, atomic absorption spectrometry (AAS), atomic fluorescence spectrometry (AFS), atomic emission detection (AED) and electron capture detection (ECD). Instrumental neutron activation analysis (INAA) and k0-neutron activation analysis (k0-NAA) were also used as analytical techniques. Each of the five analytes under investigation was measured with at least two of these analytical techniques. IAEA reported two results for arsenic and lead. They were measured with ICP-MS and AAS, respectively. JSI reported two results for mercury, measured with NAA and AAS, and furthermore two results for methylmercury measured with GC-ECD and GC-CV-AFS. This report presents the participants' results in CCQM-P39.1 for all analytes under investigation. In Annex 1, the results are displayed with the CCQM-K43 KCRV. In Annex 2, the different approaches for methlymercury measurements are presented in more detail. In Annex 3, the questionnaire data are presented. Annex 4 compiles all the CCQM-P39.1 information documents. The key comparison CCQM-K43 was carried out in parallel to this pilot study for the same measurands in the same salmon material. Participation was meant for IAWG members, to support their CMCs in Appendix C. Main text. To reach the main text of this paper, click on Final Report. The final report has been peer-reviewed and approved for publication by the CCQM Working Group on Inorganic Analysis.
FeO "Orange Arc" Emission Detected in Optical Spectrum of Leonid Persistent Trains

NASA Technical Reports Server (NTRS)

Jenniskens, Peter; Lacey, Matt; Allan, Beverly J.; Self, Daniel E.; Plane, John M. C.; DeVincenzi, Donald L. (Technical Monitor)

2000-01-01

We report the detection of a broad continuum emission dominating the visual spectrum of a Leonid persistent train. A comparison with laboratory spectra of FeO 1 "orange arc" emission at I mbar shows a general agreement of the band position and shape. The detection of FeO confirms the classical mechanism of metal atom catalyzed recombination of ozone and oxygen atoms as the driving force behind optical emission from persistent trains. Sodium and iron atoms are now confirmed catalysts.
Micro-scale flow system for on-line multielement preconcentration from saliva digests and determination by inductively coupled plasma optical emission spectrometry

NASA Astrophysics Data System (ADS)

Menegário, Amauri A.; Fernanda Giné, Maria

2001-10-01

A micro-scale flow system is proposed for on-line preconcentration of Cd, Cu, Mn, Ni and Pb in saliva samples and their determination by inductively coupled plasma optical emission spectrometry (ICP-OES). A small column containing 8 μl of AG50W-X8 resin was inserted into the flow system, assembled with capillary tubes and connected to a micro-concentric nebulizer. The elution of the analytes was performed with 3 mol l -1 HCl at a flow rate of 82 μl min -1. The ICP-OES signal acquisition program permits measurements for 5 s in the concentrated portion of the transient elution peaks. A sample volume of 1 ml was required to obtain enrichment factors of 46, 23, 17, 18 and 44 for Cd, Cu, Mn, Ni and Pb, respectively. The relative standard deviations for a 50-μg l -1 multi-analyte solution were ≤6.5%. The recoveries for Cd, Cu, Mn, Ni and Pb in digested human saliva samples were between 86 and 111%. The sample throughput was 24 h -1.
Anchoring of Cu(II) onto surface of porous metal-organic framework through post-synthesis modification for the synthesis of benzimidazoles and benzothiazoles

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

Kardanpour, Reihaneh; Tangestaninejad, Shahram, E-mail: stanges@sci.ui.ac.ir; Mirkhani, Valiollah, E-mail: mirkhani@sci.ui.ac.ir

2016-03-15

Efficient synthesis of various benzimidazoles and benzothiazoles under mild conditions catalyzed by Cu(II) anchored onto UiO-66–NH{sub 2} metal organic framework is reported. In this manner, first, the aminated UiO-66 was modified with thiophene-2-carbaldehyde and then the prepared Schiff base was reacted with CuCl{sub 2}. The prepared catalyst was characterized by FT-IR, UV–vis, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), N{sub 2} adsorption, inductively coupled plasma atomic emission spectroscopy (ICP-AES) and field emission scanning electron microscopy (FE-SEM). The UiO-66–NH{sub 2}–TC–Cu was applied as a highly efficient catalyst for synthesis of benzimidazole and benzothiazole derivatives by the reaction of aldehydes with 1,2-diaminobenzenemore » or 2-aminothiophenol. The Cu(II)-containing MOF was reused several times without any appreciable loss of its efficiency. - Graphical abstract: Efficient synthesis of benzimidazoles and benzothiazoles catalyzed by Cu(II) anchored onto UiO-66–NH{sub 2} metal organic framework is reported. - Highlights: • A copper Schiff base was immobilized on UiO-66 via postsynthetic modification. • The modified MOFs were fully characterized by a variety of methods. • The catalyst was used for the preparation of benzimidazoles and benzothiazoles. • In comparison of other catalysts, our catalyst was more efficient and forceful.« less
Tuning the morphology, luminescence and magnetic properties of hexagonal-phase NaGdF4: Yb, Er nanocrystals via altering the addition sequence of the precursors

NASA Astrophysics Data System (ADS)

Zhao, Shuwen; Xia, Donglin; Zhao, Ruimin; Zhu, Hao; Zhu, Yiru; Xiong, Yuda; Wang, Youfa

2017-01-01

Hexagonal-phase NaGdF4: Yb, Er upconversion nanocrystals (UCNCs) with tunable morphology and properties were successfully prepared via a thermal decomposition method. The influences of the adding sequence of the precursors on the morphology, chemical composition, luminescence and magnetic properties were investigated by transmission electron microscopy (TEM), inductively coupled plasma-atomic emission spectrometry (ICP-AES), upconversion (UC) spectroscopy, and a vibrating sample magnetometer (VSM). It was found that the resulting nanocrystals, with different sizes ranging from 24 to 224 nm, are in the shape of spheres, hexagonal plates and flakes; moreover, the composition percentage of Yb3+-Er3+ and Gd3+ ions was found to vary in a regular pattern with the adding sequence. Furthermore, the intensity ratios of emission colors (f g/r, f g/p), and the magnetic mass susceptibility of hexagonal-phase NaGdF4: Yb, Er nanocrystals change along with the composition of the nanocrystals. A positive correlation between the susceptibility and f g/r of NaGdF4: Yb, Er was proposed. The decomposition processes of the precursors were investigated by a thermogravimetric (TG) analyzer. The result indicated that the decomposition of the resolved lanthanide trifluoroacetate is greatly different from lanthanide trifluoroacetate powder. It is of tremendous help to recognize the decomposition process of the precursors and to understand the related reaction mechanism.
Detection of hazardous pollutants in chrome-tanned leather using locally developed laser-induced breakdown spectrometer.

PubMed

Nasr, M M; Gondal, Mohammed Asharf; Seddigi, Z S

2011-04-01

Highly toxic contaminants like Cr, As, and Pb were detected in chrome-tanning process of animal skin to produce leather by applying locally developed laser-induced breakdown spectrometer. An Nd-YAG laser with 1,064 nm wavelength was focused on the surface of leather samples (natural and manufactured) to generate a plasma spark and spectrally resolved spectra were used for identification and quantification of contaminants. The leather samples were collected from a tannery located in industrial cities of Riyadh and Jeddah, Saudi Arabia. The study was carried out on fully, half manufactured (wet blue leather), and natural hide (skin). To the best of our knowledge, this is the first attempt where laser-induced breakdown spectroscopy (LIBS) technique has been applied for the analysis of leather before and after tanning process. The maximum concentration of different elements of environmental significance like chromium, lead, arsenic, sulfur, magnesium were 199, 289, 31, 38, and 39 ppm, respectively, in one of the manufactured leather samples. The limit of detection (LOD) of our LIBS system for chromium, lead, arsenic, sulfur, and magnesium were 2, 3, 1.5,7, and 3 ppm, respectively. The safe permissible limit for tanned leather for highly toxic elements like chromium, lead, and arsenic are 1, 0.5, 0.01 ppm, respectively, as prescribed in Environmental Regulation Standards for Saudi Industries set by Royal Commission Jubail, Saudi Arabia. The LIBS technique is superior to other conventional techniques like ICP or atomic absorption that a little or no sample preparation is required, no chemicals are needed, multi-elemental analysis is possible for all kinds of samples (natural and anthropogenic materials), microgram of sample is essential, and LIBS could be applied for remote analysis. It is highly selective and sensitivity higher than ICP, and as no sample and chemicals are required, it is cost effective for multi-sample analysis per unit time as compared with other conventional techniques. The concentration of some toxic elements (Cr, Pb, As) is much higher than the safe permissible limits set by Occupational Safety and Health Administration in USA or Saudi environmental regulatory agencies. Results obtained with our LIBS systems were in close agreement with the results obtained using other standard analytical technique such as the inductively coupled plasma atomic emission spectroscopy.
Combustor exhaust-emissions and blowout-limits with diesel number 2 and Jet A fuels utilizing air-atomizing and pressure-atomizing nozzles

NASA Technical Reports Server (NTRS)

Ingebo, R. D.; Norgren, C. T.

1975-01-01

The effect of fuel properties on exhaust emissions and blowout limits of a high-pressure combustor segment is evaluated using a splash-groove air-atomizing fuel injector and a pressure-atomizing simplex fuel nozzle to burn both diesel number 2 and Jet A fuels. Exhaust emissions and blowout data are obtained and compared on the basis of the aromatic content and volatility of the two fuels. Exhaust smoke number and emission indices for oxides of nitrogen, carbon monoxide, and unburned hydrocarbons are determined for comparison. As compared to the pressure-atomizing nozzle, the air-atomizing nozzle is found to reduce nitrogen oxides by 20%, smoke number by 30%, carbon monoxide by 70%, and unburned hydrocarbons by 50% when used with diesel number 2 fuel. The higher concentration of aromatics and lower volatility of diesel number 2 fuel as compared to Jet A fuel appears to have the most detrimental effect on exhaust emissions. Smoke number and unburned hydrocarbons are twice as high with diesel number 2 as with Jet A fuel.
Axially and radially viewed inductively coupled plasmas — a critical review

NASA Astrophysics Data System (ADS)

Brenner, I. B.; Zander, A. T.

2000-08-01

The present status of axially viewed inductively coupled plasmas (ICP) is reviewed with special emphasis placed on the analytical performance of currently available systems. Descriptions are given of the various designs of the plasma-spectrometer configuration. Conventional figures of merit such as limits of detection, background behavior, interferences due to easily ionized elements (EIE), Ca and acids, and the Mg II 280.270 nm/Mg I 285.213 nm intensity ratio, are used to compare the performance of axially viewed and radially viewed ICPs. Various modes of sample introduction, including conventional pneumatic and ultrasonic nebulization (USN), thermospray and a direct injection probe will be described. For axially viewed ICPs, limits of detection (LOD) are improved by factors varying from approximately 2 to 30. Additional improvements by factors of 2-20 can be obtained using USN. The improvement factors generally depend on energy potentials of the spectral lines and the element. Although limits of detection in the presence of Ca and Na are degraded relative to an aqueous solution 10-30-fold, USN LODs using an axially viewed ICP are improved relative to those obtained using a pneumatic nebulizer for solutions containing Ca and Na. With normal aerosol load and under robust plasma conditions (as evidenced by Mg II/Mg I intensity ratios >8), EIE, Ca and mineral acid induced interferences are relatively small and are similar in axial and conventional radial configurations. However, interferences due to Ca are larger than those caused by Na due to the larger amount of energy required to dissociate the matrix. Matrix effects increase considerably when an USN is employed. For robust plasmas, ICP operating conditions and performance for multi-element quantitative analysis do not differ significantly from those of conventional radial configurations. In cases where robustness decreases, matrix interferences should be taken into account when establishing optimum conditions for operation. In robust axially viewed ICPs, a single internal standard can compensate for ionic line intensity suppression due to Na. However, owing to the variable influence of Ca on spectral response, more than one internal standard is required to compensate for these matrix effects. In this situation, linear energy potential-interference functions can be used to improve accuracy using spectral lines varying over wide ranges of energy potentials. In axially viewed ICPs, Mg II/ Mg I ratios vary widely as a function of applied RF power, aerosol flow rates and load, diameter of the central torch injector, and composition of the aspirated solution. The highest values of 9-13 have been observed for a pure aqueous solution using conventional nebulization and argon carrier flow rates (0.5-0.7 ml min -1) and forward powers of 1.2-1.5 kW. Mg II/Mg I ratios decrease when the RF power decreases, when Na and Ca are added to the plasma, and when the aerosol load is increased. A low value of 2 was obtained when the carrier gas flow rate was high and when the aerosol load was high using an USN. The use of a copper metal skimmer below the analytical observation zone to isolate the axial channel of the ICP and to deflect the outer cool fringe results in 5-20 times improvement of the LODs compared to those obtained using a conventional configuration (a normal radially viewed ICP). A direct He purged plasma-spectrometer interface for end-on detection of the vacuum UV (VUV) emission from the axial region of an ICP allows the determination of Cl, Br and other analytes in the μg l -1 range. The characteristics of a secondary discharge at the orifice of a Cu cone when the axial channel of the ICP is extracted into a vacuum chamber will be discussed. The characteristics of the emission in the Mach disk region extracted from the axial column will be surveyed. Several applications and techniques are described: determination of major, minor and trace elements in geological, environmental and biological materials, analysis of brines, nuclear materials and organic solvents and solutions. Several unique techniques are described: elemental speciation, determination of the halides and other analytes with VUV spectral lines using a He purged direct plasma-spectrometer interface. Direct solids analysis using slurries, laser and spark ablation and direct solids insertion further extends the scope of axially viewed ICPs.
Reduction of Solvent Effect in Reverse Phase Gradient Elution LC-ICP-MS

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

Sullivan, Patrick Allen

2005-12-17

Quantification in liquid chromatography (LC) is becoming very important as more researchers are using LC, not as an analytical tool itself, but as a sample introduction system for other analytical instruments. The ability of LC instrumentation to quickly separate a wide variety of compounds makes it ideal for analysis of complex mixtures. For elemental speciation, LC is joined with inductively coupled plasma mass spectrometry (ICP-MS) to separate and detect metal-containing, organic compounds in complex mixtures, such as biological samples. Often, the solvent gradients required to perform complex separations will cause matrix effects within the plasma. This limits the sensitivity ofmore » the ICP-MS and the quantification methods available for use in such analyses. Traditionally, isotope dilution has been the method of choice for LC-ICP-MS quantification. The use of naturally abundant isotopes of a single element in quantification corrects for most of the effects that LC solvent gradients produce within the plasma. However, not all elements of interest in speciation studies have multiple naturally occurring isotopes; and polyatomic interferences for a given isotope can develop within the plasma, depending on the solvent matrix. This is the case for reverse phase LC separations, where increasing amounts of organic solvent are required. For such separations, an alternative to isotope dilution for quantification would be is needed. To this end, a new method was developed using the Apex-Q desolvation system (ESI, Omaha, NE) to couple LC instrumentation with an ICP-MS device. The desolvation power of the system allowed greater concentrations of methanol to be introduced to the plasma prior to destabilization than with direct methanol injection into the plasma. Studies were performed, using simulated and actual linear methanol gradients, to find analyte-internal standard (AIS) pairs whose ratio remains consistent (deviations {+-} 10%) over methanol concentration ranges of 5%-35% (simulated) and 8%-32% (actual). Quadrupole (low resolution) and sector field (high resolution) ICP-MS instrumentation were utilized in these studies. Once an AIS pair is determined, quantification studies can be performed. First, an analysis is performed by adding both elements of the AIS pair post-column while performing the gradient elution without sample injection. A comparison of the ratio of the measured intensities to the atomic ratio of the two standards is used to determine a correction factor that can be used to account for the matrix effects caused by the mobile phase. Then, organic and/or biological molecules containing one of the two elements in the AIS pair are injected into the LC column. A gradient method is used to vary the methanol-water mixture in the mobile phase and to separate out the compounds in a given sample. A standard solution of the second ion in the AIS pair is added continuously post-column. By comparing the ratio of the measured intensities to the atomic ratio of the eluting compound and internal standard, the concentration of the injected compound can be determined.« less
Control of spontaneous emission from a microwave-field-driven four-level atom in an anisotropic photonic crystal

NASA Astrophysics Data System (ADS)

Zhang, Duo; Li, Jiahua; Ding, Chunling; Yang, Xiaoxue

2012-05-01

The spontaneous emission properties of a microwave-field-driven four-level atom embedded in anisotropic double-band photonic crystals (PCs) are investigated. We discuss the influences of the band-edge positions, Rabi frequency and detuning of the microwave field on the emission spectrum. It is found that several interesting features such as spectral-line enhancement, spectral-line suppression, spectral-line overlap, and multi-peak structures can be observed in the spectra. The proposed scheme can be achieved by use of a microwave-coupled field into hyperfine levels in rubidium atom confined in a photonic crystal. These theoretical investigations may provide more degrees of freedom to manipulate the atomic spontaneous emission.
High-pressure combustor exhaust emissions with improved air-atomizing and conventional pressure-atomizing fuel nozzles

NASA Technical Reports Server (NTRS)

Ingebo, R. D.; Norgren, C. T.

