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Sample records for plasma-atomic emission spectrometry

  1. Modified Babington nebulizer for inductively coupled plasma atomic emission spectrometry.

    PubMed

    Isoyama, Hirofumi; Uchida, Tetsuo; Nagashima, Takashi; Ohira, Osamu

    2003-04-01

    A PTFE Babingtonnebulizer equipped with a hood was investigated for inductively coupled plasma atomicemission spectrometry in conjunction with a PTFE cyclone chamber, in order to nebulize various sample solutions containing high salts, hydrofluoric acid and/or suspended solid. A hood of 3 mmphi (nozzle side) - 5 mmphi (outlet side) and 6 mm in length gave a comparable or higher sensitivity compared to a system with a commercially available concentric nebulizer and a glass cyclone chamber. Moreover, the present nebulizer was fully interchangeable with a concentric one at normal argon pressure, attaining sufficient stability, a short wash-out time and good nebulizing of high matrices solutions. The present system was successfully applied to the determination of trace impurities in highly pure silica powders.

  2. Preconcentration of heavy metals in urine and quantification by inductively coupled plasma atomic emission spectrometry.

    PubMed

    López-Artíguez, M; Cameán, A; Repetto, M

    1993-01-01

    This paper describes a method for the determination of heavy metals (Co, Ni, Cu, Cd, Pb) in urine by inductively coupled plasma atomic emission spectrometry (ICP-AES). The method proposed requires purification of the samples with activated charcoal under acidic conditions before preconcentration by complexation with ammonium pyrrolidinedithiocarbamate (APDC). The formed complexes are extracted with methyl isobutyl ketone (MIBK) and the resulting residue is finally digested under acid oxidant conditions. Because of its low detection limit (below 10 micrograms/L), this procedure can be applied conveniently for toxicological diagnostic purposes. PMID:8429621

  3. Matrix-Assisted Plasma Atomization Emission Spectrometry for Surface Sampling Elemental Analysis

    PubMed Central

    Yuan, Xin; Zhan, Xuefang; Li, Xuemei; Zhao, Zhongjun; Duan, Yixiang

    2016-01-01

    An innovative technology has been developed involving a simple and sensitive optical spectrometric method termed matrix-assisted plasma atomization emission spectrometry (MAPAES) for surface sampling elemental analysis using a piece of filter paper (FP) for sample introduction. MAPAES was carried out by direct interaction of the plasma tail plume with the matrix surface. The FP absorbs energy from the plasma source and releases combustion heating to the analytes originally present on its surface, thus to promote the atomization and excitation process. The matrix-assisted plasma atomization excitation phenomenon was observed for multiple elements. The FP matrix served as the partial energy producer and also the sample substrate to adsorb sample solution. Qualitative and quantitative determinations of metal ions were achieved by atomic emission measurements for elements Ba, Cu, Eu, In, Mn, Ni, Rh and Y. The detection limits were down to pg level with linear correlation coefficients better than 0.99. The proposed MAPAES provides a new way for atomic spectrometry which offers advantages of fast analysis speed, little sample consumption, less sample pretreatment, small size, and cost-effective. PMID:26762972

  4. Matrix-Assisted Plasma Atomization Emission Spectrometry for Surface Sampling Elemental Analysis

    NASA Astrophysics Data System (ADS)

    Yuan, Xin; Zhan, Xuefang; Li, Xuemei; Zhao, Zhongjun; Duan, Yixiang

    2016-01-01

    An innovative technology has been developed involving a simple and sensitive optical spectrometric method termed matrix-assisted plasma atomization emission spectrometry (MAPAES) for surface sampling elemental analysis using a piece of filter paper (FP) for sample introduction. MAPAES was carried out by direct interaction of the plasma tail plume with the matrix surface. The FP absorbs energy from the plasma source and releases combustion heating to the analytes originally present on its surface, thus to promote the atomization and excitation process. The matrix-assisted plasma atomization excitation phenomenon was observed for multiple elements. The FP matrix served as the partial energy producer and also the sample substrate to adsorb sample solution. Qualitative and quantitative determinations of metal ions were achieved by atomic emission measurements for elements Ba, Cu, Eu, In, Mn, Ni, Rh and Y. The detection limits were down to pg level with linear correlation coefficients better than 0.99. The proposed MAPAES provides a new way for atomic spectrometry which offers advantages of fast analysis speed, little sample consumption, less sample pretreatment, small size, and cost-effective.

  5. Matrix-Assisted Plasma Atomization Emission Spectrometry for Surface Sampling Elemental Analysis.

    PubMed

    Yuan, Xin; Zhan, Xuefang; Li, Xuemei; Zhao, Zhongjun; Duan, Yixiang

    2016-01-01

    An innovative technology has been developed involving a simple and sensitive optical spectrometric method termed matrix-assisted plasma atomization emission spectrometry (MAPAES) for surface sampling elemental analysis using a piece of filter paper (FP) for sample introduction. MAPAES was carried out by direct interaction of the plasma tail plume with the matrix surface. The FP absorbs energy from the plasma source and releases combustion heating to the analytes originally present on its surface, thus to promote the atomization and excitation process. The matrix-assisted plasma atomization excitation phenomenon was observed for multiple elements. The FP matrix served as the partial energy producer and also the sample substrate to adsorb sample solution. Qualitative and quantitative determinations of metal ions were achieved by atomic emission measurements for elements Ba, Cu, Eu, In, Mn, Ni, Rh and Y. The detection limits were down to pg level with linear correlation coefficients better than 0.99. The proposed MAPAES provides a new way for atomic spectrometry which offers advantages of fast analysis speed, little sample consumption, less sample pretreatment, small size, and cost-effective. PMID:26762972

  6. Expressing self-absorption in the analytical function of inductively coupled plasma atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Kántor, Tibor; Bartha, András

    2015-11-01

    The self-absorption of spectral lines was studied with up to date multi-element inductively coupled plasma atomic emission spectrometry (ICP-AES) instrumentation using radial and axial viewing of the plasma, as well, performing line peak height and line peak area measurements. Two resonance atomic and ionic lines of Cd and Mg were studied, the concentration range was extended up to 2000 mg/L. At the varying analyte concentration, constant matrix concentration of 10,000 mg/L Ca was ensured in the pneumatically nebulized solutions. The physical and the phenomenological formulation of the emission analytical function is overviewed and as the continuity of the earlier results the following equation is offered:

  7. The Kalman filter approach to inductively coupled plasma atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Van Veen, E. H.; Bosch, S.; De Loos-Vollebregt, M. T. C.

    1994-07-01

    This article is an electronic publication in Spectrochimica Acta Electronica (SAE), the electronic section of Spectrochimica Acta Part B (SAB). The hardcopy text, comprising the main article and two appendices, is accompanied by a disk containing the compiled program, a reference manual and data files. The work deals with data handling in inductively coupled plasma atomic emission spectrometry (ICP-AES). With this technique, the analyte signal is superimposed on a background signal. When separating the signals by manual or automated three-point background correction, there are many instances in which the data reduction fails. Based on scans recorded in a fast-scanning mode and on a library of pure-component scans, the Kaiman filter approach models the emission in the spectral window (about 100 pm) of the analyte and mathematically solves the problem of background correction. By using a criterion-based algorithm to correct for optical instability, the uncertainty in the determination of the interferent line signal is eliminated. Therefore, the present filter implementation yields more accurate and precise results, especially in the case of line overlap. The Kalman filter Approach to Atomic Spectrometry (KAAS) software automatically processes Perkin-Elmer Plasma 1000/2000 text files, but can also handle ASCII data files. Practical and comprehensive examples are given to evoke the "Kalman filter feeling" in the crucial step of creating the emission model.

  8. Methods for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry

    DOEpatents

    Chan, George C. Y.; Hieftje, Gary M.

    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.

  9. 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.

  10. Differentiation of colloidal and dissolved silica: Analytical separation using spectrophotometry and inductively coupled plasma atomic emission spectrometry

    USGS Publications Warehouse

    Lewis-Russ, A.; Ranville, J.; Kashuba, A.T.

    1991-01-01

    A method is described that differentiates between solutions containing silica-dominated colloids and solutions that are essentially free of colloids. Suspensions of tuff particles were treated to remove colloids by centrifugation, filtration or both. Agreement of silica concentrations determined by inductively coupled plasma atomic emission spectrometry and by a spectrophotometric method was taken as an indication of colloid-free solutions. For two tuffs, centrifugation was effective for removing colloids. For the third, highly altered tuff, filtration was more effective for removing colloids.

  11. Inelastic collisional deactivation in plasma-related non-spectroscopic matrix interferences in inductively coupled plasma atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Al-Ammar, Assad S.; Barnes, Ramon M.

    1999-07-01

    Inelastic collisional deactivation of the analyte excited state is demonstrated as a dominant cause for non-spectroscopic matrix interference in inductively coupled plasma atomic emission spectrometry (ICP-AES) for commonly used plasma operating conditions in routine analysis. A mathematical simulation of the inelastic collisional model was examined. Comparison between the theoretical model and experimental results using atomic and ionic lines of the analytes Zn, Ba, Mg, Mn and Sr validates the inelastic collisional deactivation model as a dominant cause for non-spectroscopic matrix effect. Matrices evaluated were NH 4Cl, NH 4SCN, (NH 4) 2SO 4, and H 2SO 4 to represent difficult-to-ionize matrices (DIE) and NaCl and CaCl 2 to represent easy-to-ionize element matrices (EIE).

  12. Subnanogram determination of inorganic and organic mercury by helium-microwave induced plasma-atomic emission spectrometry

    SciTech Connect

    Fukushi, K. ); Willie, S.N.; Sturgeon, R.E. )

    1993-02-01

    Inorganic and organic mercury were determined by helium-microwave induced plasma-atomic emission spectrometry following cold vapor generation. Whereas only inorganic mercury was reduced by stannous ion in an acidic medium, both inorganic and organic mercury (total mercury) were reduced by stannous ion in the presence of cupric ion in a basic medium. Organic mercury was determined as the difference between total and inorganic mercury. Detection limits for inorganic and organic mercury were 11 and 10 pg, respectively. The accuracy of the proposed method was verified through the determination of inorganic, total and organic mercury in two marine biological standard reference materials, DORM-1 and TORT-1. 21 refs., 1 fig., 4 tabs.

  13. Determination of Vanadium, Tin and Mercury in Atmospheric Particulate Matter and Cement Dust Samples by Direct Current Plasma Atomic Emission Spectrometry.

    ERIC Educational Resources Information Center

    Hindy, Kamal T.; And Others

    1992-01-01

    An atmospheric pollution study applies direct current plasma atomic emission spectrometry (DCP-AES) to samples of total suspended particulate matter collected in two industrial areas and one residential area, and cement dust collected near major cement factories. These samples were analyzed for vanadium, tin, and mercury. The results indicate the…

  14. 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.

  15. NEW METHOD FOR REMOVAL OF SPECTRAL INTERFERENCES FOR BERYLLIUM ASSAY USING INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY

    SciTech Connect

    Maxwell, S; Matthew Nelson, M; Linda Youmans, L; Maureen Bernard, M

    2008-01-14

    Beryllium has been used widely in specific areas of nuclear technology. Frequent monitoring of air and possible contaminated surfaces in U.S Department of Energy (DOE) facilities is required to identify potential health risks and to protect DOE workers from beryllium-contaminated dust. A new method has been developed to rapidly remove spectral interferences prior to beryllium (Be) measurement by inductively-coupled plasma atomic emission spectrometry (ICP-AES). The ion exchange separation removes uranium (U), thorium (Th), niobium (Nb), vanadium (V), molybdenum (Mo), zirconium (Zr), tungsten (W), iron (Fe), chromium (Cr), cerium (Ce), erbium (Er) and titanium (Ti). A stacked column consisting of Diphonix Resin{reg_sign} and TEVA Resin{reg_sign} reduces the levels of the spectral interferences so that low level Be measurements can be performed accurately. If necessary, an additional anion exchange separation can be used for further removal of interferences, particularly chromium. The method has been tested using spiked filters, spiked wipe samples and certified reference material standards with high levels of interferences added. The method provides very efficient removal of spectral interferences with very good accuracy and precision for beryllium on filters or wipes. A vacuum box system is employed to reduce analytical time and reduce labor costs.

  16. 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.

  17. Development of a partial least-squares calibration model for simultaneous determination of elements by inductively coupled plasma-atomic emission spectrometry.

    PubMed

    Chaloosi, Marzieh; Asadollahi, Seyed Azadeh; Khanchi, Ali Reza; FirozZare, Mahmoud; Mahani, Mohamad Khayatzadeh

    2009-01-01

    A partial least-squares (PLS) calibration model was developed for simultaneous multicomponent elemental analysis with inductively coupled plasma-atomic emission spectrometry (ICP-AES) in the presence of spectral interference. The best calibration model was obtained using a PLS2 algorithm. Validation was performed with an artificial test set. Multivariate calibration models were constructed using 2 series of synthetic mixtures (Zn, Cu, Fe, and U, V). Accuracy of the method was evaluated with unknown synthetic and real samples. PMID:19382589

  18. Spectral interferences in the determination of trace elements in environmental materials by inductively coupled plasma atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Daskalova, N.; Boevski, I. V.

    1999-07-01

    This paper deals with spectral interferences in inductively coupled plasma atomic emission spectrometry (ICP-AES) encountered with environmental materials. These samples normally contain high concentrations of aluminium, calcium, magnesium, iron, titanium, potassium and sodium. The investigations cover: (a) spectral data for Al, Ca, Mg, Fe, Ti, K and Na as interferents for 200 pm wide windows centred (±100 pm) around the prominent lines of As, B, Ba, Be, Cd, Cr, Cu, Hg, Mn, P, Pb, Sb, Se, Sn, Tl, U and Zn; (b) a data base of Q-values for line interference [ QI j(λ a)] and Q-values for wing background interference [ QW j(Δλ a)] for two values of the excitation temperature 6200 K and 7200 K. The lines free or negligibly influenced by line interference were selected for analyte determination. Q-values were used for calculation of correction factors under a spectral line without the measurement of a reference blank at the wavelength of the prominent analysis lines. The accuracy of ICP-AES with the Q-concept as a basic methodology is checked by the analysis of a certified reference material IAEA/Sediment SD-N-1/2/. The precision of the method is characterised by an RSD of 0.6-1.7%. Extraction of trace elements soluble in aqua regia was used as a decomposition method. This article is an electronic publication in Spectrochimica Acta Electronica (SAE), a section of Spectrochimica Acta, Part B (SAB). The hardcopy text is accompanied by an electronic archive, stored on the SAE homepage at http://www.elsevier.nl/locate/sabe. The archive contains the tabular material of this article in electronic form.

  19. Application of microwave plasma atomic emission spectrometry (MP-AES) for environmental monitoring of industrially contaminated sites in Hyderabad city.

    PubMed

    Kamala C T; Balaram V; Dharmendra V; Satyanarayanan M; Subramanyam K S V; Krishnaiah A

    2014-11-01

    Recently introduced microwave plasma-atomic emission spectroscopy (MP-AES) represents yet another and very important addition to the existing array of modern instrumental analytical techniques. In this study, an attempt is made to summarize the performance characteristics of MP-AES and its potential as an analytical tool for environmental studies with some practical examples from Patancheru and Uppal industrial sectors of Hyderabad city. A range of soil, sediment, water reference materials, particulate matter, and real-life samples were chosen to evaluate the performance of this new analytical technique. Analytical wavelengths were selected considering the interference effects of other concomitant elements present in different sample solutions. The detection limits for several elements were found to be in the range from 0.05 to 5 ng/g. The trace metals analyzed in both the sectors followed the topography with more pollution in the low-lying sites. The metal contents were found to be more in ground waters than surface waters. Since a decade, the pollutants are transfered from Patancheru industrial area to Musi River. After polluting Nakkavagu and turning huge tracts of agricultural lands barren besides making people residing along the rivulet impotent and sick, industrialists of Patancheru are shifting the effluents to downstream of Musi River through an 18-km pipeline from Patancheru. Since the effluent undergoes primary treatment at Common Effluent Treatment Plant (CETP) at Patanchru and travels through pipeline and mixes with sewage, the organic effluents will be diluted. But the inorganic pollutants such as heavy and toxic metals tend to accumulate in the environmental segments near and downstreams of Musi River. The data generated by MP-AES of toxic metals like Zn, Cu, and Cr in the ground and surface waters can only be attributed to pollution from Patancheru since no other sources are available to Musi River.

  20. The use of ion chromatography-dc plasma atomic emission spectrometry for the speciation of trace metals

    SciTech Connect

    Urasa, I.T.

    1991-09-20

    The original objects of this research program were: to interface d.c. plasma atomic emission spectrometer with an ion chromatograph; to characterize and optimize the combined systems for application in the speciation of metals in aqueous solutions; to use this system in the study of the solution chemistry of various metals; and to find ways in which the measurement sensitivity of the method can be enhanced, thereby allowing the detection of metal species at low ppb concentration levels. This approach has been used to study the chemistry of and speciate several elements in solution including: arsenic, chromium, iron, manganese, nickel phosphorus, platinum, selenium, and vanadium. During the course of this research, we have found that the solution chemistry of the elements studied and the speciation data obtained can vary considerably depending on the solution, and the chromatographic conditions employed. The speciation of chromium, iron, and vanadium was found to be highly influenced by the acidity of the sample. The element selective nature of the d.c. plasma detector allows these changes to be monitored, thereby providing quantitative information on the new moieties formed. New approaches are being developed including the use of chelating ligands as preconcentration agents for purposes of reducing further the detection limits of the elements of interest and to improve the overall element speciation scheme. New thrusts are being directed towards the employment of post-column derivatization method coupled with colorimetric measurements to detect and quantify metal species eluting from the chromatographic column. The influence of sample acidity on these investigations will be carefully evaluated. These new thrusts are described in the accompanying Project Renewal Proposal.

  1. Determination of iron, cobalt, nickel, manganese, zinc, copper, cadmium and lead in human hair by inductively coupled plasma-atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Sreenivasa Rao, K.; Balaji, T.; Prasada Rao, T.; Babu, Y.; Naidu, G. R. K.

    2002-08-01

    A method was standardized for the dissolution of hair samples and analysis was carried out by inductively coupled plasma atomic emission spectrometry (ICP-AES). Hair samples were brought into solution by using a mixture of nitric acid and hydrogen peroxide. Various parameters that influence the sample preparation, namely temperature, digestion time and ratio of acid mixture were studied and standardized. The optimized method has been employed to digest standard reference materials and hair samples of residents of India, collected from different age groups and sex, and analyzed for Fe, Co, Ni, Mn, Zn, Cu, Cd and Pb. The values agree for most of the metals with the data reported for human hair samples of residents of India. The NIES CRM Human Hair No. 5 and IAEA Reference Hair HH-1 certified reference materials were used in order to verify the accuracy of the method and the results were in excellent agreement with the certified values.

  2. 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.

  3. 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.

  4. Pressure dissolution and real sample matrix calibration for multielement analysis of raw agricultural crops by inductively coupled plasma atomic emission spectrometry

    SciTech Connect

    Kuennen, R.W.; Woinik, K.A.; Fricke, F.L.; Caruso, J.A.

    1982-11-01

    A method utilizing a pressure dissolution technique to minimize sample pretreatment is described for multielement analysis of raw agricultural crops by inductively coupled argon plasma atomic emission spectrometry. The procedure employs a 30-min pressure dissolution of sample composite with 6 M HCI at 80/sup 8/C in 60-mL linear polyethylene bottles. A sample introduction system is also described which permits direct atomization of complex organic matrices. Combined with a real sample matrix callbration technique, this introduction system allows rapid and accurate multielement analysis of complex HCl sample matrix solutions. The procedure compares favorably to more time-consuming conventional wet ashing methods for the determination of major, minor, and trace elements occurring in lettuce, potatoes, peanuts, soybeans, spinach, sweet corn, and wheat. Recoveries for spiked samples, precision studies, and analyses of NBS reference materials demonstrate the reliability and accuracy of the procedure. Advantages and limitations of this technique relative to conventional wet ashing methods are discussed. 2 figures, 7 tables.

  5. Effect of surfactant addition on ultrasonic leaching of trace elements from plant samples in inductively coupled plasma-atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Borkowska-Burnecka, Jolanta; Jankowiak, Urszula; Zyrnicki, Wieslaw; Anna Wilk, Kazimiera

    2004-04-01

    The applicability of surfactants in sample preparation of plant materials followed by analysis by inductively coupled plasma atomic emission spectrometry has been examined. Reference materials (INCT-MPH-2-Mixed Polish Herbs, INCT-TL-1 black tea leaves and CTA-VTL-2 -Virginia tobacco leaves) and commercially available tea leaves were analyzed. Effects of addition surfactants (Triton X-100, didodecyldimethylammonium bromide and cetyltrimethylammonium bromide) on efficiency of ultrasonic leaching of elements from the plant samples and on plasma parameters were investigated. Low concentrations of the surfactants in solutions did not affect, in practice, analytical line intensities and the nebulization process. Quantitative recovery of some elements could be obtained by ultrasonic diluted acid leaching with the aid of surfactants. However, the element recovery depended on type of surfactant, as well as element and sample material. Plasma parameters, i.e. the excitation temperatures of Ar I, Fe II and Ca II as well as the electron number density and the Mg II/Mg I intensity ratio did not vary significantly due to the surfactants in solutions.

  6. Multielement determination of heavy metals in water samples by continuous powder introduction microwave-induced plasma atomic emission spectrometry after preconcentration on activated carbon

    NASA Astrophysics Data System (ADS)

    Jankowski, Krzysztof; Yao, Jun; Kasiura, Krzysztof; Jackowska, Adrianna; Sieradzka, Anna

    2005-03-01

    A novel continuous powder introduction microwave-induced plasma atomic emission spectrometry method (CPI-MIP-AES) has been developed for trace determination of metals in ground and tap water samples after preconcentration on activated carbon. The experimental setup consisted of integrated rectangular cavity TE 101 and vertically positioned plasma torch. The technical arrangement of the sample introduction system has been designed based on the fluidized bed concept. The satisfactory signal stability required for sequential analysis was attained owing to the vertical plasma configuration, as well as the plasma gas flow rate compatibility with sample introduction flow rate. The elements of interest (Cd, Cu, Cr, Fe, Mn, Pb, Zn) were preconcentrated in a batch procedure at pH 8-8.5 after addition of activated carbon and then, after filtering and drying of the activated carbon suspension, introduced to the MIP by the CPI system. An enrichment factor of about 1000-fold for a sample volume of 1 l was obtained. The detection limit values for the proposed method were 17-250 ng l -1. The proposed method was validated by analyzing the certified reference materials: SRW "Warta" Synthetic River Water and BCR CRM 399 major elements in freshwater. The method was successfully applied to the determination of the heavy metals in tap water samples.

  7. Method development for the determination of calcium, copper, magnesium, manganese, iron, potassium, phosphorus and zinc in different types of breads by microwave induced plasma-atomic emission spectrometry.

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2016-06-01

    A novel method was developed for the determination of calcium, magnesium, potassium, iron, copper, zinc, and manganese and phosphorous in various kinds of breads samples sold in Turkey by microwave plasma-atomic emission spectrometry (MIP-AES). Breads were dried at 100 °C for one day, ground thoroughly and then digested using nitric acid/hydrogen per oxide (3:1). The analytes in certified reference wheat flour and maize flour samples were determined in the uncertainty limits of the certified values as well as the analytes added to the mixture of ground bread and acid mixture prior to digestion were recovered quantitatively (>90%). Therefore, all determinations were made by linear calibration technique using aqueous standards. The LOD values for Ca, Cu, Fe, K, Mg, Mn, P and Zn were 13.1, 0.28, 4.47, 118, 1.10, 0.41, 7550 and 3.00 ng mL(-1), respectively. No spectral interference was detected at the working wavelengths of the analytes. PMID:26830585

  8. Method development for the determination of calcium, copper, magnesium, manganese, iron, potassium, phosphorus and zinc in different types of breads by microwave induced plasma-atomic emission spectrometry.

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2016-06-01

    A novel method was developed for the determination of calcium, magnesium, potassium, iron, copper, zinc, and manganese and phosphorous in various kinds of breads samples sold in Turkey by microwave plasma-atomic emission spectrometry (MIP-AES). Breads were dried at 100 °C for one day, ground thoroughly and then digested using nitric acid/hydrogen per oxide (3:1). The analytes in certified reference wheat flour and maize flour samples were determined in the uncertainty limits of the certified values as well as the analytes added to the mixture of ground bread and acid mixture prior to digestion were recovered quantitatively (>90%). Therefore, all determinations were made by linear calibration technique using aqueous standards. The LOD values for Ca, Cu, Fe, K, Mg, Mn, P and Zn were 13.1, 0.28, 4.47, 118, 1.10, 0.41, 7550 and 3.00 ng mL(-1), respectively. No spectral interference was detected at the working wavelengths of the analytes.

  9. Determination of rare earth elements in geological materials by inductively coupled argon plasma/atomic emission spectrometry

    USGS Publications Warehouse

    Crock, J.G.; Lichte, F.E.

    1982-01-01

    Inductively coupled argon plasma/optical emission spectrometery (ICAP/OES) is useful as a simultaneous, multielement analytical technique for the determination of trace elements in geological materials. A method for the determination of trace-level rare earth elements (REE) in geological materials using an ICAP 63-channel emission spectrometer is described. Separation and preconcentration of the REE and yttrium from a sample digest are achieved by a nitric acid gradient cation exchange and hydrochloric acid anion exchange. Precision of 1-4% relative standard deviation and comparable accuracy are demonstrated by the triplicate analysis of three splits of BCR-1 and BHVO-1. Analyses of other geological materials including coals, soils, and rocks show comparable precision and accuracy.

  10. Determination of microamounts of hafnium in zirconium using inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry during their separation by ion exchange on Diphonix chelating resin.

    PubMed

    Smolik, Marek; Jakóbik-Kolon, Agata

    2009-04-01

    Inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICPMS) methods were applied to check the possibility of determination of hafnium in zirconium at a level lower than 100 ppm. A zirconium matrix of hafnium content lower than 10 ppm was obtained using a worked-out separation method exploiting ion exchange on Diphonix resin. Both methods give results in good agreement with each other as well as with those for certified reference material BCR-098 (Zircaloy-4). They were utilized in determination of Hf in the samples collected during separation of microamounts of hafnium from zirconium by the mentioned ion exchange. These results proved the earlier described method of separation on Diphonix resin to be effective even when the initial concentration of hafnium in zirconium decreases from 2.4% to 0.0082%.

  11. Determination of hafnium at the 10(-4)% level (relative to zirconium content) using neutron activation analysis, inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry.

    PubMed

    Smolik, Marek; Polkowska-Motrenko, Halina; Hubicki, Zbigniew; Jakóbik-Kolon, Agata; Danko, Bożena

    2014-01-01

    Hafnium at the very low level of 1-8 ppm (in relation to zirconium) was determined in zirconium sulfate solutions (originating from investigations of the separation of ca. 44 ppm Hf from zirconium by means of the ion exchange method) by using three independent methods: inductively coupled plasma mass spectrometry (ICP MS), neutron activation analysis (NAA) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The results of NAA and ICP MS determinations were consistent with each other across the entire investigated range (the RSD of both methods did not exceed 38%). The results of ICP-AES determination were more diverse, particularly at less than 5 ppm Hf (RSD was significantly higher: 29-253%). The ion exchange method exploiting Diphonix(®) resin proved sufficient efficiency in Zr-Hf separation when the initial concentration ratio of the elements ([Zr]0/[Hf]0) ranged from 1200 to ca. 143,000.

  12. Determination of aluminum and silicon in biological materials by inductively coupled plasma atomic emission spectrometry with electrothermal vaporization

    NASA Astrophysics Data System (ADS)

    Matusiewicz, Henryk; Barnes, Ramon M.

    An atomic emission spectrometric method is described for the determination of trace elements in microvolume samples especially of biological materials. Based upon the arrangement of a commercial electrothermal vaporizer and a 40-MHz inductively coupled plasma, the direct determination of aluminum and silicon in human body fluids such as urine and serum and aluminum in hemodialysis solution is performed. The instrumental system involves vaporizing the sample from a modified graphite electrode followed by atomization and excitation of the vapors in the ICP discharge. Compromise experimental conditions are reported and calibration functions compared. Limits of detection in 5-μl samples were 8 pg Al and 2.5 ng Si, and after preconcentration of Al with a poly(acrylamidoxime) resin, the detection limit was 1 pg Al. Recovery of 5 μg Si/ml and 10 ng Al/ml from aqueous and synthetic standards was 80-85% and 96-103%, respectively.

  13. MPTS-silica coated capillary microextraction on line hyphenated with inductively coupled plasma atomic emission spectrometry for the determination of Cu, Hg and Pb in biological samples.

    PubMed

    Zheng, Fei; Hu, Bin

    2007-09-15

    A novel sol-gel 3-mercaptopropyltrimethoxysilane (MPTS) modified silica coating was developed for capillary microextraction (CME) of trace Cu, Hg and Pb prior to their on line determination by inductively coupled plasma-atomic emission spectrometry (ICP-AES). This organic-inorganic hybrid coating was in situ created on the inner walls of fused silica capillary using a sol solution containing TMOS (tetramethoxysilane) as a precursor, MPTS as a co-precursor, ethanol as the solvent and hydrochloric acid as a catalyst. The structure of the capillary coating was characterized by FT-IR spectroscopy, Raman spectroscopy, SEM and TEM. The factors affecting on the capillary microextraction of analytes such as pH, sample flow rate and volume, elution solution and interfering ions had been investigated, and the optimized experimental parameters were obtained. Under the optimized conditions, the absorption capacity of MPTS-silica coated capillary was found to be 1.17, 1.96 and 1.19mugm(-1) for Cu, Hg and Pb, and the limits of detection were as low as 0.17 0.22 and 0.52ngmL(-1), respectively. With a sampling frequency of 12h(-1), the relative standard deviations (R.S.D.s) were 4.2, 2.6 and 3.8% (C=4ngmL(-1), n=7, sample volume=1mL) for Cu, Hg and Pb, respectively. The proposed method had been successfully applied to the determination of Cu, Hg and Pb in human urine, human serum and preserved egg. To validate the proposed method, certified reference materials of BCR151 milk powder, GBW07601 (GSH-1) human hair, GSBZ 50016-90 and GSB 07-1183-2000 water samples were analyzed and the determined values were in a good agreement with the certified values.

  14. Separation and preconcentration of ultra trace amounts of beryllium in water samples using mixed micelle-mediated extraction and determination by inductively coupled plasma-atomic emission spectrometry.

    PubMed

    Beiraghi, Assadollah; Babaee, Saeed

    2008-01-28

    In the present study a cloud point extraction process using mixed micelle of the cationic surfactant cetyl-pyridinium chloride (CPC) and non-ionic surfactant Triton X-114 for extraction of beryllium from aqueous solutions is developed. The extraction of analyte from aqueous samples was performed in the presence of 1,8-dihydroxyanthrone as chelating agent in buffer media of pH 9.5. After phase separation, the surfactant-rich phase was diluted with 0.4mL of a 60:40 methanol-water mixture containing 0.03 mL HNO(3). Then, the enriched analyte in the surfactant-rich phase was determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The different variables affecting the complexation and extraction conditions were optimized. Under the optimum conditions (i.e. 1.6 x 10(-4) molL(-1) 1,8-dihydroxyanthrone, 1.2 x 10(-4) molL(-1) CPC, 0.15% (v/v) Triton X-114, 50 degrees C equilibrium temperature) the calibration graph was linear in the range of 0.006-80 ngmL(-1) with detection limit of 0.001 ngmL(-1) and the precision (R.S.D.%) for five replicate determinations at 18 ngmL(-1) of Be(II) was better than 2.9%. In this manner the preconcentration and enrichment factors were 16.7 and 24.8, respectively. Under the presence of foreign ions no significant interference was observed. Finally, the proposed method was successfully utilized for the determination of this cation in water samples.

  15. Element analysis and characteristic identification of non-fumigated and sulfur-fumigated Fritillaria thunbergii Miq. using microwave digestion-inductively coupled plasma atomic emission spectrometry combined with Fourier transform infrared spectrometry

    PubMed Central

    Lou, Yajing; Cai, Hao; Liu, Xiao; Tu, Sicong; Pei, Ke; Zhao, Yingying; Cao, Gang; Li, Songlin; Qin, Kunming; Cai, Baochang

    2014-01-01

    Background: Sulfur-fumigation may induce chemical transformation of traditional Chinese medicines leading to harmful effects following patient ingestion. For quality control, it is urgently needed to develop a reliable and efficient method for sulfur-fumigation identification. Materials and Methods: The spectrochemical identification of non-fumigated and sulfur-fumigated Fritillaria thunbergii Miq. was carried out to evaluate inorganic elements and organic components. The concentrations of 12 elements, including Zn, Mn, Cu, Fe, Li, Mg, Sr, Pb, As, Cd, Hg, and S of samples were determined by microwave digestion - inductively coupled plasma atomic emission spectrometry (ICP-AES). Meanwhile, Fourier transform infrared spectrometry (FTIR) was used for the study of chemical group characteristic reactions after sulfur-fumigation. Results: The concentrations of Fe, Mg, Hg, and S elements showed significant differences between non-fumigated and sulfur-fumigated Fritillaria thunbergii Miq. The characteristic stretching vibrations of some groups in FTIR spectra, such as -OH, -S = O and -S-O, provided the identification basis for the discrimination of non-fumigated and sulfur-fumigated Fritillaria thunbergii Miq. Conclusion: The application of microwave digestion - ICP-AES was successfully used in combination with FTIR to authenticate and evaluate the quality of medicinal Fritillaria thunbergii Miq. Further applications of this technique should be explored. PMID:24914306

  16. 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.

  17. 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. PMID:27591646

  18. The use of ion chromatography-dc plasma atomic emission spectrometry for the speciation of trace metals. Annual performance report, February 1, 1989--January 31, 1992

    SciTech Connect

    Urasa, I.T.