1973-01-01

A high-pressure combustor segment 0.456 meter (18 in.) long with a maximum cross section of 0.153 by 0.305 meter (6 by 12 in.) was tested with specially designed air-atomizing and conventional pressure-atomizing fuel nozzles at inlet-air temperatures of 340 to 755 k (610 deg to 1360 R), reference velocities of 12.4 to 26.1 meters per second (41 to 86 ft/sec), and fuel-air ratios of 0.008 to 0.020. Increasing inlet-air pressure from 4 to 20 atmospheres generally increased smoke number and nitric oxide, but decreased carbon monoxide and unburned hydrocarbon concentrations with air-atomizing and pressure-atomizing nozzles. Emission indexes for carbon monoxide and unburned hydrocarbons were lower at 4, 10, and 20 atmospheres, and nitric oxide emission indexes were lower at 10 and 20 atmospheres with air-atomizing than with pressure-atomizing nozzles.
Spectrophotometric determination of gold(III) in forensic and pharmaceutical samples and results complemented with ICP AES and EDXRF analysis

NASA Astrophysics Data System (ADS)

Nagaraja, Vani; Kumar, M. Kiran; Giddappa, Nagendrappa

2017-02-01

Spectrophotometric method with three systems were developed here for the determination of gold(III) using o-dianisidine, aniline sulphate and catechol. Gold(III),in the system 1 it oxidizes o-dianisidine, in the system 2 it oxidizes catechol followed by its coupling with o-dianisidine, in the system 3 it oxidizes catechol followed by its coupling with aniline sulphate forming dye products with respective λmax 446 nm, 540 nm, and 505 nm. All the three systems were optimized and analytical parameters were calculated. The molar absorptivity values were 9.27 × 104, 1.97 × 104 and 1.62 × 104 respectively for the systems 1, 2 and 3 with the corresponding Sandell sensitivity values (μg cm- 2), 0.0021, 0.0096 and 0.011. The optimized systems were used for the determination of gold present in some forensic jewellery and pharmaceutical samples and the results obtained were compared with the results of all samples determined by Inductively Coupled Plasma - Atomic Emission Spectrometric method and a few of them were also complemented by Energy Dispersive X-Ray Fluorescent spectral analysis.
Integrative functional genomics of salt acclimatization in the model legume Lotus japonicus.

PubMed

Sanchez, Diego H; Lippold, Felix; Redestig, Henning; Hannah, Matthew A; Erban, Alexander; Krämer, Ute; Kopka, Joachim; Udvardi, Michael K

2008-03-01

The model legume Lotus japonicus was subjected to non-lethal long-term salinity and profiled at the ionomic, transcriptomic and metabolomic levels. Two experimental designs with various stress doses were tested: a gradual step acclimatization and an initial acclimatization approach. Ionomic profiling by inductively coupled plasma/atomic emission spectrometry (ICP-AES) revealed salt stress-induced reductions in potassium, phosphorus, sulphur, zinc and molybdenum. Microarray profiling using the Lotus Genechip allowed the identification of 912 probesets that were differentially expressed under the acclimatization regimes. Gas chromatography/mass spectrometry-based metabolite profiling identified 147 differentially accumulated soluble metabolites, indicating a change in metabolic phenotype upon salt acclimatization. Metabolic changes were characterized by a general increase in the steady-state levels of many amino acids, sugars and polyols, with a concurrent decrease in most organic acids. Transcript and metabolite changes exhibited a stress dose-dependent response within the range of NaCl concentrations used, although threshold and plateau behaviours were also observed. The combined observations suggest a successive and increasingly global requirement for the reprogramming of gene expression and metabolic pathways to maintain ionic and osmotic homeostasis. A simple qualitative model is proposed to explain the systems behaviour of plants during salt acclimatization.
Influence of heavy metal stress on antioxidant status and DNA damage in Urtica dioica.

PubMed

Gjorgieva, Darinka; Kadifkova Panovska, Tatjana; Ruskovska, Tatjana; Bačeva, Katerina; Stafilov, Trajče

2013-01-01

Heavy metals have the potential to interact and induce several stress responses in the plants; thus, effects of heavy metal stress on DNA damages and total antioxidants level in Urtica dioica leaves and stems were investigated. The samples are sampled from areas with different metal exposition. Metal content was analyzed by Inductively Coupled Plasma-Atomic Emission Spectrometer (ICP-AES), for total antioxidants level assessment the Ferric-Reducing Antioxidant Power (FRAP) assay was used, and genomic DNA isolation from frozen plant samples was performed to obtain DNA fingerprints of investigated plant. It was found that heavy metal contents in stems generally changed synchronously with those in leaves of the plant, and extraneous metals led to imbalance of mineral nutrient elements. DNA damages were investigated by Random Amplified Polymorphic DNA (RAPD) technique, and the results demonstrated that the samples exposed to metals yielded a large number of new fragments (total 12) in comparison with the control sample. This study showed that DNA stability is highly affected by metal pollution which was identified by RAPD markers. Results suggested that heavy metal stress influences antioxidant status and also induces DNA damages in U. dioica which may help to understand the mechanisms of metals genotoxicity.
Effects of Ion-Releasing Tooth-Coating Material on Demineralization of Bovine Tooth Enamel

PubMed Central

Kawasaki, Koji; Kambara, Masaki

2014-01-01

We compared the effect of a novel ion-releasing tooth-coating material that contained S-PRG (surface-reaction type prereacted glass-ionomer) filler to that of non-S-PRG filler and nail varnish on the demineralization of bovine enamel subsurface lesions. The demineralization process of bovine enamel was examined using quantitative light-induced fluorescence (QLF) and electron probe microanalyzer (EPMA) measurement. Ion concentrations in demineralizing solution were measured using inductively coupled plasma atomic (ICP) emission spectrometry and an ion electrode. The nail varnish group and the non-S-PRG filler group showed linear demineralization. Although the nail varnish group and the non-S-PRG filler group showed linear demineralization, the S-PRG filler group did not. Further, plane-scanning by EPMA analysis in the S-PRG filler group showed no changes in Ca ion distribution, and F ions showed peak levels on the surface of enamel specimens. Most ions in the demineralizing solution were present at higher concentrations in the S-PRG filler group than in the other two groups. In conclusion, only the S-PRG filler-containing tooth-coating material released ions and inhibited demineralization around the coating. PMID:24578706
Automatic flow system for simultaneous determination of iron and chromium in steel alloys employing photometers based on LEDs as radiation source

PubMed Central

Fernandes, Ridvan N.; Campos, Luís Fernando P.

2003-01-01

A multicommutated flow system for simultaneous determination of iron and chromium in steel alloys by photometry is described. The flow network consisted of an automatic injector and four solenoid valves assembled to form two independent analytical pathways, each one comprising reaction coils and a flow cell. The light source (LED) and detector (photodiode) were attached to the flow cells to form a compact unit. The flow system was microcomputer controlled by Quick BASIC 4.5 software, which carried out all steps of the analytical procedure. The feasibility of the system was proved by the determination of iron and chromium in steel alloys and its accuracy was accessed by comparing results with those obtained by plasma atomic emission spectrometry (ICP-AES). No significant difference at the 95% confidence level was observed. Other profitable features such as low reagent consumption (0.33 mg 1,10-phenantroline and 0.03 mg 1,5-diphenylcarbazide per determination); relative standard deviations (n = 5) of 0.4% for iron and 1.2% for chromium; and an analytical throughput of 160 determinations per h were also achieved. PMID:18924884
A preliminary study of the phycological degradation of natural stone masonry.

PubMed

Welton, Ryan G; Cuthbert, Simon J; Mclean, Roger; Hursthouse, Andrew; Hughes, John

2003-03-01

For many years it has been realised that the weathering of stone is not merely determined by physical and chemical factors but also by biological agents. When the stone in question is a historic building or monument, the damage done constitutes an irretrievable loss of our heritage and history. Laboratory studies have commenced in Paisley to study the effect of photoautotrophs on the major sedimentary rock forming minerals, with a view to expanding this work to study the overall effect of these micro-organisms on heritage masonry. Tests were carried out on Albite, Calcite, Dolomite, Orthoclase, Siderite and Quartz, using axenic cultures of the following: Chlorella vulgaris, Chlorococcum tetrasporum, Scenedesmus obliquus, Oocystis marsonii, Stichococcus bacillaris. The rock chips were immersed in either water or bolds basal media and exposed to a mix of the micro-organisms listed above and then tested weekly for their pH, fortnightly for the waters chemical composition using inductively coupled plasma-atomic emission spectrometry (ICP-AES) and visually utilising the university's SEM facilities. Work so far has revealed biologically mediated etching of minerals, a well-defined pH profile over a period of 90 days, as well as a variety of elemental release patterns for the different minerals.
Biology and survival of extremely halophilic archaeon Haloarcula marismortui RR12 isolated from Mumbai salterns, India in response to salinity stress.

PubMed

Thombre, Rebecca S; Shinde, Vinaya D; Oke, Radhika S; Dhar, Sunil Kumar; Shouche, Yogesh S

2016-05-27

Haloarchaea are unique microorganism's resistant to environmental and osmotic stresses and thrive in their habitats despite extreme fluctuating salinities. In the present study, haloarchaea were isolated from hypersaline thalossohaline salterns of Bhandup, Mumbai, India and were identified as Haloferax prahovense, Haloferax alexandrines, Haloferax lucentense, Haloarcula tradensis, Haloarcula marismortui and Haloarcula argentinensis. The mechanism of adaptation to contrasting salinities (1.5 M and 4.5 M) was investigated in the extreme haloarchaeon, Hal. marismortui RR12. Hal. marismortui RR12 increased the intracellular sequestration of K(+) and Cl(-) ions in hypo salinity and hyper salinity respectively as detected by Energy-dispersive X-ray spectroscopy microanalysis (EDAX) and Inductively Coupled Plasma- atomic Emission Spectroscopy (ICP-AES) indicating the presence of 'salt-in' strategy of osmoadaptation. As a cellular response to salinity stress, it produced small heat shock like proteins (sHSP) identified using MALDI-TOF MS and increased the production of protective red carotenoid pigment. This is the first report on the study of the concomitant cellular, molecular and physiological mechanism adapted by Hal. marismortui RR12 when exposed to contrasting salinities in external environment.
A phosphorescent silver(I)-gold (I) cluster complex that specifically lights up the nucleolus of living cells with FLIM imaging.

PubMed

Chen, Min; Lei, Zhen; Feng, Wei; Li, Chunyan; Wang, Quan-Ming; Li, Fuyou

2013-06-01

The phosphorescent silver(I)-gold(I) cluster complex [CAu6Ag2(dppy)6](BF4)4 (N1) selectively stains the nucleolus, with a much lower uptake in the nucleus and cytoplasm, and exhibits excellent photostability. This Ag-Au cluster, which has a photoluminescent lifetime of microseconds, is particularly attractive as a probe in applications of time-gated microscopy. Investigation of the pathway of cellular entry indicated that N1 permeates the outer membrane and nuclear membrane of living cells through an energy-dependent and non-endocytic route within 10 min. High concentrations of N1 in the nucleolus have been quantified by inductively coupled plasma atomic emission spectroscopy (ICP-AES) and transmission electron microscopy coupled with an energy dispersive X-ray analysis (TEM-EDXA), which also helped to elucidate the mechanism of the specific staining. Intracellular selective staining may be correlated with the microenvironment of the nucleolus, which is consistent with experiments conducted at different phases of the cell cycle. These results prove that N1 is a very attractive phosphorescent staining reagent for visualizing the nucleolus of living cells. Copyright © 2013 Elsevier Ltd. All rights reserved.

Synthesis, characterization, magnetic and electrochemical properties of a new 3D hexa-copper-substituted germanotungstate

NASA Astrophysics Data System (ADS)

Li, Yanzhou; Luo, Jie; Zhang, Yanting; Zhao, Junwei; Chen, Lijuan; Ma, Pengtao; Niu, Jingyang

2013-09-01

An inorganic-organic hybrid hexa-copper-substituted germanotungstate Na2[Cu(dap)2]2[Cu(dap)2] {[Cu6(H2O)2(dap)2][B-α-GeW9O34]2}·4H2O (1) (dap=1,2-diaminopropane) has been hydrothermally prepared and characterized by elemental analyses, inductively coupled plasma atomic emission spectrometry (ICP-AES) analyses, IR spectra, powder X-ray diffraction (PXRD), thermogravimetric analysis (TGA) and single-crystal X-ray diffraction. 1 displays the six-connected 3D network with the long topological (O'Keefe) vertex symbol is 4·4·64·4·4·4·4·64·4·4·4·64·4·4·4 and the short vertex (Schläfli) symbol of 41263. Magnetic measurements indicate that there are the overall ferromagnetic exchange interactions in the belt-like hexa-CuII cluster in 1. Furthermore, the electrochemical behavior and electrocatalysis of 1 modified carbon paste electrode (1-CPE) have been studied. The reductions of nitrite, bromate and hydrogen peroxide are principally mediated by the WVI-based wave.
Development of Processing Techniques for Advanced Thermal Protection Materials

NASA Technical Reports Server (NTRS)

Selvaduray, Guna; Cox, Michael; Srinivasan, Vijayakumar

1997-01-01

Thermal Protection Materials Branch (TPMB) has been involved in various research programs to improve the properties and structural integrity of the existing aerospace high temperature materials. Specimens from various research programs were brought into the analytical laboratory for the purpose of obtaining and refining the material characterization. The analytical laboratory in TPMB has many different instruments which were utilized to determine the physical and chemical characteristics of materials. Some of the instruments that were utilized by the SJSU students are: Scanning Electron Microscopy (SEM), Energy Dispersive X-ray analysis (EDX), X-ray Diffraction Spectrometer (XRD), Fourier Transform-Infrared Spectroscopy (FTIR), Ultra Violet Spectroscopy/Visible Spectroscopy (UV/VIS), Particle Size Analyzer (PSA), and Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES). The above mentioned analytical instruments were utilized in the material characterization process of the specimens from research programs such as: aerogel ceramics (I) and (II), X-33 Blankets, ARC-Jet specimens, QUICFIX specimens and gas permeability of lightweight ceramic ablators. In addition to analytical instruments in the analytical laboratory at TPMB, there are several on-going experiments. One particular experiment allows the measurement of permeability of ceramic ablators. From these measurements, physical characteristics of the ceramic ablators can be derived.
Effects of Precipitant and pH on Coprecipitation of Nanosized Co-Cr-V Alloy Powders.

PubMed

Chen, Xiaoyu; Li, Yongxia; Huang, Lan; Zou, Dan; Wu, Enxi; Liu, Yanjun; Xie, Yuanyan; Yao, Rui; Liao, Songyi; Wang, Guangrong; Zheng, Feng

2017-09-21

Nanosized Co-Cr-V alloy powders were synthesized via coprecipitation method. Effects of precipitants ((NH₄)₂C₂O₄·H₂O and Na₂CO₃) and pH were investigated by X-ray diffraction (XRD), Zeta potential analyzer, thermogravimetry-differential scanning calorimetry (TG-DSC), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and scanning electron microscopy (SEM). Co-Cr-V alloy powders were consisted of major face-centered cubic Co (fcc Co) and minor hexagonal close-packed Co (hcp Co). Grain sizes of precursors and Co-Cr-V alloy powders were increased with pH value (7-10) within the ranges of 3~39 and 39~66 nm, respectively. Rod-like or granular Co-Cr-V alloy particles were assembled by interconnected nanograins. At pH = 7, Na₂CO₃ precipitant was found to be beneficial to maintain the desirable composition of Co-Cr-V powders. It was also found that lower pH favors the maintenance of pre-designed composition, while grain coarsens at higher pH. Effects of variation for precipitant and pH on the morphology and composition of Co-Cr-V alloy powder were discussed in detail and relevant mechanism was further proposed.
Human exposure assessment of silver and copper migrating from an antimicrobial nanocoated packaging material into an acidic food simulant.

PubMed

Hannon, Joseph Christopher; Kerry, Joseph P; Cruz-Romero, Malco; Azlin-Hasim, Shafrina; Morris, Michael; Cummins, Enda

2016-09-01

To examine the human exposure to a novel silver and copper nanoparticle (AgNP and CuNP)/polystyrene-polyethylene oxide block copolymer (PS-b-PEO) food packaging coating, the migration of Ag and Cu into 3% acetic acid (3% HAc) food simulant was assessed at 60 °C for 10 days. Significantly lower migration was observed for Ag (0.46 mg/kg food) compared to Cu (0.82 mg/kg food) measured by inductively coupled plasma - atomic emission spectrometry (ICP-AES). In addition, no distinct population of AgNPs or CuNPs were observed in 3% HAc by nanoparticle tracking analysis (NTA) and transmission electron microscopy (TEM). The predicted human exposure to Ag and Cu was used to calculate a margin of exposure (MOE) for ionic species of Ag and Cu, which indicated the safe use of the food packaging in a hypothetical scenario (e.g. as fruit juice packaging). While migration exceeded regulatory limits, the calculated MOE suggests current migration limits may be conservative for specific nano-packaging applications. Copyright © 2016 Elsevier Ltd. All rights reserved.
Spectrophotometric determination of gold(III) in forensic and pharmaceutical samples and results complemented with ICP AES and EDXRF analysis.

PubMed

Nagaraja, Vani; Kumar, M Kiran; Giddappa, Nagendrappa

2017-02-15

Spectrophotometric method with three systems were developed here for the determination of gold(III) using o-dianisidine, aniline sulphate and catechol. Gold(III),in the system 1 it oxidizes o-dianisidine, in the system 2 it oxidizes catechol followed by its coupling with o-dianisidine, in the system 3 it oxidizes catechol followed by its coupling with aniline sulphate forming dye products with respective λ max 446nm, 540nm, and 505nm. All the three systems were optimized and analytical parameters were calculated. The molar absorptivity values were 9.27×10 4 , 1.97×10 4 and 1.62×10 4 respectively for the systems 1, 2 and 3 with the corresponding Sandell sensitivity values (μgcm -2 ), 0.0021, 0.0096 and 0.011. The optimized systems were used for the determination of gold present in some forensic jewellery and pharmaceutical samples and the results obtained were compared with the results of all samples determined by Inductively Coupled Plasma - Atomic Emission Spectrometric method and a few of them were also complemented by Energy Dispersive X-Ray Fluorescent spectral analysis. Copyright © 2016 Elsevier B.V. All rights reserved.
[Separation/preconcentration of trace rare earth elements in Tricholoma giganteum by micro-column with nanometer A1203 and their determination by ICP-AES].