    1991-09-20

    The original objects of this research program were: to interface d.c. plasma atomic emission spectrometer with an ion chromatograph; to characterize and optimize the combined systems for application in the speciation of metals in aqueous solutions; to use this system in the study of the solution chemistry of various metals; and to find ways in which the measurement sensitivity of the method can be enhanced, thereby allowing the detection of metal species at low ppb concentration levels. This approach has been used to study the chemistry of and speciate several elements in solution including: arsenic, chromium, iron, manganese, nickel phosphorus, platinum, selenium, and vanadium. During the course of this research, we have found that the solution chemistry of the elements studied and the speciation data obtained can vary considerably depending on the solution, and the chromatographic conditions employed. The speciation of chromium, iron, and vanadium was found to be highly influenced by the acidity of the sample. The element selective nature of the d.c. plasma detector allows these changes to be monitored, thereby providing quantitative information on the new moieties formed. New approaches are being developed including the use of chelating ligands as preconcentration agents for purposes of reducing further the detection limits of the elements of interest and to improve the overall element speciation scheme. New thrusts are being directed towards the employment of post-column derivatization method coupled with colorimetric measurements to detect and quantify metal species eluting from the chromatographic column. The influence of sample acidity on these investigations will be carefully evaluated. These new thrusts are described in the accompanying Project Renewal Proposal.

  19. High-temperature liquid chromatography inductively coupled plasma atomic emission spectrometry hyphenation for the combined organic and inorganic analysis of foodstuffs.

    PubMed

    Terol, Amanda; Paredes, Eduardo; Maestre, Salvador E; Prats, Soledad; Todolí, José L

    2010-10-01

    The coupling of a High-Temperature Liquid Chromatography system (HTLC) with an Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES) is reported for the first time. This hyphenation combines the separation efficiency of HTLC with the detection power of a simultaneous ICP-AES system and allows the combined determination of organic compound and metals. The effluents of the column were introduced into the spectrometer and the chromatograms for organic compounds were obtained by plotting the carbon emission signal at a characteristic wavelength versus time. As regards metals, they were determined by injecting a small sample volume between the exit of the column and the spectrometer and taking the emission intensity for each one of the elements simultaneously. Provided that in HTLC the effluents emerged at high temperatures, an aerosol was easily generated at the exit of the column. Therefore, the use of a pneumatic nebulizer as a component of a liquid sample introduction system in the ICP-AES could be avoided, thus reducing the peak dispersion and limits of detection by a factor of two. The fact that a hot liquid stream was nebulized made it necessary to use a thermostated spray chamber so as to avoid the plasma cooling as a cause of the excessive mass of solvent delivered to it. Due to the similarity in sample introduction, an Evaporative Light Scattering Detector (ELSD) was taken as a reference. Comparatively speaking, limits of detection were of the same order for both HTLC-ICP-AES and HTLC-ELSD, although the latter provided better results for some compounds (from 10 to 20 mg L(-1) and 5-10 mg L(-1), respectively). In contrast, the dynamic range for the new hyphenation was about two orders of magnitude wider. More importantly, HTLC-ICP-AES provided information about the content of both organic (glucose, sucrose, maltose and lactose at concentrations from roughly 10 to 400 mg L(-1)) as well as inorganic (magnesium, calcium, sodium, zinc, potassium and

  20. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of dissolved aluminum and boron in water by inductively coupled plasma-atomic emission spectrometry

    USGS Publications Warehouse

    Struzeski, T.M.; DeGiacomo, W.J.; Zayhowski, E.J.

    1996-01-01

    Inductively coupled plasma-atomic emission spectrometry is a sensitive, rapid, and accurate method for determining the dissolved concentration of aluminum and boron in water samples. The method detection limits are 5 micrograms per liter for aluminum and 4 micrograms per liter for boron. For aluminum, low-level (about 30 micrograms per liter) short-term precision (single-operator, seven days) is about 5 percent relative standard deviation and the low-level long-term precision (single-operator, nine months) is about 8 percent relative standard deviation. For boron, the low-level short-term precision is about 4 percent relative standard deviation, and the low-level long-term precision is about 5 percent relative standard deviation. Spike recoveries for aluminum ranged from 86 to 100 percent, and recoveries for boron ranged from 92 to 109 percent.

  1. 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

  2. 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.

  3. Determination of soluble toxic arsenic species in alga samples by microwave-assisted extraction and high performance liquid chromatography-hydride generation-inductively coupled plasma-atomic emission spectrometry.

    PubMed

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

    2006-09-29

    A microwave-based procedure for arsenic species extraction in alga samples (Sargassum fulvellum, Chlorella vulgaris, Hizikia fusiformis and Laminaria digitata) is described. Extraction time and temperature were tested in order to evaluate the extraction efficiency of the process. Arsenic compounds were extracted in 8 ml of deionised water at 90 degrees C for 5 min. The process was repeated three times. Soluble arsenic compounds extracted accounted for about 78-98% of total arsenic. The results were compared with those obtained in a previous work, where the extraction process was carried out by ultrasonic focussed probe for 30 s. Speciation studies were carried out by high performance liquid chromatography-hydride generation-inductively coupled plasma-atomic emission spectrometry (HPLC-HG-ICP-AES). The chromatographic method allowed us to separate As(III), As(V), monomethylarsonic acid and dimethylarsinic acid in less than 13 min. The chromatographic analysis of the samples allowed us to identify and quantify As(V) in Hizikia sample and Sargasso material, while the four arsenic species studied were found in Chlorella sample. In the case of Laminaria sample, none of these species was identified by HPLC-HG-ICP-AES. However, in the chromatographic analysis of this alga by HPLC-ICP-AES, an unknown arsenic species was detected.

  4. Determination of soluble toxic arsenic species in alga samples by microwave-assisted extraction and high performance liquid chromatography-hydride generation-inductively coupled plasma-atomic emission spectrometry.

    PubMed

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

    2006-09-29

    A microwave-based procedure for arsenic species extraction in alga samples (Sargassum fulvellum, Chlorella vulgaris, Hizikia fusiformis and Laminaria digitata) is described. Extraction time and temperature were tested in order to evaluate the extraction efficiency of the process. Arsenic compounds were extracted in 8 ml of deionised water at 90 degrees C for 5 min. The process was repeated three times. Soluble arsenic compounds extracted accounted for about 78-98% of total arsenic. The results were compared with those obtained in a previous work, where the extraction process was carried out by ultrasonic focussed probe for 30 s. Speciation studies were carried out by high performance liquid chromatography-hydride generation-inductively coupled plasma-atomic emission spectrometry (HPLC-HG-ICP-AES). The chromatographic method allowed us to separate As(III), As(V), monomethylarsonic acid and dimethylarsinic acid in less than 13 min. The chromatographic analysis of the samples allowed us to identify and quantify As(V) in Hizikia sample and Sargasso material, while the four arsenic species studied were found in Chlorella sample. In the case of Laminaria sample, none of these species was identified by HPLC-HG-ICP-AES. However, in the chromatographic analysis of this alga by HPLC-ICP-AES, an unknown arsenic species was detected. PMID:16876177

  5. Automated detection and interpretation of spectral information using cross-correlation, millilitre volumes, pneumatic nebulization sample introduction and inductively coupled plasma-atomic emission spectrometry with photodiode array detection

    NASA Astrophysics Data System (ADS)

    Karanassios, V.; Drouin, P. J.; Spiers, G. A.

    1998-08-01

    A method for automated detection and interpretation of spectral information from ˜230 nm spectral windows, millilitre volume samples for 15 elements is presented. The basic approach involves cross-correlation of a spectral pattern obtained by running laboratory prepared multi-element `unknowns' with a reference spectral pattern obtained by running a single element standard. From the resultant cross-correlogram, it can be decided whether or not the sought-for reference spectral pattern (and the corresponding element) are present in the unknown. Spectral patterns were acquired using an inductively coupled plasma-atomic emission spectrometry (ICP-AES) system equipped with a linear, 1024-element, photo-diode array (Leco, Plasmarray). Reference spectral patterns for Al, Au, Be, Cd, Cu, Ga, Mg, Mn, Ni, Pd, Si, Sc, Y, Sr and Zn were converted to noise-free and interference-free binary software masks and, subsequently, to analogue software masks. Cross-correlation of the analogue masks with spectral patterns acquired by running multi-element unknowns is discussed, an algorithm that does not rely on fast Fourier transforms (FFT) to calculate cross-correlations is presented and a context-sensitive, colour-coded and interrogatable periodic table graphical user-interface that presents the likely composition of an unknown on the computer screen is described in detail.

  6. Assessing oral bioaccessibility of trace elements in soils under worst-case scenarios by automated in-line dynamic extraction as a front end to inductively coupled plasma atomic emission spectrometry.

    PubMed

    Rosende, María; Magalhães, Luis M; Segundo, Marcela A; Miró, Manuel

    2014-09-01

    A novel biomimetic extraction procedure that allows for the in-line handing of ≥400 mg solid substrates is herein proposed for automatic ascertainment of trace element (TE) bioaccessibility in soils under worst-case conditions as per recommendations of ISO norms. A unified bioaccessibility/BARGE method (UBM)-like physiological-based extraction test is evaluated for the first time in a dynamic format for accurate assessment of in-vitro bioaccessibility of Cr, Cu, Ni, Pb and Zn in forest and residential-garden soils by on-line coupling of a hybrid flow set-up to inductively coupled plasma atomic emission spectrometry. Three biologically relevant operational extraction modes mimicking: (i) gastric juice extraction alone; (ii) saliva and gastric juice composite in unidirectional flow extraction format and (iii) saliva and gastric juice composite in a recirculation mode were thoroughly investigated. The extraction profiles of the three configurations using digestive fluids were proven to fit a first order reaction kinetic model for estimating the maximum TE bioaccessibility, that is, the actual worst-case scenario in human risk assessment protocols. A full factorial design, in which the sample amount (400-800 mg), the extractant flow rate (0.5-1.5 mL min(-1)) and the extraction temperature (27-37°C) were selected as variables for the multivariate optimization studies in order to obtain the maximum TE extractability. Two soils of varied physicochemical properties were analysed and no significant differences were found at the 0.05 significance level between the summation of leached concentrations of TE in gastric juice plus the residual fraction and the total concentration of the overall assayed metals determined by microwave digestion. These results showed the reliability and lack of bias (trueness) of the automatic biomimetic extraction approach using digestive juices.

  7. On-line collection/concentration and determination of transition and rare-earth metals in water samples using Multi-Auto-Pret system coupled with inductively coupled plasma-atomic emission spectrometry.

    PubMed

    Katarina, Rosi Ketrin; Oshima, Mitsuko; Motomizu, Shoji

    2009-05-15

    On-line preconcentration and determination of transition and rare-earth metals in water samples was performed using a Multi-Auto-Pret system coupled with inductively coupled plasma-atomic emission spectrometry (ICP-AES). The Multi-Auto-Pret AES system proposed here consists of three Auto-Pret systems with mini-columns that can be used for the preconcentration of trace metals sequentially or simultaneously, and can reduce analysis time to one-third and running cost of argon gas and labor. A newly synthesized chelating resin, ethylenediamine-N,N,N'-triacetate-type chitosan (EDTriA-type chitosan), was employed in the Multi-Auto-Pret system for the collection of trace metals prior to their measurement by ICP-AES. The proposed resin showed very good adsorption ability for transition and rare-earth metal ions without any interference from alkali and alkaline-earth metal ions in an acidic media. For the best result, pH 5 was adopted for the collection of metal ions. Only 5 mL of samples could be used for the determination of transition metals, while 20 mL of samples was necessary for the determination of rare-earth metals. Metal ions adsorbed on the resin were eluted using 1.5 M nitric acid, and were measured by ICP-AES. The proposed method was evaluated by the analysis of SLRS-4 river water reference materials for trace metals. Good agreement with certified and reference values was obtained for most of the metals examined; it indicates that the proposed method using the newly synthesized resin could be favorably used for the determination of transition and rare-earth metals in water samples by ICP-AES.

  8. In situ calibration of inductively coupled plasma-atomic emission and mass spectroscopy

    DOEpatents

    Braymen, Steven D.

    1996-06-11

    A method and apparatus for in situ addition calibration of an inductively coupled plasma atomic emission spectrometer or mass spectrometer using a precision gas metering valve to introduce a volatile calibration gas of an element of interest directly into an aerosol particle stream. The present situ calibration technique is suitable for various remote, on-site sampling systems such as laser ablation or nebulization.

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

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2016-02-01

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

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

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2016-02-01

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

  11. In situ calibration of inductively coupled plasma-atomic emission and mass spectroscopy

    DOEpatents

    Braymen, S.D.

    1996-06-11

    A method and apparatus are disclosed for in situ addition calibration of an inductively coupled plasma atomic emission spectrometer or mass spectrometer using a precision gas metering valve to introduce a volatile calibration gas of an element of interest directly into an aerosol particle stream. The present in situ calibration technique is suitable for various remote, on-site sampling systems such as laser ablation or nebulization. 5 figs.

  12. Inductively coupled plasma -- Atomic emission spectroscopy glove box assembly system at the West Valley Demonstration Project

    SciTech Connect

    Marlow, J.H.; McCarthy, K.M.; Tamul, N.R.

    1999-12-17

    The inductively coupled plasma/atomic emission spectroscopy [ICP/AES (ICP)] system for elemental analyses in support of vitrification processing was first installed in 1986. The initial instrument was a Jobin Yvon (JY) Model JY-70 ICP that consisted of sequential and simultaneous spectrometers for analysis of nonradioactive samples as radioactive surrogates. The JY-70 ICP continued supporting nonradioactive testing during the Functional and Checkout Testing of Systems (FACTS) using the full-scale melter with ``cold'' (nonradioactive) testing campaigns. As a result, the need for another system was identified to allow for the analysis of radioactive samples. The Mass Spec (Spectrometry) Lab was established for the installation of the modified ICP system for handling radioactive samples. The conceptual setup of another ICP was predicated on the use of a hood to allow ease of accessibility of the torch, nebulizer, and spray chamber, and the minimization of air flow paths. However, reconsideration of the radioactive sample dose rate and contamination levels led to the configuration of the glovebox system with a common transfer interface box for the ICP and the inductively coupled plasma-mass spectrometer (ICP-MS) glovebox assemblies. As a result, a simultaneous Model JY-50P ICP with glovebox was installed in 1990 as a first generation ICP glovebox system. This was one of the first ICP glovebox assemblies connected with an ICP-MS glovebox system. Since the economics of processing high-level radioactive waste (HLW) required the availability of an instrument to operate 24 hours a day throughout the year without any downtime, a second generation ICP glovebox assembly was designed, manufactured, and installed in 1995 using a Model JY-46P ICP. These two ICP glovebox systems continue to support vitrification of the HLW into canisters for storage. The ICP systems have been instrumental in monitoring vitrification batch processing. To date, remote sample preparation and

  13. Measurement of lanthanum and technetium in uranium fuels by inductively coupled plasma atomic emission spectroscopy.

    SciTech Connect

    Carney, K.; Crane, P.; Cummings, D.; Krsul, J.; McKnight, R.

    1999-06-10

    An important parameter in characterizing an irradiated nuclear fuel is determining the amount of uranium fissioned. By determining the amount of uranium fissioned in the fuel a burnup performance parameter can be calculated, and the amount of fission products left in the fuel can be predicted. The quantity of uranium fissioned can be calculated from the amount of lanthanum and technetium present in the fuel. Lanthanum and technetium were measured in irradiated fuel samples using an Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) instrument and separation equipment located in a shielded glove-box. A discussion of the method, interferences, detection limits, quality control and a comparison to other work will be presented.

  14. Slurry sample introduction with microwave induced plasma atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Matusiewicz, Henryk; Sturgeon, Ralph E.

    1993-04-01

    The successful direct introduction of aqueous slurry samples into a highly efficient TE 101 microwave plasma has been demonstrated. Slurry samples from a spray chamber are fed directly into the cavity with no desolvation apparatus. A V-groove, clog-free Babington-type nebulizer was evaluated for use with high solids content solutions. Slurry concentrations up to 10% m/v were used for the microwave induced plasma work with calibration by the standard additions method. Results are presented for the analysis of two NRCC Standard Reference Materials, i.e. TORT-1 (Lobster Hepatopancreas) and PACS-21 (Marine Sediment). Agreement between analytical results and certified values for the test elements Cd, Cu, Fe and Zn (in the range of 28-850 μg/g) was good. No memory effects were evident and the nebulizer system had a rapid clean-out time.

  15. Determination of total tin in canned food using inductively coupled plasma atomic emission spectroscopy.

    PubMed

    Perring, Loïc; Basic-Dvorzak, Marija

    2002-09-01

    Tin is considered to be a priority contaminant by the Codex Alimentarius Commission. Tin can enter foods either from natural sources, environmental pollution, packaging material or pesticides. Higher concentrations are found in processed food and canned foods. Dissolution of the tinplate depends on the of food matrix, acidity, presence of oxidising reagents (anthocyanin, nitrate, iron and copper) presence of air (oxygen) in the headspace, time and storage temperature. To reduce corrosion and dissolution of tin, nowadays cans are usually lacquered, which gives a marked reduction of tin migration into the food product. Due to the lack of modern validated published methods for food products, an ICP-AES (Inductively coupled plasma-atomic emission spectroscopy) method has been developed and evaluated. This technique is available in many laboratories in the food industry and is more sensitive than atomic absorption. Conditions of sample preparation and spectroscopic parameters for tin measurement by axial ICP-AES were investigated for their ruggedness. Two methods of preparation involving high-pressure ashing or microwave digestion in volumetric flasks were evaluated. They gave complete recovery of tin with similar accuracy and precision. Recoveries of tin from spiked products with two levels of tin were in the range 99+/-5%. Robust relative repeatabilities and intermediate reproducibilities were <5% for different food matrices containing >30 mg/kg of tin. Internal standard correction (indium or strontium) did not improve the method performance. Three emission lines for tin were tested (189.927, 283.998 and 235.485 nm) but only 189.927 nm was found to be robust enough with respect to interferences, especially at low tin concentrations. The LOQ (limit of quantification) was around 0.8 mg/kg at 189.927 nm. A survey of tin content in a range of canned foods is given. PMID:12324843

  16. Multielement analysis of geologic materials by inductively coupled plasma-atomic emission spectroscopy

    SciTech Connect

    Christensen, O.D.; Kroneman, R.L.; Capuano, R.M.

    1980-03-01

    Atomic emission spectroscopy using an inductively coupled plasma (ICP) source permits the rapid acquisition of multielement geochemical data from a wide variety of geologic materials. Rocks or other solid samples are taken into solution with a four acid digestion procedure and introduced directly into the plasma; fluid samples are acidified or analyzed directly. The entire process is computer-controlled, fully-automated, and requires less than five minutes per sample for quantitative determination of 37 elements. The procedures and instrumentation employed at the ESL for multielement ICP analysis of geologic materials are described and these are intended as a guide for evaluating analytic results reported from this laboratory. The quality of geochemical data can be characterized by precision, limits of quantitative determination, and accuracy. Precision values are a measure of the repeatability of analyses. In general, major element and analyses have precision of better than 5% and trace elements of better than 10% of the amount present. (MHR)

  17. High speed analysis of agricultural samples using inductively coupled plasma-atomic emission spectroscopy

    NASA Astrophysics Data System (ADS)

    Isaac, R. A.; Johnson, W. C.

    The determination of potassium, phosphorus, calcium, magnesium, zinc and manganese in soil extracts are reported at an analysis rate of 200 samples h -1. A 4 cm 3volume of soil is extracted with a 20 ml solution of 0.025 N H 2SO 4-0.05 N HCl (Mehlich I). The filtered solution is then placed on a Technicon Sampler IV, which is interfaced to an 1CP emission spectrometer. This extract is analyzed for all the nutrients above. In addition to soil extracts, the ICP is used for mineral analyses of feed samples at a sample rate of 120 samples h -1. Several "American Association of Feed Control Officials" check feed samples have been analyzed and the results will be discussed comparing the ICP results with other laboratories participating in the program. The preparation of feed samples involves ashing a 1 g sample at 500°C for 4 h. The ashed sample was then taken up in hot HCl and diluted to 250 ml. Analyses are also performed by ICP on water, heavy metals in sewage sludge, and on other materials. The ICP technique has increased the efficiency of our laboratory to the extent that one technician can do the same work that formerly required four technicians.

  18. Laser Ablation Solid Sampling processes investigated usinginductively coupled plasma - atomic emission spectroscopy (ICP-AES)

    SciTech Connect

    Mao, X.L.; Ciocan, A.C.; Borisov, O.V.; Russo, R.E.

    1997-07-01

    The symbiotic relationship between laser ablation mechanismsand analytical performance using inductively coupled plasma-atomicemission spectroscopy are addressed in this work. For both cases, it isimportant to ensure that the ICP conditions (temperature and electronnumber density) are not effected by the ablated mass. By ensuring thatthe ICP conditions are constant, changes in spectral emission intensitywill be directly related to changes in laser ablation behavior. Mg ionicline to atomic line ratios and excitation temperature were measured tomonitor the ICP conditions during laser-ablation sample introduction. Thequantity of ablated mass depends on the laser pulse duration andwavelength. The quantity of mass removed per unit energy is larger whenablating with shorter laser wavelengths and pulses. Preferential ablationof constituents from a multicomponent sample was found to depend on thelaser beam properties (wavelength and pulse duration). Fornanosecond-pulsed lasers, thermal vaporization dominates the ablationprocess. For picosecond-pulsed lasers, a non-thermal mechanism appears todominate the ablation process. This work will describe the mass ablationbehavior during nanosecond and picosecond laser sampling into the ICP.The behavior of the ICP under mass loading conditions is firstestablished, followed by studies of the ablation behavior at variouspower densities. A thermal vaporization model is used to explainnanosecond ablation, and a possible non-thermal mechanism is proposed toexplain preferential ablation of Zn and Cu from brass samples duringpicosecond ablation.

  19. LASER ABLATION-INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION SPECTROSCOPY STUDY AT THE 222-S LABORATORY USING HOT-CELL GLOVE BOX PROTOTYPE SYSTEM

    SciTech Connect

    SEIDEL CM; JAIN J; OWENS JW

    2009-02-23

    This report describes the installation, testing, and acceptance of the Waste Treatment and Immobilization Plant (WTP) procured laser ablation-inductively coupled plasma-atomic emission spectroscopy (LA-ICP-AES) system for remotely analyzing high-level waste (HLW) samples in a hot cell environment. The work was completed by the Analytical Process Development (APD) group in accordance with Task Order 2005-003; ATS MP 1027, Management Plan for Waste Treatment Plant Project Work Performed by Analytical Technical Services. The APD group at the 222-S Laboratory demonstrated acceptable turnaround time (TAT) and provide sufficient data to assess sensitivity, accuracy, and precision of the LA-ICP-AES method.

  20. LASER ABLATION-INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION SPECTROSCOPY STUDY AT THE 222-S LABORATORY USING HOT-CELL GLOVE BOX PROTOTYPE SYSTEM

    SciTech Connect

    LOCKREM LL; OWENS JW; SEIDEL CM

    2009-03-26

    This report describes the installation, testing and acceptance of the Waste Treatment and Immobilization Plant procured laser ablation-inductively coupled plasma-atomic emission spectroscopy (LA-ICP-AES) system for remotely analyzing high-level waste samples in a hot cell environment. The 2005-003; ATS MP 1027, Management Plan for Waste Treatment Plant Project Work Performed by Analytical Technical Services. The APD group at the 222-S laboratory demonstrated acceptable turnaround time (TAT) and provide sufficient data to assess sensitivity, accuracy, and precision of the LA-ICP-AES method.

  1. Determination of Ca, Mg, Na, Cd, Cu, Fe, K, Li and Zn in acid mine and reference water samples by inductively coupled plasma atomic fluorescence spectrometry

    USGS Publications Warehouse

    Sanzolone, R.F.; Meier, A.L.

    1986-01-01

    An inductively coupled plasma atomic fluorescence spectrometric (ICP-AFS) method was used for the determination of nine elements in natural water. Reference and acid mine water samples were analysed by this method to demonstrate its usefulness for hydrogeochemical exploration. The elements were determined in two groups based on the compatibility of operating conditions and consideration of element abundance levels in natural water. Ca, Mg and Na were determined as a group using one set of instrumental conditions and a 1 + 99 dilution of the sample, and Cd, Cu, Fe, K, Li and Zn were determined using another set of conditions and the undiluted sample. The detection limits for the elements are as follows: Ca, 1.4; Mg, 1.7; Na, 2.0; Cd, 1.8; Cu, 6.2; Fe, 15.8; K, 3.5; Li, 0.3; and Zn, 1.2 ng m1-1. Each element has a linear range spanning about four orders of magnitude. The method has good precision and accuracy, as shown by statistics on replicate analyses and by the agreement between values obtained and those recommended for the reference water samples, and also those obtained by atomic absorption spectrometry for the acid mine water samples.

  2. 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. PMID:20047806

  3. 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.

  4. Selection of operating conditions and analytical procedure in multi-metal analysis of animal tissues by d.c. plasma-atomic emission spectroscopy

    NASA Astrophysics Data System (ADS)

    Frank, Adrian; Petersson, Lars R.

    In order to expand the analytical capacity and achieve better utilization of tissue materials (liver, kidney, etc.) so as to assess the degrees of environmental pollution, a method for simultaneous determination of 14 metals (Al, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Ni, Pb, V, W, and Zn) has been developed by applying d.c. plasma-atomic emission spectroscopy. The analytical emission lines were chosen after considering the absence of more important interfering emission lines from elements present in the matrix, and taking into account their intensity, background, range of linearity and working range. At increasing ionic buffer concentration most metals seem to have a region of relatively little change in intensity. A 0.25 M LiNO 3 solution was chosen as ionic buffer. Optimization of plasma position to obtain maximum light intensity at each of the analytical wavelengths was studied with both single- and multi-element cassettes. The intention was to find a plasma position with satisfactory light intensity for all metals to be determined simultaneously. Spectral interferences, stray light effects included, from elements present in the matrix were investigated and linear relationships were usually found between the "false" signal contribution and the concentration of the interfering element. These signals were expressed as spectral interference correction coefficients (SICC values) on a concentration equivalent basis, viz. μ ml -1 per μ ml -1. The effect of Ca on the analytical emission lines of Al, Pb, and W was not linear in contrast to the usual relationship. Organ tissues are prepared by automated wet digestion. Transfer of sample solution from the sample tray into the plasma is performed automatically. A microcomputer is used for evaluation of metal contents in the solutions, background correction by use of SICC values, and final calculation of metal concentrations in the tissues.

  5. Evaluation of a direct injection nebulizer interface for flow injection analysis and high performance liquid chromatography with inductively coupled plasma-atomic emission spectroscopic detection

    SciTech Connect

    LaFreniere, K.E.

    1986-06-01

    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, 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.

  6. Evaluation of a direct injection nebulizer interface for flow injection analysis and high performance liquid chromatography with inductively coupled plasma-atomic emission spectroscopic detection

    SciTech Connect

    LaFreniere, K.E.

    1986-01-01

    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 the 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.

  7. Comparison of several spray chambers operating at very low liquid flow rates in inductively coupled plasma atomic emission spectrometry.

    PubMed

    Todolí, J L; Maestre, S; Mora, J; Canals, A; Hernandis, V

    2000-12-01

    Four different spray chambers were evaluated in ICP-AES at very low liquid flow rates: a double-pass (Scott type), a conventional cyclonic, and two low-volume cyclonic-type spray chambers (i.e., Cinnabar and Genie). A glass concentric pneumatic micro nebulizer (Atom Mist) was used in conjunction with all four chambers. The liquid flow rate was varied from 10 to 160 microL min(-1). The conventional cyclonic spray chamber gave rise to coarser tertiary aerosols, higher analyte and solvent transport rates, higher sensitivity and lower limits of detection than the remaining ones. The low-volume spray chambers afforded analytical figures of merit similar to the double-pass one, despite their very different designs. However, these spray chambers exhibited shorter wash-out times. The matrix effects were significant only for the double-pass. This fact allowed the analysis of reference samples by employing aqueous standards at a minimum level of sample consumption. The recoveries obtained for the cyclonic spray chambers and several certified samples were close to 100%, being always lower in the case of the double-pass spray chamber.

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

    USGS Publications Warehouse

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

    1990-01-01

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

  9. Determination of gaseous semi- and low-volatile organic halogen compounds by barrier-discharge atomic emission spectrometry.

    PubMed

    Sun, Yifei; Watanabe, Nobuhisa; Wang, Wei; Zhu, Tianle

    2013-01-01

    A group parameter approach using "total organic halogen" is effective for monitoring gaseous organic halogen compounds, including fluorine, chlorine, and bromine compounds, generated from combustion. We described the use of barrier-discharge radiofrequency-helium-plasma/atomic emission spectrometry, for the detection of semi- and low-volatile organic halogen compounds (SLVOXs), which can be collected by Carbotrap adsorbents and analyzed using thermal desorption. The optimal carrier gas flow rates at the injection and desorption lines were established to be 100 mL/min. The detection range for SLVOXs in the gaseous samples was from 10 ng to tens of micrograms. Measuring F was more difficult than measuring C1 or Br, because the wavelength of F is close to that of air. The barrier-discharge radiofrequency-helium-plasma/atomic emission spectrometry measured from 85% to 103% of the SLVOXs in the gas sample. It has been found that Carbotrap B is appropriate for high-boiling-point compounds, and Carbotrap C is suitable for the determination of organic halogen compounds with lower boiling points, in the range 200-2300C. Under optimal analysis conditions, a chlorine-containing plastic was destroyed using different oxygen concentrations. Lower oxygen concentrations resulted in the production of lower amounts of organic halogen compounds. PMID:23586317

  10. Determination of gaseous semi- and low-volatile organic halogen compounds by barrier-discharge atomic emission spectrometry.

    PubMed

    Sun, Yifei; Watanabe, Nobuhisa; Wang, Wei; Zhu, Tianle

    2013-01-01

    A group parameter approach using "total organic halogen" is effective for monitoring gaseous organic halogen compounds, including fluorine, chlorine, and bromine compounds, generated from combustion. We described the use of barrier-discharge radiofrequency-helium-plasma/atomic emission spectrometry, for the detection of semi- and low-volatile organic halogen compounds (SLVOXs), which can be collected by Carbotrap adsorbents and analyzed using thermal desorption. The optimal carrier gas flow rates at the injection and desorption lines were established to be 100 mL/min. The detection range for SLVOXs in the gaseous samples was from 10 ng to tens of micrograms. Measuring F was more difficult than measuring C1 or Br, because the wavelength of F is close to that of air. The barrier-discharge radiofrequency-helium-plasma/atomic emission spectrometry measured from 85% to 103% of the SLVOXs in the gas sample. It has been found that Carbotrap B is appropriate for high-boiling-point compounds, and Carbotrap C is suitable for the determination of organic halogen compounds with lower boiling points, in the range 200-2300C. Under optimal analysis conditions, a chlorine-containing plastic was destroyed using different oxygen concentrations. Lower oxygen concentrations resulted in the production of lower amounts of organic halogen compounds.

  11. Developments in glow discharge emission spectrometry

    NASA Astrophysics Data System (ADS)

    Ferreira, N. P.; Strauss, J. A.; Human, H. G. C.

    Developments in the field of glow discharge emission spectrometry at the National Physical Research Laboratory of the Council for Scientific and Industrial Research comprise measurement of fundamental plasma parameters, instrumental development and analytical applications. While reference is only made to published material, recent developments are described in more detail, e.g. the use of a fluorescent atomic vapour as spectral line isolator and the use of a microwave auxiliary discharge to augment excitation of sputtered material.

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

    PubMed

    Zachariadis, G A; Rosenberg, E

    2009-04-30

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

  13. Determination of methylmercury and butyltin compounds in marine biota and sediments using microwave-assisted acid extraction, solid-phase microextraction, and gas chromatography with microwave-induced plasma atomic emission spectrometric detection.