PubMed

Liu, Hong-gao; Wang, Yuan-zhong

2010-01-01

Using a micro-column packed with immobilized 1-phenyl-3-methyl-4-bonzoil-5-pyrazone(PMBP) on nanometer Al2O3 powder as the adsorption material, the adsorption and elution behaviors of rare earth ions (Sc3+, Y3+ and La3+) on the above material under dynamic conditions were studied with inductively coupled plasma-atomic emission spectrometry. The conditions for preconcentration of rare earth ions were optimized, and the results show that the studied ions can be adsorbed quantitatively on the above material at pH 4.5 and the analytes adsorbed on the column can be eluted with 0.5 mol x L(-1) HCl solution. The detection limits of the method for Sc, Y and La were 0.15, 0.18 and 0.34 microg x L(-1), respectively, and the relative standard deviations were 2.5%, 3.0% and 1.7%, respectively (n=12, c = 0.5 mg x L(-1)). The proposed method was applied to the determination of trace amount of Sc, Y and La in Tricholoma giganteum with satisfactory results.
Production and Characterization of a Ag- and Zn-Doped Glass-Ceramic Material and In Vitro Evaluation of Its Biological Effects

NASA Astrophysics Data System (ADS)

Baghbani, Fatemeh; Moztarzadeh, Fathollah; Mozafari, Masoud; Raz, Majid; Rezvani, Hamideh

2016-08-01

Bioactive glasses in the system SiO2-CaO-Na2O-P2O5-MgO with different amounts of zinc (Zn) and silver (Ag) were synthesized by the sol-gel technique and characterized. The bioactivity was studied during in vitro assays: the ability of hydroxycarbonate apatite (HCA) layer to form on the glass surface was examined after contact with simulated body fluid (SBF). The x-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, and inductively coupled plasma atomic emission spectrometry (ICP) studies were performed after immersion in vitro assays. Also, the antibacterial and antifungal activities of glass samples against Pseudomonas aeruginosa (ATCC 27853), E. coli (ATCC 25922), and Candida albicans were measured by the halo zone test. Introduction of zinc and silver as the trace elements induces several modifications on the observed phenomena at the glass surface and in SBF solution after immersion of the samples. The chemical durability of the glasses, the formation of the silica-rich layer, and the crystallization of the HCA layer were affected. Samples with the higher content of zinc and silver exhibited an excellent antibacterial/antifungal activity.
Application of Solid Phase Extraction on Multiwalled Carbon Nanotubes of Some Heavy Metal Ions to Analysis of Skin Whitening Cosmetics Using ICP-AES

PubMed Central

ALqadami, Ayoub A.; Abdalla, Mohammad Abulhassan; ALOthman, Zeid A.; Omer, Kamal

2013-01-01

A novel and highly sensitive method for the determination of some heavy metals in skin whitening cosmetics creams using multiwalled carbon nanotubes MWCNTs as solid phase extraction sorbent for the preconcentration of these heavy metals prior to their determination by inductively coupled plasma atomic emission spectrometry is described. Different practical parameters have been thoroughly investigated and the optimum experimental conditions were employed. The developed method was then applied for the determination of arsenic, bismuth, cadmium, mercury, lead and titanium in samples of skin whitening cosmetics. The detection limits under these conditions for As, Bi, Cd, Pb, Hg and Ti were 2.4, 4.08, 0.3, 2.1, 1.8, and 1.8 ng·mL−1, respectively. The relative standard deviations (RSDs) were found to be less than 2.0%. For validation, a certified reference material of NIST SRM 1570a spinach leaves was analyzed and the determined values were in good agreement with the certified values. The recoveries for spiked samples were found to be in the range of 89.6–104.4%. PMID:23343988
Posture systematically alters ear-canal reflectance and DPOAE properties

PubMed Central

Voss, Susan E.; Adegoke, Modupe F.; Horton, Nicholas J.; Sheth, Kevin N.; Rosand, Jonathan; Shera, Christopher A.

2010-01-01

Several studies have demonstrated that the auditory system is sensitive to changes in posture, presumably through changes in intracranial pressure (ICP) that in turn alter the intracochlear pressure, which affects the stiffness of the middle-ear system. This observation has led to efforts to develop an ear-canal based noninvasive diagnostic measure for monitoring ICP, which is currently monitored invasively via access through the skull or spine. Here, we demonstrate the effects of postural changes, and presumably ICP changes, on distortion product otoacoustic emissions (DPOAE) magnitude, DPOAE angle, and power reflectance. Measurements were made on 12 normal-hearing subjects in two postural positions: upright at 90 degrees and tilted at −45 degrees to the horizontal. Measurements on each subject were repeated five times across five separate measurement sessions. All three measures showed significant changes (p < 0.001) between upright and tilted for frequencies between 500 and 2000 Hz, and DPOAE angle changes were significant at all measured frequencies (500–4000 Hz). Intrasubject variability, assessed via standard deviations for each subject’s multiple measurements, were generally smaller in the upright position relative to the tilted position. PMID:20227475
Real-time measurement of size-resolved elemental composition ratio for flame synthesized composite nanoparticle aggregates using a tandem SMPS-ICP-OES

PubMed Central

Reed, Nathan; Fang, Jiaxi; Chavalmane, Sanmathi; Biswas, Pratim

2017-01-01

Composite nanoparticles find application in catalysis, drug delivery, and energy storage and require increasingly fine control of their physical properties and composition. While composite nanoparticles have been widely synthesized and characterized, little work has systematically correlated the initial concentration of precursors and the final composition of flame synthesized composite nanoparticles. This relationship is explored in a diffusion flame aerosol reactor by coupling a scanning mobility particle sizer (SMPS) with an inductively coupled plasma optical emission spectrometer (ICP-OES). A framework for studying the relationship between the initial precursor concentrations of different elements and the final nanoparticle composition is explored. The size-resolved elemental composition was measured by directly injecting size-selected fractions of aggregated magnetite and silicon dioxide composite nanoparticles into the ICP-OES plasma. This work showed a correlation between precursor molar ratio and the measured elemental ratio in the mobility size range of 50 to 140 nm. Building on previous work studying size resolved elemental composition of engineered nanoparticles, the analysis is extended to flame synthesized composite nanoparticle aggregates in this work. PMID:28435179
[Determination of 22 inorganic elements in different parts of Lantana camara by ICP-OES].

PubMed

Zhou, Wei-ming; Wang, Ru-yi; Chen, Liu-sheng; Huang, Chuan-bin

2014-09-01

To determine the contents of 22 inorganic elements in different parts of Lantana camara by inductively coupled plasma optical emission spectroscopy (ICP-OES). HNO3-H2 02 digested system was used to completely decomposed the organic compounds effectually by microwave digestion. 22 inorganic elements such as K, Ca, Mg, Fe, Al, Na, Zn, Mn and Cr were determined by ICP-OES under set up working conditions. The contents of K, Ca and Mg were the most in different parts of Lantana camrnara; The contents of K, Ca, Mg, Mn, Sr and Cu in the leaves of Lantana camara were more than that in the root and the branch. The contents of Fe and Na in the root of Lantana camara were more than that in the leaves and the branch. The contents of Pb and Cd were higher than the national standard and Cr had high content in different parts of Lantana camara. The determination method is quick, easy and accurate with high sensitivity,which can determine the contents of 22 inorganic elements accurately in different parts of Lantana camara.
Real-time measurement of size-resolved elemental composition ratio for flame synthesized composite nanoparticle aggregates using a tandem SMPS-ICP-OES.

PubMed

Reed, Nathan; Fang, Jiaxi; Chavalmane, Sanmathi; Biswas, Pratim

2017-01-01

Composite nanoparticles find application in catalysis, drug delivery, and energy storage and require increasingly fine control of their physical properties and composition. While composite nanoparticles have been widely synthesized and characterized, little work has systematically correlated the initial concentration of precursors and the final composition of flame synthesized composite nanoparticles. This relationship is explored in a diffusion flame aerosol reactor by coupling a scanning mobility particle sizer (SMPS) with an inductively coupled plasma optical emission spectrometer (ICP-OES). A framework for studying the relationship between the initial precursor concentrations of different elements and the final nanoparticle composition is explored. The size-resolved elemental composition was measured by directly injecting size-selected fractions of aggregated magnetite and silicon dioxide composite nanoparticles into the ICP-OES plasma. This work showed a correlation between precursor molar ratio and the measured elemental ratio in the mobility size range of 50 to 140 nm. Building on previous work studying size resolved elemental composition of engineered nanoparticles, the analysis is extended to flame synthesized composite nanoparticle aggregates in this work.
Assessment of the Effects Exerted by Acid and Alkaline Solutions on Bone: Is Chemistry the Answer?

PubMed

Amadasi, Alberto; Camici, Arianna; Porta, Davide; Cucca, Lucia; Merli, Daniele; Milanese, Chiara; Profumo, Antonella; Rassifi, Nabila; Cattaneo, Cristina

2017-09-01

The treatment of corpses with extremely acid or basic liquids is sometimes performed in criminal contexts. A thorough characterization by chemical analysis may provide further help to macroscopic and microscopic analysis; 63 porcine bone samples were treated with solutions at different pH (1-14) for immersion periods up to 70 days, as well as in extremely acidic sulfuric acid solutions (9 M/18 M) and extremely basic sodium hydroxide. Inductively coupled optical emission spectrometry (ICP-OES)/plasma mass spectrometry (ICP-MS), Fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray analysis (EDX), X-ray powder diffraction (XRPD), and scanning electron microscopy (SEM) showed that only the sulfuric acid solution 18 M was able to completely dissolve the sample. In addition, chemical analysis allowed to recognize the contact between bone and substances. Hydrated calcium sulfate arose from extreme pH. The possibility of detecting the presence of human material within the residual solution was demonstrated, especially with FT-IR, ICP-OES, and EDX. © 2017 American Academy of Forensic Sciences.
Simultaneous trace multielement determination by ICP-OES after solid phase extraction with modified octadecyl silica gel.

PubMed

Karbasi, Mohamad-Hadi; Jahanparast, Babak; Shamsipur, Mojtaba; Hassan, Jalal

2009-10-15

Multielement simultaneous determination of 35 trace elements in environmental samples was carried out by inductively coupled plasma emission spectrometry (ICP-OES) after preconcentration with octadecyl silicagel, modified with aurin tricarboxylic acid (Aluminon). Optimal experimental conditions including pH of sample solution, sample volume, sample and eluent flow rate, type, concentration and volume of eluent and foreign ions effect were investigated and established. Trace element ions in aqueous solution were quantitatively adsorbed onto octadecyl silicagel modified with aurin tricarboxylic acid at pH 8.0 with a flow rate of 11.0 mL min(-1). The adsorbed element ions were eluted with 3-5 mL of 0.5 mol L(-1) HNO(3) at a flow rate of 10.0 mL min(-1) and analyzed by ICP-OES simultaneously. The proposed method has at least preconcentration factor of 100 in water samples, which results high sensitive detection of ultra-trace and trace analysis. The present methodology gave recoveries better than 70% and RSD less than 16%.
Determination of cobalt species in nutritional supplements using ICP-OES after microwave-assisted extraction and solid-phase extraction.

PubMed

Bartosiak, Magdalena; Jankowski, Krzysztof; Giersz, Jacek

2018-06-05

Cobalt content (as vitamin B 12 and inorganic cobalt) in two nutritional supplements, namely Spirulina platensis and Saccharomyces cerevisiae known as a "superfood", has been determined using inductively coupled plasma optical emission spectrometry (ICP-OES). Several sample pre-treatment protocols have been applied and compared. Microwave-assisted acid digestion efficiently decomposed all cobalt-containing compounds, thus allowed obtaining total cobalt content in supplements examined. Vitamin B 12 was extracted from the samples with acetate buffer and potassium cyanide solution exposed to mild microwave radiation for 30 min, and cyanocobalamin was separated from the extract by on-column solid phase extraction using C-18 modified silica bed. About 100% of cobalt species was extracted using the triple microwave-assisted extraction procedure. Total cobalt content was 20-fold greater in Spirulina tablets than the declared cobalamin content (as Co). The ICP-OES method precision was about 3% and detection limit was 1.9 and 2.7 ng Co mL -1 for inorganic cobalt or cyanocobalamin, respectively. Copyright © 2018 Elsevier B.V. All rights reserved.
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.
Method for atmospheric pressure reactive atom plasma processing for surface modification

DOEpatents

Carr, Jeffrey W [Livermore, CA

2009-09-22

Reactive atom plasma processing can be used to shape, polish, planarize and clean the surfaces of difficult materials with minimal subsurface damage. The apparatus and methods use a plasma torch, such as a conventional ICP torch. The workpiece and plasma torch are moved with respect to each other, whether by translating and/or rotating the workpiece, the plasma, or both. The plasma discharge from the torch can be used to shape, planarize, polish, and/or clean the surface of the workpiece, as well as to thin the workpiece. The processing may cause minimal or no damage to the workpiece underneath the surface, and may involve removing material from the surface of the workpiece.
Improving catchment scale water quality modelling with continuous high resolution monitoring of metals in runoff

NASA Astrophysics Data System (ADS)

Saari, Markus; Rossi, Pekka; Blomberg von der Geest, Kalle; Mäkinen, Ari; Postila, Heini; Marttila, Hannu

2017-04-01

High metal concentrations in natural waters is one of the key environmental and health problems globally. Continuous in-situ analysis of metals from runoff water is technically challenging but essential for the better understanding of processes which lead to pollutant transport. Currently, typical analytical methods for monitoring elements in liquids are off-line laboratory methods such as ICP-OES (Inductively Coupled Plasma Optical Emission Spectroscopy) and ICP-MS (ICP combined with a mass spectrometer). Disadvantage of the both techniques is time consuming sample collection, preparation, and off-line analysis at laboratory conditions. Thus use of these techniques lack possibility for real-time monitoring of element transport. We combined a novel high resolution on-line metal concentration monitoring with catchment scale physical hydrological modelling in Mustijoki river in Southern Finland in order to study dynamics of processes and form a predictive warning system for leaching of metals. A novel on-line measurement technique based on micro plasma emission spectroscopy (MPES) is tested for on-line detection of selected elements (e.g. Na, Mg, Al, K, Ca, Fe, Ni, Cu, Cd and Pb) in runoff waters. The preliminary results indicate that MPES can sufficiently detect and monitor metal concentrations from river water. Water and Soil Assessment Tool (SWAT) catchment scale model was further calibrated with high resolution metal concentration data. We show that by combining high resolution monitoring and catchment scale physical based modelling, further process studies and creation of early warning systems, for example to optimization of drinking water uptake from rivers, can be achieved.
Application of ICP-OES for evaluating energy extraction and production wastewater discharge impacts on surface waters in Western Pennsylvania.

PubMed

Pancras, Joseph Patrick; Norris, Gary A; Landis, Matthew S; Kovalcik, Kasey D; McGee, John K; Kamal, Ali S

2015-10-01

Oil and gas extraction and coal-fired electrical power generating stations produce wastewaters that are treated and discharged to rivers in Western Pennsylvania with public drinking water system (PDWS) intakes. Inductively coupled plasma optical emission spectroscopy (ICP-OES) was used to quantify inorganic species in wastewater and river samples using a method based on EPA Method 200.7 rev4.4. A total of 53 emission lines from 30 elements (Al, As, B, Ba, Ca, Cd, Ce, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, S, Sb, Se, Si, Sn, Sr, Ti, Tl, V, and Zn) were investigated. Samples were prepared by microwave-assisted acid digestion using a mixture of 2% HNO3 and 0.5% HCl. Lower interferences and better detection characteristics resulted in selection of alternative wavelengths for Al, As, Sb, Mg, Mo, and Na. Radial view measurements offered accurate determinations of Al, Ba, K, Li, Na, and Sr in high-brine samples. Spike recovery studies and analyses of reference materials showed 80-105% recoveries for most analytes. This method was used to quantify species in samples with high to low brine concentrations with method detection limits a factor of 2 below the maximum contaminant limit concentrations of national drinking water standards. Elements B, Ca, K, Li, Mg, Na, and Sr were identified as potential tracers for the sources impacting PDWS intakes. Usability of the ICP-OES derived data for factor analytic model applications was also demonstrated. Published by Elsevier B.V.
Spontaneous emission and atomic line shift in causal perturbation theory

NASA Astrophysics Data System (ADS)

Marzlin, Karl-Peter; Fitzgerald, Bryce

2018-04-01

We derive a spontaneous emission rate and line shift for two-level atoms coupled to the radiation field using causal perturbation theory. In this approach, employing the theory of distribution splitting prevents the occurrence of divergent integrals. Our method confirms the result for an atomic decay rate but suggests that the cutoff frequency for the atomic line shift is determined by the atomic mass, rather than the Bohr radius or electron mass.

Investigation of mass dependence effects for the accurate determination of molybdenum isotope amount ratios by MC-ICP-MS using synthetic isotope mixtures.

PubMed

Malinovsky, Dmitry; Dunn, Philip J H; Petrov, Panayot; Goenaga-Infante, Heidi

2015-01-01

Methodology for absolute Mo isotope amount ratio measurements by multicollector inductively coupled plasma-mass spectrometry (MC-ICP-MS) using calibration with synthetic isotope mixtures (SIMs) is presented. For the first time, synthetic isotope mixtures prepared from seven commercially available isotopically enriched molybdenum metal powders ((92)Mo, (94)Mo, (95)Mo, (96)Mo, (97)Mo, (98)Mo, and (100)Mo) are used to investigate whether instrumental mass discrimination of Mo isotopes in MC-ICP-MS is consistent with mass-dependent isotope distribution. The parent materials were dissolved and mixed as solutions to obtain mixtures with accurately known isotope amount ratios. The level of elemental impurities in the isotopically enriched molybdenum metal powders was quantified by ICP-MS by using both high-resolution and reaction cell instruments to completely resolve spectral interferences. The Mo isotope amount ratio values with expanded uncertainty (k = 2), determined by MC-ICP-MS for a high-purity Mo rod from Johnson Matthey, were as follows: (92)Mo/(95)Mo = 0.9235(9), (94)Mo/(95)Mo = 0.5785(8), (96)Mo/(95)Mo = 1.0503(9), (97)Mo/(95)Mo = 0.6033(6), (98)Mo/(95)Mo = 1.5291(20), and (100)Mo/(95)Mo = 0.6130(7). A full uncertainty budget for the measurements is presented which shows that the largest contribution to the uncertainty budget comes from correction for elemental impurities (∼51%), followed by the contribution from weighing operations (∼26 %). The atomic weight of molybdenum was calculated to be 95.947(2); the uncertainty in parentheses is expanded uncertainty with the coverage factor of 2. A particular advantage of the developed method is that calibration factors for all six Mo isotope amount ratios, involving the (95)Mo isotope, were experimentally determined. This allows avoiding any assumption on mass-dependent isotope fractions in MC-ICP-MS, inherent to the method of double spike previously used for Mo isotope amount ratio measurements. However, data obtained in this study show that instrumental mass discrimination in MC-ICP-MS is consistent with mass-dependent Mo isotope fractionation. This was demonstrated by a good agreement between experimentally obtained and theoretically expected values of the exponent of isotope fractionation, β, for each triad of Mo isotopes.
Identification of platinum nanoparticles in road dust leachate by single particle inductively coupled plasma-mass spectrometry.

PubMed

Folens, Karel; Van Acker, Thibaut; Bolea-Fernandez, Eduardo; Cornelis, Geert; Vanhaecke, Frank; Du Laing, Gijs; Rauch, Sebastien

2018-02-15

Elevated platinum (Pt) concentrations are found in road dust as a result of emissions from catalytic converters in vehicles. This study investigates the occurrence of Pt in road dust collected in Ghent (Belgium) and Gothenburg (Sweden). Total Pt contents, determined by tandem ICP-mass spectrometry (ICP-MS/MS), were in the range of 5 to 79ngg -1 , comparable to the Pt content in road dust of other medium-sized cities. Further sample characterization was performed by single particle (sp) ICP-MS following an ultrasonic extraction procedure using stormwater runoff for leaching. The method was found to be suitable for the characterization of Pt nanoparticles in road dust leachates. The extraction was optimized using road dust reference material BCR-723, for which an extraction efficiency of 2.7% was obtained by applying 144kJ of ultrasonic energy. Using this method, between 0.2% and 18% of the Pt present was extracted from road dust samples. spICP-MS analysis revealed that Pt in the leachate is entirely present as nanoparticles of sizes between 9 and 21nm. Although representing only a minor fraction of the total content in road dust, the nanoparticulate Pt leachate is most susceptible to biological uptake and hence most relevant in terms of bioavailability. Copyright © 2017 Elsevier B.V. All rights reserved.
Metal characterization of white hawthorn organs and infusions.

PubMed

Juranović Cindrić, Iva; Zeiner, Michaela; Konanov, Darija Mihajlov; Stingeder, Gerhard

2015-02-18

Hawthorn is one of the most commonly used European and North American phytopharmaceuticals. Because there is no information on metals in seeds, and only rare data for leaves and flowers, the aim of the present study was elemental analysis of the white hawthorn (Crataegus monogyna) by inductively coupled plasma emission spectrometry (ICP-AES) or inductively coupled plasma mass spectrometry (ICP-MS) after digestion in a microwave-assisted system. The limits of detection are below 2 μg/g for ICP-AES and 0.5 μg/g for ICP-MS. Hawthorn leaves and flowers contain essential elements at concentrations (mean values, RSD 2-8%) in mg/g of Ca, 1-4; K, 4-5; Mg, 1-2; and Na, <0.2); and at μg/g levels of Ba, 1-10; Co, <0.16; Cr, <1.4; Cu, 0.6-7; Fe, 1-37; Li, <0.5; Mn, 1-13; Mo, <0.17; Ni, <0.6; Sr, 0.2-2; and Zn, 1-31. Toxic elements were found in low quantities: As (<0.04), Cd (0.04-0.1), and Pb (0.1-2). Up to 10% of the metals is extracted into the infusions. The analyzed plant parts and infusions contain essential elements justifying its use as a medicinal plant, whereas the low quantities of harmful elements will not pose any risk to humans when consumed.
Multiple Method Analysis of TiO2 Nanoparticle Uptake in Rice (Oryza sativa L.) Plants.

PubMed

Deng, Yingqing; Petersen, Elijah J; Challis, Katie E; Rabb, Savelas A; Holbrook, R David; Ranville, James F; Nelson, Bryant C; Xing, Baoshan

2017-09-19

Understanding the translocation of nanoparticles (NPs) into plants is challenging because qualitative and quantitative methods are still being developed and the comparability of results among different methods is unclear. In this study, uptake of titanium dioxide NPs and larger bulk particles (BPs) in rice plant (Oryza sativa L.) tissues was evaluated using three orthogonal techniques: electron microscopy, single-particle inductively coupled plasma mass spectroscopy (spICP-MS) with two different plant digestion approaches, and total elemental analysis using ICP optical emission spectroscopy. In agreement with electron microscopy results, total elemental analysis of plants exposed to TiO 2 NPs and BPs at 5 and 50 mg/L concentrations revealed that TiO 2 NPs penetrated into the plant root and resulted in Ti accumulation in above ground tissues at a higher level compared to BPs. spICP-MS analyses revealed that the size distributions of internalized particles differed between the NPs and BPs with the NPs showing a distribution with smaller particles. Acid digestion resulted in higher particle numbers and the detection of a broader range of particle sizes than the enzymatic digestion approach, highlighting the need for development of robust plant digestion procedures for NP analysis. Overall, there was agreement among the three techniques regarding NP and BP penetration into rice plant roots and spICP-MS showed its unique contribution to provide size distribution information.
EVALUATION OF IODINE BASED IMPINGER SOLUTIONS FOR THE EFFICIENT CAPTURE OF HG USING DIRECT INJECTION NEBULIZATION INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY (DIN-ICP/MS) ANALYSIS

EPA Science Inventory

Currently there are no EPA reference sampling methods that have been promulgated for measuring stack emissions of Hg from coal combustion sources, however, EPA Method 29 is most commonly applied. The draft ASTM Ontario Hydro Method for measuring oxidized, elemental, particulate-b...
Liquid-Arc/Spark-Excitation Atomic-Emission Spectroscopy

NASA Technical Reports Server (NTRS)

Schlagen, Kenneth J.

1992-01-01

Constituents of solutions identified in situ. Liquid-arc/spark-excitation atomic-emission spectroscopy (LAES) is experimental variant of atomic-emission spectroscopy in which electric arc or spark established in liquid and spectrum of light from arc or spark analyzed to identify chemical elements in liquid. Observations encourage development of LAES equipment for online monitoring of process streams in such industries as metal plating, electronics, and steel, and for online monitoring of streams affecting environment.
Spreadsheet-Based Program for Simulating Atomic Emission Spectra

ERIC Educational Resources Information Center

Flannigan, David J.

2014-01-01

A simple Excel spreadsheet-based program for simulating atomic emission spectra from the properties of neutral atoms (e.g., energies and statistical weights of the electronic states, electronic partition functions, transition probabilities, etc.) is described. The contents of the spreadsheet (i.e., input parameters, formulas for calculating…
High concentrations of heavy metals in PM from ceramic factories of Southern Spain

NASA Astrophysics Data System (ADS)

Sánchez de la Campa, Ana M.; de la Rosa, Jesús D.; González-Castanedo, Yolanda; Fernández-Camacho, Rocío; Alastuey, Andrés; Querol, Xavier; Pio, Casimiro

2010-06-01

In this study, physicochemical characterization of Atmospheric Particulate Matter (PM) was performed in an urban-industrial site background (Bailén, Southern Spain), highly influenced by the impact of emission plumes from ceramic factories. This area is considered one of the towns with the highest PM 10 levels and average SO 2 concentration in Spain. A three stages methodology was used: 1) real-time measurements of levels of PM 10 and gaseous pollutants, and sampling of PM; 2) chemical characterization using ICP-MS, ICP-OES, CI and TOT, and source apportionment analysis (receptor modelling) of PM; and 3) chemical characterization of emission plumes derived from representative factories. High ambient air concentrations were found for most major components and trace elements compared with other industrialized towns in Spain. V and Ni are considered fingerprints of PM derived from the emissions of brick factories in this area, and were shown to be of particular interest. This highlights the high V and Ni concentrations in PM 10 (122 ngV/m 3 and 23.4 ngNi/m 3), with Ni exceeding the 2013 annual target value for the European Directive 2004/107/EC (20 ng/m 3). The methodology of this work can be used by Government departments responsible for Environment and Epidemiology in planning control strategies for improving air quality.
Remote air lasing for trace detection

NASA Astrophysics Data System (ADS)

Dogariu, Arthur; Michael, James B.; Miles, Richard B.

2011-05-01

We demonstrate coherent light propagating backwards from a remotely generated high gain air laser. A short ultraviolet laser pulse tuned to a two-photon atomic oxygen electronic resonance at 226 nm simultaneously dissociates the oxygen molecules in air and excites the resulting atomic oxygen fragments. Due to the focal depth of the pumping laser, a millimeter long region of high gain is created in air for the atomic oxygen stimulated emission at 845nm. We demonstrate that the gain in excess of 60 cm-1 is responsible for both forward and backwards emission of a strong, collimated, coherent laser beam. We present evidence for coherent emission and characterize the backscattered laser beam while varying the pumping conditions. The optical gain and directional emission allows for six orders of magnitude enhancement for the backscattered emission when compared with the fluorescence emission collected into the same solid angle. . This opens new opportunities for the remote detection capabilities of trace species, and provides much greater range for the detection of optical molecular and atomic features from a distant target.
Effect of the cesium and potassium doping of multiwalled carbon nanotubes grown in an electrical arc on their emission characteristics

NASA Astrophysics Data System (ADS)

Izrael'yants, K. R.; Orlov, A. P.; Ormont, A. B.; Chirkova, E. G.

2017-04-01

The effect of cesium and potassium atoms deposited onto multiwalled carbon nanotubes grown in an electrical arc on their emission characteristics was studied. The current-voltage characteristics of the field electron emission of specimens with cesium or potassium doped multiwalled carbon nanotubes of this type were revealed to retain their linear character in the Fowler-Nordheim coordinates within several orders of magnitude of change in the emission current. The deposition of cesium and potassium atoms was shown to lead to a considerable increase in the emission current and a decrease in the work function φ of studied emitters with multiwalled nanotubes. The work function was established to decrease to φ 3.1 eV at an optimal thickness of coating with cesium atoms and to φ 2.9 eV in the case of doping with potassium atoms. Cesium and potassium deposition conditions optimal for the attainment of a maximum emission current were found.
Occupational exposure to manganese-containing welding fumes and pulmonary function indices among natural gas transmission pipeline welders.

PubMed

Hassani, Hamid; Golbabaei, Farideh; Ghahri, Asghar; Hosseini, Mostafa; Shirkhanloo, Hamid; Dinari, Behnam; Eskandari, Davood; Fallahi, Majid

2012-01-01

The objectives of this study were to evaluate manganese (Mn)-containing welding fumes' exposure, assess urinary Mn as a biomarker for Mn exposure and investigate the correlation of Mn in air, total fumes and urinary Mn with pulmonary function indices in 118 welders and 37 unexposed controls from two regions in Iran, Assaluyeh and Borujen. Air samples were collected on mixed cellulose ester membrane filters in personal air samplers and then analyzed using inductively coupled plasma atomic emission spectroscopy (ICP-AES) (NIOSH Method 7300). For all participants, urine samples were collected during the entire work shift, and Mn in urine was determined by graphite furnace atomic absorption spectroscopy according to NIOSH Method 8310. Spirometric measurements were also done for participants. The maximum exposures to airborne Mn and total fumes were 0.304 ± 0.256 mg/m(3) and 21.52 ± 9.40 mg/m(3), respectively. The urine Mn levels in the various groups ranged between 0.77 to 7.58 μg/l. The correlation between airborne Mn and urinary Mn was significant for total whole participants. Some values of spirometric indices were statistically lower in welders rather than controls. Our results indicate that many welders have been exposed to higher concentrations of Mn-containing welding fumes. Urinary Mn can be used as a biomarker for Mn exposure. There were weak inverse correlations between Mn-containing welding fumes and pulmonary function indices, and the inverse correlation between urinary Mn with forced vital capacities (FVC) and forced expiratory volume in 1 s (FEV1) was significant.
Lead levels of edibles grown in contaminated residential soils: a field survey.

PubMed

Finster, Mary E; Gray, Kimberly A; Binns, Helen J

2004-03-29

Plants grown in lead contaminated soils can accumulate lead from the adherence of dust and translocation into the plant tissue. In order to evaluate the potential health hazard due to the consumption of plants grown in residential gardens contaminated by lead, a survey of the lead concentrations in a typical array of edible vegetables, fruits and herbs was conducted. Samples of garden plants harvested from the field were washed with detergent or water alone to remove adhered soil. They were dried, separated into sections including root, shoot and edible fruit, and then analyzed for lead content using inductively coupled plasma-atomic emission spectrometry (ICP-AES). Soil samples, taken in conjunction with the plant harvesting, were analyzed using flame atomic absorbance (FAA). A pattern of lead transference from soil through the root to the stem and leaves of garden crops was found. The majority of the lead was concentrated in the roots (root:soil ranging from 0.02 to 0.51), with some translocation into the shoots (shoot:soil as high as 0.10). This pattern is a concern particularly for crops in which the root, stems, stalks or leaves are edible. The lead concentration in fruiting vegetables was less than the detection limit of 10 ppm (microgram lead/gram dry plant matter). Some edible portions of the leafy vegetables and herbs, however, were found to have lead levels that, if consumed, could contribute to the total body burden of lead. Therefore, urban gardeners should test the lead levels in their soils and develop strategies to ensure safety.
Stoichiometry determination of (Pb,La)(Zr,Ti)O3-type nano-crystalline ferroelectric ceramics by wavelength-dispersive X-ray fluorescence spectrometry.

PubMed

Sitko, Rafał; Zawisza, Beata; Kita, Andrzej; Płońska, Małgorzata

2006-07-01

Analysis of small samples of lanthanum-doped lead zirconate titanate (PLZT) by wavelength-dispersive X-ray fluorescence spectrometry (WDXRF) is presented. The powdered material in ca. 30 mg was suspended in water and collected on the membrane filter. The pure oxide standards (PbO, La2O3, ZrO2 and TiO2) were used for calibration. The matrix effects were corrected using a theoretical influence coefficients algorithm for intermediate-thickness specimens. The results from XRF method were compared with the results from the inductively coupled plasma optical emission spectrometry (ICP-OES). Agreement between XRF and ICP-OES analysis was satisfactory and indicates the usefulness of XRF method for stoichiometry determination of PLZT.
Multielement analysis and antioxidant capacity of Merlot wine clones developed in Montenegro.

PubMed

Đorđević, Neda O; Pejin, Boris; Novaković, Miroslav M; Stanković, Dalibor M; Mutić, Jelena J; Pajović, Snežana B; Tešević, Vele V

2018-02-01

The overall aim of this paper was to compare the multielement composition and antioxidant capacity of two Montenegrin Merlot wines obtained from specific vine clones (VCR1 and VCR 101) along with commercial Merlot wine throughout the consecutive vintages in 2010 and 2011. Elemental composition was analysed using inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). Additionally, antioxidant capacity was assessed by cyclic voltammetry. VCR 1 wine from 2011 stood out for its elemental composition. On the other hand, antioxidant capacity of VCR 101 wines was the highest one for the both vintages. According to the experimental data obtained, all three wines are good source of essential elements and products with a significant antioxidant activity and specific geographical origin.
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.
Gunshot residue (GSR) analysis by single particle inductively coupled plasma mass spectrometry (spICP-MS).

PubMed

Heringer, Rodrigo D; Ranville, James F

2018-05-25

Single particle inductively coupled plasma mass spectrometry (spICP-MS) was investigated as a screening-level technique for the analysis and characterization of inorganic gunshot residue (IGSR) nanoparticles. spICP-MS works with undigested samples whereby nanoparticles (NPs) in a suspension are individually atomized and ionized as they reach the plasma, each resulting in a pulse of analyte ions that can be quantified. The method is rapid, and signals from hundreds of NPs can be collected in 1-2min per sample. The technique is quantitative for NP mass and number concentration when only one element (single element mode) is measured using a quadrupole MS. Likewise, a qualitative elemental fingerprint can be obtained for individual NPs when peak-hopping between two elements (dual element mode). For this proof of concept study, each shooter's hand was sampled with ultrapure water or swab to obtain NPs suspensions. Measurements of antimony, barium, and lead were performed using both analysis modes. With no sample preparation and fully automated sample introduction, it is possible to analyze more than 100 samples in a day. Results show that this technique opens a new perspective for future research on GSR sample identification and characterization and can complement SEM/EDX analysis. Copyright © 2018 Elsevier B.V. All rights reserved.
Selective hydride generation- cryotrapping- ICP-MS for arsenic speciation analysis at picogram levels: analysis of river and sea water reference materials and human bladder epithelial cells

PubMed Central

Matoušek, Tomáš; Currier, Jenna M.; Trojánková, Nikola; Saunders, R. Jesse; Ishida, María C.; González-Horta, Carmen; Musil, Stanislav; Mester, Zoltán; Stýblo, Miroslav; Dědina, Jiří

2013-01-01

An ultra sensitive method for arsenic (As) speciation analysis based on selective hydride generation (HG) with preconcentration by cryotrapping (CT) and inductively coupled plasma- mass spectrometry (ICP-MS) detection is presented. Determination of valence of the As species is performed by selective HG without prereduction (trivalent species only) or with L-cysteine prereduction (sum of tri- and pentavalent species). Methylated species are resolved on the basis of thermal desorption of formed methyl substituted arsines after collection at −196°C. Limits of detection of 3.4, 0.04, 0.14 and 0.10 pg mL−1 (ppt) were achieved for inorganic As, mono-, di- and trimethylated species, respectively, from a 500 μL sample. Speciation analysis of river water (NRC SLRS-4 and SLRS-5) and sea water (NRC CASS-4, CASS-5 and NASS-5) reference materials certified to contain 0.4 to 1.3 ng mL−1 total As was performed. The concentrations of methylated As species in tens of pg mL−1 range obtained by HG-CT-ICP-MS systems in three laboratories were in excellent agreement and compared well with results of HG-CT-atomic absorption spectrometry and anion exchange liquid chromatography- ICP-MS; sums of detected species agreed well with the certified total As content. HG-CT-ICP-MS method was successfully used for analysis of microsamples of exfoliated bladder epithelial cells isolated from human urine. Here, samples of lysates of 25 to 550 thousand cells contained typically tens pg up to ng of iAs species and from single to hundreds pg of methylated species, well within detection power of the presented method. A significant portion of As in the cells was found in the form of the highly toxic trivalent species. PMID:24014931
The Means: Cytometry and Mass Spectrometry Converge in a Single Cell Deep Profiling Platform

PubMed Central

Weis-Garcia, Frances; Bandura, Dmitry; Baranov, Vladimir; Ornatsky, Olga; Tanner, Scott

2013-01-01

Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a distinct flavor of mass spectrometry that has had little association with cell biology: it remains the state of the art for the determination of the atomic composition of materials. Unrelatedly, flow cytometry is the superior method for distinguishing the heterogeneity of cells through the determination of antigen signatures using tagged antibodies. Simply replacing fluorophore tags with stable isotopes of the heavy metals, and measuring these cell-by-cell with ICP-MS, dramatically increases the number of probes that can be simultaneously measured in cytometry and enables a transformative increase in the resolution of rare cell populations in complex biological samples. While this can be thought of as a novel incarnation of single-cell targeted proteomics, the metal-labeling reagents, ICP-MS of single cells, and accompanying informatics comprise a new field of technology termed Mass Cytometry. While the conception of mass cytometry is simple the embodiment to address the issues of multi-parameter flow cytometry has been far more challenging. There are many elements, and many more stable isotopes of those elements, that might be used as distinct reporter tags. Still, there are many approaches to conjugating metals to antibodies (or other affinity reagents) and work in this area along with developing new applications is ongoing. The mass resolution and linear (quantitative) dynamic range of ICP-MS allows those many stable isotopes to be measured simultaneously and without the spectral overlap issues that limit fluorescence assay. However, the adaptation of ICP-MS to allow high-speed simultaneous measurement with single cell distinction at high throughput required innovation of the cell introduction system, ion optics (sampling, transmission and beam-shaping), mass analysis, and signal handling and processing. An overview of “the nuts and bolts” of Mass Cytometry is presented.
Multianalytical determination of trace elements in atmospheric biomonitors by k0-INAA, ICP-MS and AAS

NASA Astrophysics Data System (ADS)

Freitas, M. C.; Pacheco, A. M. G.; Dionísio, I.; Sarmento, S.; Baptista, M. S.; Vasconcelos, M. T. S. D.; Cabral, J. P.