    PubMed

    Tutschku, Silke; Schantz, Michele M; Wise, Stephen A

    2002-09-15

    A method is described for the determination of methylmercury and butyltin compounds in marine sediment and tissue using microwave-assisted acid extraction or digestion and solid-phase microextraction (SPME) followed by analysis using gas chromatography with microwave-induced plasma atomic emission spectrometric detection (GC-MIP-AES). Using the SPME-GC-MIP-AES method, enrichment factors for methylmercury and butyltin compounds of 50-100 were achieved, as compared to the typical hexane extraction, and measurements in marine tissue and sediment matrixes were possible at 1-2 microg/kg (methylmercury) and 10-100 ng/kg (butyltins). The SPME-GC-MIP-AES method was validated using several marine sediment and tissue matrix certified reference materials (CRMs) with certified values for methylmercury and butyltin compounds. The SPME-GC-MIP-AES method was used to measure methylmercury in four marine tissue CRMs ranging from oyster tissue at 13.0 +/- 1.0 microg/kg to fish tissue at 397 +/- 13 microg/kg (as Hg dry mass). Results from the SPME-GC-MIP-AES method were used in conjunction with results from other techniques to assign certified values for methylmercury in oyster, mussel, and fish tissue CRMs. Mono-, di-, and tributyltin were measured in three sediment CRMs at concentration levels of (0.08 +/- 0.03)-(0.35 +/- 0.05) mg/kg (as Sn dry mass). PMID:12349972

  14. Digital image-based flame emission spectrometry.

    PubMed

    Silva Lyra, Wellington; Dos Santos, Vagner Bezerra; Dionízio, Amália Geiza Gama; Martins, Valdomiro Lacerda; Almeida, Luciano Farias; Nóbrega Gaião, Edvaldo; Diniz, Paulo Henrique Gonçalves Dias; Silva, Edvan Cirino; Araújo, Mário César Ugulino

    2009-03-15

    A digital image-based flame emission spectrometric (DIB-FES) method for the quantitative chemical analysis is proposed here for the first time. The DIB-FES method employs a webcam to capture the digital images which are associated to a radiation emitted by the analyte into an air-butane flame. Since the detection by webcam is based on the RGB (red-green-blue) colour system, a novel mathematical model was developed in order to build DIB-FES analytical curves and estimate figures of merit for the proposed method. In this approach, each image is retrieved in the three R, G and B individual components and their values were used to define a position vector in RGB three-dimensional space. The norm of this vector is then adopted as the RGB-based value (analytical response) and it has revealed to be linearly related to the analyte concentration. The feasibility of the DIB-FES method is illustrated in three applications involving the determination of lithium, sodium and calcium in anti-depressive drug, physiological serum and water, respectively. In comparison with the traditional flame emission spectrometry (trad-FES), no statistic difference has been observed between the results by applying the paired t-test at the 95% confidence level. However, the DIB-FES method has offered the largest sensitivities and precision, as well as the smallest limits of detection and quantification for the three analytes. These advantageous characteristics are attributed to the trivariate nature of the detection by webcam. PMID:19159768

  15. Tin Content Determination in Canned Fruits and Vegetables by Hydride Generation Inductively Coupled Plasma Optical Emission Spectrometry

    PubMed Central

    Rončević, Sanda; Benutić, Anica; Nemet, Ivan; Gabelica, Buga

    2012-01-01

    Tin content in samples of canned fruits and vegetables was determined by hydride generation inductively coupled plasma atomic emission spectrometry (HG-ICP-OES), and it was compared with results obtained by standard method of flame atomic absorption spectrometry (AAS). Selected tin emission lines intensity was measured in prepared samples after addition of tartaric acid and followed by hydride generation with sodium borohydride solution. The most favorable line at 189.991 nm showed the best detection limit (1.9 μg L−1) and limit of quantification (6.4 μg kg−1). Good linearity and sensitivity were established from time resolved analysis and calibration tests. Analytical accuracy of 98–102% was obtained by recovery study of spiked samples. Method of standard addition was applied for tin determination in samples from fully protected tinplate. Tin presence at low-concentration range was successfully determined. It was shown that tenth times less concentrations of Sn were present in protected cans than in nonprotected or partially protected tinplate. PMID:22550488

  16. METHOD 200.5 - DETERMINATION OF TRACE ELEMENTS IN DRINKING WATER BY AXIALLY VIEWED INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION SPECTROMETRY

    EPA Science Inventory

    2.0 SUMMARY OF METHOD
    2.1. A 50 mL aliquot of a well-mixed, non-filtered, acid preserved aqueous sample is accurately transferred to clean 50-mL plastic disposable digestion tube containing a mixture of nitric and hydrochloric acids. The aliquot is heated to 95 degrees C (+ o...

  17. Simultaneous preconcentration of copper and mercury in water samples by cloud point extraction and their determination by inductively coupled plasma atomic emission spectrometry.

    PubMed

    Shoaee, Hamta; Roshdi, Mina; Khanlarzadeh, Nasibeh; Beiraghi, Asadollah

    2012-12-01

    A cloud-point extraction process coupled to ICP-OES by using 3-nitro benzaldehyde thiosemicarbazone (3-NBT) as complexing agent was developed for the simultaneous preconcentration and determination of copper and mercury in water samples. The variables affecting the complexation and extraction steps were optimized. Under the optimum conditions (i.e. 1.5×10(-5) mol L(-1) ligand, 0.3% (v/v) Triton X-114, 55 °C equilibrium temperature, incubation time of 30 min) the calibration graphs were linear in the range of 5-120 and 10-100 ng mL(-1) with enhancement factor of 82.7 and 51.3 for Cu(2+) and Hg(2+), respectively. The preconcentration factors were 28.6 in both cases and detection limits were obtained 0.48 for Cu and 1.1 ng mL(-1) for Hg. The precisions (R.S.D.%) for five replicate determinations at 50 ng mL(-1) of copper and mercury were better than 1.8% and 3.2%, respectively. The accuracy of the proposed method is validated by analyzing a certified reference material of water (RTC-QCI-049) with satisfactory results. Finally, the proposed method was utilized successfully for the determination of copper and mercury in surface water (river), tap water and bottled mineral water samples.

  18. Simultaneous preconcentration of copper and mercury in water samples by cloud point extraction and their determination by inductively coupled plasma atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Shoaee, Hamta; Roshdi, Mina; Khanlarzadeh, Nasibeh; Beiraghi, Asadollah

    2012-12-01

    A cloud-point extraction process coupled to ICP-OES by using 3-nitro benzaldehyde thiosemicarbazone (3-NBT) as complexing agent was developed for the simultaneous preconcentration and determination of copper and mercury in water samples. The variables affecting the complexation and extraction steps were optimized. Under the optimum conditions (i.e. 1.5 × 10-5 mol L-1 ligand, 0.3% (v/v) Triton X-114, 55 °C equilibrium temperature, incubation time of 30 min) the calibration graphs were linear in the range of 5-120 and 10-100 ng mL-1 with enhancement factor of 82.7 and 51.3 for Cu2+ and Hg2+, respectively. The preconcentration factors were 28.6 in both cases and detection limits were obtained 0.48 for Cu and 1.1 ng mL-1 for Hg. The precisions (R.S.D.%) for five replicate determinations at 50 ng mL-1 of copper and mercury were better than 1.8% and 3.2%, respectively. The accuracy of the proposed method is validated by analyzing a certified reference material of water (RTC-QCI-049) with satisfactory results. Finally, the proposed method was utilized successfully for the determination of copper and mercury in surface water (river), tap water and bottled mineral water samples.

  19. The use of ion chromatography-D.C. plasma atomic emission spectrometry for the speciation of trace metals. Final performance technical report, February 1, 1995--January 31, 1998

    SciTech Connect

    Urasa, I.T.

    1998-06-12

    The chemistry of heavy metals in natural waters, industrial waste streams, and the environment is influenced by a number of factors including the prevailing matrix, their relative concentrations, and biologically or chemically induced transformations. Speciation, which entails the identification and quantification of all the forms of a metal or any other chemical entity present in a sample, is a necessary step in assessing the toxic and pollution effects and the overall impact of these entities on environmental systems. Analytical methods and protocols that can provide analytical data in the parts per billion concentration range and below are needed for these kinds of measurements. The thrust of this research was to develop metal speciation methods and techniques using direct current plasma (DCPAES) in combination with ion chromatography (IC), whereby the DCPAES serves as an element selective detector (ESD) for the metal species separated in the chromatographic column. While the metal speciation work carried out in this program has utilized the IC-DCPAES as the primary analytical measurement tool, other sample processing and preparation approaches have also been developed to enhance the effectiveness and capability of the chromatographic-element selective method of metal speciation. Post-column derivatization and solid phase extraction are two protocols which were incorporated with IC-ESD with significant improvements in the capability of the method.

  20. 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.

  1. Secondary ion mass spectrometry: Polyatomic and molecular ion emission

    NASA Astrophysics Data System (ADS)

    Colton, Richard J.; Ross, Mark M.; Kidwell, David A.

    1986-03-01

    Secondary ion mass spectrometry (SIMS) has become a diverse tool for the study of many substances such as metals, semiconductors, inorganic compounds and organic compounds, including polymers and biomolecules. This paper discusses the formation and emission of polyatomic and molecular ions from surfaces of these materials. The mass, energy, and abundance distribution of cluster ions emitted from various solids — Van der Waals, molecular, metallic, ionic and covalent — are compared. Trends in their emission patterns are discussed in terms of a recombination or a direct emission mechanism. For example, the ion abundance of cluster ions sputtered from metals decreases monotonically with increasing cluster size due to a decreasing formation probability for large clusters. The emission from metal oxides, however, shows a broad distribution of M mO ±n cluster ions whose formation can be described by both recombination and direct emission mechanisms. Covalently bonded molecules tend to eject as intact species. The emission of molecular ions is also discussed with respect to the method of ionization and the various sample preparation and matrix-assisted and derivatization procedures used. For example, the emission of molecular ions from metal surfaces is strongly influenced by the nature of the adsorption site; and matrix-assisted and derivatization procedures enhance the ionization efficiency of the analyte.

  2. Resolving Emissions Dynamics via Mass Spectrometry: Time Resolved Measurements of Emission Transients by Mass Spectrometry

    SciTech Connect

    Partridge, William P.

    2000-08-20

    Transient emissions occur throughout normal engine operation and can significantly contribute to overall system emissions. Such transient emissions may originate from various sources including cold start, varying load and exhaust-gas recirculation (EGR) rates; all of which are dynamic processes in the majority of engine operation applications (1). Alternatively, there are systems which are inherently dynamic even at steady-state engine-operation conditions. Such systems include catalytic exhaust-emissions treatment devices with self-initiated and sustained oscillations (2) and NOX adsorber systems (3,4,5). High-speed diagnostics, capable of temporally resolving such emissions transients, are required to characterize the process, verify calculated system inputs, and optimize the system.

  3. 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)

    SciTech Connect

    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, 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.

  4. HPLC-ICP atomic emission spectrometry in environmental analysis

    SciTech Connect

    Frame, E.M.S.

    1996-10-01

    Trace concentrations of many compounds are difficult to determine directly by traditional chromatographic techniques. Organosilicon compounds, for example, have no chromophoric groups. Size exclusion (SEC) and high performance liquid chromatography (HPLC) can separate high and low molecular weight organosilicon compounds, but routinely employ detectors with insufficient sensitivity for trace concentrations in environmental samples. Elemental analysis methods such as inductively coupled plasma optical emission spectrometry (ICP) provide excellent element sensitivity but no speciation information. Interfacing of a chromatographic method with ICP has been shown to provide quantitative determination of trace compounds while retaining the chemical speciation information. This work will describe the power of the HPLC-ICP combination for trace compounds in environmental samples to identify and determine ppm levels of organometallics.

  5. Evaluation of flow injection-solution cathode glow discharge-atomic emission spectrometry for the determination of major elements in brines.

    PubMed

    Yang, Chun; Wang, Lin; Zhu, Zhenli; Jin, Lanlan; Zheng, Hongtao; Belshaw, Nicholas Stanley; Hu, Shenghong

    2016-08-01

    A new method for the determination of major metal elements in high salinity brines was developed by solution cathode glow discharge (SCGD) with flow injection analysis (FIA). The matrix interferences of major cations and anions in brines have been evaluated. It was found that high concentration of Na(+) and K(+) could interfere each other, K(+) at a concentration of 400mgL(-1) enhanced the signal intensity of Na(+) more than 20%. The effect of the anions was observed and it was noted that the signal intensity of both Ca(2+) and Mg(2+) were suppressed significantly when the SO4(2-) reached 100mgL(-1). It was demonstrated that some low molecular weight organic substances such as formic acid, glycerol and ascorbic acid could eliminate interference of SO4(2-) even with volume percentages of 0.5%. Under the optimized condition, the proposed FIA-SCGD can determine K, Na, Ca and Mg with the limits of detection of 0.49 (K), 0.14 (Na), 11 (Ca) and 5.5 (Mg) ngmL(-1). The proposed method has been successfully applied to the analysis of 5 salt lake samples and compared with those obtained with inductively coupled plasma atomic emission spectrometry (ICP-AES). The advantages of small size, low energy consumption, good stability and repeatability indicated that the SCGD is promising for the determination of major ions in brine samples. PMID:27216688

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

    ERIC Educational Resources Information Center

    Horlick, Gary

    1984-01-01

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

  7. High-capacity chitosan-based chelating resin for on-line collection of transition and rare-earth metals prior to inductively coupled plasma-atomic emission spectrometry measurement.

    PubMed

    Katarina, Rosi Ketrin; Oshima, Mitsuko; Motomizu, Shoji

    2009-10-15

    High-capacity chitosan-based chelating resin, N-(2-hydroxyethyl)glycine-type chitosan, was synthesized using chloromethyloxirane (CMO) as a cross-linker and a coupling arms and hydroxylethylamine and bromoacetic acid as a synthesizer for the N-(2-hydroxyethyl)glycine chelating moiety. The CMO could bind with both of hydroxyl and amino group of the chitosan resin, and then couple with the chelating moiety. Increasing the amounts of chelating moiety could increase the capacity of the resin toward metal ions. Most transition and rare-earth metals could adsorb quantitatively on the resin at wide pH ranges and could be separated from alkaline and alkaline-earth metals. The resin was packed in a mini-column (40 mm length x 2 mm i.d.) which was installed in a Multi-Auto-Pret system. The Multi-Auto-Pret system coupled with ICP-AES was successfully applied to the determination of transition and rare-earth metals in river water samples.

  8. Pulsed, atmospheric pressure plasma source for emission spectrometry

    DOEpatents

    Duan, Yixiang; Jin, Zhe; Su, Yongxuan

    2004-05-11

    A low-power, plasma source-based, portable molecular light emission generator/detector employing an atmospheric pressure pulsed-plasma for molecular fragmentation and excitation is described. The average power required for the operation of the plasma is between 0.02 W and 5 W. The features of the optical emission spectra obtained with the pulsed plasma source are significantly different from those obtained with direct current (dc) discharge higher power; for example, strong CH emission at 431.2 nm which is only weakly observed with dc plasma sources was observed, and the intense CN emission observed at 383-388 nm using dc plasma sources was weak in most cases. Strong CN emission was only observed using the present apparatus when compounds containing nitrogen, such as aniline were employed as samples. The present apparatus detects dimethylsulfoxide at 200 ppb using helium as the plasma gas by observing the emission band of the CH radical. When coupled with a gas chromatograph for separating components present in a sample to be analyzed, the present invention provides an apparatus for detecting the arrival of a particular component in the sample at the end of the chromatographic column and the identity thereof.

  9. Constraining Anthropogenic and Biogenic Emissions Using Chemical Ionization Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Spencer, Kathleen M.

    Numerous gas-phase anthropogenic and biogenic compounds are emitted into the atmosphere. These gases undergo oxidation to form other gas-phase species and particulate matter. Whether directly or indirectly, primary pollutants, secondary gas-phase products, and particulate matter all pose health and environmental risks. In this work, ambient measurements conducted using chemical ionization mass spectrometry are used as a tool for investigating regional air quality. Ambient measurements of peroxynitric acid (HO2NO2) were conducted in Mexico City. A method of inferring the rate of ozone production, PO3, is developed based on observations of HO2NO 2, NO, and NO2. Comparison of this observationally based PO3 to a highly constrained photochemical box model indicates that regulations aimed at reducing ozone levels in Mexico City by reducing NOx concentrations may be effective at higher NO x levels than predicted using accepted photochemistry. Measurements of SO2 and particulate sulfate were conducted over the Los Angeles basin in 2008 and are compared to measurements made in 2002. A large decrease in SO2 concentration and a change in spatial distribution are observed. Nevertheless, only a modest reduction in sulfate concentration is observed at ground sites within the basin. Possible explanations for these trends are investigated. Two techniques, single and triple quadrupole chemical ionization mass spectrometry, were used to quantify ambient concentrations of biogenic oxidation products, hydroxyacetone and glycolaldehyde. The use of these techniques demonstrates the advantage of triple quadrupole mass spectrometry for separation of mass analogues, provided the collision-induced daughter ions are sufficiently distinct. Enhancement ratios of hydroxyacetone and glycolaldehyde in Californian biomass burning plumes are presented as are concentrations of these compounds at a rural ground site downwind of Sacramento.

  10. Atomic absorption spectrometry with a flame emission source

    NASA Astrophysics Data System (ADS)

    Calloway, Clifton P.; Jones, Bradley T.

    1994-12-01

    An atomic absorption spectrometer with flame atomization and a flame emission light source is described. The light source is prepared by aspirating a solution containing a high concentration of analyte into the emission flame. Two different source flames (air/acetylene and nitrous oxide/acetylene) have been evaluated, with the N 2O flame providing better signal to noise ratios ( S/N) in most cases. Source S/N values as high as 5900 (Cr) have been observed. Experimental parameters have been optimized for nine test elements to give limits of detection obtained with this system that are in some cases as good as those obtained with the traditional hollow cathode lamp source; for example, Cu (4 ng/ml), Mn (3 ng/ml) and Ni (5 ng/ml). Linear dynamic ranges typically span 2-3 orders of magnitude. This system offers an inexpensive emission source with the ability to quickly change the setup to accommodate different analytes.

  11. Apparatus and method for transient thermal infrared emission spectrometry

    DOEpatents

    McClelland, John F.; Jones, Roger W.

    1991-12-24

    A method and apparatus for enabling analysis of a solid material (16, 42) by applying energy from an energy source (20, 70) top a surface region of the solid material sufficient to cause transient heating in a thin surface layer portion of the solid material (16, 42) so as to enable transient thermal emission of infrared radiation from the thin surface layer portion, and by detecting with a spectrometer/detector (28, 58) substantially only the transient thermal emission of infrared radiation from the thin surface layer portion of the solid material. The detected transient thermal emission of infrared radiation is sufficiently free of self-absorption by the solid material of emitted infrared radiation, so as to be indicative of characteristics relating to molecular composition of the solid material.

  12. Determination of microelements in uncontaminated natural water from the Baikal region by atomic emission spectrometry

    SciTech Connect

    Kuznetsova, A.I.; Chumakova, N.L.

    1995-10-01

    In this study, concentration by evaporation was used to determine 17 microelements (B, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Sr, Mo, Ag, Sn, Ba, and Pb) in water from Lake Baikal and its tributaries by atomic-emission spectrometry with the arc excitation of spectra.

  13. Dynamics of secondary ion emission: Novel energy and angular spectrometry

    NASA Astrophysics Data System (ADS)

    Jalowy, T.; Neugebauer, R.; Hattass, M.; Fiol, J.; Afaneh, F.; Pereira, J. A. M.; Collado, V.; da Silveira, E. F.; Schmidt-Böcking, H.; Groeneveld, K. O.

    2002-06-01

    A new spectrometer has been developed based on the combination of standard time-of-flight technique and position sensitive delay line detectors. The basic features of the spectrometer, particularly of the multi-hit capable detector, are described. To demonstrate the performance of this new system, the dynamic emission characteristics, i.e. the three-dimensional velocity distribution, of desorbed H 2+ from Al target by Ar 0 impact (570 keV) is presented. It is found that the desorption yield is maximum for radial and axial emission velocities at 1.2 and 12 km/s respectively, corresponding to 1.5 eV ions emitted at 57° to normal (following the projectile radial direction). The initial energy distribution spreads out over 16 eV.

  14. Narrowband emission line imaging spectrometry using Savart plates

    NASA Astrophysics Data System (ADS)

    Maione, Bryan; Brickson, Leandra; Kudenov, Michael; Escuti, Michael

    2016-05-01

    Polarization spatial heterodyne interferometry (PSHI) allows for the development of compact, vibration insensitive, high spectral resolution sensors. Introducing the imaging qualities of a lenslet array extends the advantages of PSHI to imaging interferometers. The use of Savart plates enables a birefringent interferometer that obtains higher spectral resolution with fewer optical aberrations when compared to alternative designs. In this paper, we describe the design, construction, calibration and validation of a narrowband emission line imaging spectrometer (NELIS), based on Savart plates and liquid crystal polarization gratings, along with its associated theoretical model. This sensor is advantageous for spectral imaging in the areas of remote sensing, biomedical imaging and machine vision.

  15. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

    SciTech Connect

    Montaser, A.

    1992-01-01

    New high temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. Emphasis was placed on atmospheric pressure He inductively coupled plasmas (ICP) suitable for atomization, excitation, and ionization of elements; simulation and computer modeling of plasma sources with potential for use in spectrochemical analysis; spectroscopic imaging and diagnostic studies of high temperature plasmas, particularly He ICP discharges; and development of new, low-cost sample introduction systems, and examination of techniques for probing the aerosols over a wide range. Refs., 14 figs. (DLC)

  16. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

    NASA Astrophysics Data System (ADS)

    Montaser, A.

    In this project, new high temperature plasmas and new sample introduction systems are developed for rapid elemental and isotopic analysis of gases, solutions, and solids using atomic emission spectrometry (AES) and mass spectrometry (MS). These devices offer promise of solving singularly difficult analytical problems that either exist now or are likely to arise in the future in the various fields of energy generation, environmental pollution, nutrition, and biomedicine. Emphasis is being placed on: (1) generation of annular, helium inductively coupled plasmas (He ICPs) that are suitable for atomization, excitation, and ionization of elements possessing high excitation and ionization energies, with the intent of enhancing the detecting powers of a number of elements; (2) computer modelings of ICP discharges to predict the behavior of new and existing plasmas; (3) diagnostic studies of high temperature plasmas and sample introduction systems to quantify their fundamental properties, with the ultimate aim to improve analytical performance of atomic spectrometry; (4) development and characterization of new, low cost sample introduction systems that consume microliter or microgram quantities of samples; and (5) investigation of new membrane separators for stripping solvent from sample aerosol to reduce various interferences and to enhance sensitivity and selectivity in plasma spectrometry.

  17. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

    SciTech Connect

    Montaser, A.

    1990-01-01

    In this project, new high temperature plasmas and new sample introduction systems are developed for rapid elemental and isotopic analysis of gases, solutions, and solids using atomic emission spectrometry (AES) and mass spectrometry (MS). These devices offer promise of solving singularly difficult analytical problems that either exist now or are likely to arise in the future in the various fields of energy generation, environmental pollution, biomedicine and nutrition. Emphasis is being placed on: generation of annular, helium inductively coupled plasmas (He ICPs) that are suitable for atomization, excitation, and ionization of elements possessing high excitation and ionization energies, with the intent of enhancing the detecting powers of a number of elements; diagnostic studies of high-temperature plasmas to quantify their fundamental properties, with the ultimate aim to improve analytical performance of atomic spectrometry; development and characterization of new sample introduction systems that consume microliter or microgram quantities of samples, and investigation of new membrane separators for striping solvent from sample aerosol to reduce various interferences and to enhance sensitivity in plasma spectrometry.

  18. 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.

  19. Alpha-particle emission probabilities of ²³⁶U obtained by alpha spectrometry.

    PubMed

    Marouli, M; Pommé, S; Jobbágy, V; Van Ammel, R; Paepen, J; Stroh, H; Benedik, L

    2014-05-01

    High-resolution alpha-particle spectrometry was performed with an ion-implanted silicon detector in vacuum on a homogeneously electrodeposited (236)U source. The source was measured at different solid angles subtended by the detector, varying between 0.8% and 2.4% of 4π sr, to assess the influence of coincidental detection of alpha-particles and conversion electrons on the measured alpha-particle emission probabilities. Additional measurements were performed using a bending magnet to eliminate conversion electrons, the results of which coincide with normal measurements extrapolated to an infinitely small solid angle. The measured alpha emission probabilities for the three main peaks - 74.20 (5)%, 25.68 (5)% and 0.123 (5)%, respectively - are consistent with literature data, but their precision has been improved by at least one order of magnitude in this work.

  20. Dielectric barrier discharge plasma atomizer for hydride generation atomic absorption spectrometry-Performance evaluation for selenium

    NASA Astrophysics Data System (ADS)

    Duben, Ondřej; Boušek, Jaroslav; Dědina, Jiří; Kratzer, Jan

    2015-09-01

    Atomization of selenium hydride in a quartz dielectric barrier discharge (DBD) atomizer was optimized and its performance was compared to that of the externally heated quartz multiatomizer. Argon was found as the best DBD discharge gas employing a flow rate of 75 ml min- 1 Ar while the DBD power was optimized at 14 W. The detection limits reached 0.24 ng ml- 1 Se in the DBD and 0.15 ng ml- 1 Se in the multiatomizer. The tolerance of DBD to interferences is even better than with the multiatomizer.

  1. Sampling and analysis of particulate matter by glow discharge atomic emission and mass spectrometries.

    PubMed

    Marcus, R K; Dempster, M A; Gibeau, T E; Reynolds, E M

    1999-08-01

    The direct introduction of particulate matter into glow discharge atomic emission and mass spectrometry sources through a particle beam/momentum separator apparatus is described. Vacuum action through a narrow (0.0625 in. i.d.) stainless steel tube allows the introduction of discrete samples of NIST SRM 1648 urban particulate matter (UPM) and caffeine in powder form. Introduction of "ambient" airborne particulate matter is also possible. Particles passing through the aerodynamic momentum separator impinge on the heated (∼200-250 °C) inner surface of the glow discharge plasma volume and are flash-vaporized. The resultant atoms/molecules are subjected to excitation/ionization collisions within the low-pressure (0.5-5 Torr of He or Ar) plasma, producing characteristic photon emission and/or signature ionic species. In this way, atomic emission and mass spectrometry identification of particle constituents is possible. Basic design aspects of the apparatus are presented, and demonstrations of atomic emission detection of the constituents in the NIST SRM illustrate the general characteristics of the approach. Transient atomic emission signals are captured for the introduction of preweighed, discrete samples, with the integrated areas used to construct analytical response curves. Limits of detection using this relatively simple atomic emission system are on the order of tens of nanograms for sample masses of ∼50 μg. Mass spectrometric monitoring of introduced caffeine particles and a mixture of polycyclic aromatic hydrocarbons (PAHs) illustrates the ability of the glow discharge plasma to produce high-quality, library (electron impact) searchable mass spectra of molecular species while also yielding isotopic identification of elemental components of the UPM. Limits of detection for Fe in the NIST SRM are on the order of 175 ng of material, equivalent to ∼7 ng of analyte Fe. It is believed that the small size, low power consumption, ease of operation, and multimode

  2. Dielectric barrier discharge micro-plasma emission spectrometry for the detection of acetone in exhaled breath.

    PubMed

    Yang, Ting; Gao, Dong-Xue; Yu, Yong-Liang; Chen, Ming-Li; Wang, Jian-Hua

    2016-01-01

    Acetone is a predominant volatile organic compound (VOC) in the exhaled breath and a promising biomarker for diabetes and ketoacidosis. A non-thermal micro-plasma generated in a planar dielectric barrier discharge (DBD) is used as a radiation source for the excitation of gaseous acetone followed by its quantification with optical emission spectrometry (OES). Gaseous acetone can be directly sampled, while liquid acetone is evaporated by heated tungsten coil and then introduced into the DBD micro-plasma by a helium carrier flow for performing optical emission and detection at a 519 nm emission line. In the present study, the exhaled breath is collected and transferred into aqueous medium for sampling. With a sampling volume of 7 μL in a micro-drop, a linear range of 40-1600 mg L(-1) is obtained along with a detection limit of 44 ng and a precision of 5.7% RSD. The present system is successfully applied to the determination of breath acetone for both diabetic patients and healthy volunteers.

  3. Dielectric barrier discharge micro-plasma emission spectrometry for the detection of acetone in exhaled breath.

    PubMed

    Yang, Ting; Gao, Dong-Xue; Yu, Yong-Liang; Chen, Ming-Li; Wang, Jian-Hua

    2016-01-01

    Acetone is a predominant volatile organic compound (VOC) in the exhaled breath and a promising biomarker for diabetes and ketoacidosis. A non-thermal micro-plasma generated in a planar dielectric barrier discharge (DBD) is used as a radiation source for the excitation of gaseous acetone followed by its quantification with optical emission spectrometry (OES). Gaseous acetone can be directly sampled, while liquid acetone is evaporated by heated tungsten coil and then introduced into the DBD micro-plasma by a helium carrier flow for performing optical emission and detection at a 519 nm emission line. In the present study, the exhaled breath is collected and transferred into aqueous medium for sampling. With a sampling volume of 7 μL in a micro-drop, a linear range of 40-1600 mg L(-1) is obtained along with a detection limit of 44 ng and a precision of 5.7% RSD. The present system is successfully applied to the determination of breath acetone for both diabetic patients and healthy volunteers. PMID:26695309

  4. 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.

  5. PLANE-INTEGRATED OPEN-PATH FOURIER TRANSFORM INFRARED SPECTROMETRY METHODOLOGY FOR ANAEROBIC SWINE LAGOON EMISSION MEASUREMENTS

    EPA Science Inventory

    Emissions of ammonia and methane from an anaerobic lagoon at a swine animal feeding operation were evaluated five times over a period of two years. The plane-integrated (PI) open-path Fourier transform infrared spectrometry (OP-FTIR) methodology was used to transect the plume at ...

  6. Flame Emission Spectrometry in General Chemistry Labs: Solubility Product (K[subscript sp]) of Potassium Hydrogen Phthalate

    ERIC Educational Resources Information Center

    Nyasulu, Frazier W.; Cusworth, William, III; Lindquist, David; Mackin, John

    2007-01-01

    In this general chemistry laboratory, flame emission spectrometry is used to determine the potassium ion concentration in saturated solutions of potassium hydrogen phthalate (KHP) in the 0-65 [degree]C temperature range. From these data the solubility products (K[subscript sp]), the Gibbs free energies of solution ([Delta][subscript…

  7. ANALYSIS OF TRACE-LEVEL ORGANIC COMBUSTION PROCESS EMISSIONS USING NOVEL MULTIDIMENSIONAL GAS CHROMATOGRAPHY-MASS SPECTROMETRY PROCEDURES

    EPA Science Inventory

    The paper discusses the analysis of trace-level organic combustion process emissions using novel multidimensional gas chromatography-mass spectrometry (MDGC-MS) procedures. It outlines the application of the technique through the analyses of various incinerator effluent and produ...

  8. Determination of phosphorus impurity that directly affects quantification of microbial genomic DNA using inductively coupled plasma optical emission spectrometry.

    PubMed

    Yang, Hyo-Jin; Yang, Inchul; Choi, Jun-Hyuk; Kang, Dukjin; Han, Myung-Sub; Kim, Sook-Kyung

    2014-04-01

    We prepared genomic DNA from human placenta, Escherichia coli, and Bacillus subtilis using various DNA extraction methods and quantified the genomic DNA using ultraviolet (UV) spectrophotometry, capillary electrophoresis (CE), and inductively coupled plasma optical emission spectrometry (ICP-OES). Application of ICP-OES unexpectedly led to a serious overestimation of phosphorus in B. subtilis genomic DNA prepared using cetyltrimethyl ammonium bromide (CTAB). Further investigations using reversed-phase high-performance liquid chromatography (RP-HPLC), ultra-performance liquid chromatography electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS), and (31)P nuclear magnetic resonance (NMR) identified the phosphorus impurity as lipoteichoic acid (LTA). PMID:24486318

  9. Rapid analysis of tile industry gaseous emissions by ion mobility spectrometry and comparison with solid phase micro-extraction/gas chromatography/mass spectrometry.

    PubMed

    Pozzi, R; Bocchini, P; Pinelli, F; Galletti, G C

    2006-12-01

    The present paper reports on a rapid method for the analysis of gaseous emissions from ceramic industry, based on ion mobility spectrometry (IMS) as a means for on-site monitoring of volatile organic compounds (VOCs) produced during tile baking. IMS was calibrated with a set of reference compounds (i.e. ethyl acetate, ethanol, ethylene glycol, diethylene glycol, acetaldehyde, formaldehyde, 2-methyl-1,3-dioxolane, 2,2-dimethyl-1,3-dioxolane, 1,3-dioxolane, 1,4-dioxane, benzene, toluene, cyclohexane, acetone, acetic acid) via air-flow permeation. The technique was tested on a laboratory-scale kiln and tiles prepared with selected glycol- and resin-based additives. Finally, the analytical method was applied to emissions from two industries in the Modena (Italy) ceramic area. The results of all experimental phases were compared to those obtained by solid phase micro-extraction/gas chromatography/mass spectrometry (SPME/GC/MS). IMS showed potential as a real-time monitoring device for quality assessment in ceramic industry emissions. IMS spectra, SPME/GC/MS data, relationship between additives/baking conditions and produced VOCs and advantages and limitations of both techniques will be discussed.

  10. Finite Larmor radii effects in fast ion measurements with neutron emission spectrometry

    NASA Astrophysics Data System (ADS)

    Eriksson, J.; Hellesen, C.; Andersson Sundén, E.; Cecconello, M.; Conroy, S.; Ericsson, G.; Gatu Johnson, M.; Pinches, S. D.; Sharapov, S. E.; Weiszflog, M.; EFDA contributors, JET

    2013-01-01

    When analysing data from fast ion measurements it is normally assumed that the gyro-phase distribution of the ions is isotropic within the field of view of the measuring instrument. This assumption is not valid if the Larmor radii of the fast ions are comparable to—or larger than—the gradient scale length in the spatial distribution of the ions, and if this scale length is comparable to—or smaller than—the width of the field of view of the measuring instrument. In this paper the effect of such an anisotropy is demonstrated by analysing neutron emission spectrometry data from a JET experiment with deuterium neutral beams together with radiofrequency heating at the third harmonic of the deuterium cyclotron frequency. In the experiment, the neutron time-of-flight spectrometer TOFOR was used to measure the neutrons from the d(d,n)3He-reaction. Comparison of the experimental data with Monte Carlo calculations shows that the finite Larmor radii of the fast ions need to be included in the modelling to get a good description of the data. Similar effects are likely to be important for other fast ion diagnostics, such as γ-ray spectroscopy and neutral particle analysis, as well.

  11. Standard dilution analysis of beverages by microwave-induced plasma optical emission spectrometry.

    PubMed

    Goncalves, Daniel A; McSweeney, Tina; Santos, Mirian C; Jones, Bradley T; Donati, George L

    2016-02-25

    In this work, standard dilution analysis (SDA) is combined with microwave-induced plasma optical emission spectrometry (MIP OES) to determine seven elements in coffee, green tea, energy drink, beer, whiskey and cachaça (Brazilian hard liquor). No sample preparation other than simple dilution in HNO3 1% v v(-1) is required. Due to relatively low plasma temperatures, matrix effects may compromise accuracies in MIP OES analyzes of complex samples. The method of standard additions (SA) offers enhanced accuracies, but is time-consuming and labor intensive. SDA offers a simpler, faster approach, with improved accuracies for complex matrices. In this work, SDA's efficiency is evaluated by spike experiments, and the results are compared to the traditional methods of external calibration (EC), internal standard (IS), and standard additions (SA). SDA is comparable to the traditional calibration methods, and it provides superior accuracies for applications involving ethanol-containing beverage samples. The SDA-MIP OES procedure is effective. Using only two calibration solutions, it may be easily automated for accurate and high sample throughput routine applications.