2006-08-01

Elemental contents of atmospheric biomonitors—epiphytic lichens and tree bark, exposed in continuous and discontinuous modes—have been assessed through k0-standardised instrumental neutron activation analysis ( k0-INAA) (two different institutions), inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectrometry (AAS). Certified reference materials—ISE-921 (river clay), NIST-1547 (peach leaves), ICHTJ-INCT-TL-1 (tea leaves; TL-1 hereinafter) and IAEA-336 (lichen material), and nonparametric statistics—rank-order correlations (Spearman RS) and enhanced-sign tests (Wilcoxon T)—were used for analytical control and data comparison, respectively. In general, quality of procedures was deemed good, except for k0-INAA in determining Br, Cu and Na, all likely affected by high counting statistics, and/or contamination issues (the latter). Results for Cu, Ni, Pb and Sr (by both ICP-MS and AAS) revealed that, despite an outstanding correlation (asymptotic p=0.000), they could be viewed as statistically equal for Cu only: AAS tended to yield higher values for Pb and Ni, and lower ones for Sr. The comparison between ICP-MS and k0-INAA data from TUDelft, for Al, Ca, Cu, Mg, Mn, Na, Ti and V, showed an excellent correlation (as above) and random (relative) magnitude for Cu, Mg, Mn and Ti only: ICP-MS tended to yield higher values for Al, Na and V, and lower ones for Ca, whereas between k0-INAA data from TUDelft and ITN, for Br, Ca and Na, resulted in systematically higher [Br] and [Ca] variates from TUDelft, even if all corresponding data sets were found to correlate at stringent significance levels. In a few cases, though—Ca, Sr in lichens; Pb in bark—matrix effects did appear to interfere in the outcome of matched-pairs, signed-rank tests, since random hierarchy of variates could be asserted just when lichen and bark data sets were processed separately.
Fate of Lu(III) sorbed on 2-line ferrihydrite at pH 5.7 and aged for 12 years at room temperature. I: insights from ICP-OES, XRD, ESEM, AsFlFFF/ICP-MS, and EXAFS spectroscopy.

PubMed

Finck, Nicolas; Bouby, Muriel; Dardenne, Kathy

2018-01-31

Two-line ferrihydrite (2LFh) was aged for 12 years under ambient conditions and sheltered from light in the presence of Lu(III) used as surrogate for trivalent actinides. 2LFh aging produced hematite rhombohedra with overgrown acicular goethite particles. Analysis of the homogeneous suspension by asymmetrical flow field-flow fractionation (AsFlFFF) coupled to ICP-MS indicated that particles have a mean hydrodynamic diameter of about 140 nm and the strong correlation of the Fe and Lu fractograms hinted at a structural association of the lanthanide with the solid phase(s). Unfortunately, recoveries were low and thus results cannot be considered representative of the whole sample. The suspension was centrifuged and X-ray absorption spectroscopy (XAS) at the Lu L 3 -edge on the settled particles indicated that Lu(III) is sixfold coordinated by oxygen atoms, pointing to a retention by structural incorporation within particles. This result is consistent with AsFlFFF results on the same suspension without centrifugation. The detection of next nearest Fe and O atoms were consistent with the structure of goethite, ruling out incorporation within hematite. After centrifugation of the suspension, only nanoparticulate needle-like particles, very likely goethite, could be detected in the supernatant by ESEM. AsFlFFF data of the supernatant were comparable to that obtained for the homogeneous suspension, whereas XAS indicated that Lu(III) is predominantly present as dissolved species in the supernatant. Results from both techniques can be interpreted as a major fraction of Lu present as aqueous ions and a minor fraction as structurally incorporated. Findings from this study are corroborated by STEM-HAADF data and results from DFT calculations in a companion paper.

Determination of ultra-low level plutonium isotopes (239Pu, 240Pu) in environmental samples with high uranium.

PubMed

Xing, Shan; Zhang, Weichao; Qiao, Jixin; Hou, Xiaolin

2018-09-01

In order to measure trace plutonium and its isotopes ratio ( 240 Pu/ 239 Pu) in environmental samples with a high uranium, an analytical method was developed using radiochemical separation for separation of plutonium from matrix and interfering elements including most of uranium and ICP-MS for measurement of plutonium isotopes. A novel measurement method was established for extensively removing the isobaric interference from uranium ( 238 U 1 H and 238 UH 2 + ) and tailing of 238 U, but significantly improving the measurement sensitivity of plutonium isotopes by employing NH 3 /He as collision/reaction cell gases and MS/MS system in the triple quadrupole ICP-MS instrument. The results show that removal efficiency of uranium interference was improved by more than 15 times, and the sensitivity of plutonium isotopes was increased by a factor of more than 3 compared to the conventional ICP-MS. The mechanism on the effective suppress of 238 U interference for 239 Pu measurement using NH 3 -He reaction gases was explored to be the formation of UNH + and UNH 2 + in the reactions of UH + and U + with NH 3 , while no reaction between NH 3 and Pu + . The detection limits of this method were estimated to be 0.55 fg mL -1 for 239 Pu, 0.09 fg mL -1 for 240 Pu. The analytical precision and accuracy of the method for Pu isotopes concentration and 240 Pu/ 239 Pu atomic ratio were evaluated by analysis of sediment reference materials (IAEA-385 and IAEA-412) with different levels of plutonium and uranium. The developed method were successfully applied to determine 239 Pu and 240 Pu concentrations and 240 Pu/ 239 Pu atomic ratios in soil samples collected in coastal areas of eastern China. Copyright © 2018 Elsevier B.V. All rights reserved.
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.
PM 10 metal concentrations and source identification using positive matrix factorization and wind sectoring in a French industrial zone

NASA Astrophysics Data System (ADS)

Alleman, Laurent Y.; Lamaison, Laure; Perdrix, Esperanza; Robache, Antoine; Galloo, Jean-Claude

2010-06-01

The elemental composition data of ambient aerosols collected upon selected wind sectors in the highly industrialised harbour of Dunkirk (France) were interpreted using pollution roses, elemental ratios, Enrichment Factors (EF), Principal Component Analysis (PCA) and Positive Matrix Factorization (PMF) receptor model. The objective was to identify the possible sources of PM10 aerosols, their respective chemical tracers and to determine their relative contribution at the sampling site. PM10 particles samples were collected from June 2003 to March 2005 in order to analyse up to 35 elements (Ag, Al, As, Ba, Bi, Ca, Cd, Ce, Co, Cr, Cs, Cu, Eu, Fe, K, La, Mg, Mn, Mo, Na, Ni, Pb, Rb, S, Sb, Sc, Si, Sm, Sr, Th, Ti, U, V, Zn and Zr) using Inductively Coupled Plasma (ICP)-Atomic Emission Spectrometry (AES) and ICP-Mass Spectrometry (MS). A significant effort has been made on estimating the total uncertainty of each result by regularly analysing blanks, quality controls and SRM NIST standards. Based on this procedure, a selected set of 24 "robust" elements was compared to the 35-element matrix in order to evaluate the sturdiness of our PMF statistical treatment. Eight source factors were resolved by PCA for all the wind sectors explaining 90% of the total data variance. The PMF results confirmed that eight physically interpretable factors contributed to the ambient particulate pollution at the sampling site: crustal dust (11%), marine aerosols (12%), petrochemistry activities (9.2%), metallurgical sintering plant (8.6%), metallurgical coke plant (12.6%), ferromanganese plant (6.6%), road transport (15%) and a less clearly interpretable profile probably associated to dust resuspension (13%). These weighted contributions against wind direction frequencies demonstrate that industrial sources are the most important contributors to this site (37%) followed by the natural sources (detrital and marine sources) (23%) and the road transport (15%).
Assessment of the migration potential of nanosilver from nanoparticle-coated low-density polyethylene food packaging into food simulants.

PubMed

Hannon, Joseph Christopher; Kerry, Joseph P; Cruz-Romero, Malco; Azlin-Hasim, Shafrina; Morris, Michael; Cummins, Enda

2016-01-01

An experimental nanosilver-coated low-density polyethylene (LDPE) food packaging was incubated with food simulants using a conventional oven and tested for migration according to European Commission Regulation No. 10/2011. The commercial LDPE films were coated using a layer-by-layer (LbL) technique and three levels of silver (Ag) precursor concentration (0.5%, 2% and 5% silver nitrate (AgNO3), respectively) were used to attach antimicrobial Ag. The experimental migration study conditions (time, temperature and food simulant) under conventional oven heating (10 days at 60°C, 2 h at 70°C, 2 h at 60°C or 10 days at 70°C) were chosen to simulate the worst-case storage period of over 6 months. In addition, migration was quantified under microwave heating. The total Ag migrant levels in the food simulants were quantified by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Mean migration levels obtained by ICP-AES for oven heating were in the range 0.01-1.75 mg l(-1). Migration observed for microwave heating was found to be significantly higher when compared with oven heating for similar temperatures (100°C) and identical exposure times (2 min). In each of the packaging materials and food simulants tested, the presence of nanoparticles (NPs) was confirmed by scanning electron microscopy (SEM). On inspection of the migration observed under conventional oven heating, an important finding was the significant reduction in migration resulting from the increased Ag precursor concentration used to attach Ag on the LDPE LbL-coated films. This observation merits further investigation into the LbL coating process used, as it suggests potential for process modifications to reduce migration. In turn, any reduction in NP migration below regulatory limits could greatly support the antimicrobial silver nanoparticle (AgNP)-LDPE LbL-coated films being used as a food packaging material.
A Multi-Analytical Approach for the Evaluation of the Efficiency of the Conservation-Restoration Treatment of Moroccan Historical Manuscripts Dating to the 16th, 17th, and 18th Centuries.

PubMed

Hajji, Latifa; Boukir, Abdellatif; Assouik, Jamal; Kerbal, Abdelali; Kajjout, Mohamed; Doumenq, Pierre; De Carvalho, Maria Luisa

2015-08-01

The most critical steps during the conservation-restoration treatment applied in Moroccan libraries are the deacidification using immersion in a saturated aqueous calcium hydroxide (Ca(OH)2) solution and the consolidation of degraded manuscripts using Japanese paper. The present study aims to assess the efficiency of this restoration method using a multi-analytical approach. For this purpose, three ancient Arabic Moroccan manuscript papers dating back to the 16th, 17th, and 18th centuries were investigated to characterize the paper support and make a comparative study between pre-restoration and post-restoration states. Three structural and molecular characterization techniques including solid-state nuclear magnetic resonance spectroscopy on (13)C with cross-polarization and magic-angle spinning nuclear magnetic resonance ((13)C CP-MAS NMR), attenuated total reflectance Fourier transform infrared spectroscopy (ATR FT-IR), and X-ray diffraction (XRD) were used to elucidate the cellulose main features, to identify the inorganic composition of the papers, and to study the crystallinity of the samples. Inductively coupled plasma atomic emission spectrometry (ICP-AES) allowed us to obtain a qualitative and quantitative characterization of the mineral fillers used in the manufacturing of the papers. Scanning electron microscopy coupled to energy dispersive spectrometry (SEM-EDS) ascertained the state of conservation of the different papers and helped us to study the elemental composition of the samples. After restoration, it was shown that the deacidification improved the stability of papers by providing an important alkaline buffer, as demonstrated using FT-IR and energy dispersive spectrometry (EDS) results. However, XRD and ICP-AES did not confirm the pertinence of the treatment for all samples because of the unequal distribution of Ca on the paper surface during the restoration. The consolidation process was studied using SEM analysis; its effectiveness in restoring torn areas was found to be significant.
Toxic and trace metal concentrations in liver and kidney of dogs: influence of diet, sex, age, and pathological lesions.

PubMed

Löpez-Alonso, Marta; Miranda, Marta; García-Partida, Paulino; Mendez, Adriana; Castillo, Cristina; Benedito, José Luis

2007-05-01

The aim of this study was to provide data on the main toxic and trace metals in the liver and kidney of domestic dogs in Galicia, NW Spain and to evaluate the influence of diet, sex, age, and pathological lesions on metal accumulation. Samples of the liver and kidney from 77 male and female dogs, aged between 6 mo and 18 yr, were collected during ordinary necropsy. Samples were acid-digested and metal concentrations determined by inductively coupled plasma (ICP)-mass spectrometry and ICP-atomic emission spectrometry. Mean toxic metal concentrations (geometric means for liver and kidney respectively) were 11.5 and 15.8 microg/kg wet weight for As, 56.3 and 166 microg/kg for Cd, 32.7 and 51.9 microg/kg for Hg, and 60.1 and 23.6 microg/kg for Pb. For the trace metals, these concentrations were respectively 16.3 and 21.0 microg/kg for Co, 57.6 and 43.9 microg/kg for Cr, 42.1 and 5.95 mg/kg for Cu, 394 mg/kg and 95.7 mg/kg for Fe, 2.39 and 0.956 mg/kg for Mn, 0.522 and 0.357 mg/kg for Mo, 23.8 and 26.8 microg/kg for Ni, 0.686 and 1.39 mg/kg for Se, and 46.7 and 26.0 mg/kg for Zn. Cd concentrations in the kidney significantly increased with age, and Co concentrations in the liver and kidney significantly decreased with age. Hepatic Pb concentrations were significantly higher in growing (<1 yr) and old (>10 yr) dogs. Animals with pathological lesions showed significantly higher Co and lower Mn and Zn concentrations in liver than animals without macroscopic abnormalities. Dogs that received commercial diets in general showed low variability in hepatic mineral status compared to animals that receive homemade feeds or a mixture of commercial and homemade feeds.
Assessment of heavy metal contamination in core sediment samples in Gulf of Izmir, Aegean Sea, Turkey (by inductively coupled plasma-optical emission spectrometry (ICP-OES))

NASA Astrophysics Data System (ADS)

Ünal Yumun, Zeki; Kam, Erol; Kurt, Dilek

2017-04-01

Heavy metal and radionuclide analysis studies are crucial in explaining biotic and abiotic interactions in ecosystems. This type of analysis is highly needed in environments such as coastal areas, gulfs or lakes where human activities are generally concentrated. Sediments are one of the best biological indicators for the environment since the pollution accumulates in the sediments by descent to the sea floor. In this study, sediments were collected from the Gulf of Izmir (Eastern Aegean Sea, Turkey) considering the accumulated points of domestic and industrial wastes to make an anthropogenic pollution analysis. The core sediments had different depths of 0.00-30.00 m at four different locations where Karsiyaka, Bayrakli, Incialti and Cesmealti in the Gulf of Izmir. The purpose of the study was determining Cd, Co, Cr, Cu, Mn, Ni, Pb, and Zn concentrations in the drilling samples to assess their levels and spatial distribution in crucial areas of the Aegean Sea by inductively coupled plasma-optical emission spectrometry (ICP-OES) with microwave digestion techniques. The heavy metal concentrations found in sediments varied for Cd:
The time variation of atomic oxygen emission around Io during a volcanic event observed with Hisaki/EXCEED

NASA Astrophysics Data System (ADS)

Koga, Ryoichi; Tsuchiya, Fuminori; Kagitani, Masato; Sakanoi, Takeshi; Yoneda, Mizuki; Yoshioka, Kazuo; Kimura, Tomoki; Murakami, Go; Yamazaki, Atsushi; Yoshikawa, Ichiro; Smith, H. Todd

2018-01-01

Io has an atmosphere produced by volcanism and sublimation of frosts deposited around active volcanoes. However, the time variation of atomic oxygen escaping Io's atmosphere is not well known. In this paper, we show a significant increase in atomic oxygen around Io during a volcanic event. Brightening of Io's extended sodium nebula was observed in the spring of 2015. We used the Hisaki satellite to investigate the time variation of atomic oxygen emission around Io during the same period. This investigation reveals that the duration of atomic oxygen brightness increases from a volcanically quiet level to a maximum level during the same approximate time period of 30 days as the observed sodium brightness. On the other hand, the recovery of the atomic oxygen brightness from the maximum to the quiet level (60 days) was longer than that of the sodium nebula decreasing (40 days). Additionally, a dawn-dusk asymmetry of the atomic oxygen emission is observed.
The effect of sampling scheme in the survey of atmospheric deposition of heavy metals in Albania by using moss biomonitoring.

PubMed

Qarri, Flora; Lazo, Pranvera; Bekteshi, Lirim; Stafilov, Trajce; Frontasyeva, Marina; Harmens, Harry

2015-02-01

The atmospheric deposition of heavy metals in Albania was investigated by using a carpet-forming moss species (Hypnum cupressiforme) as bioindicator. Sampling was done in the dry seasons of autumn 2010 and summer 2011. Two different sampling schemes are discussed in this paper: a random sampling scheme with 62 sampling sites distributed over the whole territory of Albania and systematic sampling scheme with 44 sampling sites distributed over the same territory. Unwashed, dried samples were totally digested by using microwave digestion, and the concentrations of metal elements were determined by inductively coupled plasma atomic emission spectroscopy (ICP-AES) and AAS (Cd and As). Twelve elements, such as conservative and trace elements (Al and Fe and As, Cd, Cr, Cu, Ni, Mn, Pb, V, Zn, and Li), were measured in moss samples. Li as typical lithogenic element is also included. The results reflect local emission points. The median concentrations and statistical parameters of elements were discussed by comparing two sampling schemes. The results of both sampling schemes are compared with the results of other European countries. Different levels of the contamination valuated by the respective contamination factor (CF) of each element are obtained for both sampling schemes, while the local emitters identified like iron-chromium metallurgy and cement industry, oil refinery, mining industry, and transport have been the same for both sampling schemes. In addition, the natural sources, from the accumulation of these metals in mosses caused by metal-enriched soil, associated with wind blowing soils were pointed as another possibility of local emitting factors.
First survey of atmospheric heavy metal deposition in Kosovo using moss biomonitoring.

PubMed

Maxhuni, Albert; Lazo, Pranvera; Kane, Sonila; Qarri, Flora; Marku, Elda; Harmens, Harry

2016-01-01

Bryophytes act as bioindicators and bioaccumulators of metal deposition in the environment. The atmospheric deposition of Cd, Cr, Cu, Fe, Hg, Ni, Mn, Pb, and Zn in Kosovo was investigated by using carpet-forming moss species (Pseudocleropodium purum and Hypnum cupressiforme) as bioindicators. This research is part of the European moss survey coordinated by the ICP Vegetation, an International Cooperative Programme reporting on the effects of air pollution on vegetation to the UNECE Convention on Long-range Transboundary Air Pollution. Sampling was performed during the summer of 2011 at 25 sampling sites homogenously distributed over Kosovo. Unwashed, dried samples were digested by using wet digestion in Teflon tubes. The concentrations of metal elements were determined by atomic absorption spectrometry (AAS) equipped with flame and/or furnace systems. The heavy metal concentration in mosses reflected local emission sources. The data obtained in this study were compared with those of similar studies in neighboring countries and Europe (2010-2014 survey). The geographical distribution maps of the elements over the sampled territory were constructed using geographic information system (GIS) technology. The concentrations of Cr, Ni, Pb, and Zn were higher than the respective median values of Europe, suggesting that the zones with heavy vehicular traffic and industry emission input are important emitters of these elements. Selected zones are highly polluted particularly by Cd, Pb, Hg, and Ni. The statistical analyses revealed that a strong correlation exists between the Pb and Cd content in mosses, and the degree of pollution in the studied sites was assessed.
A novel plasminogen activator from Agkistrodon blomhoffii Ussurensis venom (ABUSV-PA): Purification and characterization

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

Liu Shuqing; Sun Mingzhong; Greenaway, Frederick T.

2006-10-06

A plasminogen activator with arginine ester hydrolysis activity (ABUSV-PA) has been identified and purified to homogeneity from Chinese Agkistrodon blomhoffii Ussurensis snake venom. ABUSV-PA, a monomeric protein with molecular mass of 27815.2 Da, was purified 180-fold with 0.02% recovery for protein and 3.6% recovery for esterase activity. ABUSV-PA reacts optimally with its substrate N {sub {alpha}}-tosyl-L-arginine-methyl ester (TAME) at {approx}pH 7.5 and at 51 {sup o}C. Measurement from inductively coupled plasma-atomic emission spectroscopy (ICP-AES) reveals that ABUSV-PA is a Zn{sup 2+}-containing protein with a stoichiometry of 1:1 [Zn{sup 2+}]:[ABUSV-PA]. Analyses of esterase hydrolysis and UV absorption and CD spectra indicatemore » that Zn{sup 2+} plays an important role in maintaining the structural integrity rather than the esterase activity of ABUSV-PA. Divalent metal ions, including Ca{sup 2+}, Mg{sup 2+}, Cu{sup 2+}, Ni{sup 2+}, Mn{sup 2+}, and Co{sup 2+}, increase the TAME hydrolysis activity of ABUSV-PA. A red-shift of the emission wavelengths of the synchronous fluorescence of ABUSV-PA, compared to those of free Tyr and Trp, indicates a conformation where the Tyr and Trp residues are in exposed hydrophilic environments. The presence of zinc increases the hydrophobicity of the conformational environments surrounding the Trp residues of ABUSV-PA and affects the secondary structure of ABUSV-PA, as proved by UV absorption and CD spectroscopy.« less
40 CFR Appendix C to Part 136 - Inductively Coupled Plasma-Atomic Emission Spectrometric Method for Trace Element Analysis of...

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Inductively Coupled Plasma-Atomic... to Part 136—Inductively Coupled Plasma—Atomic Emission Spectrometric Method for Trace Element... technique. Samples are nebulized and the aerosol that is produced is transported to the plasma torch where...
40 CFR Appendix C to Part 136 - Inductively Coupled Plasma-Atomic Emission Spectrometric Method for Trace Element Analysis of...

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 23 2011-07-01 2011-07-01 false Inductively Coupled Plasma-Atomic... to Part 136—Inductively Coupled Plasma—Atomic Emission Spectrometric Method for Trace Element... technique. Samples are nebulized and the aerosol that is produced is transported to the plasma torch where...
Rapid Detection of Transition Metals in Welding Fumes Using Paper-Based Analytical Devices

PubMed Central

Volckens, John

2014-01-01

Metals in particulate matter (PM) are considered a driving factor for many pathologies. Despite the hazards associated with particulate metals, personal exposures for at-risk workers are rarely assessed due to the cost and effort associated with monitoring. As a result, routine exposure assessments are performed for only a small fraction of the exposed workforce. The objective of this research was to evaluate a relatively new technology, microfluidic paper-based analytical devices (µPADs), for measuring the metals content in welding fumes. Fumes from three common welding techniques (shielded metal arc, metal inert gas, and tungsten inert gas welding) were sampled in two welding shops. Concentrations of acid-extractable Fe, Cu, Ni, and Cr were measured and independently verified using inductively coupled plasma-optical emission spectroscopy (ICP-OES). Results from the µPAD sensors agreed well with ICP-OES analysis; the two methods gave statistically similar results in >80% of the samples analyzed. Analytical costs for the µPAD technique were ~50 times lower than market-rate costs with ICP-OES. Further, the µPAD method was capable of providing same-day results (as opposed several weeks for ICP laboratory analysis). Results of this work suggest that µPAD sensors are a viable, yet inexpensive alternative to traditional analytic methods for transition metals in welding fume PM. These sensors have potential to enable substantially higher levels of hazard surveillance for a given resource cost, especially in resource-limited environments. PMID:24515892
Rapid detection of transition metals in welding fumes using paper-based analytical devices.

PubMed

Cate, David M; Nanthasurasak, Pavisara; Riwkulkajorn, Pornpak; L'Orange, Christian; Henry, Charles S; Volckens, John

2014-05-01

Metals in particulate matter (PM) are considered a driving factor for many pathologies. Despite the hazards associated with particulate metals, personal exposures for at-risk workers are rarely assessed due to the cost and effort associated with monitoring. As a result, routine exposure assessments are performed for only a small fraction of the exposed workforce. The objective of this research was to evaluate a relatively new technology, microfluidic paper-based analytical devices (µPADs), for measuring the metals content in welding fumes. Fumes from three common welding techniques (shielded metal arc, metal inert gas, and tungsten inert gas welding) were sampled in two welding shops. Concentrations of acid-extractable Fe, Cu, Ni, and Cr were measured and independently verified using inductively coupled plasma-optical emission spectroscopy (ICP-OES). Results from the µPAD sensors agreed well with ICP-OES analysis; the two methods gave statistically similar results in >80% of the samples analyzed. Analytical costs for the µPAD technique were ~50 times lower than market-rate costs with ICP-OES. Further, the µPAD method was capable of providing same-day results (as opposed several weeks for ICP laboratory analysis). Results of this work suggest that µPAD sensors are a viable, yet inexpensive alternative to traditional analytic methods for transition metals in welding fume PM. These sensors have potential to enable substantially higher levels of hazard surveillance for a given resource cost, especially in resource-limited environments.
Using ICP-OES and SEM-EDX in biosorption studies

PubMed Central

Chojnacka, Katarzyna; Marycz, Krzysztof

2010-01-01

We have compared the analytical results obtained by inductively coupled plasma optical emission spectroscopy (ICP-OES) and by scanning electron microscopy with an energy dispersive X-ray analytical system (SEM-EDX) in order to explore the mechanism of metal ions biosorption by biomass using two independent methods. The marine macroalga Enteromorpha sp. was enriched with Cu(II), Mn(II), Zn(II), and Co(II) ions via biosorption, and the biosorption capacity of alga determined from the solution and biomass composition before and after biosorption process was compared. The first technique was used to analyze the composition of the natural and metal-loaded biomass, and additionally the composition of the solution before and after biosorption. The second technique was used to obtain a picture of the surface of natural and metal ion-loaded macroalgae, to map the elements on the cell wall of dry biomass, and to determine their concentration before and after biosorption. ICP-OES showed a better precision and lower detection limit than EDX, but SEM-EDX gave more information regarding the sample composition of Enteromorpha sp. Both techniques confirmed that biosorption is a surface phenomenon, in which alkali and alkaline earth metal ions were exchanged by metal ions from aqueous solution. Figure The advantages and disadvantages of ICP-OES and SEM-EDX techniques Electronic supplementary material The online version of this article (doi:10.1007/s00604-010-0468-0) contains supplementary material, which is available to authorized users. PMID:21423317
Using ICP-OES and SEM-EDX in biosorption studies.

PubMed

Michalak, Izabela; Chojnacka, Katarzyna; Marycz, Krzysztof

2011-02-01

We have compared the analytical results obtained by inductively coupled plasma optical emission spectroscopy (ICP-OES) and by scanning electron microscopy with an energy dispersive X-ray analytical system (SEM-EDX) in order to explore the mechanism of metal ions biosorption by biomass using two independent methods. The marine macroalga Enteromorpha sp. was enriched with Cu(II), Mn(II), Zn(II), and Co(II) ions via biosorption, and the biosorption capacity of alga determined from the solution and biomass composition before and after biosorption process was compared. The first technique was used to analyze the composition of the natural and metal-loaded biomass, and additionally the composition of the solution before and after biosorption. The second technique was used to obtain a picture of the surface of natural and metal ion-loaded macroalgae, to map the elements on the cell wall of dry biomass, and to determine their concentration before and after biosorption. ICP-OES showed a better precision and lower detection limit than EDX, but SEM-EDX gave more information regarding the sample composition of Enteromorpha sp. Both techniques confirmed that biosorption is a surface phenomenon, in which alkali and alkaline earth metal ions were exchanged by metal ions from aqueous solution.FigureThe advantages and disadvantages of ICP-OES and SEM-EDX techniques ELECTRONIC SUPPLEMENTARY MATERIAL: The online version of this article (doi:10.1007/s00604-010-0468-0) contains supplementary material, which is available to authorized users.
Determination of Heavy Metals in Almonds and Mistletoe as a Parasite Growing on the Almond Tree Using ICP-OES or ICP-MS.

PubMed

Kamar, Veysi; Dağalp, Rukiye; Taştekin, Mustafa

2017-12-28

In this study, the elements of Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Ni, Sr, Pb, Ti, and Zn were determined in the leaves, fruits, and branches of mistletoe, (Viscum albüm L.), used as a medicinal plant, and in the leaves, branches and barks of almond tree which mistletoe grows on. The aim of the study is to investigate whether the mistletoe are more absorbent than the almond tree in terms of the heavy metal contents and the determination of the amount of the elements penetrated into the mistletoe from the almond tree. ICP-MS (inductively coupled plasma-mass spectrometry) was used for the analysis of As, Cd, Mo, and Pb, whereas ICP-OES (inductively coupled plasma optical emission spectrometry) was used for the other elements. The results obtained were statistically evaluated at 95% confidence level. Within the results obtained in this study, it was determined whether there is a significant difference between metal elements in almond tree and mistletoe, or not. As a result, it was observed that there were higher contents of B, Ba, K, Mg, and Zn in the mistletoe than in the almond tree. K was found much higher than other elements in the mistletoe. On the other hand, Al, As, Ca, Cd, Cr, Cu, Fe, Mo, Ni, Sr, Pb, and Ti contents were determined to be more in almond tree than mistletoe.
First-principles calculations of orientation dependence of Si thermal oxidation based on Si emission model

NASA Astrophysics Data System (ADS)

Nagura, Takuya; Kawachi, Shingo; Chokawa, Kenta; Shirakawa, Hiroki; Araidai, Masaaki; Kageshima, Hiroyuki; Endoh, Tetsuo; Shiraishi, Kenji

2018-04-01

It is expected that the off-state leakage current of MOSFETs can be reduced by employing vertical body channel MOSFETs (V-MOSFETs). However, in fabricating these devices, the structure of the Si pillars sometimes cannot be maintained during oxidation, since Si atoms sometimes disappear from the Si/oxide interface (Si missing). Thus, in this study, we used first-principles calculations based on the density functional theory, and investigated the Si emission behavior at the various interfaces on the basis of the Si emission model including its atomistic structure and dependence on Si crystal orientation. The results show that the order in which Si atoms are more likely to be emitted during thermal oxidation is (111) > (110) > (310) > (100). Moreover, the emission of Si atoms is enhanced as the compressive strain increases. Therefore, the emission of Si atoms occurs more easily in V-MOSFETs than in planar MOSFETs. To reduce Si missing in V-MOSFETs, oxidation processes that induce less strain, such as wet or pyrogenic oxidation, are necessary.
A Multi-Pumping Flow System for In Situ Measurements of Dissolved Manganese in Aquatic Systems

PubMed Central

Meyer, David; Prien, Ralf D.; Dellwig, Olaf; Waniek, Joanna J.; Schuffenhauer, Ingo; Donath, Jan; Krüger, Siegfried; Pallentin, Malte; Schulz-Bull, Detlef E.

2016-01-01

A METals In Situ analyzer (METIS) has been used to determine dissolved manganese (II) concentrations in the subhalocline waters of the Gotland Deep (central Baltic Sea). High-resolution in situ measurements of total dissolved Mn were obtained in near real-time by spectrophotometry using 1-(2-pyridylazo)-2-naphthol (PAN). PAN is a complexing agent of dissolved Mn and forms a wine-red complex with a maximum absorbance at a wavelength of 562 nm. Results are presented together with ancillary temperature, salinity, and dissolved O2 data. Lab calibration of the analyzer was performed in a pressure testing tank. A detection limit of 77 nM was obtained. For validation purposes, discrete water samples were taken by using a pump-CTD system. Dissolved Mn in these samples was determined by an independent laboratory based method (inductively coupled plasma–optical emission spectrometry, ICP-OES). Mn measurements from both METIS and ICP-OES analysis were in good agreement. The results showed that the in situ analysis of dissolved Mn is a powerful technique reducing dependencies on heavy and expensive equipment (pump-CTD system, ICP-OES) and is also cost and time effective. PMID:27916898

[Determination of 22 inorganic elements in different parts of Lantana camara by ICP-OES].

PubMed

Zhou, Wei-ming; Wang, Ru-yi; Chen, Liu-sheng; Huang, Chuan-bin

2014-10-01

To determine the contents of 22 inorganic elements in different parts of Lantana camara by inductively coupled plasma optical emission spectroscopy (ICP-OES). HNO3-H2O2 digested system was used to completely decompose the organic compounds effectually by microwave digestion. The 22 inorganic elements such as K, Ca, Mg, Fe, Al, Na, Zn, Mn and Cr were determined by ICP-OES under set up working conditions. The contents of K, Ca and Mg were the most in different parts of Lantana camara; The contents of K, Ca, Mg, Mn, Sr and Cu in the leaf were more those that in the root and branch; The contents of Fe, Na, Cr and Ni in the root were more than those in the leaf and branch; The contents of Mn, Zn, Sr and Cu in the branch were more than those in the root and the leaf; The contents of Pb and Cd were higher than the national standard and Cr had high content in different parts of Lantana camara. The determination method is quick, easy and accurate with high sensitivity, which can determine the contents of 22 inorganic elements accurately in different parts of Lantana camara.
[Analysis and Evaluation of Inorganic Elements in Euryale Semen from Different Habitats by Microwave Digestion-ICP-OES].

PubMed

Wang, Hong; Wu, Qi-nan; Wu, Cheng-ying; Fan, Xiu-he; Jiang, Zheng; Gu, Wei; Yue, Wei

2015-01-01

To establish a simple, rapid and efficient method for determination of different inorganic elements in Euryale Semen from different habitats. Inductively coupled plasma-optical emission spectrometry(ICP-OES) was applied to determine inorganic elements in Euryale Semen, and the results were analyzed by principal component analysis. Euryale Semen from different habitats contained the kind of inorganic elements ranging from 22 to 26, including micronutrient elements like Iron, Zinc, Selenium, Copper, Molybdenum, Chrome and Cobalt, as well as macronutrient elements such as Potassium, Calcium, Sodium, Magnesium and Phosphorus. Five factors were extracted and used to comprehensively evaluate Euryale Semen from 20 different habitats covered almost China. The comprehensive function was F = 0. 38828F1 + 0. 25603F2 + 0. 07617F3 + 0. 06860F4 + 0. 04868F5, which resulted in the top three samples coming from Jiangsu Gaoyou, Hunan Xiangxi and Jiangsu Suzhou respectively. The study indicates that ICP-OES is a quick, accurate and sensitive method to determine the contents of inorganic elements in Euryale Semen,which provides scientific and reliable reference for its quality control and safety assessment.
Effect of sample preparation procedure for the determination of As, Sb and Se in fruit juices by HG-ICP-OES.