  12. [Atomic emission spectrometry determination of Au, Pt and Pd after separation and enrichment by hyperbranched polymer].

    PubMed

    Li, Hui-Zhi; Zhai, Dian-Tang; Shou, Chong-Qi; Zhao, Shu-Ying; Wei, Qin

    2006-09-01

    The present paper shows that the trace amount of gold, platinum and palladium in hydrochloric acid solution can be concentrated by hyperbranched polymer. The new reagent has a rapid adsorption rate and big concentrating capacity. The determination of trace Au, Pt and Pd in sample using carbon powder and strontium carbonate as buffer was carried out by atomic emission spectrometry(AES). Zirconium was selected as internal standard line. The sample was directly loaded into ordinary electrode. The method is simple, rapid and accurate. The condition of determination, and factors of influence were studied. The analysis line of Au, Pt and Pd is 312.3, 306.5 and 311.4 nm respectively. The internal standard line of Zr is 310.7 nm. The linear range of the determination of Au, Pt and Pd is 0-0. 20%, 0-0. 40% and 0-0. 20% respectively. The detection limit of Au, Pt and Pd is 0.010%, 0.0030% and 0.0030% respectively. The method has been applied to the determination of Au, Pt and Pd with satisfactory results.

  13. [Determination of trace zirconium and hafniumin sample by atomic emission spectrometry].

    PubMed

    Li, Hui-zhi; Yang, Chun-xia; Zhai, Dian-tang

    2005-02-01

    This paper describes the determination of trace Zr and Hf in the sample using carbon powder and titanium oxide as the buffer by Atomic Emission Spectrometry (AES). Titanium was selected for the internal standard line. Sample separation and chemical treatment were not required. The sample was directly loaded into an ordinary electrode. The method is simple, rapid and accurate. The conditions for the determination, and the factors of influence have been studied. A new method has been developed for the determination of zirconium and hafnium. The analytical lines of Zr and Hf were 327.3 and 286.6 nm respectively. The internal standard line of Ti was 308.8 nm. The linear range of the determination of Zr and Hf was 0-0.50% and 0-0.25% respectively. The detection limit of Zr and Hf was 0.0010% and 0.010% respectively. The range of the recovery of zirconium and hafnium was 96.67%-105.0%. The results for these elements in standard sample are in agreement with certified values with a precision of 3.61% RSD for Zr (n = 9), and 4.82% RSD for Hf (n = 9). The method has been applied to the determination of Zr and Hf with satisfactory results.

  14. Multielemental inductively coupled plasma optical emission spectrometry analysis of nickeliferous minerals.

    PubMed

    Abad-Peña, Elizabet; Larrea-Marín, María Teresa; Villanueva-Tagle, Margarita Edelia; Pomares-Alfonso, Mario Simeón

    2014-06-01

    An inductively coupled plasma optical emission spectrometry method for the quantitative simultaneous determination of Al, Ca, Co, Cu, Cr, Fe, K, Mg, Mn, Na, Ni, P and Zn in Cuban laterite and serpentine minerals has been developed. Additionally, V and Ti can be quantitatively determined in laterite mineral; Li, Sr, and Zr can be detected in both mineral types and Pb can be detected just in laterite mineral. The microwave-assisted total acid digestion of samples was achieved with HCl+HNO3+HF and HNO3+HClO4+HF acid mixtures for laterite and serpentine samples, respectively. In non-robust plasma operating conditions, the matrix effect characteristics of the laterite sample were dictated by the principal component Fe; while the character of the Mg principal component matrix effect was some how modified by the concomitants Fe and Ni in serpentine sample. The selection of robust conditions decreased the matrix effect. Additionally, the simulation of the matrix samples by introducing the principal component Fe or Mg, correspondingly, in calibration dissolutions was needed to overcome completely the matrix effect over the analysis accuracy. Precision of analysis was very near or lower than 10% for most elements, except Sr (15%) in L-1; and K (15%) and Li (15%) in SNi sample. Accuracy of analysis was around or lowers than 10% for most elements, except K (15%), Na (19%), P (19%) and V (19%) in L-1 sample; and Ca (14%) and P (20%) in SNi sample. PMID:24767449

  15. The survival of gunshot residues in cremated bone: an inductively coupled plasma optical emission spectrometry study.

    PubMed

    Amadasi, Alberto; Merli, Daniele; Brandone, Alberto; Poppa, Pasquale; Gibelli, Daniele; Cattaneo, Cristina

    2013-07-01

    Gunshot residue (GSR) has been sought and demonstrated on many types of material and with many techniques. Inductively coupled plasma optical emission spectrometry (ICP-OES) could be a useful method on difficult substrates, but a systematic study on burnt material has never been performed. Hence, this study aims at evaluating the usefulness and reliability of this method on burnt samples. Sixteen adult bovine ribs (eight with soft tissues, eight totally skeletonized) were shot using two kinds of projectile (both 9 mm full metal-jacketed or unjacketed). Then, every sample was led to complete calcination in an electric oven. The area of the gunshot entrance wound was swabbed and analyzed by ICP-OES; the results were also correlated with a previously published parallel study by scanning electron microscopy (SEM) equipped with an SEM-energy dispersive X-ray analyzer. ICP-OES proved to be very sensitive and reliable even on degraded material and can be an appropriate nondestructive method for detecting residues on difficult and delicate substrates such as burnt bone. PMID:23692414

  16. Standard dilution analysis of beverages by microwave-induced plasma optical emission spectrometry.

    PubMed

    Goncalves, Daniel A; McSweeney, Tina; Santos, Mirian C; Jones, Bradley T; Donati, George L

    2016-02-25

    In this work, standard dilution analysis (SDA) is combined with microwave-induced plasma optical emission spectrometry (MIP OES) to determine seven elements in coffee, green tea, energy drink, beer, whiskey and cachaça (Brazilian hard liquor). No sample preparation other than simple dilution in HNO3 1% v v(-1) is required. Due to relatively low plasma temperatures, matrix effects may compromise accuracies in MIP OES analyzes of complex samples. The method of standard additions (SA) offers enhanced accuracies, but is time-consuming and labor intensive. SDA offers a simpler, faster approach, with improved accuracies for complex matrices. In this work, SDA's efficiency is evaluated by spike experiments, and the results are compared to the traditional methods of external calibration (EC), internal standard (IS), and standard additions (SA). SDA is comparable to the traditional calibration methods, and it provides superior accuracies for applications involving ethanol-containing beverage samples. The SDA-MIP OES procedure is effective. Using only two calibration solutions, it may be easily automated for accurate and high sample throughput routine applications. PMID:26851081

  17. The survival of gunshot residues in cremated bone: an inductively coupled plasma optical emission spectrometry study.

    PubMed

    Amadasi, Alberto; Merli, Daniele; Brandone, Alberto; Poppa, Pasquale; Gibelli, Daniele; Cattaneo, Cristina

    2013-07-01

    Gunshot residue (GSR) has been sought and demonstrated on many types of material and with many techniques. Inductively coupled plasma optical emission spectrometry (ICP-OES) could be a useful method on difficult substrates, but a systematic study on burnt material has never been performed. Hence, this study aims at evaluating the usefulness and reliability of this method on burnt samples. Sixteen adult bovine ribs (eight with soft tissues, eight totally skeletonized) were shot using two kinds of projectile (both 9 mm full metal-jacketed or unjacketed). Then, every sample was led to complete calcination in an electric oven. The area of the gunshot entrance wound was swabbed and analyzed by ICP-OES; the results were also correlated with a previously published parallel study by scanning electron microscopy (SEM) equipped with an SEM-energy dispersive X-ray analyzer. ICP-OES proved to be very sensitive and reliable even on degraded material and can be an appropriate nondestructive method for detecting residues on difficult and delicate substrates such as burnt bone.

  18. Multielemental inductively coupled plasma optical emission spectrometry analysis of nickeliferous minerals.

    PubMed

    Abad-Peña, Elizabet; Larrea-Marín, María Teresa; Villanueva-Tagle, Margarita Edelia; Pomares-Alfonso, Mario Simeón

    2014-06-01

    An inductively coupled plasma optical emission spectrometry method for the quantitative simultaneous determination of Al, Ca, Co, Cu, Cr, Fe, K, Mg, Mn, Na, Ni, P and Zn in Cuban laterite and serpentine minerals has been developed. Additionally, V and Ti can be quantitatively determined in laterite mineral; Li, Sr, and Zr can be detected in both mineral types and Pb can be detected just in laterite mineral. The microwave-assisted total acid digestion of samples was achieved with HCl+HNO3+HF and HNO3+HClO4+HF acid mixtures for laterite and serpentine samples, respectively. In non-robust plasma operating conditions, the matrix effect characteristics of the laterite sample were dictated by the principal component Fe; while the character of the Mg principal component matrix effect was some how modified by the concomitants Fe and Ni in serpentine sample. The selection of robust conditions decreased the matrix effect. Additionally, the simulation of the matrix samples by introducing the principal component Fe or Mg, correspondingly, in calibration dissolutions was needed to overcome completely the matrix effect over the analysis accuracy. Precision of analysis was very near or lower than 10% for most elements, except Sr (15%) in L-1; and K (15%) and Li (15%) in SNi sample. Accuracy of analysis was around or lowers than 10% for most elements, except K (15%), Na (19%), P (19%) and V (19%) in L-1 sample; and Ca (14%) and P (20%) in SNi sample.

  19. Oxygen bomb combustion of biological samples for inductively coupled plasma optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    Souza, Gilberto B.; Carrilho, Elma Neide V. M.; Oliveira, Camila V.; Nogueira, Ana Rita A.; Nóbrega, Joaquim A.

    2002-12-01

    A rapid sample preparation method is proposed for decomposition of milk powder, corn bran, bovine and fish tissues, containing certified contents of the analytes. The procedure involves sample combustion in a commercial stainless steel oxygen bomb operating at 25 bar. Most of the samples were decomposed within 5 min. Diluted nitric acid or water-soluble tertiary amines 10% v/v were used as absorption solutions. Calcium, Cu, K, Mg, Na, P, S and Zn were recovered with the bomb washings and determined by inductively coupled plasma optical emission spectrometry (ICP-OES). Ethanol mixed with paraffin was used as a combustion aid to allow complete combustion. A cooling step prior releasing of the bomb valve was employed to increase the efficiency of sample combustion. Iodine was also determined in milk samples spiked with potassium iodide to evaluate the volatilization and collection of iodine in amine CFA-C medium and the feasibility of its determination by ICP-OES with axial view configuration. Most of the element recoveries in the samples were between 91 and 105% and the certified and found contents exhibited a fair agreement at a 95% confidence level.

  20. Mechanical Modulation of Phonon-Assisted Field Emission in a Silicon Nanomembrane Detector for Time-of-Flight Mass Spectrometry

    PubMed Central

    Park, Jonghoo; Blick, Robert H.

    2016-01-01

    We demonstrate mechanical modulation of phonon-assisted field emission in a free-standing silicon nanomembrane detector for time-of-flight mass spectrometry of proteins. The impacts of ion bombardment on the silicon nanomembrane have been explored in both mechanical and electrical points of view. Locally elevated lattice temperature in the silicon nanomembrane, resulting from the transduction of ion kinetic energy into thermal energy through the ion bombardment, induces not only phonon-assisted field emission but also a mechanical vibration in the silicon nanomembrane. The coupling of these mechanical and electrical phenomenon leads to mechanical modulation of phonon-assisted field emission. The thermal energy relaxation through mechanical vibration in addition to the lateral heat conduction and field emission in the silicon nanomembrane offers effective cooling of the nanomembrane, thereby allowing high resolution mass analysis. PMID:26861329

  1. Mechanical Modulation of Phonon-Assisted Field Emission in a Silicon Nanomembrane Detector for Time-of-Flight Mass Spectrometry.

    PubMed

    Park, Jonghoo; Blick, Robert H

    2016-01-01

    We demonstrate mechanical modulation of phonon-assisted field emission in a free-standing silicon nanomembrane detector for time-of-flight mass spectrometry of proteins. The impacts of ion bombardment on the silicon nanomembrane have been explored in both mechanical and electrical points of view. Locally elevated lattice temperature in the silicon nanomembrane, resulting from the transduction of ion kinetic energy into thermal energy through the ion bombardment, induces not only phonon-assisted field emission but also a mechanical vibration in the silicon nanomembrane. The coupling of these mechanical and electrical phenomenon leads to mechanical modulation of phonon-assisted field emission. The thermal energy relaxation through mechanical vibration in addition to the lateral heat conduction and field emission in the silicon nanomembrane offers effective cooling of the nanomembrane, thereby allowing high resolution mass analysis. PMID:26861329

  2. [A genetic algorithm approach to qualitative analysis in inductively coupled plasma-atomic emission spectroscopy].

    PubMed

    Peng, Bin; Liu, Ke-ling; Li, Zhi-min; Wang, Yue-song; Huang, Tu-jiang

    2002-06-01

    Genetic algorithm (GA) is used in automatic qualitative analysis by a sequential inductively coupled plasma spectrometer (ICP-AES) and a computer program is developed in this paper. No any standard samples are needed, and spectroscopic interferences can be eliminated. All elements and their concentration ranges of an unknown sample can be reported. The replication rate Pr, crossover rate Pc, and mutation rate of the genetic algorithm were adjusted to be 0.6, 0.4 and 0 respectively. The analytical results of GA are in good agreement with the reference values. It indicates that, combined with the intensity information, the GA can be applied to spectroscopic qualitative analysis and expected to become an effective method in qualitative analysis in ICP-AES after further work. PMID:12938334

  3. Improved voltage transfer coefficients for nonconductive materials in radiofrequency glow discharge optical emission spectrometry.

    PubMed

    Therese, L; Ghalem, Z; Guillot, P; Belenguer, P

    2006-09-01

    In radiofrequency glow discharge emission spectrometry (RF-GDOES), the excitation voltage used to create the plasma is applied to the back or front end of the sample to be analyzed. In this paper we focus on back-applied voltage systems (a configuration that represents about half of the instruments available on the market), and on applied voltage problems (the power coupling efficiency and materials analysis are beyond the scope of this study). In the RF-GDOES of nonconductive samples, a voltage drop develops inside the material. The voltage transfer coefficient is defined as the ratio between the peak voltage in front of the sample (facing the plasma) and the peak voltage applied to the back of the sample. In this work, we show that it is possible to increase the voltage transfer coefficient by increasing the capacitance of the sample. The capacitance of a given nonconductive material depends on its surface, its thickness and its permittivity. Increasing the voltage transfer coefficient permits higher power deposition in the plasma. This study is based on an electrical equivalent circuit for the discharge device, which takes into account the sample and reactor capacitances as well as the voltage probes used for the measurements. This circuit, when modeled by a commercial electrical circuit simulator, gives the voltage transfer coefficient as a function of the sample capacitance. Different approaches to increasing the sample capacitance and their influence on the voltage transfer coefficient are presented and related to the 750.4 nm argon line intensity, which is correlated to the electron density. PMID:16724217

  4. [A Study of FTIR Spectrometry Based on a Long Optical Path on the Emission Rules of Nitrous Oxide from Soil].

    PubMed

    Xiao, Guang-dong; Zheng, Ling; Dong, Da-ming; Zhang, Dong-yan; Zhang, Bao-hua; Liao, Tong-qing

    2015-11-01

    The excessive emission of N₂O (Nitrous oxide) will destroy the ozone layer, reasonable fertilization and adopting measures of emission reduction of N₂O are of great significance to slowing down the greenhouse effect. The article studied the impact of fertilization and water on the emission of N2 0 from the cabbage farmland using FTIR spectrometry. To enhance the sensitivity of the measuring system, we used multi-reflecting mirrors to increase the optical pathlength. By comparing the infrared spectra between the before and after fertilizer application and the NIST spectral library, finally, the band at 2160-2225 cm⁻¹ was chosen as the spectral characteristics band of quantitative calculation of N₂O through analyzing. The research found that fertilization and water could promote the emission of N2 0 from the cabbage farmland soil, which could supply theory bases for emission reduction of N₂O and slowing down the greenhouse effect. Finally, we also studied the diurnal emission rules of N₂O from the fertilized soil; the results showed that the emission of N₂O was lower at night and the results were compared with that of previous' studies, which verifies the feasibility of this method. The results proved that FTIR with long optical path was a rapid and effective method to measure the emission rules of N₂O from the cabbage farmland soil, which can measure the gas emissions of N₂O from the fertilized cabbage farmland soil and compared with other traditional measuring methods, it had the advantages such as rapidness and convenience. PMID:26978909

  5. [A Study of FTIR Spectrometry Based on a Long Optical Path on the Emission Rules of Nitrous Oxide from Soil].

    PubMed

    Xiao, Guang-dong; Zheng, Ling; Dong, Da-ming; Zhang, Dong-yan; Zhang, Bao-hua; Liao, Tong-qing

    2015-11-01

    The excessive emission of N₂O (Nitrous oxide) will destroy the ozone layer, reasonable fertilization and adopting measures of emission reduction of N₂O are of great significance to slowing down the greenhouse effect. The article studied the impact of fertilization and water on the emission of N2 0 from the cabbage farmland using FTIR spectrometry. To enhance the sensitivity of the measuring system, we used multi-reflecting mirrors to increase the optical pathlength. By comparing the infrared spectra between the before and after fertilizer application and the NIST spectral library, finally, the band at 2160-2225 cm⁻¹ was chosen as the spectral characteristics band of quantitative calculation of N₂O through analyzing. The research found that fertilization and water could promote the emission of N2 0 from the cabbage farmland soil, which could supply theory bases for emission reduction of N₂O and slowing down the greenhouse effect. Finally, we also studied the diurnal emission rules of N₂O from the fertilized soil; the results showed that the emission of N₂O was lower at night and the results were compared with that of previous' studies, which verifies the feasibility of this method. The results proved that FTIR with long optical path was a rapid and effective method to measure the emission rules of N₂O from the cabbage farmland soil, which can measure the gas emissions of N₂O from the fertilized cabbage farmland soil and compared with other traditional measuring methods, it had the advantages such as rapidness and convenience.

  6. Depth profile characterization of Zn-TiO2 nanocomposite films by pulsed radiofrequency glow discharge-optical emission spectrometry.

    PubMed

    Alberts, Deborah; Fernández, Beatriz; Frade, Tania; Gomes, Anabela; Pereira, Maria Isabel da Silva; Pereiro, Rosario; Sanz-Medel, Alfredo

    2011-04-15

    In recent years particular effort is being devoted towards the development of radiofrequency (rf) pulsed glow discharges (GDs) coupled to optical emission spectrometry (OES) for depth profile analysis of materials with technological interest. In this work, pulsed rf-GD-OES is investigated for the fast and sensitive depth characterization of Zn-TiO(2) nanocomposite films deposited on conductive substrates (Ti and steel). The first part of this work focuses on assessing the advantages of pulsed GDs, in comparison with the continuous GD, in terms of analytical emission intensities and emission yields. Next, the capability of pulsed rf-GD-OES for determination of thickness and compositional depth profiles is demonstrated by resorting to a simple multi-matrix calibration procedure. A rf forward power of 75 W, a pressure of 600 Pa, 10 kHz pulse frequency and 50% duty cycle were selected as GD operation parameters.Quantitative depth profiles obtained with the GD proposed methodology for Zn-TiO(2) nanocomposite films, prepared by the occlusion electrodeposition method using pulsed reverse current electrolysis, have proved to be in good agreement with results achieved by complementary techniques, including scanning electron microscopy and inductively coupled plasma-mass spectrometry. The work carried out demonstrates that pulsed rf-GD-OES is a promising tool for the fast analytical characterization of nanocomposite films. PMID:21376989

  7. Uncertainty Estimation of Metals and Semimetals Determination in Wastewater by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES)

    NASA Astrophysics Data System (ADS)

    Marques, J. R.; Villa-Soares, S. M.; Stellato, T. B.; Silva, T. B. S. C.; Faustino, M. G.; Monteiro, L. R.; Pires, M. A. F.; Cotrim, M. E. B.

    2016-07-01

    The measurement uncertainty is a parameter that represents the dispersion of the results obtained by a method of analysis. The estimation of measurement uncertainty in the determination of metals and semimetals is important to compare the results with limits defined by environmental legislation and conclude if the analytes are meeting the requirements. Therefore, the aim of this paper is present all the steps followed to estimate the uncertainty of the determination of amount of metals and semimetals in wastewater by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). Measurement uncertainty obtained was between 4.6 and 12.2% in the concentration range of mg.L-1.

  8. Initial reaction of hafnium oxide deposited by remote plasma atomic layer deposition method

    SciTech Connect

    Won, Youngdo; Park, Sangwook; Koo, Jaehyoung; Kim, Seokhoon; Kim, Jinwoo; Jeon, Hyeongtag

    2005-12-26

    A remote plasma atomic layer deposition (RPALD) method has been applied to grow a hafnium oxide thin film on the Si substrate. The deposition process was monitored by in situ XPS and the as-deposited structure and chemical bonding were examined by TEM and XPS. The in situ XPS measurement showed the presence of a hafnium silicate phase at the initial stage of the RPALD process up to the 20th cycle and indicated that no hafnium silicide was formed. The initial hafnium silicate was amorphous and grew to a thickness of approximately 2 nm. Based on these results and model reactions for silicate formation, we proposed an initial growth mechanism that includes adatom migration at nascent step edges. Density functional theory calculations on model compounds indicate that the hafnium silicate is thermodynamically favored over the hafnium silicide by as much as 250 kJ/mol.

  9. Automatable on-line generation of calibration curves and standard additions in solution-cathode glow discharge optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    Schwartz, Andrew J.; Ray, Steven J.; Hieftje, Gary M.

    2015-03-01

    Two methods are described that enable on-line generation of calibration standards and standard additions in solution-cathode glow discharge optical emission spectrometry (SCGD-OES). The first method employs a gradient high-performance liquid chromatography pump to perform on-line mixing and delivery of a stock standard, sample solution, and diluent to achieve a desired solution composition. The second method makes use of a simpler system of three peristaltic pumps to perform the same function of on-line solution mixing. Both methods can be computer-controlled and automated, and thereby enable both simple and standard-addition calibrations to be rapidly performed on-line. Performance of the on-line approaches is shown to be comparable to that of traditional methods of sample preparation, in terms of calibration curves, signal stability, accuracy, and limits of detection. Potential drawbacks to the on-line procedures include signal lag between changes in solution composition and pump-induced multiplicative noise. Though the new on-line methods were applied here to SCGD-OES to improve sample throughput, they are not limited in application to only SCGD-OES-any instrument that samples from flowing solution streams (flame atomic absorption spectrometry, ICP-OES, ICP-mass spectrometry, etc.) could benefit from them.

  10. 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. PMID:26860569

  11. Emissions of volatile organic compounds from Quercus ilex L. measured by Proton Transfer Reaction Mass Spectrometry under different environmental conditions

    NASA Astrophysics Data System (ADS)

    Holzinger, R.; Sandoval-Soto, L.; Rottenberger, S.; Crutzen, P. J.; Kesselmeier, J.

    2000-08-01

    Volatile organic compound (VOC) emissions of the Mediterranean holm oak (Quercus ilex L.) were investigated using a fast Proton Transfer Reaction Mass Spectrometry (PTR-MS) instrument for analysis. This technique is able to measure compounds with a proton affinity higher than water with a high time resolution of 1 s per compound. Hence nearly all VOCs can be detected on-line. We could clearly identify the emission of methanol, acetaldehyde, ethanol, acetone, acetic acid, isoprene, monoterpenes, toluene, and C10-benzenes. Some other species could be tentatively denominated. Among these are the masses 67 (cyclo pentadiene), mass 71 (tentatively attributed to methyl vinyl ketone (MVK) and metacrolein (MACR)), 73 (attributed to methyl ethyl ketone (MEK)), 85 (C6H12 or hexanol), and 95 (vinylfuran or phenol). The emissions of all these compounds (identified as well as nonidentified) together represent 99% of all masses detected and account for a carbon loss of 0.7-2.9% of the net photosynthesis. Of special interest was a change in the emission behavior under changing environmental conditions such as flooding or fast light/dark changes. Flooding of the root system caused an increase of several VOCs between 60 and 2000%, dominated by the emission of ethanol and acetaldehyde, which can be explained by the well described production of ethanol under anoxic conditions of the root system and the recently described subsequent transport and partial oxidation to acetaldehyde within the green leaves. However, ethanol emissions were dominant. Additionally, bursts of acetaldehyde with lower ethanol emission were also found under fast light/dark changes. These bursts are not understood.

  12. Arsenic and antimony determination in non- and biodegradable materials by hydride generation capacitively coupled plasma microtorch optical emission spectrometry.

    PubMed

    Mihaltan, Alin I; Frentiu, Tiberiu; Ponta, Michaela; Petreus, Dorin; Frentiu, Maria; Darvasi, Eugen; Marutoiu, Constantin

    2013-05-15

    A sensitive method using a miniature analytical system with a capacitively coupled plasma microtorch (25 W, 13.56 MHz, 0.4 l min(-1) Ar) was developed and evaluated for the determination of As and Sb in recyclable plastics and biodegradable materials by hydride generation optical emission spectrometry. Given their toxicity, As and Sb should be subject to monitoring in such materials despite not being included within the scope of Restriction of Hazardous Substances Directive. The advantages of the proposed approach are better detection limits and lower analysis cost relative to conventional systems based on inductively coupled plasma optical emission and flame atomic absorption spectrometry with/without derivatization. Samples were subjected to acidic microwave-assisted digestion in a nitric-sulfuric acid mixture. Chemical hydride generation with 0.5% NaBH4 after the prereduction of As(V) and Sb(V) with 0.3% L-cysteine in 0.01 mol l(-1) HCl (10 min contact time at 90±5°C) was used. Under the optimal hydride generation conditions and analytical system operation the detection limits (mg kg(-1)) were 0.5 (As) and 0.1 (Sb), whereas the precision was 0.4-7.1% for 10.2-46.2 mg kg(-1) As and 0.4-3.2% for 7.1-156 mg kg(-1) Sb. Analysis of two polyethylene CRMs revealed recoveries of 101±2% As and 100±1% Sb.

  13. Characterization of direct current He-N{sub 2} mixture plasma using optical emission spectroscopy and mass spectrometry

    SciTech Connect

    Flores, O.; Castillo, F.; Martinez, H.; Villa, M.; Reyes, P. G.; Villalobos, S.

    2014-05-15

    This study analyses the glow discharge of He and N{sub 2} mixture at the pressure of 2.0 Torr, power of 10 W, and flow rate of 16.5 l/min, by using optical emission spectroscopy and mass spectrometry. The emission bands were measured in the wavelength range of 200–1100 nm. The principal species observed were N{sub 2}{sup +} (B{sup 2}Σ{sup +}{sub u}→X{sup 2}Σ{sup +}{sub g}), N{sub 2} (C{sup 3}Π{sub u}→B{sup 3}Π{sub g}), and He, which are in good agreement with the results of mass spectrometry. Besides, the electron temperature and ion density were determined by using a double Langmuir probe. Results indicate that the electron temperature is in the range of 1.55–2.93 eV, and the electron concentration is of the order of 10{sup 10} cm{sup −3}. The experimental results of electron temperature and ion density for pure N{sub 2} and pure He are in good agreement with the values reported in the literature.

  14. Sulfur Limits of Detection and Spectral Interference Corrections for DWPF Sludge Matrices by Inductively Coupled Plasma Emission Spectrometry

    SciTech Connect

    JURGENSEN, AR

    2004-04-20

    The Savannah River Technology Center (SRTC) has been requested to perform sulfur (S) analysis on digested radioactive sludge and supernatant samples by Inductively Coupled Plasma Emission Spectrometry (ICP-ES). The amount of sulfur is a concern because there are sulfur limits for the incoming feed, due to glass melter, process vessel, and off-gas line corrosion concerns and limited sulfur solubility in the glass wasteform. Recent changes in the washing strategy and stream additions change the amount of sulfur in the sludge. Increasing the sulfur concentration in the sludge challenges the current limits, so accurately determining the amount of sulfur present in a sludge batch is paramount. There are two important figures of merit that need to be evaluated for this analysis. The first is the detection limit (LOD), the smallest concentration of an element that can be detected with a defined certainty. This issue is important since the sulfur concentration in these process streams is l ow. Another critical analytical parameter is the effect on the S quantitation from potential spectral interferences. Spectral interferences are caused by background emission from plasma recombination events, scattered and stray light from the line emission of high concentration elements, or molecular band emission and from direct or tailing spectral line overlap from a matrix element. Any existing spectral overlaps could give false positives or increase the measured S concentrations in these matrices.

  15. Source Attribution of Methane Emission from Petroleum Production Operations using High-Resolution Airborne Thermal-Infrared Imaging Spectrometry

    NASA Astrophysics Data System (ADS)

    Tratt, D. M.; Buckland, K. N.; Young, S. J.; Riley, D.; Leifer, I.

    2012-12-01

    High spatio-spectral resolution airborne thermal-infrared (TIR) imaging spectrometry is shown to be effective in detecting and tracking gaseous emissions from petroleum production facilities. The high spatial resolution (1-2 m) of the sensor permits unequivocal trace-back of emission plumes to their source. The high spectral resolution (44 nm across the 7.5-13.5 μm TIR band) enables precise identification and discrimination of primary and subsidiary plume components through the application of spectral matched filtering and adaptive coherence estimation techniques. Operation in the TIR spectral region allows operations to be conducted throughout the diurnal cycle, since the measurement relies on observation of emissive radiation and the intrinsic thermal contrast between the fugitive plume gases and the underlying scene. Methane plumes associated with petroleum production operations and natural emissions have been identified in a variety of environmental settings. The accompanying figure shows a grayscale thermal image of a marine production platform off the California coast. A gas plume (identified as methane) being released from a venting boom is shown superimposed in false color.

  16. Mass spectrometry.

    NASA Technical Reports Server (NTRS)

    Burlingame, A. L.; Johanson, G. A.

    1972-01-01

    Review of the current state of mass spectrometry, indicating its unique importance for advanced scientific research. Mass spectrometry applications in computer techniques, gas chromatography, ion cyclotron resonance, molecular fragmentation and ionization, and isotope labeling are covered. Details are given on mass spectrometry applications in bio-organic chemistry and biomedical research. As the subjects of these applications are indicated alkaloids, carbohydrates, lipids, terpenes, quinones, nucleic acid components, peptides, antibiotics, and human and animal metabolisms. Particular attention is given to the mass spectra of organo-inorganic compounds, inorganic mass spectrometry, surface phenomena such as secondary ion and electron emission, and elemental and isotope analysis. Further topics include mass spectrometry in organic geochemistry, applications in geochronology and cosmochemistry, and organic mass spectrometry.

  17. Determination of methane emission rates on a biogas plant using data from laser absorption spectrometry.

    PubMed

    Groth, Angela; Maurer, Claudia; Reiser, Martin; Kranert, Martin

    2015-02-01

    The aim of the work was to establish a method for emission control of biogas plants especially the observation of fugitive methane emissions. The used method is in a developmental stage but the topic is crucial to environmental and economic issues. A remote sensing measurement method was adopted to determine methane emission rates of a biogas plant in Rhineland-Palatinate, Germany. An inverse dispersion model was used to deduce emission rates. This technique required one concentration measurement with an open path tunable diode laser absorption spectrometer (TDLAS) downwind and upwind the source and basic wind information, like wind speed and direction. Different operating conditions of the biogas plant occurring on the measuring day (December 2013) could be represented roughly in the results. During undisturbed operational modes the methane emission rate averaged 2.8 g/s, which corresponds to 4% of the methane gas production rate of the biogas plant.

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

    PubMed

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

    2004-02-18

    Metals have been investigated in different plant materials in order to establish their normal concentration range and consider their role in plants as part of human medicinal treatment. Metal monitoring as a pattern recognition method is a promising tool in the characterization and/or standardization of phytomedicines. In the present work measurable amounts of Ca, Cu, K, Li, Mg, Mn, Na, Ni, and Zn were detected in phytopharmaceutical derivatives of Hypericum perforatum by atomic techniques. Atomic methodologies like flame atomic absorption spectrometry (FAAS) and electrothermal atomic absorption spectrometry (ETAAS) allow reliable determination of mineral content in pharmaceutical quality control of medicinal plants. Additionally, capillary electrophoresis (CE) patterns of characteristic components (fingerprints) have been performed for the search of adulterants in phytopharmaceutical products. PMID:15127813

  19. Sample introduction in ICP spectrometry by hydraulic high-pressure nebulization

    NASA Astrophysics Data System (ADS)

    Luo, S. K.; Berndt, H.

    1994-05-01

    Hydraulic high-pressure nebulization (HHPN) is a new aerosol generation technique in atomic spectrometry. Owing to the high aerosol yield of about 50%, the application of HHPN in ICP spectrometry requires a desolvation unit. The constructed unit consists of a heated tube and a two-stage condenser (liquid cooler, Peltier module cooler). The liquid cooled Peltier module offers variability of condensation temperature between +15 and -40°C. This temperature range is also sufficient for solvent-plasma load control of highly volatile organic solvents. The desolvation unit offers condensation efficiency of 97% for aqueous samples (-5°C) and 94% for methanol (-25°C). The analyte mass transport efficiency amounts to about 24%. In inductively coupled plasma atomic emission spectrometry (ICP-AES), significant improvements in sensitivity and detection limits of about one order of magnitude were obtained for most of the elements under investigation. Using an HPLC pump (100-400 bar), the additional facilities of an on-line high-performance flow system is offered (high-performance flow atomic spectrometry).

  20. Characterizing Methane Emissions at Local Scales with a 20 Year Total Hydrocarbon Time Series, Imaging Spectrometry, and Web Facilitated Analysis

    NASA Astrophysics Data System (ADS)

    Bradley, Eliza Swan

    Methane is an important greenhouse gas for which uncertainty in local emission strengths necessitates improved source characterizations. Although CH4 plume mapping did not motivate the NASA Airborne Visible InfraRed Imaging Spectrometer (AVIRIS) design and municipal air quality monitoring stations were not intended for studying marine geological seepage, these assets have capabilities that can make them viable for studying concentrated (high flux, highly heterogeneous) CH4 sources, such as the Coal Oil Point (COP) seep field (˜0.015 Tg CH4 yr-1) offshore Santa Barbara, California. Hourly total hydrocarbon (THC) data, spanning 1990 to 2008 from an air pollution station located near COP, were analyzed and showed geologic CH4 emissions as the dominant local source. A band ratio approach was developed and applied to high glint AVIRIS data over COP, resulting in local-scale mapping of natural atmospheric CH4 plumes. A Cluster-Tuned Matched Filter (CTMF) technique was applied to Gulf of Mexico AVIRIS data to detect CH4 venting from offshore platforms. Review of 744 platform-centered CTMF subsets was facilitated through a flexible PHP-based web portal. This dissertation demonstrates the value of investigating municipal air quality data and imaging spectrometry for gathering insight into concentrated methane source emissions and highlights how flexible web-based solutions can help facilitate remote sensing research.

  1. 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)

  2. The microwave induced plasma with optical emission spectrometry (MIP-OES) in 23 elements determination in geological samples.

    PubMed

    Niedzielski, P; Kozak, L; Wachelka, M; Jakubowski, K; Wybieralska, J

    2015-01-01

    The article presents the optimisation, validation and application of the microwave induced plasma optical emission spectrometry (MIP-OES) dedicated for a routine determination of Ag, Al, B, Ba, Bi, Ca, Cd, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Ni, Pb, Sr, Tl, Zn, in the geological samples. The three procedures of sample preparation has been proposed: sample digestion with the use of hydrofluoric acid for determination of total concentration of elements, extraction by aqua regia for determination of the quasi-total element concentration and extraction by hydrochloric acid solution to determine contents of the elements in acid leachable fraction. The detection limits were on the level 0.001-0.121 mg L(-1) (from 0.010-0.10 to 1.2-12 mg kg(-1) depend on the samples preparation procedure); the precision: 0.20-1.37%; accuracy 85-115% (for recovery for certified standards materials analysis and parallel analysis by independent analytical techniques: X-ray fluorescence (XRF) and flame absorption spectrometry (FAAS)). The conformity of the results obtained by MIP-OES analytical procedures with the results obtained by XRF and FAAS analysis allows to propose the procedures for studies of elemental composition of the fraction of the geological samples. Additionally, the MIP-OES technique is much less expensive than ICP techniques and much less time-consuming than AAS techniques.

  3. Evaluation of the mineral profile of textile materials using inductively coupled plasma optical emission spectrometry and chemometrics.

    PubMed

    Menezes, E A; Carapelli, R; Bianchi, S R; Souza, S N P; Matos, W O; Pereira-Filho, E R; Nogueira, A R A

    2010-10-15

    The content of Al, Ba, Ca, Cr, Cu, Fe, Ni, P, Zn, Cd and Pb was determined in textile material samples after microwave-assisted decomposition in a cavity oven and extraction with an artificial sweat solution. Radial viewing inductively coupled plasma optical emission spectrometry (ICP OES) was the main detection technique, but Cd and Pb were determined by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) to increase the sensitivity. Principal components analysis (PCA) was applied to the data sets to characterize the samples with respect to their geographic origin and color difference. The PCA for Brazilian single-color samples showed separation, with one group consisting of blue and green textiles and another with all the other materials evaluated. The geographic origin study showed a clear separation between Brazilian and Chinese textiles. The metals amount extracted with sweat extractable solution were lower than limits values pointed by the International Testing and Certification System for Textiles, Oko Tex Standard 100, in the all considered classes. Recoveries varied from 85 to 112% for additions ranging from 3.0 to 25 mg kg(-1) for Ca and from 0.3 to 7.0 mg kg(-1) for all other analytes through the microwave-assisted decomposition procedure. PMID:20599322

  4. Solid phase microextraction capillary gas chromatography combined with furnace atomization plasma emission spectrometry for speciation of mercury in fish tissues

    NASA Astrophysics Data System (ADS)

    Grinberg, Patricia; Campos, Reinaldo C.; Mester, Zoltan; Sturgeon, Ralph E.

    2003-03-01

    The use of solid phase microextraction in conjunction with tandem gas chromatography-furnace atomization plasma emission spectrometry (SPME-GC-FAPES) was evaluated for the determination of methylmercury and inorganic mercury in fish tissue. Samples were digested with methanolic potassium hydroxide, derivatized with sodium tetraethylborate and extracted by SPME. After the SPME extraction, species were separated by GC and detected by FAPES. All experimental parameters were optimized for best separation and analytical response. A repeatability precision of typically 2% can be achieved with long-term (3 months) reproducibility precision of 4.3%. Certified Reference Materials DORM-2, DOLT-2 and TORT-2 from the National Research Council of Canada were analyzed to verify the accuracy of this technique. Detection limits of 1.5 ng g -1 for methylmercury and 0.7 ng g -1 for inorganic mercury in biological tissues were obtained.

  5. 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.

  6. Effects of Ar plasma treatment for deposition of ruthenium film by remote plasma atomic layer deposition

    SciTech Connect

    Park, Taeyong; Lee, Jaesang; Park, Jingyu; Jeon, Heeyoung; Jeon, Hyeongtag; Lee, Ki-Hoon; Cho, Byung-Chul; Kim, Moo-Sung; Ahn, Heui-Bok

    2012-01-15

    Ruthenium thin films were deposited on argon plasma-treated SiO{sub 2} and untreated SiO{sub 2} substrates by remote plasma atomic layer deposition using bis(ethylcyclopentadienyl)ruthenium [Ru(EtCp){sub 2}] as a Ru precursor and ammonia plasma as a reactant. The results of in situ Auger electron spectroscopy (AES) analysis indicate that the initial transient region of Ru deposition was decreased by Ar plasma treatment at 400 deg. C, but did not change significantly at 300 deg. C The deposition rate exhibited linearity after continuous film formation and the deposition rates were about 1.7 A/cycle and 0.4 A/cycle at 400 deg. C and 300 deg. C, respectively. Changes of surface energy and polar and dispersive components were measured by the sessile drop test. The quantity of surface amine groups was measured from the surface nitrogen concentration with AES. Furthermore, the Ar plasma-treated SiO{sub 2} contained more amine groups and less hydroxyl groups on the surface than on untreated SiO{sub 2}. Auger spectra exhibited chemical shifts by Ru-O bonding, and larger shifts were observed on untreated substrates due to the strong adhesion of Ru films.

  7. Uniform GaN thin films grown on (100) silicon by remote plasma atomic layer deposition.

    PubMed

    Shih, Huan-Yu; Lin, Ming-Chih; Chen, Liang-Yih; Chen, Miin-Jang

    2015-01-01

    The growth of uniform gallium nitride (GaN) thin films was reported on (100) Si substrate by remote plasma atomic layer deposition (RP-ALD) using triethylgallium (TEG) and NH3 as the precursors. The self-limiting growth of GaN was manifested by the saturation of the deposition rate with the doses of TEG and NH3. The increase in the growth temperature leads to the rise of nitrogen content and improved crystallinity of GaN thin films, from amorphous at a low deposition temperature of 200 °C to polycrystalline hexagonal structures at a high growth temperature of 500 °C. No melting-back etching was observed at the GaN/Si interface. The excellent uniformity and almost atomic flat surface of the GaN thin films also infer the surface control mode of the GaN thin films grown by the RP-ALD technique. The GaN thin films grown by RP-ALD will be further applied in the light-emitting diodes and high electron mobility transistors on (100) Si substrate.

  8. Inductively coupled plasma atomic fluorescence spectrometric determination of cadmium, copper, iron, lead, manganese and zinc

    USGS Publications Warehouse

    Sanzolone, R.F.

    1986-01-01

    An inductively coupled plasma atomic fluorescence spectrometric method is described for the determination of six elements in a variety of geological materials. Sixteen reference materials are analysed by this technique to demonstrate its use in geochemical exploration. Samples are decomposed with nitric, hydrofluoric and hydrochloric acids, and the residue dissolved in hydrochloric acid and diluted to volume. The elements are determined in two groups based on compatibility of instrument operating conditions and consideration of crustal abundance levels. Cadmium, Cu, Pb and Zn are determined as a group in the 50-ml sample solution under one set of instrument conditions with the use of scatter correction. Limitations of the scatter correction technique used with the fluorescence instrument are discussed. Iron and Mn are determined together using another set of instrumental conditions on a 1-50 dilution of the sample solution without the use of scatter correction. The ranges of concentration (??g g-1) of these elements in the sample that can be determined are: Cd, 0.3-500; Cu, 0.4-500; Fe, 85-250 000; Mn, 45-100 000; Pb, 5-10 000; and Zn, 0.4-300. The precision of the method is usually less than 5% relative standard deviation (RSD) over a wide concentration range and acceptable accuracy is shown by the agreement between values obtained and those recommended for the reference materials.

  9. Evaluation of Five Phase Digitally Controlled Rotating Field Plasma Source for Photochemical Mercury Vapor Generation Optical Emission Spectrometry.

    PubMed

    Matusiewicz, Henryk; Ślachciński, Mariusz; Pawłowski, Paweł; Portalski, Marek

    2015-01-01

    A new sensitive method for total mercury determination in reference materials using a 5-phase digitally controlled rotating field plasma source (RFP) for optical emission spectrometry (OES) was developed. A novel synergic effect of ultrasonic nebulization (USN) and ultraviolet-visible light (UV-Vis) irradiation when used in combination was exploited for efficient Hg vapor generation. UV- and Vis-based irradiation systems were studied. It was found that the most advantageous design was an ultrasonic nebulizer fitted with a 6 W mercury lamp supplying a microliter sample to a quartz oscillator, converting liquid into aerosol at the entrance of the UV spray chamber. Optimal conditions involved using a 20% v/v solution of acetic acid as the generation medium. The mercury cold vapor, favorably generated from Hg(2+) solutions by UV irradiation, was rapidly transported into a plasma source with rotating field generated within the five electrodes and detected by digitally controlled rotating field plasma optical emission spectrometry (RFP-OES). Under optimal conditions, the experimental concentration detection limit for the determination, calculated as the concentration giving a signal equal to three times the standard deviation of the blank (LOD, 3σblank criterion, peak height), was 4.1 ng mL(-1). The relative standard deviation for samples was equal to or better than 5% for liquid analysis and microsampling capability. The methodology was validated through determination of mercury in three certified reference materials (corresponding to biological and environmental samples) (NRCC DOLT-2, NRCC PACS-1, NIST 2710) using the external aqueous standard calibration techniques in acetic acid media, with satisfactory recoveries. Mercury serves as an example element to validate the capability of this approach. This is a simple, reagent-saving, cost-effective and green analytical method for mercury determination. PMID:26460362

  10. 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.K.

    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

  11. Measurement of Hydrogen Chloride in Coal-Fired Power Plant Emissions Using Tunable Diode Laser Spectrometry

    NASA Astrophysics Data System (ADS)

    Mackay, K. L.; Chanda, A.; Mackay, G.; Pisano, J. T.; Durbin, T. D.; Crabbe, K.; Smith, T.

    2016-09-01

    In this paper, we report on TDL HCl measurements obtained at a coal-fi red power plant which indicate that there is a significant perturbation of the HCl absorption feature. A methodology was also developed to remediate this effect and provide accurate measurement that will meet the EPA precision and detection limits currently being developed for HCl measurements of process gas emissions.

  12. Chemical ionization mass spectrometry using carbon nanotube field emission electron sources.

    PubMed

    Radauscher, Erich J; Keil, Adam D; Wells, Mitch; Amsden, Jason J; Piascik, Jeffrey R; Parker, Charles B; Stoner, Brian R; Glass, Jeffrey T

    2015-11-01

    A novel chemical ionization (CI) source has been developed based on a carbon nanotube (CNT) field emission electron source. The CNT-based electron source was evaluated and compared with a standard filament thermionic electron source in a commercial explosives trace detection desktop mass spectrometer. This work demonstrates the first reported use of a CNT-based ion source capable of collecting CI mass spectra. Both positive and negative modes were investigated. Spectra were collected for a standard mass spectrometer calibration compound, perfluorotributylamine (PFTBA), as well as trace explosives including trinitrotoluene (TNT), Research Department explosive (RDX), and pentaerythritol tetranitrate (PETN). The electrical characteristics, lifetime at operating pressure, and power requirements of the CNT-based electron source are reported. The CNT field emission electron sources demonstrated an average lifetime of 320 h when operated in constant emission mode under elevated CI pressures. The ability of the CNT field emission source to cycle on and off can provide enhanced lifetime and reduced power consumption without sacrificing performance and detection capabilities. Graphical Abstract ᅟ. PMID:26133527

  13. Chemical Ionization Mass Spectrometry Using Carbon Nanotube Field Emission Electron Sources

    NASA Astrophysics Data System (ADS)

    Radauscher, Erich J.; Keil, Adam D.; Wells, Mitch; Amsden, Jason J.; Piascik, Jeffrey R.; Parker, Charles B.; Stoner, Brian R.; Glass, Jeffrey T.

    2015-11-01

    A novel chemical ionization (CI) source has been developed based on a carbon nanotube (CNT) field emission electron source. The CNT-based electron source was evaluated and compared with a standard filament thermionic electron source in a commercial explosives trace detection desktop mass spectrometer. This work demonstrates the first reported use of a CNT-based ion source capable of collecting CI mass spectra. Both positive and negative modes were investigated. Spectra were collected for a standard mass spectrometer calibration compound, perfluorotributylamine (PFTBA), as well as trace explosives including trinitrotoluene (TNT), Research Department explosive (RDX), and pentaerythritol tetranitrate (PETN). The electrical characteristics, lifetime at operating pressure, and power requirements of the CNT-based electron source are reported. The CNT field emission electron sources demonstrated an average lifetime of 320 h when operated in constant emission mode under elevated CI pressures. The ability of the CNT field emission source to cycle on and off can provide enhanced lifetime and reduced power consumption without sacrificing performance and detection capabilities.

  14. Quantification of the Rubidium in Beverage Products Micro Samples by Platinum-wire Loop in Flame Atomization Atomic Emission Spectrometry.

    PubMed

    Kékedy-Nagy, Ladislau; Zsigmond, Andreea R; Cordoş, Emil A

    2010-12-01

    The rubidium content in 3 µL of some beverage products (beer, wine, vegetable and fruit juices) atomized from a Ptwire in the methaneair flame has been determined by atomic emission spectrometry. The flame atomization conditions of rubidium were optimized, they are: λ = 780.0 nm, the height of 8 mm over the burner head, gas flow rates of 300 L h-1 air and 34 L h-1 methane. The effect of Na, K, Cs, Sr and acetone on the emission of rubidium was studied too. The limit of quantification (6σ) obtained is of 4.3±1.8 pg in the presence of 50 mg L-1 K and 5% v/v acetone (P = 0.05). The rubidium content of the samples has been determined with continuous nebulization and by atomization from the Ptwire, using the standard calibration curve and the standard addition method. The results of the two procedures agree within the determination errors. PMID:24061895

  15. 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. PMID:23816124

  16. A mass quadrupole spectrometry investigation on proton emission by nanosecond laser ablation

    SciTech Connect

    Caridi, F.

    2015-02-15

    A nanosecond pulsed Nd:YAG laser operating at the fundamental wavelength of 1064 nm and at an intensity of about 10{sup 10} W/cm{sup 2} was employed to irradiate hydrogenated polymers in vacuum. The produced plasma was characterized in terms of thermal and Coulomb interactions evaluating the equivalent temperature and the acceleration voltage developed in the non-equilibrium plasma core. Particles emission along the normal to the target surface was investigated by measuring, with the Hiden EQP 300 mass quadrupole spectrometer, ion energy distributions and fitting experimental data with the “Coulomb-Boltzmann-shifted” function. Time-of-flight technique was employed in order to measure the proton energy and yield. A comparison between experimental results is presented and discussed, with a special regard to the protons emission.

  17. Comparison in the analytical performance between krypton and argon glow discharge plasmas as the excitation source for atomic emission spectrometry.

    PubMed

    Wagatsuma, Kazuaki

    2009-04-01

    The emission characteristics of ionic lines of nickel, cobalt, and vanadium were investigated when argon or krypton was employed as the plasma gas in glow discharge optical emission spectrometry. A dc Grimm-style lamp was employed as the excitation source. Detection limits of the ionic lines in each iron-matrix alloy sample were compared between the krypton and the argon plasmas. Particular intense ionic lines were observed in the emission spectra as a function of the discharge gas (krypton or argon), such as the Co II 258.033 nm for krypton and the Co II 231.707 nm for argon. The explanation for this is that collisions with the plasma gases dominantly populate particular excited levels of cobalt ion, which can receive the internal energy from each gas ion selectively, for example, the 3d(7)4p (3)G(5) (6.0201 eV) for krypton and the 3d(7)4p (3)G(4) (8.0779 eV) for argon. In the determination of nickel as well as cobalt in iron-matrix samples, more sensitive ionic lines could be found in the krypton plasma rather than the argon plasma. Detection limits in the krypton plasma were 0.0039 mass% Ni for the Ni II 230.299-nm line and 0.002 mass% Co for the Co II 258.033-nm line. However, in the determination of vanadium, the argon plasma had better analytical performance, giving a detection limit of 0.0023 mass% V for the V II 309.310-nm line.

  18. Detection of some industrially relevant elements in water by electrolyte cathode atmospheric glow discharge optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    Bencs, László; Laczai, Nikoletta; Mezei, Pál; Cserfalvi, Tamás

    2015-05-01

    An electrolyte cathode atmospheric glow discharge optical emission spectrometry (ELCAD-OES) method was developed for the detection of the industrially relevant In, Rh and Te in water samples. Acid/additive type, sample pH and flow rate were optimized. The UV-Vis spectrum was scanned for analytical lines, free from spectral overlap interferences, and sensitive enough for quantifying the analytes at mg L- 1 or lower levels. In several cases, the background spectrum of the ELCAD hindered the use of conventional, resonant analytical lines in the UV due to overlaps with bands of molecular species (e.g., OH, NO, N2). Te and Rh showed lower emission intensities than In (determined at In I 451.1 nm), even using the most sensitive, interference-free transitions (i.e., Te I 214.3 nm, Te I 238.6 nm and Rh I 437.5 nm). The emission intensities were highly sample pH dependent, i.e., analytical signals could only be detected at pH levels lower than 2. Conversely, the use of acidity lower than pH 1 caused lower plasma volume, due to its contraction into the sample introduction capillary, and discharge instability in terms of its frequent self-extinction. The detection limits for In, Rh and Te were 0.01, 0.5 and 2.4 mg L- 1, respectively. Calibration curves were linear up to 100-150 mg L- 1. The precision for In, Rh and Te in aqueous standards, expressed as relative standard deviation (RSD), was not higher than 4.6%, 6.4% and 7.4%, respectively. Samples with high salt content (e.g., well water) caused positive matrix effects (i.e., 2.0- to 3.6-fold signal enhancements), but also ~ 1.5 times higher RSDs.

  19. Single Nanoparticle Mass Spectrometry as a High Temperature Kinetics Tool: Sublimation, Oxidation, and Emission Spectra of Hot Carbon Nanoparticles.

    PubMed

    Howder, Collin R; Long, Bryan A; Gerlich, Dieter; Alley, Rex N; Anderson, Scott L

    2015-12-17

    In single nanoparticle mass spectrometry, individual charged nanoparticles (NPs) are trapped in a quadrupole ion trap and detected optically, allowing their mass, charge, and optical properties to be monitored continuously. Previous experiments of this type probed NPs that were either fluorescent or large enough to detect by light scattering. Alternatively, small NPs can be heated to temperatures where thermally excited emission is strong enough to allow detection, and this approach should provide a new tool for measurements of sublimation and surface reaction kinetics of materials at high temperatures. As an initial test, we report a study of carbon NPs in the 20-50 nm range, heated by 10.6 μm, 532 nm, or 445 nm lasers. The kinetics for sublimation and oxidation of individual carbon NPs were studied, and a model is presented for the factors that control the NP temperature, including laser heating, and cooling by sublimation, buffer gas collisions, and radiation. The estimated NP temperatures were in the 1700-2000 K range, and the NP absorption cross sections ranged from ∼0.8 to 0.2% of the geometric cross sections for 532 nm and 10.6 μm excitation, respectively. Emission spectra of single NPs and small NP ensembles show a feature in the IR that appears to be the high energy tail of the thermal (blackbody-like) emission expected from hot particles but also a discrete feature peaking around 750 nm. Both the IR tail and 750 nm peak are observed for all particles and for both IR and visible laser excitation. No significant difference was observed between graphite and amorphous carbon NPs. PMID:26513667

  20. Determination of trace elements in bee honey, pollen and tissue by total reflection and radioisotope X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Kump, P.; Nečemer, M.; Šnajder, J.

    1996-04-01

    Multielemental determinations in samples of various types of bee honey, pollen and bee tissue have been carried out using total reflection X-ray fluorescence spectrometry (TXRF) and radioisotope excited X-ray fluorescence spectrometry (XRF). The objective was to establish whether the elemental content of bee honey, in particular, correlates with any useful information about the environment, variety of honey, etc. An attempt has also been made to determine the X-ray techniques' ability to compete with atomic absorption spectrometry (AAS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES), with regard to elemental sensitivity, accuracy, sample preparation procedures, and in particular, economic performance, which is very important in selecting an appropriate technique for the analysis of large numbers of samples. The results confirm the advantages of the TXRF method for trace element analysis, but only when utilising monochromatic excitation and selecting a proper sample preparation procedure. The radioisotope XRF technique, which does not require any sample preparation, is still very competitive in analysis of elements with concentrations above a few ten ppm. Preliminary results also confirm some correlations between the elemental content of honey and the status of the environment, and encourage further work in this direction

  1. Near-infrared emission spectrometry based on an acousto-optical tunable filter.

    PubMed

    Gonzaga, Fabiano Barbieri; Pasquini, Celio

    2005-02-15

    A spectrometer has been constructed to detect the radiation emitted by thermally excited samples in the near-infrared spectral region extending from 1500 to 3000 nm. The instrument employs an acousto-optical tunable filter (AOTF) made of TeO2 and attains maximum sensitivity by making effective use of the two diffracted beams produced by the anisotropic AOTF. The full exploitation of the transmitted power of the monochromatic beams is reported for the first time and became possible because the detector does not saturate when employed for the acquisition of the weak emission signal in the NIR region, even when exposed to the total (nondiffracted) beam. Thus, modulation and lock-in-based detection can be employed to find the intensity of the diffracted beams superimposed on the nondiffracted beam. The resolution is slighted degraded in view of the small (approximately 10 nm) difference in the wavelength diffracted in the ordinary and extraordinary beams. The instrument has been evaluated in terms of signal-to-noise ratio, effect of sample thickness, and excitation temperature and for its potential in analytical applications in monitoring high-temperature kinetics, for qualitative identification of inorganic solids, for use with a closed cell to obtain spectra of species that evaporate at the temperatures (> 150 degrees C) necessary for sample excitation, and for quantitative purposes in the determination of soybean oil content in olive oil. The feasibility of near-infrared emission spectroscopy has been demonstrated together with some of its advantages over mid-infrared emission spectroscopy, such as greater tolerance to sample thickness, suitable signal-to-noise, and its use in the investigation of kinetic phenomena and phase transitions at high temperatures.

  2. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry. Progress report, January 1, 1990--December 31, 1992

    SciTech Connect

    Montaser, A.

    1992-09-01

    New high temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. Emphasis was placed on atmospheric pressure He inductively coupled plasmas (ICP) suitable for atomization, excitation, and ionization of elements; simulation and computer modeling of plasma sources with potential for use in spectrochemical analysis; spectroscopic imaging and diagnostic studies of high temperature plasmas, particularly He ICP discharges; and development of new, low-cost sample introduction systems, and examination of techniques for probing the aerosols over a wide range. Refs., 14 figs. (DLC)

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

    PubMed

    Lajunen, L H; Kubin, A

    1986-03-01

    Methods are presented for determination of molybdenum in plant tissue by flame and graphite-furnace atomic-absorption spectrometry and direct-current argon-plasma emission spectrometry. The samples are digested in HNO(3)-H(2)SO(4)-HC1O(4) mixture, and Mo is separated and concentrated by chelation and extraction. Three organic solvents (methyl isobutyl ketone, di-isobutyl ketone and isoamyl alcohol) and two ligands (8-hydroxyquinoline and toluene-3,4-dithiol) were studied. The procedure were tested on pine needle and birch leaf samples. PMID:18964076

  4. Direct determination of sodium, potassium, chromium and vanadium in biodiesel fuel by tungsten coil atomic emission spectrometry.

    PubMed

    Dancsak, Stacia E; Silva, Sidnei G; Nóbrega, Joaquim A; Jones, Bradley T; Donati, George L

    2014-01-01

    High levels of sodium and potassium can be present in biodiesel fuel and contribute to corrosion, reduced performance and shorter engine lifetime. On the other hand, trace amounts of chromium and vanadium can increase the emission of pollutants during biodiesel combustion. Sample viscosity, immiscibility with aqueous solutions and high carbon content can compromise biodiesel analyzes. In this work, tungsten filaments extracted from microscope light bulbs are used to successively decompose biodiesel's organic matrix, and atomize and excite the analytes to determine sodium, potassium, chromium and vanadium by tungsten coil atomic emission spectrometry (WCAES). No sample preparation other than simple dilution in methanol or ethanol is required. Direct analysis of 10-μL sample aliquots using heating cycles with less than 150 s results in limits of detection (LOD) as low as 20, 70, 70 and 90 μg kg(-1) for Na, K, Cr and V, respectively. The procedure's accuracy is checked by determining Na and K in a biodiesel reference sample and carrying out spike experiments for Cr and V. No statistically significant differences were observed between reference and determined values for all analytes at a 95% confidence level. The procedure was applied to three different biodiesel samples and concentrations between 6.08 and 95.6 mg kg(-1) for Na and K, and between 0.22 and 0.43 mg kg(-1) for V were obtained. The procedure is simple, fast and environmentally friendly. Small volumes of reagents, samples and gases are used and no residues are generated. Powers of detection are comparable to other traditional methods.

  5. Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    de Oliveira Souza, Sidnei; da Costa, Silvânio Silvério Lopes; Santos, Dayane Melo; dos Santos Pinto, Jéssica; Garcia, Carlos Alexandre Borges; Alves, José do Patrocínio Hora; Araujo, Rennan Geovanny Oliveira

    2014-06-01

    An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg- 1 for Mn to 77.3 mg kg- 1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento - MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES).

  6. Correlation between calcium carbonate content and emission characteristics of incense.

    PubMed

    Yang, Chi-Ru; Lin, Ta-Chang; Chang, Feng-Hsiang

    2006-12-01

    In Taiwan and China, calcium carbonate is commonly added as a filler during incense production to lower the cost. This study has found an unexpected benefit for this practice: it reduces particulate emission. Nine types of the popular incense on the local market were chosen for this study. The calcium content in raw material incense was analyzed by inductively coupled plasma atomic emission spectrometry, followed by X-ray diffraction (XRD) spectroscopy. The correlation between the calcium content and emission characteristics of incense was investigated. The calcium content varied from 1.8 to 60 mg/g (incense burned) among those nine different types of incense. Very little calcium (< 1%) was found in natural wood or plants, which is mainly the raw material of incense. Instead, most calcium was artificially added in the form of CaCO3 during manufacturing. The combustion characteristics, including burning rate, emission factors of particulate, ash, and solid-phase polycyclic aromatic hydrocarbons (S-PAHs), varied significantly among the nine types of incense. Incense containing 2% calcium would emit 30% less S-PAHs, compared with those with little (< 0.2%) calcium. More importantly, increasing the calcium content from 0.5 to 5% by adding CaCO3 reduced the particulate emission from incense by approximately 50%.

  7. Comparison of four analytical techniques based on atomic spectrometry for the determination of total tin in canned foodstuffs.

    PubMed

    Boutakhrit, K; Crisci, M; Bolle, F; Van Loco, J

    2011-02-01

    Different techniques for the determination of total tin in beverages and canned foods by atomic spectrometry were compared. The performance characteristics of inductively coupled plasma-mass spectrometry (ICP-MS), hydride generation-inductively coupled plasma-atomic emission spectrometry (HG-ICP-AES), electrothermal atomisation-atomic absorption spectrometry (ETA-AAS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) were determined in terms of linearity, precision, recovery, limit of detection, decision limit (CCα) and detection capability (CCβ) (Decision 2002/657/EC). Calibration ranges were covered from ng l⁻¹ to mg l⁻¹ level. Limits of detection that ranged from 0.01, 0.05, 2.0 to 200 µg l⁻¹ were reached for ICP-MS; HG-ICP-AES; ETA-AAS and ICP-AES, respectively. Precision, calculated according to ISO 5725-2 for repeatability and within-laboratory reproducibility and expressed as relative standard deviation (RSD), ranged from 1.6% to 4.9%; and recovery, based on Decision 2002/657/EC, was found to be between 95% and 110%. Procedures for the mineralisation or extraction of total tin were compared. Wet digestion, sequentially, with nitric acid and hydrogen peroxide provided the best results. The influence of possible interferences present in canned food and beverage was studied, but no interference in the determination of tin was observed. Since maximum levels for tin established by European Union legislation vary from 50 mg kg⁻¹ in canned baby foods and infant foods up to 200 mg kg⁻¹ in canned food, ICP-AES was chosen as the preferred technique for routine analysis thanks to its good precision, reliability and ease of use. The accuracy of this routine method was confirmed by participation in six proficiency test schemes with z-scores ranging from -1.9 to 0.6. Several canned foodstuffs and beverage samples from a local market were analysed with this technique.

  8. Elemental determination of microsamples by liquid film dielectric barrier discharge atomic emission spectrometry.

    PubMed

    He, Qian; Zhu, Zhenli; Hu, Shenghong; Zheng, Hongtao; Jin, Lanlan

    2012-05-01

    In this study, a new liquid-film dielectric barrier discharge (LFDBD) atomic emission source was developed for microsample elemental determination. It consists of a copper electrode, a tungsten wire electrode, and a piece of glass slide between them, which serves as the dielectric barrier as well as the sample plate. The sample solution with 1 mol L(-1) nitric acid, when deposited onto the surface of the glass slide, forms a thin liquid film. The plasma is generated between the tip of the tungsten wire electrode and the liquid film surface when alternating-current (ac) high voltage (peak voltage ~3.7 kV, frequency ~30 kHz) is applied on the electrodes. Qualitative and quantitative determinations of metal ions in the sample solution were achieved by atomic emission measurements in the plasma and were demonstrated in this study with elements Na, K, Cu, Zn, and Cd. Detection limits were in the range from 0.6 ng (7 μg L(-1)) for Na to 6 ng (79 μg L(-1)) for Zn. Repeatability, expressed as relative standard deviation from seven repetitive analyses of samples with analyte concentrations at 1 mg L(-1), varied from 2.1% to 4.4%. Compared with other liquid discharge systems that operate at atmospheric pressure, the current system offers several advantages: First, it eliminates the use of a sample flow system (e.g., syringe or peristaltic pump); instead, a small aliquot of sample is directly pipetted onto the glass slide for analysis. Second, it is a microanalysis system and requires sample volume ≤80 μL, a benefit when a limited amount of sample is available. Third, because the sample is applied in aliquot, there is no washout time, and the analysis can be easily extended to sample array for high-throughput analysis. The proposed LFDBD is promising for in-field elemental determination because of its simplicity, cost effectiveness, low power supply, and no inert gas requirement. PMID:22486234

  9. Improvement of sensitivity of electrolyte cathode discharge atomic emission spectrometry (ELCAD-AES) for mercury using acetic acid medium.

    PubMed

    Shekhar, R

    2012-05-15

    A method has been developed to improve the sensitivity of the electrolyte cathode discharge atomic emission spectrometry (ELCAD-AES) for mercury determination. Effects of various low molecular weight organic solvents at different volume percentages as well as at different acid molarities on the mercury signal were investigated using ELCAD-AES. The addition of few percent of organic solvent, acetic acid produced significant enhancement in mercury signal. Acetic acid of 5% (v/v) with the 0.2M acidity has been found to give 500% enhancement for mercury signal in flow injection mode. Under the optimized parameters the repeatability, expressed as the percentage relative standard deviation of spectral peak area for mercury with 5% acetic acid was found to be 10% for acid blank solution and 5% for 20 ng/mL mercury standard based on multiple measurements with a multiple sample loading in flow injection mode. Limit of detection of this method was determined to be 2 ng/mL for inorganic mercury. The proposed method has been validated by determining mercury in certified reference materials, Tuna fish (IAEA-350) and Aquatic plant (BCR-060). Accuracy of the method for the mercury determination in the reference materials has been found to be between 3.5% and 5.9%. This study enhances the utility of ELCAD-AES for various types of biological and environmental materials to quantify total mercury at very low levels. PMID:22483872

  10. Improvement of sensitivity of electrolyte cathode discharge atomic emission spectrometry (ELCAD-AES) for mercury using acetic acid medium.