PubMed

Welna, Maja; Szymczycha-Madeja, Anna

2014-09-15

Various sample preparation procedures for the simultaneous determination of As, Sb and Se in fruit juices by hydride generation inductively coupled plasma optical emission spectrometry (HG-ICP-OES) were examined. Applicability of total wet digestion with HNO3/H2O2, partial decomposition (solubilisation in aqua regia), 1:1 dilution with 2% (v/v) HNO3 and direct analysis were evaluated. Hydrides were generated in the reaction of an acidified sample with NaBH4 after pre-reduction with KI-ascorbic acid for total As and Sb, and boiling with HCl for total Se. Best results, i.e. limits of detection (LODs) of 0.51-0.73 ng mL(-1), precision (RSD) within 1.7-3.6% and recoveries for spiked samples between 101% and 106% were found using aqua regia treatment. This procedure simplifying and improving sample preparation step prior to As, Sb and Se measurements in fruit juices by HG-ICP-OES, thus could be adequate for the routine analysis in terms of the quality control of these drinks. Copyright © 2014 Elsevier Ltd. All rights reserved.
40 CFR 65.83 - Performance requirements.

Code of Federal Regulations, 2012 CFR

2012-07-01

... stream nonhalogenated by reducing the vent stream halogen atom mass emission rate to less than 0.45... requirements of paragraph (a)(1) or (2) of this section. The mass emission rate of halogen atoms contained in...
40 CFR 65.83 - Performance requirements.

Code of Federal Regulations, 2011 CFR

2011-07-01

... stream nonhalogenated by reducing the vent stream halogen atom mass emission rate to less than 0.45... requirements of paragraph (a)(1) or (2) of this section. The mass emission rate of halogen atoms contained in...
40 CFR 65.83 - Performance requirements.

Code of Federal Regulations, 2010 CFR

2010-07-01

... stream nonhalogenated by reducing the vent stream halogen atom mass emission rate to less than 0.45... requirements of paragraph (a)(1) or (2) of this section. The mass emission rate of halogen atoms contained in...
40 CFR 65.83 - Performance requirements.

Code of Federal Regulations, 2013 CFR

2013-07-01

... stream nonhalogenated by reducing the vent stream halogen atom mass emission rate to less than 0.45... requirements of paragraph (a)(1) or (2) of this section. The mass emission rate of halogen atoms contained in...
40 CFR 65.83 - Performance requirements.

Code of Federal Regulations, 2014 CFR

2014-07-01

... stream nonhalogenated by reducing the vent stream halogen atom mass emission rate to less than 0.45... requirements of paragraph (a)(1) or (2) of this section. The mass emission rate of halogen atoms contained in...
Spatial Dependent Spontaneous Emission of an Atom in a Semi-Infinite Waveguide of Rectangular Cross Section

NASA Astrophysics Data System (ADS)

Song, Hai-Xi; Sun, Xiao-Qi; Lu, Jing; Zhou, Lan

2018-01-01

We study a quantum electrodynamics (QED) system made of a two-level atom and a semi-infinite rectangular waveguide, which behaves as a perfect mirror in one end. The spatial dependence of the atomic spontaneous emission has been included in the coupling strength relevant to the eigenmodes of the waveguide. The role of retardation is studied for the atomic transition frequency far away from the cutoff frequencies. The atom-mirror distance introduces different phases and retardation times into the dynamics of the atom interacting resonantly with the corresponding transverse modes. It is found that the upper state population decreases from its initial as long as the atom-mirror distance does not vanish, and is lowered and lowered when more and more transverse modes are resonant with the atom. The atomic spontaneous emission can be either suppressed or enhanced by adjusting the atomic location for short retardation time. There are partial revivals and collapses due to the photon reabsorbed and re-emitted by the atom for long retardation time. Supported by National Natural Science Foundation of China under Grant Nos. 11374095, 11422540, 11434011, and 11575058, National Fundamental Research Program of China (the 973 Program) under Grant No. 2012CB922103, and Hunan Provincial Natural Science Foundation of China under Grant No. 11JJ7001
Entanglement and nonlocality versus spontaneous emission in two-atom systems

NASA Astrophysics Data System (ADS)

Jakóbczyk, L.; Jamróz, A.

2003-11-01

We study evolution of entanglement of two two-level atoms in the presence of dissipation caused by spontaneous emission. We find explicit formulas for the amount of entanglement as a function of time, in the case of destruction of the initial entanglement and possible creation of a transient entanglement between atoms. We also discuss how spontaneous emission influences nonlocality of states expressed by violation of Bell-CHSH inequality. It is shown that evolving system very quickly becomes local, even if entanglement is still present or produced.
Method for determining the concentration of atomic species in gases and solids

DOEpatents

Loge, Gary W.

1999-01-01

Method for determining the concentration of atomic species in gases and solids. Measurement of at least two emission intensities from a species in a plasma containing the species after a sufficient time period has elapsed after the generation of the plasma and during a second time period, permits an instantaneous temperature to be established within the sample. The concentration of the atomic species to be determined is then derived from the known emission intensity of a predetermined concentration of that species in the sample at the measured temperature, a quantity which is measured prior to the determination of the unknown concentration, and the actual measured emission from the unknown species, or by this latter emission and the emission intensity of a species having known concentration within the sample.
The reaction of N/2D/ with O2 as a source of O/1D/ atoms in aurorae

NASA Technical Reports Server (NTRS)

Rusch, D. W.; Sharp, W. E.; Gerard, J.-C.

1978-01-01

The source of O(1D) atoms in the auroral ionosphere is investigated using sounding rocket data. Previously, it has been shown that the conventional sources of O(1D) atoms in the aurora, dissociative recombination of O2(plus) and electron impact excitation of atomic oxygen, fail to explain the measured 6300 A volume emission rate profile. It is suggested that the atom-atom interchange reaction of N(2D) with O2 can be the major source of auroral 6300 A emission if O(1D) is created with high efficiency.
Theoretical study for heterojunction surface of NEA GaN photocathode dispensed with Cs activation

NASA Astrophysics Data System (ADS)

Xia, Sihao; Liu, Lei; Wang, Honggang; Wang, Meishan; Kong, Yike

2016-09-01

For the disadvantages of conventional negative electron affinity (NEA) GaN photocathodes activated by Cs or Cs/O, new-type NEA GaN photocathodes with heterojunction surface dispensed with Cs activation are investigated based on first-principle study with density functional theory. Through the growth of an ultrathin n-type GaN cap layer on p-type GaN emission layer, a p-n heterojunction is formed on the surface. According to the calculation results, it is found that Si atoms tend to replace Ga atoms to result in an n-type doped cap layer which contributes to the decreasing of work function. After the growth of n-type GaN cap layer, the atom structure near the p-type emission layer is changed while that away from the surface has no obvious variations. By analyzing the E-Mulliken charge distribution of emission surface with and without cap layer, it is found that the positive charge of Ga and Mg atoms in the emission layer decrease caused by the cap layer, while the negative charge of N atom increases. The conduction band moves downwards after the growth of cap layer. Si atom produces donor levels around the valence band maximum. The absorption coefficient of GaN emission layer decreases and the reflectivity increases caused by n-type GaN cap layer.
Evaluation of a tunable bandpass reaction cell for an inductively coupled plasma mass spectrometer for the determination of chromium and vanadium in serum and urine

NASA Astrophysics Data System (ADS)

Nixon, David E.; Neubauer, Kenneth R.; Eckdahl, Steven J.; Butz, John A.; Burritt, Mary F.

2002-05-01

A Dynamic Reaction Cell™ inductively coupled argon plasma mass spectrometer (DRC-ICP-MS) was evaluated for the determination of chromium and vanadium in serum and urine. Reaction cell conditions were evaluated for the elimination of ArC + and ClOH + interferences on chromium at mass 52 and OCl + on vanadium at mass 51. A diluent containing only 1% nitric acid and internal standards (Y and Ga) was used to prepare serum and urine for analysis. Instrument response calibration was achieved by using aqueous acidic standards spiked into pooled sera or urine matrices. The slopes of the calibration curves prepared in urine and serum matrices were nearly identical. On average, chromium detection limits are 2.5 times lower using the DRC than Zeeman graphite furnace atomic absorption spectrometry (ZGFAAS). Vanadium detection limits are approximately 50 times lower. Average detection limits achieved with DRC-ICP-MS are 0.075 μg Cr/l and 0.028 μg V/l. Average results for the analysis of National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1598 Bovine Serum (attained over 22 days) are: 0.14 μg Cr/l and 0.068 μg V/l. The reference concentrations for vanadium and chromium in NIST SRM 1598 are (0.06) μg V/l and 0.14±0.08 μg Cr/l, respectively. Results for chromium and vanadium determinations on ICP-MS survey samples from the Toxocologie du Quebec are equivalent to those reported by high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for the same survey samples.
Elemental composition of ambient aerosols measured with high temporal resolution using an online XRF spectrometer

NASA Astrophysics Data System (ADS)

Furger, Markus; Cruz Minguillón, María; Yadav, Varun; Slowik, Jay G.; Hüglin, Christoph; Fröhlich, Roman; Petterson, Krag; Baltensperger, Urs; Prévôt, André S. H.

2017-06-01

The Xact 625 Ambient Metals Monitor was tested during a 3-week field campaign at the rural, traffic-influenced site Härkingen in Switzerland during the summer of 2015. The field campaign encompassed the Swiss National Day fireworks event, providing increased concentrations and unique chemical signatures compared to non-fireworks (or background) periods. The objective was to evaluate the data quality by intercomparison with other independent measurements and test its applicability for aerosol source quantification. The Xact was configured to measure 24 elements in PM10 with 1 h time resolution. Data quality was evaluated for 10 24 h averages of Xact data by intercomparison with 24 h PM10 filter data analysed with ICP-OES for major elements, ICP-MS for trace elements, and gold amalgamation atomic absorption spectrometry for Hg. Ten elements (S, K, Ca, Ti, Mn, Fe, Cu, Zn, Ba, Pb) showed excellent correlation between the compared methods, with r2 values ≥ 0.95. However, the slopes of the regressions between Xact 625 and ICP data varied from 0.97 to 1.8 (average 1.28) and thus indicated generally higher Xact elemental concentrations than ICP for these elements. Possible reasons for these differences are discussed, but further investigations are needed. For the remaining elements no conclusions could be drawn about their quantification for various reasons, mainly detection limit issues. An indirect intercomparison of hourly values was performed for the fireworks peak, which brought good agreement of total masses when the Xact data were corrected with the regressions from the 24 h value intercomparison. The results demonstrate that multi-metal characterization at high-time-resolution capability of Xact is a valuable and practical tool for ambient monitoring.
Laser ablation-inductively coupled plasma mass spectrometry: an emerging technology for detecting rare cells in tissue sections.

PubMed

Managh, Amy J; Hutchinson, Robert W; Riquelme, Paloma; Broichhausen, Christiane; Wege, Anja K; Ritter, Uwe; Ahrens, Norbert; Koehl, Gudrun E; Walter, Lisa; Florian, Christian; Schlitt, Hans J; Reid, Helen J; Geissler, Edward K; Sharp, Barry L; Hutchinson, James A

2014-09-01

Administering immunoregulatory cells to patients as medicinal agents is a potentially revolutionary approach to the treatment of immunologically mediated diseases. Presently, there are no satisfactory, clinically applicable methods of tracking human cells in patients with adequate spatial resolution and target cell specificity over a sufficient period of time. Laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS) represents a potential solution to the problem of detecting very rare cells in tissues. In this article, this exquisitely sensitive technique is applied to the tracking of gold-labeled human regulatory macrophages (Mregs) in immunodeficient mice. Optimal conditions for labeling Mregs with 50-nm gold particles were investigated by exposing Mregs in culture to variable concentrations of label: Mregs incubated with 3.5 × 10(9) particles/ml for 1 h incorporated an average of 3.39 × 10(8) Au atoms/cell without loss of cell viability. Analysis of single, gold-labeled Mregs by LA-ICP-MS registered an average of 1.9 × 10(5) counts/cell. Under these conditions, 100% labeling efficiency was achieved, and label was retained by Mregs for ≥36 h. Gold-labeled Mregs adhered to glass surfaces; after 24 h of culture, it was possible to colabel these cells with human-specific (154)Sm-tagged anti-HLA-DR or (174)Yb-tagged anti-CD45 mAbs. Following injection into immunodeficient mice, signals from gold-labeled human Mregs could be detected in mouse lung, liver, and spleen for at least 7 d by solution-based inductively coupled plasma mass spectrometry and LA-ICP-MS. These promising results indicate that LA-ICP-MS tissue imaging has great potential as an analytical technique in immunology. Copyright © 2014 by The American Association of Immunologists, Inc.
40 CFR 63.128 - Transfer operations provisions-test methods and procedures.

Code of Federal Regulations, 2013 CFR

2013-07-01

... using a scrubber or other halogen reduction device to reduce the vent stream halogen atom mass emission...)(2) shall determine the halogen atom mass emission rate prior to the combustor according to the...
40 CFR 63.128 - Transfer operations provisions-test methods and procedures.

Code of Federal Regulations, 2011 CFR

2011-07-01

... using a scrubber or other halogen reduction device to reduce the vent stream halogen atom mass emission...)(2) shall determine the halogen atom mass emission rate prior to the combustor according to the...
40 CFR 63.128 - Transfer operations provisions-test methods and procedures.

Code of Federal Regulations, 2010 CFR

2010-07-01

... using a scrubber or other halogen reduction device to reduce the vent stream halogen atom mass emission...)(2) shall determine the halogen atom mass emission rate prior to the combustor according to the...
40 CFR 63.128 - Transfer operations provisions-test methods and procedures.

Code of Federal Regulations, 2014 CFR

2014-07-01

... using a scrubber or other halogen reduction device to reduce the vent stream halogen atom mass emission...)(2) shall determine the halogen atom mass emission rate prior to the combustor according to the...

40 CFR 63.128 - Transfer operations provisions-test methods and procedures.

Code of Federal Regulations, 2012 CFR

2012-07-01

... using a scrubber or other halogen reduction device to reduce the vent stream halogen atom mass emission...)(2) shall determine the halogen atom mass emission rate prior to the combustor according to the...
ENVIRONMENTAL APPLICATION OF GAS CHROMATOGRAPHY/ATOMIC EMISSION DETECTION

EPA Science Inventory

A gas chromatography/atomic emission detector (GC/AED) system has been evaluated for its applicability to environmental analysis. Detection limits, elemental response factors, and regression analysis data were determined for 58 semivolatile environmental contaminants. Detection l...
Longitudinal structure in atomic oxygen concentrations observed with WINDII on UARS. [Wind Imaging Interferometer

NASA Technical Reports Server (NTRS)

Shepherd, G. G.; Thuillier, G.; Solheim, B. H.; Chandra, S.; Cogger, L. L.; Duboin, M. L.; Evans, W. F. J.; Gattinger, R. L.; Gault, W. A.; Herse, M.

1993-01-01

WINDII, the Wind Imaging Interferometer on the Upper Atmosphere Research Satellite, began atmospheric observations on September 28, 1991 and since then has been collecting data on winds, temperatures and emissions rates from atomic, molecular and ionized oxygen species, as well as hydroxyl. The validation of winds and temperatures is not yet complete, and scientific interpretation has barely begun, but the dominant characteristic of these data so far is the remarkable structure in the emission rate from the excited species produced by the recombination of atomic oxygen. The latitudinal and temporal variability has been noted before by many others. In this preliminary report on WINDII results we draw attention to the dramatic longitudinal variations of planetary wave character in atomic oxygen concentration, as reflected in the OI 557.7 nm emission, and to similar variations seen in the Meine1 hydroxyl band emission.
Emission intensity modulation of radio-frequency helium glow-discharge emission source by laser ablation.

PubMed

Matsuta, Hideyuki; Naeem, Tariq M; Wagatsuma, Kazuaki

2003-06-01

A novel emission excitation source comprising a high repetition rate diode-pumped Q-switched Nd:YAG laser and a Grimm-style glow-discharge lamp is described. Laser-ablated atoms are introduced into the He glow discharge plasma, which then give emission signals. By using phase-sensitive detection with a lock-in amplifier, the emission signal modulated by the pulsed laser can be detected selectively. It is possible to estimate only the emission intensity of sample atoms ablated by laser irradiation with little interference from the other species in the plasma.
Multielemental analysis of prehistoric animal teeth by laser-induced breakdown spectroscopy and laser ablation inductively coupled plasma mass spectrometry

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

Galiova, Michaela; Kaiser, Jozef; Fortes, Francisco J.

2010-05-01

Laser-induced breakdown spectroscopy (LIBS) and laser ablation (LA) inductively coupled plasma (ICP) mass spectrometry (MS) were utilized for microspatial analyses of a prehistoric bear (Ursus arctos) tooth dentine. The distribution of selected trace elements (Sr, Ba, Fe) was measured on a 26 mmx15 mm large and 3 mm thick transverse cross section of a canine tooth. The Na and Mg content together with the distribution of matrix elements (Ca, P) was also monitored within this area. The depth of the LIBS craters was measured with an optical profilometer. As shown, both LIBS and LA-ICP-MS can be successfully used for themore » fast, spatially resolved analysis of prehistoric teeth samples. In addition to microchemical analysis, the sample hardness was calculated using LIBS plasma ionic-to-atomic line intensity ratios of Mg (or Ca). To validate the sample hardness calculations, the hardness was also measured with a Vickers microhardness tester.« less
Temporal VUV Emission Characteristics Related to Generations and Losses of Metastable Atoms in Xenon Pulsed Barrier Discharge

NASA Astrophysics Data System (ADS)

Motomura, Hideki; Loo, Ka Hong; Ikeda, Yoshihisa; Jinno, Masafumi; Aono, Masaharu

Although xenon pulsed dielectric barrier discharge is one of the most promising substitutes for mercury low-pressure discharge for fluorescent lamps, the efficacy of xenon fluorescent lamp is not enough for practical use for general lighting. To improve the efficacy it is indispensable to clarify mechanisms of vacuum ultraviolet (VUV) emissions, which excite phosphor, from xenon discharge related to plasma characteristics. In this paper emission waveforms and temporal change of metastable atom density are measured and temporal VUV emission characteristics related to generations and losses of metastable atoms in xenon pulsed barrier discharge is investigated. It is shown that the lamp efficacy is improved by about 10% with shorter pulse in which the two VUV emission peaks in a pulse are overlapped. It is also shown that at the lower pressure of 1.3 kPa metastable atoms generated during on-period of the voltage pulse are not efficiently consumed for VUV emissions in the off-period of the voltage pulse because of lower rate of three-body collision and quenching. This fact is thought to be one of the reasons why the lamp efficacy is low at lower pressure.
Stimulated emission by hybrid transitions via a heteronuclear molecule

NASA Astrophysics Data System (ADS)

Dinev, S. G.; Khadzhikhristov, G. B.; Stefanov, I. L.