    PubMed

    Shekhar, R

    2012-05-15

    A method has been developed to improve the sensitivity of the electrolyte cathode discharge atomic emission spectrometry (ELCAD-AES) for mercury determination. Effects of various low molecular weight organic solvents at different volume percentages as well as at different acid molarities on the mercury signal were investigated using ELCAD-AES. The addition of few percent of organic solvent, acetic acid produced significant enhancement in mercury signal. Acetic acid of 5% (v/v) with the 0.2M acidity has been found to give 500% enhancement for mercury signal in flow injection mode. Under the optimized parameters the repeatability, expressed as the percentage relative standard deviation of spectral peak area for mercury with 5% acetic acid was found to be 10% for acid blank solution and 5% for 20 ng/mL mercury standard based on multiple measurements with a multiple sample loading in flow injection mode. Limit of detection of this method was determined to be 2 ng/mL for inorganic mercury. The proposed method has been validated by determining mercury in certified reference materials, Tuna fish (IAEA-350) and Aquatic plant (BCR-060). Accuracy of the method for the mercury determination in the reference materials has been found to be between 3.5% and 5.9%. This study enhances the utility of ELCAD-AES for various types of biological and environmental materials to quantify total mercury at very low levels.

  11. Multi-element determination in acid-digested soy protein formulations by inductively coupled plasma-optical emission spectrometry.

    PubMed

    Morte, Elane S Boa; Costa, Leticia M; Nobrega, Joaquim A; Korn, Maria das Gracas A

    2008-05-01

    The concentrations of major (Ca, K, Mg, Na and P) and trace elements (Al, Cu and Fe) in soy protein formulations sold in Bahia (Brazil) were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES). Liquid and powdered soy protein formulation samples, both whole and light, were digested using a conventional heating program on a hot-plate. The powdered samples were prepared according to the label instructions for human consumption. A 5.0-ml aliquot of the soy protein emulsion was transferred to a borosilicate Erlenmeyer and concentrated nitric and sulfuric acid added. After a digestion time of approximately 50 min, hydrogen peroxide was added and heating continued to give a final volume of approximately 5 ml; the colorless digests were then made up to 15.0 ml with deionised water. Residual acid content was determined by acid-base titration. Good agreement between measured and certified values for all analytes in a non-fat milk powder (NIST SRM 1549) indicated that the method was suitable for major and trace elements determination in soy protein formulations. PMID:18473216

  12. Mercury determination in non- and biodegradable materials by cold vapor capacitively coupled plasma microtorch atomic emission spectrometry.

    PubMed

    Frentiu, Tiberiu; Mihaltan, Alin I; Ponta, Michaela; Darvasi, Eugen; Frentiu, Maria; Cordos, Emil

    2011-10-15

    A new analytical system consisting of a low power capacitively coupled plasma microtorch (20 W, 13.56 MHz, 150 ml min(-1) Ar) and a microspectrometer was investigated for the Hg determination in non- and biodegradable materials by cold-vapor generation, using SnCl(2) reductant, and atomic emission spectrometry. The investigated miniaturized system was used for Hg determination in recyclable plastics from electronic equipments and biodegradable materials (shopping bags of 98% biodegradable polyethylene and corn starch) with the advantages of easy operation and low analysis costs. Samples were mineralized in HNO(3)-H(2)SO(4) mixture in a high-pressure microwave system. The detection limits of 0.05 ng ml(-1) or 0.08 μg g(-1) in solid sample were compared with those reported for other analytical systems. The method precision was 1.5-9.4% for Hg levels of 1.37-13.9 mg kg(-1), while recovery in two polyethylene certified reference materials in the range 98.7 ± 4.5% (95% confidence level).

  13. Determination of arsenic and selenium by hydride generation and headspace solid phase microextraction coupled with optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    Tyburska, Anna; Jankowski, Krzysztof; Rodzik, Agnieszka

    2011-07-01

    A hydride generation headspace solid phase microextraction technique has been developed in combination with optical emission spectrometry for determination of total arsenic and selenium. Hydrides were generated in a 10 mL volume septum-sealed vial and subsequently collected onto a polydimethylsiloxane/Carboxen solid phase microextraction fiber from the headspace of sample solution. After completion of the sorption, the fiber was transferred into a thermal desorption unit and the analytes were vaporized and directly introduced into argon inductively coupled plasma or helium microwave induced plasma radiation source. Experimental conditions of hydride formation reaction as well as sorption and desorption of analytes have been optimized showing the significant effect of the type of the solid phase microextraction fiber coating, the sorption time and hydrochloric acid concentration of the sample solution on analytical characteristics of the method developed. The limits of detection of arsenic and selenium were 0.1 and 0.8 ng mL - 1 , respectively. The limit of detection of selenium could be improved further using biosorption with baker's yeast Saccharomyces cerevisiae for analyte preconcentration. The technique was applied for the determination of total As and Se in real samples.

  14. Analysis of Tropical Forest Fire Emissions Using in Situ Gas Chromatography/Mass Spectrometry during Sambba

    NASA Astrophysics Data System (ADS)

    Minaeian, J.; Lewis, A. C.; Edwards, P. M.; Evans, M. J.; Hopkins, J. R.; Lee, J. D.; Purvis, R.

    2014-12-01

    Vertical atmospheric profiles of volatile organic compounds (VOCs) were made over Amazonia using an in situ gas chromatography/mass spectrometer (GC/MS), including isoprene, methacrolein, methyl vinyl ketone and products of biomass burning such as benzene. Measurements were made in the Amazonian (Rondônia and Amazonas) region during September 2012, a period of extensive biomass burning. Data was obtained between 100m and 8500m from the FAAM BAe 146 research aircraft. Isoprene was observed to be constrained overwhelmingly to the boundary layer (height typically ~2500m) with mean boundary layer mixing ratio of ~2 ppbv and a peak of ~5 ppbv at the lowest flight levels of 100 m. First generation isoprene oxidation products, methyl vinyl ketone and methacrolein, were quantified individually rather than as the sum of the pair, which is more commonly found in the literature. Both MACR and MVK were constrained primarily to the boundary layer, however trace quantities could be seen in the free troposphere to a height of 8000 m. Benzene from biomass burning was observed in both boundary layer and free troposphere, with a peak mixing ratio of ~0.8 ppbv at 750 m. This work will present the spatial distribution of isoprene within the boundary as a function of underlying surface type. The vertical profiles of all species are then compared to representative simulations from the GEOS-Chem chemistry transport model and conclusions drawn on the success of the model in representing emissions and oxidation chemistry.

  15. Nonthermal Optical Emission Spectrometry: Direct Atomization and Excitation of Cadmium for Highly Sensitive Determination.

    PubMed

    Cai, Yi; Zhang, Ya-Jie; Wu, De-Fu; Yu, Yong-Liang; Wang, Jian-Hua

    2016-04-19

    The low atomization and excitation capability of nonthermal microplasma, e.g., dielectric barrier discharge (DBD), has greatly hampered its potential applications for the determination of metals in solution. In the present work, an inspiring development is reported for direct atomization and excitation of cadmium in aqueous solution by DBD and facilitates highly sensitive determination. A DBD microplasma is generated on the nozzle of a pneumatic micronebulizer to focus the DBD energy on a confined space and atomize/excite metals in the spray. Meanwhile, an appropriate sample matrix and nebulization in helium further improves the atomization and excitation capability of DBD. With cadmium as a model, its emission is recorded by a CCD spectrometer at 228.8 nm. By using an 80 μL sample solution nebulized at 3 μL s(-1), a linear range of 5-1000 μg L(-1) along with a detection limit of 1.5 μg L(-1) is achieved, which is comparable to those obtained by commercial bulky inductively coupled plasma (ICP)-based instrumentations. PMID:27030025

  16. Laser ablation inductively coupled plasma optical emission spectrometry for analysis of pellets of plant materials

    NASA Astrophysics Data System (ADS)

    Gomes, Marcos S.; Schenk, Emily R.; Santos, Dário; Krug, Francisco José; Almirall, José R.

    An evaluation of laser ablation inductively coupled plasma optical emission spectroscopy (LAICP OES) for the direct analysis of pelleted plant material is reported. Ground leaves of orange citrus, soy and sugarcane were comminuted using a high-speed ball mill, pressed into pellets and sampled directly with laser ablation and analyzed by ICP OES. The limits of detection (LODs) for the method ranged from as low as 0.1 mg kg- 1 for Zn to as high as 94 mg kg- 1 for K but were generally below 6 mg kg- 1 for most of the elements of interest. A certified reference material consisting of a similar matrix (NIST SRM 1547 peach leaves) was used to check the accuracy of the calibration and the reported method resulted in an average bias of ~ 5% for all the elements of interest. The precision for the reported method ranged from as low as 4% relative standard deviation (RSD) for Mn to as high as 17% RSD for Zn but averaged ~ 6.5% RSD for all the elements (n = 10). The proposed method was tested for the determination of Ca, Mg, P, K, Fe, Mn, Zn and B, and the results were in good agreement with those obtained for the corresponding acid digests by ICP-OES, no differences being observed by applying a paired t-test at the 95% confidence level. The reported direct solid sampling method provides a fast alternative to acid digestion that results in similar and appropriate analytical figures of merit with regard to sensitivity, accuracy and precision for plant material analysis.

  17. Evaluation of the temporal profiles and the analytical features of a laser ablation - Pulsed glow discharge coupling for optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    González de Vega, Claudia; Bordel, Nerea; Pereiro, Rosario; Sanz-Medel, Alfredo

    2016-07-01

    The coupling of a glow discharge (GD) in pulsed mode (PGD) as secondary source for excitation/ionization of the material provided by laser ablation (LA) has been investigated using optical emission spectrometry (OES). The variation of the laser pulse delay with respect to the GD pulse allows to producing the ablation process during prepeak, plateau or afterglow GD regions. Emission properties of the LA-PGD plasma in each temporal region of the GD pulse have been evaluated for analytical lines of different elements. Resonant atomic lines have shown higher emission intensity in the prepeak region compared to non-resonant lines. Non-resonant lines showed higher enhancement of the emission intensity in the afterglow region. Moreover, the coupled LA-PGD system offered better linear correlation coefficients using a set of glass standards for calibration as well as lower detection limits (by at least a factor of two) when compared to laser induced breakdown spectroscopy.

  18. 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

  19. Partial microwave-assisted wet digestion of animal tissue using a baby-bottle sterilizer for analyte determination by inductively coupled plasma optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    Matos, Wladiana O.; Menezes, Eveline A.; Gonzalez, Mário H.; Costa, Letícia M.; Trevizan, Lilian C.; Nogueira, Ana Rita A.

    2009-06-01

    A procedure for partial digestion of bovine tissue is proposed using polytetrafluoroethylene (PTFE) micro-vessels inside a baby-bottle sterilizer under microwave radiation for multi-element determination by inductively coupled plasma optical emission spectrometry (ICP OES). Samples were directly weighed in laboratory-made polytetrafluoroethylene vessels. Nitric acid and hydrogen peroxide were added to the uncovered vessels, which were positioned inside the baby-bottle sterilizer, containing 500 mL of water. The hydrogen peroxide volume was fixed at 100 µL. The system was placed in a domestic microwave oven and partial digestion was carried out for the determination of Ca, Cu, Fe, Mg, Mn and Zn by inductively coupled plasma optical emission spectrometry. The single-vessel approach was used in the entire procedure, to minimize contamination in trace analysis. Better recoveries and lower residual carbon content (RCC) levels were obtained under the conditions established through a 2 4-1 fractional factorial design: 650 W microwave power, 7 min digestion time, 50 µL nitric acid and 50 mg sample mass. The digestion efficiency was ascertained according to the residual carbon content determined by inductively coupled plasma optical emission spectrometry. The accuracy of the proposed procedure was checked against two certified reference materials.

  20. Effects of anthropogenic emissions on the molecular composition of urban organic aerosols: An ultrahigh resolution mass spectrometry study

    NASA Astrophysics Data System (ADS)

    Kourtchev, I.; O'Connor, I. P.; Giorio, C.; Fuller, S. J.; Kristensen, K.; Maenhaut, W.; Wenger, J. C.; Sodeau, J. R.; Glasius, M.; Kalberer, M.

    2014-06-01

    Identification of the organic composition of atmospheric aerosols is necessary to develop effective air pollution mitigation strategies. However, the majority of the organic aerosol mass is poorly characterized and its detailed analysis is a major analytical challenge. In this study, we applied state-of-the-art direct infusion nano-electrospray (nanoESI) ultrahigh resolution mass spectrometry (UHRMS) and liquid chromatography ESI Quadrupole Time-of-Flight (Q-TOF) MS for the analysis of the organic fraction of fine particulate matter (PM2.5) collected at an urban location in Cork, Ireland. Comprehensive mass spectral data evaluation methods (e.g., Kendrick Mass Defect and Van Krevelen) were used to identify compound classes and mass distributions of the detected species. Up to 850 elemental formulae were identified in negative mode nanoESI-UHR-MS. Nitrogen and/or sulphur containing organic species contributed up to 40% of the total identified formulae and exhibited strong diurnal variations suggesting the importance of night-time NO3 chemistry at the site. The presence of a large number of oxidised aromatic and nitroaromatic compounds in the samples indicated a strong anthropogenic influence, i.e., from traffic emissions and domestic solid fuel (DSF) burning. Most of the identified biogenic secondary organic aerosol (SOA) compounds are later-generation nitrogen- and sulphur-containing products, indicating that SOA composition is strongly affected by anthropogenic species such as NOx and SO2. Unsaturated and saturated C12-C20 fatty acids were found to be the most abundant homologs with a composition reflecting a primary marine origin. The results of this work demonstrate that the studied site is a very complex environment affected by a variety of anthropogenic activities and natural sources.

  1. Determination of rare earth and concomitant elements in magnesium alloys by inductively coupled plasma optical emission spectrometry.

    PubMed

    Fariñas, Juan C; Rucandio, Isabel; Pomares-Alfonso, Mario S; Villanueva-Tagle, Margarita E; Larrea, María T

    2016-07-01

    An Inductively Coupled Plasma Optical Emission Spectrometry method for simultaneous determination of Al, Ca, Cu, Fe, In, Mn, Ni, Si, Sr, Y, Zn, Zr and rare earth elements (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu) in magnesium alloys, including the new rare earth elements-alloyed magnesium, has been developed. Robust conditions have been established as nebulizer argon flow rate of 0.5mLmin(-1) and RF incident power of 1500W, in which matrix effects were significantly reduced around 10%. Three acid digestion procedures were performed at 110°C in closed PFA vessels heated in an oven, in closed TFM vessels heated in a microwave furnace, and in open polypropylene tubes with reflux caps heated in a graphite block. The three digestion procedures are suitable to put into solution the magnesium alloys samples. From the most sensitive lines, one analytical line with lack or low spectral interferences has been selected for each element. Mg, Rh and Sc have been studied as internal standards. Among them, Rh was selected as the best one by using Rh I 343.488nm and Rh II 249.078nm lines as a function of the analytical lines. The trueness and precision have been established by using the Certified Reference Material BCS 316, as well as by means of recovery studies. Quantification limits were between 0.1 and 9mgkg(-1) for Lu and Pr, respectively, in a 2gL(-1) magnesium matrix solution. The method developed has been applied to the commercial alloys AM60, AZ80, ZK30, AJ62, WE54 and AE44.

  2. 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%.

  3. 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.

  4. Determination of rare earth and concomitant elements in magnesium alloys by inductively coupled plasma optical emission spectrometry.

    PubMed

    Fariñas, Juan C; Rucandio, Isabel; Pomares-Alfonso, Mario S; Villanueva-Tagle, Margarita E; Larrea, María T

    2016-07-01

    An Inductively Coupled Plasma Optical Emission Spectrometry method for simultaneous determination of Al, Ca, Cu, Fe, In, Mn, Ni, Si, Sr, Y, Zn, Zr and rare earth elements (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu) in magnesium alloys, including the new rare earth elements-alloyed magnesium, has been developed. Robust conditions have been established as nebulizer argon flow rate of 0.5mLmin(-1) and RF incident power of 1500W, in which matrix effects were significantly reduced around 10%. Three acid digestion procedures were performed at 110°C in closed PFA vessels heated in an oven, in closed TFM vessels heated in a microwave furnace, and in open polypropylene tubes with reflux caps heated in a graphite block. The three digestion procedures are suitable to put into solution the magnesium alloys samples. From the most sensitive lines, one analytical line with lack or low spectral interferences has been selected for each element. Mg, Rh and Sc have been studied as internal standards. Among them, Rh was selected as the best one by using Rh I 343.488nm and Rh II 249.078nm lines as a function of the analytical lines. The trueness and precision have been established by using the Certified Reference Material BCS 316, as well as by means of recovery studies. Quantification limits were between 0.1 and 9mgkg(-1) for Lu and Pr, respectively, in a 2gL(-1) magnesium matrix solution. The method developed has been applied to the commercial alloys AM60, AZ80, ZK30, AJ62, WE54 and AE44. PMID:27154648

  5. Determination of trace elements in high purity alumina powder by helium enhanced direct current glow discharge mass spectrometry

    NASA Astrophysics Data System (ADS)

    Jung, Sehoon; Kim, Sunhye; Hinrichs, Joachim

    2016-08-01

    Trace impurities in high purity alumina powder were determined by fast flow direct current glow discharge mass spectrometry (GD-MS). The non-conductive samples were prepared with high purity graphite powder and used as a sample binder and as a secondary cathode. To improve the sensitivity of the GD-MS analysis, helium was introduced as an additional glow discharge gas to argon plasma. The quantification results of the GD-MS measurement were calculated by external calibration with matrix matched certified reference materials. The GD-MS results for the determination of Na, Mg, Si, Ca, Ti, V, Cr, Fe, Cu, Zn and Ga in the alumina samples agreed well with the certified values of a reference material and the results of chemical analysis using wet sample digestion with inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The GD-MS analysis is a rapid analysis technique to determine trace elements in non-conductive alumina to below mg·kg- 1 levels.

  6. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry. Progress report: January 1, 1993--December 31, 1993

    SciTech Connect

    Montaser, A.

    1993-12-31

    In this research, new high-temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. During the period January 1993--December 1993, emphasis was placed on (a) analytical investigations of atmospheric-pressure helium inductively coupled plasma (He ICP) that are suitable for atomization, excitation, and ionization of elements possessing high excitation and ionization energies; (b) simulation and computer modeling of plasma sources to predict their structure and fundamental and analytical properties without incurring the enormous cost of experimental studies; (c) spectrosopic imaging and diagnostic studies of high-temperature plasmas; (d) fundamental studies of He ICP discharges and argon-nitrogen plasma by high-resolution Fourier transform spectrometry; and (e) fundamental and analytical investigation of new, low-cost devices as sample introduction systems for atomic spectrometry and examination of new diagnostic techniques for probing aerosols. Only the most important achievements are included in this report to illustrate progress and obstacles. Detailed descriptions of the authors` investigations are outlined in the reprints and preprints that accompany this report. The technical progress expected next year is briefly described at the end of this report.

  7. 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.

  8. Inductively coupled plasma-atomic emission spectroscopy: a computer controlled, scanning monochromator system for the rapid determination of the elements

    SciTech Connect

    Floyd, M.A.

    1980-03-01

    A computer controlled, scanning monochromator system specifically designed for the rapid, sequential determination of the elements is described. The monochromator is combined with an inductively coupled plasma excitation source so that elements at major, minor, trace, and ultratrace levels may be determined, in sequence, without changing experimental parameters other than the spectral line observed. A number of distinctive features not found in previously described versions are incorporated into the system here described. Performance characteristics of the entire system and several analytical applications are discussed.

  9. 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

    ..., Publication No. 77-206, August 1977. 14.8“OSHA Safety and Health Standards, General Industry,” (29 CFR part...,000 mL with deionized, distilled water. 7.3.15Manganese solution, stock, 1 mL=100 µg Mn: Dissolve 0... Wavelength, nm Interferent— A1 Ca Cr Cu Fe Mg Mn Ni Ti V Aluminum 308.214 0.21 1.4 Antimony 206.833 0.47...

  10. 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

    ..., Publication No. 77-206, August 1977. 14.8“OSHA Safety and Health Standards, General Industry,” (29 CFR part...,000 mL with deionized, distilled water. 7.3.15Manganese solution, stock, 1 mL=100 µg Mn: Dissolve 0... Wavelength, nm Interferent— A1 Ca Cr Cu Fe Mg Mn Ni Ti V Aluminum 308.214 0.21 1.4 Antimony 206.833 0.47...

  11. Detailed gas and diesel vehicle emissions: PTR-MS measurements of real-time VOC profiles and comprehensive characterization of primary emissions for IVOC, SVOC, and LVOC by gas chromatography with vacuum ultra-violet ionization mass spectrometry

    NASA Astrophysics Data System (ADS)

    Drozd, G.; Frodin, B.; Zhao, Y.; Franklin, J. P.; Cross, E. S.; Saleh, R.; Saliba, G.; Lambe, A. T.; Sardar, S.; Maldonado, H.; Russell, L. M.; Kroll, J. H.; Robinson, A. L.; Goldstein, A. H.

    2015-12-01

    Over the past fifteen years US vehicle emissions standards have dramatically improved, with the goal of reducing urban air pollution. Recent studies demonstrate secondary organic aerosol (SOA) to be the dominant contributor to urban organic aerosol, but controversy remains regarding the contributions of different vehicle types to SOA. Increased potency for SOA formation from non methane hydrocarbons (NMHC) from newer vehicles that meet tighter emission standards has also been observed. Both speciation and temporal resolution of vehicular emissions are critical for predicting SOA formation. The relative importance of diesel and gasoline emissions to SOA formation depends critically on speciation. Experiments were conducted at the California Air Resources Board Haagen-Smit Laboratory to better understand SOA formation for low, ultra-low, super ultra-low and partial zero emission vehicles (LEV, ULEV, SULEV, PZEV). Exhaust was sampled on filters and adsorbent tubes to measure intermediate-, semi-, and low-volatility NMHC (IVOC, SVOC, LVOC). A proton-transfer-reaction mass spectrometer (PTR-MS) measured volatile organics (VOC) emissions with high time-resolution. Analysis of filters and adsorbent tubes using gas chromatography with vacuum-ultra-violet ionization mass spectrometry provided unprecedented characterization of emissions according to degree of branching, number of cyclic rings, aromaticity, and molecular weight. ULEV vehicles show the composition distributions of primary particulate emissions peak for compounds in the SVOC range. PZEV vehicle emissions peak in the IVOC range. Diesel vehicles have up to ten times higher emissions than gasoline vehicles; their distributions have significant IVOC levels and peak in the SVOC/LVOC range. Our measurements are used to predict potential SOA formation by vehicle standard class and the relative SOA formation for diesel and gasoline vehicles. PTR-MS measurement show VOC emissions after cold start occur almost entirely

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

    SciTech Connect

    Ombaba, J.M.

    1992-01-01

    This thesis deals with the construction and evaluation of an alternating current plasma (ACP) as an element-selective detector for high resolution capillary gas chromatography (GC) and as an excitation source for atomic absorption spectrometry (AAS) and atomic emission spectrometry (AES). The plasma, constrained in a quartz discharge tube at atmospheric pressure, is generated between two copper electrodes and utilizes helium as the plasma supporting gas. The alternating current plasma power source consists of a step-up transformer with a secondary output voltage of 14,000 V at a current of 23 mA. The chromatographic applications studied included the following: (1) the separation and selective detection of the organotin species, tributyltin chloride (TBT) and tetrabutyltin (TEBT), in environmental matrices including mussels (mytilus edullus) and sediment from Boston Harbor, industrial waste water and industrial sludge, and (2) the detection of methylcyclopentadienylmanganesetricarbonyl (MMT) and similar compounds used as gasoline additives. An ultrasonic nebulizer was utilized as a sample introduction device for aqueous solutions when the ACP was employed as an atomization source for atomic absorption spectrometry and as an excitation source for atomic emission spectrometry. Plasma diagnostic parameters studied include spatial electron number density across the discharge tube, electronic, excitation and ionization temperatures. Interference studies both in absorption and emission modes were considered. The evaluation of a computer-aided optimization program, Drylab GC, using spearmint oil and Environmental Protection Agency (EPA) standard mixture as probes is discussed. The program is used for separation optimization and prediction of gas chromatographic parameters. The program produces a relative resolution map (RRM) which guides the analyst in selecting the most favorable temperature programming rate for the separation.

  13. Scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX) and aerosol time-of-flight mass spectrometry (ATOFMS) single particle analysis of metallurgy plant emissions.

    PubMed

    Arndt, J; Deboudt, K; Anderson, A; Blondel, A; Eliet, S; Flament, P; Fourmentin, M; Healy, R M; Savary, V; Setyan, A; Wenger, J C

    2016-03-01

    The chemical composition of single particles deposited on industrial filters located in three different chimneys of an iron-manganese (Fe-Mn) alloy manufacturing plant have been compared using aerosol time-of-flight mass spectrometry (ATOFMS) and scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX). Very similar types of particles were observed using both analytical techniques. Calcium-containing particles dominated in the firing area of the sintering unit, Mn and/or Al-bearing particles were observed at the cooling area of the sintering unit, while Mn-containing particles were dominant at the smelting unit. SEM-EDX analysis of particles collected downstream of the industrial filters showed that the composition of the particles emitted from the chimneys is very similar to those collected on the filters. ATOFMS analysis of ore samples was also performed to identify particulate emissions that could be generated by wind erosion and manual activities. Specific particle types have been identified for each emission source (chimneys and ore piles) and can be used as tracers for source apportionment of ambient PM measured in the vicinity of the industrial site.

  14. Sequential cloud point extraction for the speciation of mercury in seafood by inductively coupled plasma optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    Li, Yingjie; Hu, Bin

    2007-10-01

    A novel nonchromatographic speciation technique for the speciation of mercury by sequential cloud point extraction (CPE) combined with inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. The method based on Hg 2+ was complexed with I - to form HgI 42-, and the HgI 42- reacted with the methyl green (MG) cation to form hydrophobic ion-associated complex, and the ion-associated complex was then extracted into the surfactant-rich phase of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114), which are subsequently separated from methylmercury (MeHg +) in the initial solution by centrifugation. The surfactant-rich phase containing Hg(II) was diluted with 0.5 mol L - 1 HNO 3 for ICP-OES determination. The supernatant is also subjected to the similar CPE procedure for the preconcentration of MeHg + by the addition of a chelating agent, ammonium pyrrolidine dithiocarbamate (APDC), in order to form water-insolvable complex with MeHg +. The MeHg + in the micelles was directly analyzed after disposal as describe above. Under the optimized conditions, the extraction efficiency was 93.5% for Hg(II) and 51.5% for MeHg + with the enrichment factor of 18.7 for Hg(II) and 10.3 for MeHg +, respectively. The limits of detection (LODs) were 56.3 ng L - 1 for Hg(II) and 94.6 ng L - 1 for MeHg + (as Hg) with the relative standard deviations (RSDs) of 3.6% for Hg(II) and 4.5% for MeHg + ( C = 10 μg L -1, n = 7), respectively. The developed technique was applied to the speciation of mercury in real seafood samples and the recoveries for spiked samples were found to be in the range of 93.2-108.7%. For validation, a certified reference material of DORM-2 (dogfish muscle) was analyzed and the determined values are in good agreement with the certified values.

  15. 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

    2016-09-01

    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

  16. 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

    2016-09-01

    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

  17. Particle emission from chemically enhanced electron-beam-induced etching of Si: An approach for zero-energy secondary-ion mass spectrometry

    NASA Astrophysics Data System (ADS)

    Vanhove, N.; Lievens, P.; Vandervorst, W.

    2009-01-01

    The mechanisms of particle emission resulting from electron-beam-induced etching of Si surfaces have been studied. A detailed analysis of the obtained mass spectra and kinetic-energy distributions shows that SiFx(x=0-2) species are predominantly desorbed from the surface when exposed to XeF2 etching gas and the electron beam. Based on these observations, we demonstrate a unique concept for materials analysis, termed zero-energy secondary-ion mass spectrometry, which can provide very high depth resolution and accurate near-surface profiles.

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

    NASA Astrophysics Data System (ADS)

    Ombaba, Jackson M.

    This thesis deals with the construction and evaluation of an alternating current plasma (ACP) as an element-selective detector for high resolution capillary gas chromatography (GC) and as an excitation source for atomic absorption spectrometry (AAS) and atomic emission spectrometry (AES). The plasma, constrained in a quartz discharge tube at atmospheric pressure, is generated between two copper electrodes and utilizes helium as the plasma supporting gas. The alternating current plasma power source consists of a step-up transformer with a secondary output voltage of 14,000 V at a current of 23 mA. The device exhibits a stable signal because the plasma is self-seeding and reignites itself every half cycle. A tesla coil is not required to commence generation of the plasma if the ac voltage applied is greater than the breakdown voltage of the plasma-supporting gas. The chromatographic applications studied included the following: (1) the separation and selective detection of the organotin species, tributyltin chloride (TBT) and tetrabutyltin (TEBT), in environmental matrices including mussels (Mvutilus edullus) and sediment from Boston Harbor, industrial waste water and industrial sludge, and (2) the detection of methylcyclopentadienyl manganesetricarbonyl (MMT) and similar compounds used as gasoline additives. An ultrasonic nebulizer (common room humidifier) was utilized as a sample introduction device for aqueous solutions when the ACP was employed as an atomization source for atomic absorption spectrometry and as an excitation source for atomic emission spectrometry. Plasma diagnostic parameters studied include spatial electron number density across the discharge tube, electronic, excitation and ionization temperatures. Interference studies both in absorption and emission modes were also considered. Figures of merits of selected elements both in absorption and emission modes are reported. The evaluation of a computer-aided optimization program, Drylab GC, using

  19. 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).

  20. 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). PMID:26838401

  1. 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.

  2. Inspection of non-CO2 greenhouse gases from emission sources and in ambient air by Fourier-transform-infrared-spectrometry: Measurements with FTIS-MAPS.

    PubMed

    Schäfer, K; Haus, R; Heland, J

    1994-05-01

    Infrared spectrometry is a versatile basis to analyse greenhouse gases in the atmosphere. A multicomponent air pollution software (MAPS) was developed for retrieval of gas concentrations from radiation emission as well as absorption measurements. Concentrations of CO, CH4, N2O, and H2O as well as CO2, NO, NO2, NH3, SO2, HCl, HCHO, and the temperature of warm gases are determined on-line. The analyses of greenhouse gases in gaseous emission sources and in ambient air are performed by a mobile remote sensing system using the double-pendulum interferometer K300 of the Munich company Kayser-Threde. Passive radiation measurements are performed to retrieve CO, N2O, and H2O as well as CO2, NO, SO2, and HCl concentrations in smoke stack effluents of thermal power plants and municipal incinerators and CO and H2O as well as CO2 and NO in exhausts of aircraft engines. Open-path radiation measurements are used to determine greenhouse gas concentrations at different ambient air conditions and greenhouse gas emission rates of diffusive sources as garbage deposits, open coal mining, stock farming together with additional compounds (e.g. NH3), and from road traffic together with HCHO. Some results of measurements are shown. A future task is the verification of emission cadastres by these inspection measurements.

  3. X-ray Spectrometry.

    ERIC Educational Resources Information Center

    Markowicz, Andrzej A.; Van Grieken, Rene E.

    1984-01-01

    Provided is a selective literature survey of X-ray spectrometry from late 1981 to late 1983. Literature examined focuses on: excitation (photon and electron excitation and particle-induced X-ray emission; detection (wavelength-dispersive and energy-dispersive spectrometry); instrumentation and techniques; and on such quantitative analytical…

  4. Characterization of Gas-Phase Organics Using Proton Transfer Reaction Time-of-Flight Mass Spectrometry: Cooking Emissions.

    PubMed

    Klein, Felix; Platt, Stephen M; Farren, Naomi J; Detournay, Anais; Bruns, Emily A; Bozzetti, Carlo; Daellenbach, Kaspar R; Kilic, Dogushan; Kumar, Nivedita K; Pieber, Simone M; Slowik, Jay G; Temime-Roussel, Brice; Marchand, Nicolas; Hamilton, Jacqueline F; Baltensperger, Urs; Prévôt, André S H; El Haddad, Imad

    2016-02-01

    Cooking processes produce gaseous and particle emissions that are potentially deleterious to human health. Using a highly controlled experimental setup involving a proton-transfer-reaction time-of-flight mass spectrometer (PTR-ToF-MS), we investigate the emission factors and the detailed chemical composition of gas phase emissions from a broad variety of cooking styles and techniques. A total of 95 experiments were conducted to characterize nonmethane organic gas (NMOG) emissions from boiling, charbroiling, shallow frying, and deep frying of various vegetables and meats, as well as emissions from vegetable oils heated to different temperatures. Emissions from boiling vegetables are dominated by methanol. Significant amounts of dimethyl sulfide are emitted from cruciferous vegetables. Emissions from shallow frying, deep frying and charbroiling are dominated by aldehydes of differing relative composition depending on the oil used. We show that the emission factors of some aldehydes are particularly large which may result in considerable negative impacts on human health in indoor environments. The suitability of some of the aldehydes as tracers for the identification of cooking emissions in ambient air is discussed. PMID:26766423

  5. Measurement of fugitive volatile organic compound emissions from a petrochemical tank farm using open-path Fourier transform infrared spectrometry

    NASA Astrophysics Data System (ADS)

    Wu, Chang-Fu; Wu, Tzong-gang; Hashmonay, Ram A.; Chang, Shih-Ying; Wu, Yu-Syuan; Chao, Chun-Ping; Hsu, Cheng-Ping; Chase, Michael J.; Kagann, Robert H.

    2014-01-01

    Fugitive emission of air pollutants is conventionally estimated based on standard emission factors. The Vertical Radial Plume Mapping (VRPM) technique, as described in the US EPA OTM-10, is designed to measure emission flux by directly monitoring the concentration of the plume crossing a vertical plane downwind of the site of interest. This paper describes the evaluation results of implementing VRPM in a complex industrial setting (a petrochemical tank farm). The vertical plane was constructed from five retroreflectors and an open-path Fourier transform infrared spectrometer. The VRPM configuration was approximately 189.2 m in width × 30.7 m in height. In the accompanying tracer gas experiment, the bias of the VRPM estimate was less than 2% and its 95% confidence interval contained the true release rate. Emission estimates of the target VOCs (benzene, m-xylene, o-xylene, p-xylene, and toluene) ranged from 0.86 to 2.18 g s-1 during the 14-day field campaign, while estimates based on the standard emission factors were one order of magnitude lower, possibly leading to an underestimation of the impact of these fugitive emissions on air quality and human health. It was also demonstrated that a simplified 3-beam geometry (i.e., without one dimensional scanning lines) resulted in higher uncertainties in the emission estimates.