1990-03-01

An atomic emission, identified as a four-wave parametric emission and stimulated by collision assisted hybrid transition via a heteronuclear molecule, is presented together with a diagram of excitation and emission for the relevant K and NaK energy levels. The cascading emission from the excited 7S or 5D levels to lower-lying atomic states is considered to be insignificant. The dependence of the red signal and the NaK fluorescence on the pump energy is investigated, and the results can be used to indicate the onset of a stimulated process.
Superradiance for Atoms Trapped along a Photonic Crystal Waveguide

NASA Astrophysics Data System (ADS)

Goban, A.; Hung, C.-L.; Hood, J. D.; Yu, S.-P.; Muniz, J. A.; Painter, O.; Kimble, H. J.

2015-08-01

We report observations of superradiance for atoms trapped in the near field of a photonic crystal waveguide (PCW). By fabricating the PCW with a band edge near the D1 transition of atomic cesium, strong interaction is achieved between trapped atoms and guided-mode photons. Following short-pulse excitation, we record the decay of guided-mode emission and find a superradiant emission rate scaling as Γ¯SR∝N ¯Γ1 D for average atom number 0.19 ≲N ¯≲2.6 atoms, where Γ1 D/Γ'=1.0 ±0.1 is the peak single-atom radiative decay rate into the PCW guided mode, and Γ' is the radiative decay rate into all the other channels. These advances provide new tools for investigations of photon-mediated atom-atom interactions in the many-body regime.
Partially autoionizing states of atomic oxygen

NASA Technical Reports Server (NTRS)

Samson, J. A. R.; Petrosky, V. E.

1974-01-01

Certain Rydberg states and an intershell transition of atomic oxygen were shown to partially autoionize, and to produce emission spectra competitive with autoionization. These states are forbidden to autoionize on the basis of LS coupling; but they were observed both in emission spectroscopy and in photoelectron spectroscopy. The results explain an unidentified structure in the 584 Angstrom He I atomic O spectrum observed by previous investigators.
Studies of Be migration in the JET tokamak using AMS with 10Be marker

NASA Astrophysics Data System (ADS)

Bykov, I.; Bergsåker, H.; Possnert, G.; Zhou, Y.; Heinola, K.; Pettersson, J.; Conroy, S.; Likonen, J.; Petersson, P.; Widdowson, A.

2016-03-01

The JET tokamak is operated with beryllium limiter tiles in the main chamber and tungsten coated carbon fiber composite tiles and solid W tiles in the divertor. One important issue is how wall materials are migrating during plasma operation. To study beryllium redistribution in the main chamber and in the divertor, a 10Be enriched limiter tile was installed prior to plasma operations in 2011-2012. Methods to take surface samples have been developed, an abrasive method for bulk Be tiles in the main chamber, which permits reuse of the tiles, and leaching with hot HCl to remove all Be deposited at W coated surfaces in the divertor. Quantitative analysis of the total amount of Be in cm2 sized samples was made with inductively coupled plasma atomic emission spectroscopy (ICP-AES). The 10Be/9Be ratio in the samples was measured with accelerator mass spectrometry (AMS). The experimental setup and methods are described in detail, including sample preparation, measures to eliminate contributions in AMS from the 10B isobar, possible activation due to plasma generated neutrons and effects of diffusive isotope mixing. For the first time marker concentrations are measured in the divertor deposits. They are in the range 0.4-1.2% of the source concentration, with moderate poloidal variation.
Increased cellular uptake of peptide-modified PEGylated gold nanoparticles.

PubMed

He, Bo; Yang, Dan; Qin, Mengmeng; Zhang, Yuan; He, Bing; Dai, Wenbing; Wang, Xueqing; Zhang, Qiang; Zhang, Hua; Yin, Changcheng

2017-12-09

Gold nanoparticles are promising drug delivery vehicles for nucleic acids, small molecules, and proteins, allowing various modifications on the particle surface. However, the instability and low bioavailability of gold nanoparticles compromise their clinical application. Here, we functionalized gold nanoparticles with CPP fragments (CALNNPFVYLI, CALRRRRRRRR) through sulfhydryl PEG to increase their stability and bioavailability. The resulting gold nanoparticles were characterized with transmission electron microscopy (TEM), dynamic light scattering (DLS), UV-visible spectrometry and X-ray photoelectron spectroscopy (XPS), and the stability in biological solutions was evaluated. Comparing to PEGylated gold nanoparticles, CPP (CALNNPFVYLI, CALRRRRRRRR)-modified gold nanoparticles showed 46 folds increase in cellular uptake in A549 and B16 cell lines, as evidenced by the inductively coupled plasma atomic emission spectroscopy (ICP-AES). The interactions between gold nanoparticles and liposomes indicated CPP-modified gold nanoparticles bind to cell membrane more effectively than PEGylated gold nanoparticles. Surface plasmon resonance (SPR) was used to measure interactions between nanoparticles and the membrane. TEM and uptake inhibitor experiments indicated that the cellular entry of gold nanoparticles was mediated by clathrin and macropinocytosis. Other energy independent endocytosis pathways were also identified. Our work revealed a new strategy to modify gold nanoparticles with CPP and illustrated the cellular uptake pathway of CPP-modified gold nanoparticles. Copyright © 2017 Elsevier Inc. All rights reserved.
Gram-level synthesis of core-shell structured catalysts for the oxygen reduction reaction in proton exchange membrane fuel cells

NASA Astrophysics Data System (ADS)

Luo, Mingchuan; Wei, Lingli; Wang, Fanghui; Han, Kefei; Zhu, Hong

2014-12-01

Over the past decade, Pt based core-shell structured alloys have been studied extensively as oxygen reduction reaction (ORR) catalysts for proton exchange membrane fuel cells (PEMFCs) because of their distinctive electrochemical performance and low Pt loading. In this paper, a facile route based on microwave-assisted polyol method and chemical dealloying process is proposed to synthesize carbon supported core-shell structured nanoparticles (NPs) in gram-level for ORR electrocatalysis in PEMFCs. The obtained samples are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), inductively coupled plasma atomic emission spectroscopy (ICP-AES), and X-ray photoelectron spectroscopy (XPS). These physical characterization indicate that the final synthesized NPs are highly dispersed on the carbon support, and in a core-shell structure with CuPt alloy as the core and Pt as the shell. Electrochemical measurements, conducted by cyclic voltammetry (CV) and rotating disk electrode (RDE) tests, show the core-shell structured catalyst exhibit a 3× increase in mass activity and a 2× increase in specific activity over the commercial Pt/C catalyst, respectively. These results demonstrate that this route can be a reliable way to synthesize low-Pt catalyst in large-scale for PEMFCs.
Dopant occupancy and exposure energy in Hf:Nd:LiNbO3 crystal as a function of [Li]/[Nb] ratios

NASA Astrophysics Data System (ADS)

Dai, Li; Liu, Chunrui; Han, Xianbo; Yan, Zhehua; Tan, Chao; Wang, Luping; Xu, Yuheng

2017-09-01

A series of Hf: Nd: LiNbO3 crystals with various [Li]/[Nb] ratios ([Li]/[Nb] = 0.94, 1.05, 1.20, 1.38) in the melt were grown by conventional Czochralski technique. The distribution coefficients of Hf4+ and Nd3+ ions were recorded by an inductively coupled plasma-atomic emission spectrometer (ICP-AES). The effective distribution coefficient of Hf4+ is reduced and that of Nd3+ is increased with the increase of [Li]/[Nb] ratio in the melts. In all cases, the effective distribution coefficients is less than 1. The IR transmission spectroscopy of the Hf: Nd: LiNbO3 crystals were measured, getting the results that Hf: Yb: Ho: LiNbO3 crystals with 1.05 [Li]/[Nb] ratios was the stoichiometric. The optical damage resistance ability of Hf:Nd:LiNbO3 crystals were studied by light-induced scattering exposure energy flux threshold method and it increases with the increasing of [Li]/[Nb] ratios. When the [Li]/[Nb] ratio is 1.38 in the melt (the sample 4#), the exposure energy achieves 687.35 J/cm2, approximately 441 folds than that of the sample 1# ([Li]/[Nb] = 0.94) in magnitude.
Common plants as alternative analytical tools to monitor heavy metals in soil

PubMed Central

2012-01-01

Background Herbaceous plants are common vegetal species generally exposed, for a limited period of time, to bioavailable environmental pollutants. Heavy metals contamination is the most common form of environmental pollution. Herbaceous plants have never been used as natural bioindicators of environmental pollution, in particular to monitor the amount of heavy metals in soil. In this study, we aimed at assessing the usefulness of using three herbaceous plants (Plantago major L., Taraxacum officinale L. and Urtica dioica L.) and one leguminous (Trifolium pratense L.) as alternative indicators to evaluate soil pollution by heavy metals. Results We employed Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) to assess the concentration of selected heavy metals (Cu, Zn, Mn, Pb, Cr and Pd) in soil and plants and we employed statistical analyses to describe the linear correlation between the accumulation of some heavy metals and selected vegetal species. We found that the leaves of Taraxacum officinale L. and Trifolium pratense L. can accumulate Cu in a linearly dependent manner with Urtica dioica L. representing the vegetal species accumulating the highest fraction of Pb. Conclusions In this study we demonstrated that common plants can be used as an alternative analytical tool for monitoring selected heavy metals in soil. PMID:22594441
Development of strontium and magnesium substituted porous hydroxyapatite/poly(3,4-ethylenedioxythiophene) coating on surgical grade stainless steel and its bioactivity on osteoblast cells.

PubMed

Gopi, D; Ramya, S; Rajeswari, D; Surendiran, M; Kavitha, L

2014-02-01

The present study deals with the successful development of bilayer coatings by electropolymerisation of poly(3,4-ethylenedioxythiophene) (PEDOT) on surgical grade stainless steel (316L SS) followed by the electrodeposition of strontium (Sr) and magnesium (Mg) substituted porous hydroxyapatite (Sr, Mg-HA). The bilayer coatings were characterised by Fourier transform infrared spectroscopy (FT-IR) and high resolution scanning electron microscopy (HRSEM). Corrosion resistance of the obtained coatings was investigated in Ringer's solution by electrochemical techniques and the results were in good agreement with those obtained from chemical analysis, namely inductively coupled plasma atomic emission spectrometry (ICP-AES). Also, the mechanical and biological properties of the bilayer coatings were analyzed. From the obtained results it was evident that the PEDOT/Sr, Mg-HA bilayer exhibited greater adhesion strength than the Sr, Mg-HA coated 316L SS. In vitro cell adhesion test of the Sr, Mg-HA coating on PEDOT coated specimen is found to be more bioactive compared to that of the single substituted hydroxyapatite (Sr or Mg-HA) on the PEDOT coated 316L SS. Thus, the PEDOT/Sr, Mg-HA bilayer coated 316L SS can serve as a prospective implant material for biomedical applications. Copyright © 2013 Elsevier B.V. All rights reserved.
A comparison of techniques for preparing fish fillet for ICP-AES multielemental analysis and the microwave digestion of whole fish.

PubMed

Moeller, A; Ambrose, R F; Que Hee, S S

2001-01-01

Four catfish fillet homogenate treatments before multielemental metal analysis by simultaneous inductively coupled plasma/atomic emission spectroscopy were compared in triplicate. These treatments were: nitric acid wet-ashing by Parr bomb digestion; nitric acid wet-ashing by microwave digestion; tetramethylammonium hydroxide/nitric acid wet digestion; and dry-ashing. The tetramethylammonium hydroxide/nitric acid method was imprecise (coefficients of variation > 20%). The dry-ashing method was fast and sensitive but had low recoveries of 50% for spiked Pb and Al and was not as precise as the Parr bomb or microwave treatments. The Parr bomb method was the most precise method but was less sensitive than the microwave method which had nearly the same precision. The microwave method was then adapted to homogenates of small whole fish < or = 3 cm in length. The whole fish homogenate required more vigorous digestion conditions, and addition of more acid after the evaporative step because of the presence of less oxidizable and acid-soluble components than fillet. The whole fish homogenate was also more heterogeneous than catfish fillet. A quality assurance protocol to demonstrate homogenate uniformity is essential. The use of a non-specialized microwave oven system allowed precise results for fillet and whole fish homogenates.
A microbial transformation using Bacillus subtilis B7-S to produce natural vanillin from ferulic acid

PubMed Central

Chen, Peng; Yan, Lei; Wu, Zhengrong; Li, Suyue; Bai, Zhongtian; Yan, Xiaojuan; Wang, Ningbo; Liang, Ning; Li, Hongyu

2016-01-01

Bacillus subtilis strain B7-S screened from18 strains is an aerobic, endospore-forming, model organism of Gram-positive bacteria which is capable to form vanillin during ferulic acid bioconversion. The bioconversion of ferulic acid to vanillin by Bacillus subtilis B7-S (B. subtilis B7-S) was investigated. Based on our results, the optimum bioconversion conditions for the production of vanillin by B. subtilis B7-S can be summarized as follows: temperature 35 °C; initial pH 9.0; inoculum volume 5%; ferulic acid concentration 0.6 g/L; volume of culture medium 20%; and shaking speed 200 r/min. Under these conditions, several repeated small-scale batch experiments showed that the maximum conversion efficiency was 63.30% after 3 h of bioconversion. The vanillin products were confirmed by spectral data achieved from UV–vis, inductively coupled plasma atomic emission spectroscope (ICP-AES) and Fourier transform infrared spectrometer (FT-IR) spectra. Scanning electron microscopy (SEM) and transmission electron spectroscopy (TEM) results confirmed that the cell surface of B. subtilis plays a role in the induction of ferulic acid tolerance. These results demonstrate that B. subtilis B7-S has the potential for use in vanillin production through bioconversion of ferulic acid. PMID:26841717
A microbial transformation using Bacillus subtilis B7-S to produce natural vanillin from ferulic acid.

PubMed

Chen, Peng; Yan, Lei; Wu, Zhengrong; Li, Suyue; Bai, Zhongtian; Yan, Xiaojuan; Wang, Ningbo; Liang, Ning; Li, Hongyu

2016-02-04

Bacillus subtilis strain B7-S screened from18 strains is an aerobic, endospore-forming, model organism of Gram-positive bacteria which is capable to form vanillin during ferulic acid bioconversion. The bioconversion of ferulic acid to vanillin by Bacillus subtilis B7-S (B. subtilis B7-S) was investigated. Based on our results, the optimum bioconversion conditions for the production of vanillin by B. subtilis B7-S can be summarized as follows: temperature 35 °C; initial pH 9.0; inoculum volume 5%; ferulic acid concentration 0.6 g/L; volume of culture medium 20%; and shaking speed 200 r/min. Under these conditions, several repeated small-scale batch experiments showed that the maximum conversion efficiency was 63.30% after 3 h of bioconversion. The vanillin products were confirmed by spectral data achieved from UV-vis, inductively coupled plasma atomic emission spectroscope (ICP-AES) and Fourier transform infrared spectrometer (FT-IR) spectra. Scanning electron microscopy (SEM) and transmission electron spectroscopy (TEM) results confirmed that the cell surface of B. subtilis plays a role in the induction of ferulic acid tolerance. These results demonstrate that B. subtilis B7-S has the potential for use in vanillin production through bioconversion of ferulic acid.
Assessment of functional changes in nanoparticle-exposed neuroendocrine cells with amperometry: exploring the generalizability of nanoparticle-vesicle matrix interactions.

PubMed

Love, Sara A; Haynes, Christy L

2010-09-01

Using two of the most commonly synthesized noble metal nanoparticle preparations, citrate-reduced Au and Ag, the impacts of short-term accidental nanoparticle exposure are examined in primary culture murine adrenal medullary chromaffin cells. Transmission electron microscopy (TEM), inductively coupled plasma atomic emission spectroscopy (ICP-AES) and Alamar Blue viability studies revealed that nanoparticles are taken up by cells but do not decrease cell viability within 48 hours of exposure. Carbon-fiber microelectrode amperometry (CFMA) examination of exocytosis in nanoparticle-exposed cells revealed that nanoparticle exposure does lead to decreased secretion of chemical messenger molecules, of up to 32.5% at 48 hours of Au exposure. The kinetics of intravesicular species liberation also slows after nanoparticle exposure, between 30 and 50% for Au and Ag, respectively. Repeated stimulation of exocytosis demonstrated that these effects persisted during subsequent stimulations, meaning that nanoparticles do not interfere directly with the vesicle recycling machinery but also that cellular function is unable to recover following vesicle content expulsion. By comparing these trends with parallel studies done using mast cells, it is clear that similar exocytosis perturbations occur across cell types following noble metal nanoparticle exposure, supporting a generalizable effect of nanoparticle-vesicle interactions.
Toxic and essential mineral elements content of black tea leaves and their tea infusions consumed in Iran.

PubMed

Salahinejad, Maryam; Aflaki, Fereydoon

2010-04-01

The metal contents of eleven black tea samples, four cultivated in Iran and seven imported, and their tea infusions were determined. Twelve elements consisting toxic metals (Al, As, Pb, Cr, Cd, and Ni) and essential mineral elements (Fe, Zn, Cu, Mn, Ca, and Mg) were analyzed using inductively coupled plasma atomic emission spectroscopy (ICP-AES). Al, Ca, Mg, and Mn ranged in black tea leaves at mg g(-1) levels, while Cr, Fe, Ni, Cu, Zn were at microg g(-1) levels. Analysis of variance showed no statistically significant differences among most elements determined in cultivated and imported black teas in Iran except for Ni and Cu. The extraction efficiency of each element into tea infusions was evaluated. The solubility of measured metals in infusion extracts varied widely and ranged from 0 to 59.3%. Among the studied elements, Cr, Pb, and Cd showed the lowest rates of solubility and Ni had the highest rates of solubility. The amount of toxic metals and essential mineral elements that one may take up through consumption of black tea infusion was estimated. The amount of realizing each element into tea infusions and acceptable daily intake, for safety consumption of black tea, was compared.

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