  6. Analysis of non-regulated vehicular emissions by extractive FTIR spectrometry: tests on a hybrid car in Mexico City

    NASA Astrophysics Data System (ADS)

    Reyes, F.; Grutter, M.; Jazcilevich, A.; González-Oropeza, R.

    2006-07-01

    A methodology to acquire valuable information on the chemical composition and evolution of vehicular emissions is presented. The analysis of the gases is performed by passing a constant flow of a sample gas from the tail-pipe into a 10 L multi-pass cell. The absorption spectra within the cell are obtained using an FTIR spectrometer at 0.5 cm-1 resolution along a 13.1 m optical path. Additionally, the total flow from the exhaust is continuously measured from a differential pressure sensor on a Pitot tube installed at the exit of the exhaust. This configuration aims to obtain a good speciation capability by coadding spectra during 30 s and reporting the emission (in g/km) of key and non-regulated pollutants, such as CO2, CO, NO, SO2, NH3, HCHO, NMHC, during predetermined driving routines. The advantages and disadvantages of increasing the acquisition frequency, as well as the effect of other parameters such as spectral resolution, cell volume and flow rate, are discussed. With the aim of testing and evaluating the proposed technique, experiments were performed on a dynamometer running FTP-75 and typical driving cycles of the Mexico City Metropolitan Area (MCMA) on a Toyota Prius hybrid vehicle. This car is an example of recent automotive technology to reach the market dedicated to reduce emissions and therefore pressing the need of low detection techniques. This study shows the potential of the proposed technique to measure and report in real time the emissions of a large variety of pollutants, even from a super ultra-low emission vehicle (SULEV). The emissions of HC's, NOx, CO and CO2 obtained here are similar to experiments performed in other locations with the same vehicle model. Some differences suggest that an inefficient combustion process and type of gasoline used in the MCMA may be partly responsible for lower CO2 and higher CO and NO emission factors. Also, a fast reduction of NO emission to very low values is observed after cold ignition, giving rise to

  7. Identification of lead and other elements in ceramic glazes and housewares by 109Cd-induced X-ray fluorescence emission spectrometry.

    PubMed

    Anderson, D L; Cunningham, W C; Lindstrom, T R; Olmez, I

    1995-01-01

    Radioisotope x-ray fluorescence spectrometry was investigated as a potential screening method for Pb and other elements in housewares. Thirty-six commercial houseware items and 87 ceramic test tiles (85 fired with hobby glazes and 2 blank bisques) were examined qualitatively for the presence of Pb by using 109Cd-induced L x-ray fluorescence emission spectrometry. For the housewares, the technique provided fast, nondestructive analysis of areas with about 10 cm diameters (general regions) to about 4 mm diameters (isolated design regions). Pb was found in 25 of 28 ceramicware items, in all 8 other housewares, and in all the test-tile glazes above the limit of detection of 1 count per second (cps) for Pb L beta x-rays. For housewares, Pb identification did not always correspond to Pb leachability. For 68 test-tile glazes labeled as containing Pb (39 of which were also labeled 'dinnerware safe' or 'safe for food containers'), count rates ranged from 290 to 730 cps, whereas for the other 17 glazes labeled (with one exception) 'non-toxic,' much lower count rates (5-61 cps) were obtained. Other elements found in the housewares or test glazes were As, Au, Ca, Co, Cr, Cu, Fe, Mn, Nb, Ni, Rb, Sr, Y, Zn, and Zr.

  8. Current Opportunities and Challenges of Magnetic Resonance Spectroscopy, Positron Emission Tomography, and Mass Spectrometry Imaging for Mapping Cancer Metabolism In Vivo

    PubMed Central

    Chung, Yuen-Li

    2014-01-01

    Cancer is known to have unique metabolic features such as Warburg effect. Current cancer therapy has moved forward from cytotoxic treatment to personalized, targeted therapies, with some that could lead to specific metabolic changes, potentially monitored by imaging methods. In this paper we addressed the important aspects to study cancer metabolism by using image techniques, focusing on opportunities and challenges of magnetic resonance spectroscopy (MRS), dynamic nuclear polarization (DNP)-MRS, positron emission tomography (PET), and mass spectrometry imaging (MSI) for mapping cancer metabolism. Finally, we highlighted the future possibilities of an integrated in vivo PET/MR imaging systems, together with an in situ MSI tissue analytical platform, may become the ultimate technologies for unraveling and understanding the molecular complexities in some aspects of cancer metabolism. Such comprehensive imaging investigations might provide information on pharmacometabolomics, biomarker discovery, and disease diagnosis, prognosis, and treatment response monitoring for clinical medicine. PMID:24724090

  9. A Simple But Comprehensive Methodology To Determine Gas-Phase Emissions Of Motor Vehicles With Extractive FTIR Spectrometry

    NASA Astrophysics Data System (ADS)

    Reyes, F. M.; Jaczilevich, A.; Grutter, M. A.; Huerta, M. A.; Rincón, P.; Rincón, R.; González, R.

    2004-12-01

    In this contribution, a methodology to acquire valuable information on the chemical composition and evolution of vehicular emissions is presented. With this innovative experimental set-up, it is possible to obtain real-time emissions of the combustion products without the need of dilution or sample collection. Key pollutants such as CO, CO2, H2CO, CH4, NO, N2O, NH3, SO2, CH3OH, acetylene, ethylene, ethane and total hydrocarbons, most of which are not regulated nor measured by current emissions control programs, can be accurately monitored with a single instrument. An FTIR spectrometer is used for the analysis of a constant flow of sample gas from the tail-pipe into a stainless-steel cylindrical cell of constant volume.(1) The cell is heated to 185 °C to avoid condensation, the pressure is kept constant and a multi-pass optical arrangement(2)is used to transmit the modulated infrared beam several times to improve the sensitivity. The total flow from the exhaust used for calculating the emission can be continuously determined from the differential pressure measurements from a "Pitot" tube calibrated against a hot-wire devise. This simple methodology is proposed for performing state-of-the-art evaluations on the emission behavior of new technologies, reformulated fuels and emission control devices. The results presented here were performed on a dynamometer running FTP-75 and driving cycles typical for Mexico City.(3,4) References 1. Grutter M. "Multi-Gas Analysis using FTIR Spectroscopy over Mexico City." Atmosfera 16, 1-16 (2003). 2. White J.U. "Long optical paths of large aperture. J. Opt. Soc. Am., 32, 285-288 (1942). 3. Santiago Cruz L. and P.I. Rincón. "Instrumentation of the Emission Control Laboratory at the Engineering School of the National Autonomous University of Mexico." Instrumentation and Development 4, 19-24, (2000). 4. González Oropeza R. and A. Galván Zacarías. "Desarrollo de ciclos de manejo característicos de la Ciudad de México." Memorias

  10. Polycyclic aromatic hydrocarbon emissions in diesel exhaust using gas chromatography-mass spectrometry with programmed temperature vaporization and large volume injection

    NASA Astrophysics Data System (ADS)

    Vieira de Souza, Carolina; Corrêa, Sergio Machado

    2015-02-01

    Diesel engines are significant sources of Polycyclic Aromatic Compounds (PAHs) in urban atmospheres. These compounds are widely known for their carcinogenic potential and mutagenic properties. In this study, a method was developed for the analysis of 16 priorities PAHs using gas chromatography-mass spectrometry (GC-MS) with programmable temperature vaporizer large volume injection (PTV-LVI), which allowed to be obtained detection limits below 2.0 ng mL-1. This method was evaluated in samples from stratified particulate matter and gas phase from the emissions of diesel vehicle employing diesel commercial S10 (sulfur 10 mg L-1) and B5 (biodiesel 5% v/v). A sampling system that does not employ exhaust products dilution was used to evaluate the PAHs gas-particle partition. Six PAHs were identified in extracts and gas-phase PAHs took percentage of 80% in the total PAHs emissions. The sampling system without dilution not caused a strong nucleation/condensation of the most volatile PAHs. PAHs size-particle distribution was found in higher levels in the accumulation mode.

  11. Gaseous and particulate composition of fresh and aged emissions of diesel, RME and CNG buses using Chemical Ionization Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Psichoudaki, Magda; Le Breton, Michael; Hallquist, Mattias; Watne, Ågot; Hallquist, Asa

    2016-04-01

    Urban air pollution is becoming a significant global problem, especially for large cities around the world. Traffic emissions contribute significantly to both elevated particle concentrations and to gaseous pollutants in cities. The latter also have the potential of forming more particulate mass via their photochemical oxidation in the atmosphere. The International Agency for Research on Cancer and the US EPA have characterised diesel exhausts as a likely human carcinogen that can also contribute to other health problems. In order to meet the challenges with increased transportation and enhanced greenhouse gas emissions, the European Union have decided on a 10% substitution of traditional fuels in the road transport sector by alternative fuels (e.g. biodiesel, CNG) before the year 2020. However, it is also important to study the influence of fuel switches on other primary pollutants as well as the potential to form secondary aerosol mass. This work focuses on the characterisation of the chemical composition of the gas and the condensed phase of fresh bus emissions during acceleration, in order to mimic the exhaust plume that humans would inhale under realistic conditions. In addition, photochemical aging of the exhaust emissions was achieved by employing a Potential Aerosol Mass (PAM) flow reactor, allowing the characterization of the composition of the corresponding aged emissions. The PAM reactor uses UV lamps and high concentrations of oxidants (OH radicals and O3) to oxidize the organic species present in the chamber. The oxidation that takes place within the reactor can be equivalent to up to one week of atmospheric oxidation. Preliminary tests showed that the oxidation employed in these measurements corresponded to a range from 4 to 8 days in the atmosphere. During June and July 2015, a total of 29 buses, 5 diesel, 13 CNG and 11 RME (rapeseed methyl ester), were tested in two different locations with limited influence from other types of emissions and traffic

  12. Flowing Liquid Anode Atmospheric Pressure Glow Discharge as an Excitation Source for Optical Emission Spectrometry with the Improved Detectability of Ag, Cd, Hg, Pb, Tl, and Zn.

    PubMed

    Greda, Krzysztof; Swiderski, Krzysztof; Jamroz, Piotr; Pohl, Pawel

    2016-09-01

    A novel atmospheric pressure glow discharge generated in contact with a flowing liquid anode (FLA-APGD) was developed as the efficient excitation source for the optical emission spectrometry (OES) detection. Differences in the appearance and the electrical characteristic of the FLA-APGD and a conventional system operated with a flowing liquid cathode (FLC-APGD) were studied in detail and discussed. Under the optimal operating conditions for the FLA-APGD, the emission from the analytes (Ag, Cd, Hg, Pb, Tl, and Zn) was from 20 to 120 times higher as compared to the FLC-APGD. Limits of detections (LODs) established with a novel FLA-APGD system were on average 20 times better than those obtained for the FLC-APGD. A further improvement of the LODs was achieved by reducing the background shift interferences and, as a result, the LODs for Ag, Cd, Hg, Pb, Tl, and Zn were 0.004, 0.040, 0.70, 1.7, 0.035, and 0.45 μg L(-1), respectively. The precision of the FLA-APGD-OES method was evaluated to be within 2-5% (as the relative standard deviation of the repeated measurements). The method found its application in the determination of the content of Ag, Cd, Hg, Pb, Tl, and Zn in a certified reference material (CRM) of Lobster hepatopancreas (TORT-2), four brass samples as well as mineral water and tea leaves samples spiked with the analytes. In the case of brass samples, a reference method, i.e., inductively coupled plasma optical emission spectrometry (ICP-OES) was used. A good agreement between the results obtained with FLA-APGD-OES and the certified values for the CRM TORT-2 as well as the reference values obtained with ICP-OES for the brass samples was revealed, indicating the good accuracy of the proposed method. The recoveries obtained for the spiked samples of mineral water and tea leaves were within the range of 97.5-102%. PMID:27476678

  13. Determination of dissolved boron in fresh, estuarine, and geothermal waters by d.c. argon-plasma emission spectrometry

    USGS Publications Warehouse

    Ball, J.W.; Thompson, J.M.; Jenne, E.A.

    1978-01-01

    A d.c. argon-plasma emission spectrometer is used to determine dissolved boron in natural (fresh and estuarine) water samples. Concentrations ranged from 0.02 to 250 mg l-1. The emission-concentration function is linear from 0.02 to 1000 mg l-1. Achievement of a relative standard deviation of ??? 3% requires frequent restandardization to offset sensitivity changes. Dilution may be necessary to overcome high and variable electron density caused by differences in alkali-metal content and to avoid quenching of the plasma by high solute concentrations of sodium and other easily ionized elements. The proposed method was tested against a reference method and found to be more sensitive, equally or more precise and accurate, less subject to interferences, with a wider linear analytical range than the carmine method. Analyses of standard reference samples yielded results in all cases within one standard deviation of the means. ?? 1978.

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

    PubMed

    García-Salgado, S; Quijano, M A; Bonilla, M M

    2012-02-10

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

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

    PubMed

    García-Salgado, S; Quijano, M A; Bonilla, M M

    2012-02-10

    Twelve commercially available edible marine algae from France, Japan and Spain and the certified reference material (CRM) NIES No. 9 Sargassum fulvellum were analyzed for total arsenic and arsenic species. Total arsenic concentrations were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) after microwave digestion and ranged from 23 to 126 μg g(-1). Arsenic species in alga samples were extracted with deionized water by microwave-assisted extraction and showed extraction efficiencies from 49 to 98%, in terms of total arsenic. The presence of eleven arsenic species was studied by high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation atomic-fluorescence spectrometry (HPLC-(UV)-HG-AFS) developed methods, using both anion and cation exchange chromatography. Glycerol and phosphate sugars were found in all alga samples analyzed, at concentrations between 0.11 and 22 μg g(-1), whereas sulfonate and sulfate sugars were only detected in three of them (0.6-7.2 μg g(-1)). Regarding arsenic toxic species, low concentration levels of dimethylarsinic acid (DMA) (<0.9 μg g(-1)) and generally high arsenate (As(V)) concentrations (up to 77 μg g(-1)) were found in most of the algae studied. The results obtained are of interest to highlight the need to perform speciation analysis and to introduce appropriate legislation to limit toxic arsenic species content in these food products. PMID:22244135

  16. Inductively coupled plasma spectrometry: Noise characteristics of aerosols, application of generalized standard additions method, and Mach disk as an emission source

    SciTech Connect

    Shen, Luan

    1995-10-06

    This dissertation is focused on three problem areas in the performance of inductively coupled plasma (ICP) source. The noise characteristics of aerosols produced by ICP nebulizers are investigated. A laser beam is scattered by aerosol and detected by a photomultiplier tube and the noise amplitude spectrum of the scattered radiation is measured by a spectrum analyzer. Discrete frequency noise in the aerosol generated by a Meinhard nebulizer or a direct injection nebulizer is primarily caused by pulsation in the liquid flow from the pump. A Scott-type spray chamber suppresses white noise, while a conical, straight-pass spray chamber enhances white noise, relative to the noise seen from the primary aerosol. Simultaneous correction for both spectral interferences and matrix effects in ICP atomic emission spectrometry (AES) can be accomplished by using the generalized standard additions method (GSAM). Results obtained with the application of the GSAM to the Perkin-Elmer Optima 3000 ICP atomic emission spectrometer are presented. The echelle-based polychromator with segmented-array charge-coupled device detectors enables the direct, visual examination of the overlapping lines Cd (1) 228.802 nm and As (1) 228.812 nm. The slit translation capability allows a large number of data points to be sampled, therefore, the advantage of noise averaging is gained. An ICP is extracted into a small quartz vacuum chamber through a sampling orifice in a water-cooled copper plate. Optical emission from the Mach disk region is measured with a new type of echelle spectrometer equipped with two segmented-array charge-coupled-device detectors, with an effort to improve the detection limits for simultaneous multielement analysis by ICP-AES.

  17. Inductively coupled plasma-optical emission spectrometry/mass spectrometry for the determination of Cu, Ni, Pb and Zn in seawater after ionic imprinted polymer based solid phase extraction.

    PubMed

    Otero-Romaní, Jacobo; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Pilar; Martin-Esteban, Antonio

    2009-08-15

    The capabilities of a synthesized ionic imprinted polymer (IIP), originally prepared for Ni recognition/pre-concentration from seawater, have been evaluated for other trace elements pre-concentration. The polymer has been synthesized by the precipitation polymerization technique using a ternary pre-polymerization complex formed by the template (Ni), the monomer (2-(diethylamino) ethyl methacrylate, DEM) and a non-vinylated chelating agent (8-hydroxyquinoline, 8-HQ). Since the complexing agent (8-HQ) is trapped into the polymeric matrix, but is not linked to the polymer chains, specific interactions between the functional groups (present in the monomer and the complexing agent) and other trace elements rather than Ni may occur. Results have shown that the IIP offers imprinting properties for the template (Ni(II)) and also for Cu(II), Pb(II), Zn(II), As(V) and Cd(II), with analytical recoveries close to 100% for all elements except for As(V) and Cd(II) (around 70%), whereas the non-imprinted polymer (NIP) did not show affinity for any trace element. In addition, the polymer does not interact with alkaline or alkaline-earth metals, so Na, K, Mg and Ca from the seawater salt matrix could be effectively removed. Variables affecting the IIP-solid phase extraction (SPE) process (pH, load flow rate and concentration and volume of the eluting solution) were completely studied. Inductively coupled plasma-optical emission spectrometry (ICP-OES) and inductively coupled plasma-mass spectrometry (ICP-MS) have been used as multi-element detectors. Acidified seawater samples must only be treated to fix an alkaline pH (8.5+/-0.5) and passed through IIP-SPE cartridges. After seawater sample loading (250 mL), analytes were eluted with 2.5 mL of 2.0M nitric acid, offering a pre-concentration factor of 100. Therefore, the limits of detection (LODs) of the method were 0.14, 0.15, 0.18 and 0.03 microg L(-1), for Ni, Cu, Pb and Zn, respectively, when using ICP-OES detection and 0.0022, 0

  18. Miniaturized dielectric barrier discharge carbon atomic emission spectrometry with online microwave-assisted oxidation for determination of total organic carbon.

    PubMed

    Han, Bingjun; Jiang, Xiaoming; Hou, Xiandeng; Zheng, Chengbin

    2014-07-01

    A simple, rapid, and portable system consisted of a laboratory-built miniaturized dielectric barrier discharge atomic emission spectrometer and a microwave-assisted persulfate oxidation reactor was developed for sensitive flow injection analysis or continuous monitoring of total organic carbon (TOC) in environmental water samples. The standard/sample solution together with persulfate was pumped to the reactor to convert organic compounds to CO2, which was separated from liquid phase and transported to the spectrometer for detection of the elemental specific carbon atomic emission at 193.0 nm. The experimental parameters were systematically investigated. A limit of detection of 0.01 mg L(-1) (as C) was obtained based on a 10 mL sample injection volume, and the precision was better than 6.5% (relative standard deviation, RSD) at 0.1 mg L(-1). The system was successfully applied for TOC analysis of real environmental water samples. The obtained TOC value of 30 test samples agreed well with those by the standard high-temperature combustion coupled nondispersive infrared absorption method. Most importantly, the system showed good capability of in situ continuous monitoring of total organic carbon in environmental water.

  19. Determination of metal-cofactors in enzyme complexes by total-reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Wittershagen, A.; Rostam-Khani, P.; Klimmek, O.; Groß, R.; Zickermann, V.; Zickermann, I.; Gemeinhardt, S.; Kröger, A.; Ludwig, B.; Kolbesen, B. O.

    1997-07-01

    The determination of metal-cofactors and their molar concentrations is an important requirement for the characterisation of metalloproteins and a challenge regarding the capabilities of trace analytical methods. In this respect, total-reflection X-ray fluorescence spectrometry offers many advantages for the determination of trace elements in enzymes, as compared to other well known analytical techniques such as flame atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry (ICP-AES), because of the significantly smaller amounts of sample required. Without any decomposition, elements like P, S, Fe, Ni, Cu, Zn, Mn and Mo could be determined with high accuracy, in spite of the large bio-organic matrix. The enzymes (polysulphide reductase and hydrogenase of the rumen bacterium Wolinella succinogenes, and the cytochrome c oxidase and quinol oxidase of the soil bacterium Paracoccus denitrificans) were transferred from their usual salt-buffer into a solution of 100 mmol l -1 tris(hydroxymethyl)aminomethane (tris)-acetate containing an appropriate detergent. By this procedure, an improved signal-to-noise ratio is obtained. The polysulphide reductase was found to contain copper as a hitherto existing unknown cofactor. The enzyme contains a stretch of amino acids that are typical of copper proteins and thus confirm the presence of this element. Furthermore, the data concerning cytochrome c oxidase from Paracoccus denitrificans are in good agreement with published values obtained by ICP-AES. Also, results from measurements with the quinol oxidase from the same bacterium agree with the expected values. The investigations lead to the conclusion that the method is well suited to the quantitative determination of metals in enzymes, in particular their molar fractions, and requires only small amounts of the biological sample without any extensive pretreatment.

  20. Identification and differentiation of the red ink entries of seals on document by laser desorption ionization mass spectrometry.

    PubMed

    Wang, Xiang-Feng; Zhang, Yun; Wu, Yao; Yu, Jing; Xie, Meng-Xia

    2014-03-01

    The establishment of approaches for the differentiation of the ink entries of seals on paper can provide evidence to authenticate the related documents and can play a key role in judicial expertise. The identification and discrimination method for 38 red ink entries of seals on paper has been investigated using laser desorption ionization mass spectrometry (LDI-MS). Six dye components for the ink pastes of seals, Scarlet powder (SP), Bronze Red C (BR), Fast Red R (FR), Basic Violet 3 (BV3), Pigment Red 22 (PR22) and Pigment Red 112 (PR112), have been identified by their LDI-MS spectra, and the results have been confirmed by electrospray ionization quadruple-time of flight mass spectrometry (QTOF-ESI-MS/MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The 38 ink entries were classified into six groups based on the presence or the absence of the pigments in their positive and negative LDI-MS spectra, and the discrimination power (DP) was calculated to be about 82%. The ink entries within each group were further differentiated from the relative peak areas (RPA) of the fragments for the pigments and the profile of their LDI-MS spectra, and thus the DP was increased to 98%. All the 38 ink entries could be discriminated (the DP was 100%), if including the contribution of unknown peaks. Compared with the results obtained by the FTIR and Raman methods, the established LDI-MS approach could provide more information of the dye components in the ink entries. The results showed that the developed LDI-MS method is powerful, sensitive and rapid and can directly differentiate the red ink entries of seals from paper substrates, thus offering a novel approach to judge the authenticity of documents.

  1. Speciation of inorganic and organometallic compounds in solid biological samples by thermal vaporization and plasma emission spectrometry

    SciTech Connect

    Hanamura, S.; Smith, B.W.; Winefordner, J.D.

    1983-11-01

    By means of thermal vaporization, inorganic, organic, and metallorganic species are separated and elemental emission in a microwave plasma is detected as a function of vaporization temperature. Solid samples of 250 mg or more are used to avoid problems with sample heterogeneity. The precision of characteristic appearance temperatures is +/-2/sup 0/C. The single electrode atmosphere pressure microwave plasma system is extremely tolerant to the introduction of water, organic solvents, and air. The measurement system contained a repetition wavelength scan device to allow background correction. The plasma temperature was 5500 K. The system was used to measure C, H, N, O, and Hg in orchard leaves and in tuna fish. 9 figures, 5 tables.

  2. Determination of Se in biological samples by axial view inductively coupled plasma optical emission spectrometry after digestion with aqua regia and on-line chemical vapor generation

    NASA Astrophysics Data System (ADS)

    dos Santos, Éder José; Herrmann, Amanda Beatriz; de Caires, Suzete Kulik; Frescura, Vera Lúcia Azzolin; Curtius, Adilson José

    2009-06-01

    A simple and fast method for the determination of Se in biological samples, including food, by axial view inductively coupled plasma optical emission spectrometry using on-line chemical vapor generation (CVG-ICP OES) is proposed. The concentrations of HCl and NaBH 4, used in the chemical vapor generation were optimized by factorial analysis. Six certified materials (non-fat milk powder, lobster hepatopancreas, human hair, whole egg powder, oyster tissue, and lyophilised pig kidney) were treated with 10 mL of aqua regia in a microwave system under reflux for 15 min followed by additional 15 min in an ultrasonic bath. The solutions were transferred to a 100 mL volumetric flask and the final volume was made up with water. The Se was determined directly in these solutions by CVG-ICP OES, using the analytical line at 196.026 nm. Calibration against aqueous standards in 10% v/v aqua regia in the concentration range of 0.5-10.0 µg L - 1 Se(IV) was used for the analysis. The quantification limit, considering a 0.5 g sample weight in a final volume of 100 mL - 1 was 0.10 µg g - 1. The obtained concentration values were in agreement with the total certified concentrations, according to the t-test for a 95% confidence level.

  3. Comparison of parallel flow and concentric micronebulizers for elemental determination in lubricant oil, residual fuel oil and biodiesel by Inductively Coupled Plasma Optical Emission Spectrometry

    NASA Astrophysics Data System (ADS)

    de Souza, Jefferson R.; dos Santos, Eider Fernando; Duyck, Christiane B.; Saint'Pierre, Tatiana D.

    2011-05-01

    Two micronebulizers, PFA-100 and Miramist, were evaluated using a method for elemental determination by Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) in lubricant and residual fuel oils diluted in xylene. The facility and speed of direct sample dilution in organic solvents, without additional pretreatment, combined with the multielemental capacity and robustness of ICP OES are advantageous. The operational conditions were optimized through factorial design. Improvement in the signal-to-background ratio was observed for Ag, Al, B, Ba, Ca, Cr, Cu, Fe, Mn, Si, Ti and V. Higher sensitivity was obtained with the PFA-100 micronebulizer, although the limits of detection (LOD) obtained for both micronebulizers were similar, between 0.3 μg kg -1 (Mg) and 18 μg kg -1 (Ni). The certified reference materials NIST 1634c and NIST 1085b were used for method validation and good recoveries were obtained with values between 93% (Pb) and 102% (P) for PFA-100 and 90% (Pb) and 103% (P) for Miramist. The method was also validated for analysis of biodiesel samples by recovery tests, with results from 89% to 103%. The proposed method was employed for the analysis of crude oil, lubricant oil and biodiesel from different raw materials.

  4. Reduction of Argon Consumption to Less than 2 L min(-1) by Gas Recycling in Inductively Coupled Plasma Optical Emission Spectrometry.

    PubMed

    Tirk, Paul; Wolfgang, Matthias; Wiltsche, Helmar

    2016-07-19

    An innovative interface between the torch and the entrance optics for inductively coupled plasma optical emission spectrometry (ICP-OES) is proposed. This system is capable of collecting all argon which was initially supplied to the torch, cooling and cleaning it and feeding most of the argon back to the outer gas port of the torch. Thereby, the total argon consumption could be reduced from 14 to 1.4 L min(-1) using a standard torch and without restricting the rf power. The excitation- and rotational temperature of the plasma were identical when comparing the traditional setup with the enclosed plasma interface. However, the limits of detection (LOD) and limits of quantification (LOQ) of 27 elements investigated were degraded about 5-fold, though this fact can be expected to stem from a change of the observed zone in the plasma caused by the slight overpressure of 2000 Pa within the interface. Though the enclosed plasma interface was located close to the load coil, the rf power coupled to the interface was well below 1 W and no rf arcing was observed for two different rf generator designs.

  5. Investigation on the erosion/deposition processes in the ITER-like wall divertor at JET using glow discharge optical emission spectrometry technique

    NASA Astrophysics Data System (ADS)

    Ruset, C.; Grigore, E.; Luculescu, C.; Tiseanu, I.; Likonen, J.; Mayer, M.; Rubel, M.; Matthews, G. F.; contributors, JET

    2016-02-01

    As a complementary method to Rutherford back scattering (RBS), glow discharge optical emission spectrometry (GDOES) was used to investigate the depth profiles of W, Mo, Be, O and C concentrations into marker coatings (CFC/Mo/W/Mo/W) and the substrate of divertor tiles up to a depth of about 100 μm. A number of 10 samples cored from particular areas of the divertor tiles were analyzed. The results presented in this paper are valid only for those areas and they cannot be extrapolated to the entire tile. Significant deposition of Be was measured on Tile 3 (near to the top), Tile 6 (at about 40 mm from the innermost edge) and especially on Tile 0 (HFGC). Preliminary experiments seem to indicate a penetration of Be through the pores and imperfections of CFC material up to a depth of 100 μm in some cases. No erosion and a thin layer of Be (<1 μm) was detected on Tiles 4, 7 and 8. On Tile 1 no erosion was found at about 1/3 from bottom.

  6. Simultaneous determination of macro and trace elements in biological reference materials by microwave induced plasma optical emission spectrometry with slurry sample introduction

    NASA Astrophysics Data System (ADS)

    Matusiewicz, Henryk; Golik, Bartosz

    2004-05-01

    A slurry sampling technique (SST) has been utilized for simultaneous multi-element analysis by microwave-induced plasma optical emission spectrometry (MIP-OES). Slurry samples from a spray chamber are fed directly into the microwave cavity-torch assembly (power 300 W) with no desolvation apparatus. The performance of SST-MIP-OES was demonstrated by the determination of macro (Na, K, Ca, Mg, P) and trace (Cd, Cu, Mn, Sr, Zn) elements in three biological certified reference materials using a V-groove, clog-free Babington-type nebulizer. Slurry concentrations up to 1% m/v (particles <20 μm), prepared in 10% HNO 3 (pH 1.2) containing 0.01% of Triton X-100, were used with calibration by the standard additions method. The method offers relatively good precision (R.S.D. ranged from 7 to 11%) with measured concentrations being in satisfactory agreement with certified values for NRCC TORT-1 (Lobster hepatopancreas), NRCC LUTS-1 (Lobster hepatopancreas) and IAEA-153 (Milk powder). The concentrations of Na, K, Ca, Mg, P and Cd, Cu, Mn, Sr, Zn were determined in the range 90-22 000 μg/g and 1-420 μg/g, respectively. The method could be useful as a routine procedure.

  7. 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.

  8. Assessment of trace aluminium content in parenteral solutions by combined cloud point preconcentration-flow injection inductively coupled plasma optical emission spectrometry.

    PubMed

    Sombra, Lorena L; Luconi, Marta O; Fernández, Liliana P; Olsina, Roberto A; Silva, María F; Martínez, Luis D

    2003-01-01

    A micelle-mediated phase separation without added chelating agents to preconcentrate trace levels of aluminium in parenteral solutions as a prior step to its determination by flow injection inductively coupled plasma optical emission spectrometry has been developed. The enrichment step is based on the cloud point extraction of aluminium with the non-ionic surfactant polyethyleneglycolmono-p-nonylphenylether (PONPE 7.5). The chemical variables affecting the sensitivity of the extractive-spectrometric procedure were studied in detail. After optimization, a preconcentration factor of 200 and a %E higher than 99.9 were achieved. The detection limit (DL) value of aluminium for the preconcentration of 50 ml of parenteral solution was 0.25 microgl(-1). The calibration graph using the preconcentration system for aluminium was linear with a correlation coefficient of 0.9997 at levels near the DLs up to at least 200 microgl(-1). The developed hyphenated assay, which thoroughly satisfies the typical requirements for pharmaceutical control processes, is appropriate to monitor the aluminium concentration in parenteral nutrition.

  9. Monitoring of volatile compound emissions during dry anaerobic digestion of the Organic Fraction of Municipal Solid Waste by Proton Transfer Reaction Time-of-Flight Mass Spectrometry.

    PubMed

    Papurello, Davide; Soukoulis, Christos; Schuhfried, Erna; Cappellin, Luca; Gasperi, Flavia; Silvestri, Silvia; Santarelli, Massimo; Biasioli, Franco

    2012-12-01

    Volatile Organic Compounds (VOCs) formed during anaerobic digestion of aerobically pre-treated Organic Fraction of Municipal Solid Waste (OFMSW), have been monitored over a 30 day period by a direct injection mass spectrometric technique: Proton Transfer Reaction Time-of-Flight Mass Spectrometry (PTR-ToF-MS). Most of the tentatively identified compounds exhibited a double-peaked emission pattern which is probably the combined result from the volatilization or oxidation of the biomass-inherited organic compounds and the microbial degradation of organic substrates. Of the sulfur compounds, hydrogen sulfide had the highest accumulative production. Alkylthiols were the predominant sulfur organic compounds, reaching their maximum levels during the last stage of the process. H(2)S formation seems to be influenced by the metabolic reactions that the sulfur organic compounds undergo, such as a methanogenesis induced mechanism i.e. an amino acid degradation/sulfate reduction. Comparison of different batches indicates that PTR-ToF-MS is a suitable tool providing information for rapid in situ bioprocess monitoring. PMID:23079412

  10. Determination of traces of uranium and thorium in titanium and copper used for the construction of the Russian Emission Detector 100 by inductively coupled plasma mass spectrometry.

    PubMed

    Poteshin, Sergey S; Sysoev, Alexey A; Lagunov, Sergey S; Sereda, Andrei; Sosnovtsev, Valery V; Bolozdynya, Alexander I; Efremenko, Yuriy B

    2015-01-01

    The Russian Emission Detector 100 (RED-100) under construction at the National Research Nuclear University MEPhI (Moscow Engineering Physics Institute) is designed to detect the presently undiscovered effect of coherent neutrino scattering. One of the factors limiting the sensitivity of the detector is the spontaneous decay of uranium and thorium in the detector materials. Radioactive impurities in detector materials at levels of parts per billion can significantly affect the sensitivity. Five random samples of titanium and one of copper from materials used in the construction of the detector were selected for assay. The concentration of (232)Th and (238)U were measured by inductively coupled plasma mass spectrometry (ICP- MS) in solid titanium using both: solutions in acids and direct sampling by laser ablation (LA-ICP-MS). The LA- ICP-MS method allowed us to determine (238)U and (232)Th at subnanogram per gram levels. This method is much faster than ICP-MS with liquid injection. The titanium samples studied have impurities in the range between 1 ng g(-1) and 21 ng g(-1) for (238)U and 3 ng g(-1) and 31 ng g(-1) for (232)Th. In copper we set upper limits of 0.4 ng g(-1) for (238)U and 1 ng g(-1)for (232)Th. The total activity of the cryostat constructed from materials studied was estimated to be 43 Bq.

  11. Imaging of elements in leaves of tobacco by solid sampling-electrothermal vaporization-inductively coupled plasma-optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    Masson, Pierre

    2014-12-01

    Plants take up and store elements according to the environment in which they are growing. Because plants are at the base of the food chain, the determination of essential elements or toxic elements in plant materials is of importance. However, it is assumed that the element content determined on selected tissues may provide more specific information than that derived from the whole plant analysis. In this work, we assessed the feasibility of solid sampling-electrothermal vaporization-inductively coupled plasma-optical emission spectrometry analyses for quantitative imaging of Cd and Mg in plant leaves. Leaves of tobacco (Nicotiana tabacum) were selected to be used as samples. To produce a two dimensional image, sections cut from leaf samples were analyzed. Cellulose doped with multi-element solution standards was used as calibration samples. Two certified reference materials (NIST SRM 1547 Peach Leaves and NIST SRM 1573a Tomato leaves) were used to verify the accuracy of measurements with good agreement between the measured concentrations and the certified values. Quantitative imaging revealed the inhomogeneous distribution of the selected elements. Excess of Cd and Mg tended to be focused on peripheral regions and the tip of the leaf.

  12. Simultaneous extraction and preconcentration of uranium and thorium in aqueous samples by new modified mesoporous silica prior to inductively coupled plasma optical emission spectrometry determination.

    PubMed

    Yousefi, Seyed Reza; Ahmadi, Seyed Javad; Shemirani, Farzaneh; Jamali, Mohammad Reza; Salavati-Niasari, Masoud

    2009-11-15

    A new synthesized modified mesoporous silica (MCM-41) using 5-nitro-2-furaldehyde (fural) was applied as an effective sorbent for the solid phase extraction of uranium(VI) and thorium(IV) ions from aqueous solution for the measurement by inductively coupled plasma optical emission spectrometry (ICP OES). The influences of some analytical parameters on the quantitative recoveries of the analyte ions were investigated in batch method. Under optimal conditions, the analyte ions were sorbed by the sorbent at pH 5.5 and then eluted with 1.0 mL of 1.0 mol L(-1) HNO(3). The preconcentration factor was 100 for a 100mL sample volume. The limits of detection (LOD) obtained for uranium(VI) and thorium(IV) were 0.3 microg L(-1). The maximum sorption capacity of the modified MCM-41 was found to be 47 and 49 mg g(-1) for uranium(VI) and thorium(IV), respectively. The sorbent exhibited good stability, reusability, high adsorption capacity and fast rate of equilibrium for sorption/desorption of uranium and thorium ions. The applicability of the synthesized sorbent was examined using CRM and real water samples. PMID:19782216

  13. Multi-element analysis by inductively coupled plasma optical emission spectrometry of airborne particulate matter collected with a low-pressure cascade impactor.

    PubMed

    Robache, A; Mathé, F; Galloo, J C; Guillermo, R

    2000-10-01

    A method was developed for the elemental analysis of size segregated particles ranging from 0.03 to 10 microns. Sampling and analysis problems are discussed in this paper. Particles were collected with a Dekati low-pressure cascade impactor. PTFE filters coated with oleic acid were used as substrate. Particles were microwave digested in closed vessels. The optimum digestion mixture was composed of HNO3 (1 mL), HF (50 microL) and H2O (1 mL). The optimal power setting and digestion time were studied in order to achieve an efficient digestion. A ca. 35 min microwave digestion cycle at a 650 W maximum power allowed complete digestion of the samples. Special emphasis was placed on the pressure in the closed vessels to avoid sample losses. Solution samples were analysed by inductively coupled plasma optical emission spectrometry using an ultrasonic nebuliser for 18 elements (Al, Ba, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, S, Sr, Ti, V, Zn). This procedure was tested with NIST Standard Reference Material 1648 Urban Particulate. Recoveries for certified elements ranged from 95 to 105% except for Al (90%). The influence of cascade impactor materials was investigated with 44 field samples. Strong artefacts due to contamination were shown for analysis at environmental concentrations of Al, Cr, Mn and Ni.

  14. Analysis of six heavy metals in Ortho mineral trioxide aggregate and ProRoot mineral trioxide aggregate by inductively coupled plasma-optical emission spectrometry.

    PubMed

    Kum, Kee-Yeon; Zhu, Qiang; Safavi, Kamran; Gu, Yu; Bae, Kwang-Shik; Chang, Seok Woo

    2013-12-01

    Ortho mineral trioxide aggregate (MTA) is a mineral aggregate newly developed for perforation repair, root end filling and pulp capping. The aim of this study was to investigate the levels of cadmium (Cd), copper (Cu), iron (Fe), manganese (Mn), nickel (Ni) and zinc (Zn) in Ortho MTA and ProRoot MTA. A total of 0.2 g of each MTA was digested using a mixture of hydrochloric and nitric acids and filtered. Six heavy metals in the resulting filtrates were analyzed by inductively coupled plasma-optical emission spectrometry (n = 5). The results were statistically analyzed using the Mann-Whitney U-test. The concentrations of Cd, Cu, Fe, Mn, Ni and Zn in Ortho MTA were 0.10, 7.73, 49.51, 2.58, 0.82 and 10.09 p.p.m., respectively. The concentrations of Cd, Cu, Fe, Mn, Ni and Zn in ProRoot MTA were 0.16, 9.38, 1438.11, 74.51, 18.98 and 4.05 p.p.m., respectively. In conclusion, Ortho MTA had lower levels of Cd, Cu, Fe, Mn and Ni than ProRoot MTA. PMID:24279659

  15. On-line determination of Sb(III) and total Sb using baker's yeast immobilized on polyurethane foam and hydride generation inductively coupled plasma optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    Menegário, Amauri A.; Silva, Ariovaldo José; Pozzi, Eloísa; Durrant, Steven F.; Abreu, Cassio H.

    2006-09-01

    The yeast Saccharomyces cerevisiae was immobilized in cubes of polyurethane foam and the ability of this immobilized material to separate Sb(III) and Sb(V) was investigated. A method based on sequential determination of total Sb (after on-line reduction of Sb(V) to Sb(III) with thiourea) and Sb(III) (after on-line solid-liquid phase extraction) by hydride generation inductively coupled plasma optical emission spectrometry is proposed. A flow system assembled with solenoid valves was used to manage all stages of the process. The effects of pH, sample loading and elution flow rates on solid-liquid phase extraction of Sb(III) were evaluated. Also, the parameters related to on-line pre-reduction (reaction coil and flow rates) were optimized. Detection limits of 0.8 and 0.15 μg L - 1 were obtained for total Sb and Sb(III), respectively. The proposed method was applied to the analysis of river water and effluent samples. The results obtained for the determination of total Sb were in agreement with expected values, including the river water Standard Reference Material 1640 certified by the National Institute of Standards and Technology (NIST). Recoveries of Sb(III) and Sb(V) in spiked samples were between 81 ± 19 and 111 ±15% when 120 s of sample loading were used.

  16. Reduction of Argon Consumption to Less than 2 L min(-1) by Gas Recycling in Inductively Coupled Plasma Optical Emission Spectrometry.

    PubMed

    Tirk, Paul; Wolfgang, Matthias; Wiltsche, Helmar

    2016-07-19

    An innovative interface between the torch and the entrance optics for inductively coupled plasma optical emission spectrometry (ICP-OES) is proposed. This system is capable of collecting all argon which was initially supplied to the torch, cooling and cleaning it and feeding most of the argon back to the outer gas port of the torch. Thereby, the total argon consumption could be reduced from 14 to 1.4 L min(-1) using a standard torch and without restricting the rf power. The excitation- and rotational temperature of the plasma were identical when comparing the traditional setup with the enclosed plasma interface. However, the limits of detection (LOD) and limits of quantification (LOQ) of 27 elements investigated were degraded about 5-fold, though this fact can be expected to stem from a change of the observed zone in the plasma caused by the slight overpressure of 2000 Pa within the interface. Though the enclosed plasma interface was located close to the load coil, the rf power coupled to the interface was well below 1 W and no rf arcing was observed for two different rf generator designs. PMID:27306111

  17. Speciation of inorganic selenium in environmental water samples by inductively coupled plasma optical emission spectrometry after preconcentration by using a mesoporous zirconia coating on coal cinder.

    PubMed

    Wei, Xiao-Shu; Wu, Yi-Wei; Han, Li-Juan; Guo, Jing; Sun, Hong-Li

    2014-08-01

    A simple, novel, and selective flow-injection solid-phase extraction with inductively coupled plasma optical emission spectrometry method was developed for the speciation of inorganic selenium in environmental water samples. A mesoporous zirconia film was simply introduced to coat coal cinder by means of the sol-gel technique, and the adsorptive performance of the coated material for Se(IV)/Se(VI) was investigated in different media. Both Se(IV) and Se(VI) can be retained quantitatively by the material in HCl/NaOH (pH 1.0-9.0) media, while only Se(IV) was adsorbed quantitatively in sodium acetate buffer (pH 3.5-6.0). Thus, the assay of Se(VI) is based on subtracting Se(IV) from total selenium by controlling different adsorptive media without employing any redox procedure. Under the optimum conditions, the detection limit of Se(IV) is 9.0 ng/L with an enrichment factor of 100, and the relative standard deviation is 3.6% (n = 9, C = 5.0 ng/mL). The developed method was successfully applied to the speciation of inorganic selenium in environmental water samples with satisfactory results. In order to further verify the accuracy of the developed method, it was applied to analysis of total selenium in GSBZ 50031-94 certified reference environmental water, and the determined values coincided with the certified values very well.

  18. Determination of traces of uranium and thorium in titanium and copper used for the construction of the Russian Emission Detector 100 by inductively coupled plasma mass spectrometry.

    PubMed

    Poteshin, Sergey S; Sysoev, Alexey A; Lagunov, Sergey S; Sereda, Andrei; Sosnovtsev, Valery V; Bolozdynya, Alexander I; Efremenko, Yuriy B

    2015-01-01

    The Russian Emission Detector 100 (RED-100) under construction at the National Research Nuclear University MEPhI (Moscow Engineering Physics Institute) is designed to detect the presently undiscovered effect of coherent neutrino scattering. One of the factors limiting the sensitivity of the detector is the spontaneous decay of uranium and thorium in the detector materials. Radioactive impurities in detector materials at levels of parts per billion can significantly affect the sensitivity. Five random samples of titanium and one of copper from materials used in the construction of the detector were selected for assay. The concentration of (232)Th and (238)U were measured by inductively coupled plasma mass spectrometry (ICP- MS) in solid titanium using both: solutions in acids and direct sampling by laser ablation (LA-ICP-MS). The LA- ICP-MS method allowed us to determine (238)U and (232)Th at subnanogram per gram levels. This method is much faster than ICP-MS with liquid injection. The titanium samples studied have impurities in the range between 1 ng g(-1) and 21 ng g(-1) for (238)U and 3 ng g(-1) and 31 ng g(-1) for (232)Th. In copper we set upper limits of 0.4 ng g(-1) for (238)U and 1 ng g(-1)for (232)Th. The total activity of the cryostat constructed from materials studied was estimated to be 43 Bq. PMID:26307714

  19. [Characterization of dinosaur fossils and their surrounding rocks by atomic emission spectrometry and X-ray powder diffractometry].

    PubMed

    Yang, Qun; Wang, Yi-lin; Li, Chao-zhen; Yuan, Bo

    2005-02-01

    More dinosaur fossils have been found in the Laochangqing valley, Lufeng county than anywhere else in the world, and the dinosaur fossils found here cover the longest time span (including the early and middle Jurassic ages). This excavation offers an ideal experimental base for prehistoric biology studies. This paper presents an elementary analysis of the components and structure of the dinosaur fossils in three different geologic-layers and their surrounding rocks in the above mentioned area. Atomic emission spectrum shows that the fossils are rich in the contents of calcium (>5%) and phosphor, but low in the content of silicon (3%-8%), while the surrounding rocks are high in the content of silicon (>10%). Furthermore, XRD results show that the major compound of the fossils is CaCO3 (66%), followed by SiO2 (17%); while that of the surrounding rocks is SiO2 (>80%), followed by CaCO3 (<12%). The most important difference between the fossils and the surrounding rocks is, according to the experiment, that phosphate has been identified in the former but not in the latter. This is a characteristic that can be used to distinguish the dinosaur fossils from other rocks. This paper provides valuable data for further zoological studies on the living conditions and evolution of the dinosaurs in the Laochangqing valley, Lufeng county.

  20. [Recent Development of Atomic Spectrometry in China].

    PubMed

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

    2015-09-01

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

  1. Optical Characteristics and Chemical Composition of Dissolved Organic Matter (DOM) from Riparian Soil by Using Excitation-Emission Matrix (EEM) Fluorescence Spectroscopy and Mass Spectrometry.

    PubMed

    Wang, Yulai; Yang, Changming; Zou, Limin; Cui, Hengzhao

    2015-05-01

    Understanding the quantity and quality of soil dissolved organic matter (DOM) in riparian buffer zones is critical for explaining the biogeochemical processes of soil DOM in river ecosystems. Here, we investigated the dissolved organic carbon, fluorescent DOM (FDOM), and DOM molecules from riparian soils on Chongming Island in eastern China. Simultaneously, the soil DOM was extensively characterized in terms of the total aromaticity index (TAI) and several optical indices. The excitation (Ex)-emission (Em) matrix parallel factor analysis results showed that two humic-like components were present (Ex/Em = 283(364)/454 nm; 337/410 nm), a fulvic-like component (Ex/Em = 241/426 nm) and a microbial degradation component (Ex/Em = 295/382 nm). The humic-like and fulvic-like substances were the main components in the riparian soil FDOM, accounting for ~90% of the FDOM. Mass spectrometry provided more detailed information for the soil DOM molecules. Six chemical fractions, amino acids, carbonyl compounds, fatty acids, lipids, proteins and sugars, were identified using liquid chromatography with quadrupole time-of-flight mass spectrometry. Lipids, proteins, and carbonyl compounds were dominant in the soil DOM, accounting for >85% of the detected molecules (m/z < 1000). Significant differences were observed between the quantities of the six soil DOM chemical fractions at the different sampling locations. Discriminant molecules verified the hypothesis that the chemical soil DOM fractions varied with the land use of the adjacent watersheds. The TAI for the soil DOM could provide more reliable information regarding the biogeochemical processes of DOM. The carbonyl compounds and lipid fractions controlled this index. Overall, the optical indices and TAI values can improve our understanding of soil DOM quality; however, the optical indices did not provide quantitative evidence regarding the sources or properties of the soil DOM. The observations from this study provided detailed

  2. 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…

  3. Ultrasensitive Speciation Analysis of Mercury in Rice by Headspace Solid Phase Microextraction Using Porous Carbons and Gas Chromatography-Dielectric Barrier Discharge Optical Emission Spectrometry.

    PubMed

    Lin, Yao; Yang, Yuan; Li, Yuxuan; Yang, Lu; Hou, Xiandeng; Feng, Xinbin; Zheng, Chengbin

    2016-03-01

    Rice consumption is a primary pathway for human methylmercury (MeHg) exposure in inland mercury mining areas of Asia. In addition, the use of iodomethane, a common fumigant that significantly accelerates the methylation of mercury in soil under sunlight, could increase the MeHg exposure from rice. Conventional hyphenated techniques used for mercury speciation analysis are usually too costly for most developing countries. Consequently, there is an increased interest in the development of sensitive and inexpensive methods for the speciation of mercury in rice. In this work, gas chromatography (GC) coupled to dielectric barrier discharge optical emission spectrometry (DBD-OES) was developed for the speciation analysis of mercury in rice. Prior to GC-DBD-OES analysis, mercury species were derivatized to their volatile species with NaBPh4 and preconcentrated by headspace solid phase microextraction using porous carbons. Limits of detection of 0.5 μg kg(-1) (0.16 ng), 0.75 μg kg(-1) (0.24 ng), and 1.0 μg kg(-1) (0.34 ng) were obtained for Hg(2+), CH3Hg(+), and CH3CH2Hg(+), respectively, with relative standard deviations (RSDs) better than 5.2% and 6.8% for one fiber or fiber-to-fiber mode, respectively. Recoveries of 90-105% were obtained for the rice samples, demonstrating the applicability of the proposed technique. Owing to the small size, low power, and low gas consumption of DBD-OES as well as efficient extraction of mercury species by porous carbons headspace solid phase micro-extraction, the proposed technique provides several advantages including compactness, cost-effectiveness, and potential to couple with miniature GC to accomplish the field speciation of mercury in rice compared to conventional hyphenated techniques.

  4. Dilute-and-shoot procedure for the determination of mineral constituents in vinegar samples by axially viewed inductively coupled plasma optical emission spectrometry (ICP OES).

    PubMed

    Da Silva, J C J; Cadore, S; Nobrega, J A; Baccan, N

    2007-02-01

    Samples of commercial wine vinegar were introduced in an axially viewed inductively coupled plasma optical emission spectrometry instrument (AX-ICP OES) equipped with different sample introduction systems: a cross-flow nebulizer combined with a double-path spray chamber (CF-DP) and cone spray associated with a cyclone spray chamber (CS-CC). Samples of white and red wine vinegar were diluted with water before analysis. Higher magnesium Mg II/Mg I ratios (11 and 10 for CS-CC and CF-DP, respectively) were obtained using a nebulization gas flow rate of 0.6 l min-1 and an applied power of 1.3 kW. The background equivalent concentrations (BEC) and signal-to-background ratio (SBR) of analytes were improved using scandium (Sc) as the internal standard. The limits of detection (LOD) and limits of quantification (LOQ) for mineral constituents were similar for both introduction systems. Best recoveries values were obtained using a plasma under robust conditions, CS-CC system and Sc as the internal standard. The concentration determined in 13 commercial samples of wine vinegars varied between 0.2 and 3.0, between 0.02 and 0.4, between 8.5 and 100.0, between 0.01 and 0.05, between 27.0 and 540.0, between 4.0 and 79.0, between 0.4 and 10.0, and between 0.01 and 2.0 for aluminium (Al), barium (Ba), calcium (Ca), copper (Cu), potassium (K), magnesium (Mg), manganese (Mn), and zinc (Zn), respectively. PMID:17364913

  5. A method for Ca, Fe, Ga, Na, Si and Zn determination in alumina by inductively coupled plasma optical emission spectrometry after aluminum precipitation

    NASA Astrophysics Data System (ADS)

    Souza, Alexandre L.; Lemos, Sherlan G.; Oliveira, Pedro V.

    2011-05-01

    In this present work a method for the determination of Ca, Fe, Ga, Na, Si and Zn in alumina (Al 2O 3) by inductively coupled plasma optical emission spectrometry (ICP OES) with axial viewing is presented. Preliminary studies revealed intense aluminum spectral interference over the majority of elements and reaction between aluminum and quartz to form aluminosilicate, reducing drastically the lifetime of the torch. To overcome these problems alumina samples (250 mg) were dissolved with 5 mL HCl + 1.5 mL H 2SO 4 + 1.5 mL H 2O in a microwave oven. After complete dissolution the volume was completed to 20 mL and aluminum was precipitated as Al(OH) 3 with NH 3 (by bubbling NH 3 into the solution up to a pH ~ 8, for 10 min). The use of internal standards (Fe/Be, Ga/Dy, Zn/In and Na/Sc) was essential to obtain precise and accurate results. The reliability of the proposed method was checked by analysis of alumina certified reference material (Alumina Reduction Grade-699, NIST). The found concentrations (0.037% w w -1 CaO, 0.013% w w -1 Fe 2O 3, 0.012% w w -1 Ga 2O 3, 0.49% w w -1 Na 2O, 0.014% w w -1 SiO 2 and 0.013% w w -1 ZnO) presented no statistical differences compared to the certified values at a 95% confidence level.

  6. Development of a wet digestion method for paints for the determination of metals and metalloids using inductively coupled plasma optical emission spectrometry.

    PubMed

    Silva, Francisco L F; Duarte, Thalita A O; Melo, Luciana S; Ribeiro, Livia P D; Gouveia, Sandro T; Lopes, Gisele S; Matos, Wladiana O

    2016-01-01

    Paints, a complex matrix, have a variable composition that is dependent on the application. In this work, a new wet digestion procedure for the determination of Al, As, Ba, Cd, Cr, Cu, Mn, Ni, Pb, Sn, Sr, Ti and Zn in paint samples using inductively coupled plasma optical emission spectrometry (ICP OES) has been developed. An experimental design approach was employed to determine the optimal conditions for achieving complete solubilization and/or decomposition in the sample preparation method. An efficient sample preparation was developed that consisted of a pre-digestion step at 40°C for 20 min using 1 mL of HNO3 to eliminate organic solvents followed by digestion at 120°C for 3h using 5 mL of HCl and 1 mL of HF in a block digestion. The proposed procedure promotes the complete solubilization of different bases of paints at low temperature and atmospheric pressure. The accuracy was determined by addition/recovery tests and comparing the results with those obtained using the ASTM D335-85a standard sample preparation method. The limits of quantification were 1.78, 0.11, 0.006, 0.006, 0.01, 0.04, 0.006, 0.006, 0.02, 0.07, 0.30, 1.30 and 0.30 mg kg(-1) for Al, As, Ba, Cd, Cr, Cu,Mn, Ni, Pb, Sn, Sr, Ti and Zn, respectively. The proposed method was applied for the analysis of inorganics via the ICP OES of paints with different colors and bases used to cover wall surfaces. PMID:26695251

  7. Capillary microextraction combined with fluorinating assisted electrothermal vaporization inductively coupled plasma optical emission spectrometry for the determination of trace lanthanum, europium, dysprosium and yttrium in human hair.

    PubMed

    Wu, Shaowei; Hu, Chengguo; He, Man; Chen, Beibei; Hu, Bin

    2013-10-15

    In this work, a congo red modified single wall carbon nanotubes (CR-SWCNTs) coated fused-silica capillary was prepared and used for capillary microextraction (CME) of trace amounts of lanthanum (La), europium (Eu), dysprosium (Dy) and yttrium (Y) in human hair followed by fluorinating assisted electrothermal vaporization-inductively coupled plasma-optical emission spectrometry (FETV-ICP-OES) determination. The adsorption properties and stability of the prepared CR-SWCNTs coated capillary along with the various factors affecting the separation/preconcentration of La, Eu, Dy and Y by CME were investigated in detail. Under the optimized conditions, with a consumption of 2 mL sample solution, a theoretical enrichment factor of 50 and a detection limit (3σ) of 0.12 ng mL(-1) for La, 0.03 ng mL(-1) for Eu, 0.11 ng mL(-1) for Dy and 0.03 ng mL(-1) for Y were obtained, respectively. The preparation reproducibility of the CR-SWCNTs coated capillary was investigated and the relative standard deviations (RSDs) were ranging from 4.1% (Eu) to 4.4% (La) (CLa, Dy=1.4 ng mL(-1); CY, Eu=0.25 ng mL(-1), n=7) in one batch, and from 5.7% (Eu) to 6.1% (Y) (CLa, Dy=1.4 ng mL(-1); CY, Eu=0.25 ng mL(-1), n=5) among different batches. The proposed method was applied to the analysis of real-world human hair sample and the recoveries for the spiked sample were in the range of 93-105%. The method was also applied to the determination of La, Eu, Dy and Y in Certified Reference Material of GBW07601 human hair, and the determined values were in good agreement with the certified values.

  8. Investigations on the emission of fragrance allergens from scented toys by means of headspace solid-phase microextraction gas chromatography-mass spectrometry.

    PubMed

    Masuck, Ines; Hutzler, Christoph; Luch, Andreas

    2010-04-30

    In the revised European toy safety directive 2009/48/EC the application of fragrance allergens in children's toys is restricted. The focus of the present work lies on the instrumental analytics of 13 banned fragrance allergens, as well as on 11 fragrance allergens that require declaration when concentrations surpass 100 microg per gram material. Applying a mixture of ethyl acetate and toluene solid/liquid extraction was performed prior to quantitative analysis of mass contents of fragrances in scented toys. In addition, an easy-to-perform method for the determination of emitted fragrances at 23 degrees C (handling conditions) or at 40 degrees C (worst case scenario) has been worked out to allow for the evaluation of potential risks originating from inhalation of these compounds during handling of or playing with toys. For this purpose a headspace solid-phase microextraction (HS-SPME) technique was developed and coupled to subsequent gas chromatography-mass spectrometry (GC-MS) analysis. Fragrance allergens were adsorbed (extracted) from the gas phase onto an 85 microm polyacrylate fiber while incubating pieces of the scented toys in sealed headspace vials at 23 degrees C and 40 degrees C. Quantification of compounds was performed via external calibration. The newly developed headspace method was subsequently applied to five perfumed toys. As expected, the emission of fragrance allergens from scented toys depends on the temperature and on the content of fragrance allergens present in those samples. In particular at conditions mimicking worst case (40 degrees C), fragrance allergens in toys may pose a risk to children since considerable amounts of compound might be absorbed by lung tissue via breathing of contaminated air.

  9. Comparative Analysis of Urban Atmospheric Aerosol by Particle-Induced X-ray Emission (PIXE), Proton Elastic Scattering Analysis (PESA), and Aerosol Mass Spectrometry (AMS)

    SciTech Connect

    Johnson, Kirsten S; Laskin, Alexander; Jimenez, Jose L; Shutthanandan, V; Molina, Luisa T; Salcedo, D; Dzepina, K; Molina, Mario J

    2008-09-01

    A multifaceted approach to atmospheric aerosol analysis is often desirable in field studies where an understanding of technical comparability among different measurement techniques is essential. Herein we report quantitative intercomparisons of Particle-Induced X-ray Emission (PIXE) and Proton Elastic Scattering Analysis (PESA), performed off-line under vacuum, with analysis by Aerosol Mass Spectrometry (AMS) carried out in real-time during the MCMA-2003 Field Campaign in the Mexico City Metropolitan Area. Good agreement was observed for mass concentrations of PIXE-measured sulfur (assuming it was dominated by SO42-) and AMS-measured sulfate during the most of the campaign. PESA-measured hydrogen mass was separated into sulfate H and organic H mass fractions assuming the only major contributions were (NH4)2SO4 and organic compounds. Comparison of the organic H mass with AMS organic aerosol measurements indicates that about 75% of the mass of these species evaporated under vacuum. However ~25% of the organics does remain under vacuum, which is only possible with low vapor pressure compounds, and which supports the presence of high molecular weight and/or highly oxidized organics consistent with atmospheric aging. Approximately 10% of the chloride detected by AMS was measured by PIXE, possibly in the form of metal-chloride complexes, while the majority of Cl was likely present as more volatile species including NH4Cl. This is the first comparison of PIXE/PESA and AMS, and to our knowledge also the first report of PESA hydrogen measurements for urban organic aerosols.

  10. Determination of Phosphorus and Potassium in Commercial Inorganic Fertilizers by Inductively Coupled Plasma-Optical Emission Spectrometry: Single-Laboratory Validation, First Action 2015.18.

    PubMed

    Thiex, Nancy J

    2016-07-01

    A previously validated method for the determination of both citrate-EDTA-soluble P and K and acid-soluble P and K in commercial inorganic fertilizers by inductively coupled plasma-optical emission spectrometry was submitted to the expert review panel (ERP) for fertilizers for consideration of First Action Official Method(SM) status. The ERP evaluated the single-laboratory validation results and recommended the method for First Action Official Method status and provided recommendations for achieving Final Action. Validation materials ranging from 4.4 to 52.4% P2O5 (1.7-22.7% P) and 3-62% K2O (2.5-51.1% K) were used for the validation. Recoveries from validation materials for citrate-soluble P and K ranged from 99.3 to 124.9% P and from 98.4 to 100.7% K. Recoveries from validation materials for acid-soluble "total" P and K ranged from 95.53 to 99.40% P and from 98.36 to 107.28% K. Values of r for citrate-soluble P and K, expressed as RSD, ranged from 0.28 to 1.30% for P and from 0.41 to 1.52% for K. Values of r for total P and K, expressed as RSD, ranged from 0.71 to 1.13% for P and from 0.39 to 1.18% for K. Based on the validation data, the ERP recommended the method (with alternatives for the citrate-soluble and the acid-soluble extractions) for First Action Official Method status and provided recommendations for achieving Final Action status. PMID:27455933

  11. Sensitive determination of mercury in tap water by cloud point extraction pre-concentration and flow injection-cold vapor-inductively coupled plasma optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    de Wuilloud, Jorgelina C. A.; Wuilloud, Rodolfo G.; Silva, María. F.; Olsina, Roberto A.; Martinez, Luis D.

    2002-02-01

    A pre-concentration and determination methodology for mercury at trace levels in water samples was developed. Cloud point extraction was successfully employed for the pre-concentration of mercury prior to inductively coupled plasma optical emission spectrometry coupled to a flow injection with cold vapor generation system. The mercury was extracted as mercury-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol [Hg(II)-(5-Br-PADAP)] complex, at pH 9.2 mediated by micelles of the non-ionic surfactant polyethyleneglycolmono- p-nonylphenylether (PONPE 5). Cold vapor generation was developed from 100 μl of the extracted surfactant-rich phase by means of a stannous chloride (SnCl 2) solution as reluctant. An exhaustive study of the variables affecting the cloud point extraction with PONPE 5 and cold vapor mercury generation from the surfactant phase was performed. The 50-ml sample solution pre-concentration allowed us to raise an enrichment factor of 200-fold. The lower limit of detection obtained under the optimal conditions was 4 ng l -1. The precision for 10 replicate determinations at the 0.5-μg l -1 Hg level was 3.4% relative standard deviation (R.S.D.), calculated with the peak heights. The calibration graph using the pre-concentration system for mercury was linear with a correlation coefficient of 0.9998 at levels near the detection limits up to at least 50 μg l -1. The method was successfully applied to the determination of mercury in tap water samples.

  12. Capillary microextraction combined with fluorinating assisted electrothermal vaporization inductively coupled plasma optical emission spectrometry for the determination of trace lanthanum, europium, dysprosium and yttrium in human hair.

    PubMed

    Wu, Shaowei; Hu, Chengguo; He, Man; Chen, Beibei; Hu, Bin

    2013-10-15

    In this work, a congo red modified single wall carbon nanotubes (CR-SWCNTs) coated fused-silica capillary was prepared and used for capillary microextraction (CME) of trace amounts of lanthanum (La), europium (Eu), dysprosium (Dy) and yttrium (Y) in human hair followed by fluorinating assisted electrothermal vaporization-inductively coupled plasma-optical emission spectrometry (FETV-ICP-OES) determination. The adsorption properties and stability of the prepared CR-SWCNTs coated capillary along with the various factors affecting the separation/preconcentration of La, Eu, Dy and Y by CME were investigated in detail. Under the optimized conditions, with a consumption of 2 mL sample solution, a theoretical enrichment factor of 50 and a detection limit (3σ) of 0.12 ng mL(-1) for La, 0.03 ng mL(-1) for Eu, 0.11 ng mL(-1) for Dy and 0.03 ng mL(-1) for Y were obtained, respectively. The preparation reproducibility of the CR-SWCNTs coated capillary was investigated and the relative standard deviations (RSDs) were ranging from 4.1% (Eu) to 4.4% (La) (CLa, Dy=1.4 ng mL(-1); CY, Eu=0.25 ng mL(-1), n=7) in one batch, and from 5.7% (Eu) to 6.1% (Y) (CLa, Dy=1.4 ng mL(-1); CY, Eu=0.25 ng mL(-1), n=5) among different batches. The proposed method was applied to the analysis of real-world human hair sample and the recoveries for the spiked sample were in the range of 93-105%. The method was also applied to the determination of La, Eu, Dy and Y in Certified Reference Material of GBW07601 human hair, and the determined values were in good agreement with the certified values. PMID:24054601

  13. Determination of phosphorus and potassium in commercial inorganic fertilizers by inductively coupled plasma-optical emission spectrometry: single-laboratory validation.

    PubMed

    Bartos, James M; Boggs, Barton L; Falls, J Harold; Siegel, Sanford A

    2014-01-01

    A two-part single-laboratory validation study was conducted for determination of the P and K content in commercial fertilizer materials by inductively coupled plasma-optical emission spectrometry (ICP-OES). While several methods exist for determination of P and K in fertilizer products, the main focus of this study was on ICP-OES determination, which offers several unique advantages. Fertilizer samples with consensus P and K values from the Magruder and Association of Fertilizer and Phosphate Chemists (AFPC) check sample programs were selected for this study. Validation materials ranging from 4.4 to 52.4% P205 (1.7 to 22.7% P) and 3 to 62% K20 (2.5 to 51.5% K) were utilized. Because all P and K compounds contained in fertilizer materials are not "available" for plants to use, this study was conducted in two parts. Part A focused on ammonium citrate-disodium EDTA as the extraction solvent, as it estimates the pool of fertilizer P and K that is considered available to plants. Part B focused on hydrochloric acid as the digestion solvent, as it estimates the total P and K content of the fertilizer product. Selectivity studies indicated that this method can have a high bias for fertilizer products containing sources of phosphite or organic P compared to gravimetric or colorimetric methods that measure just orthophosphate. Provided the analytical challenges outlined in this study are addressed, this method offers the potential for a quick, accurate, and safe alternative for determining the P and K content of commercial inorganic fertilizer materials.

  14. Tungsten coil atomic emission spectrometry combined with dispersive liquid-liquid microextraction: A synergistic association for chromium determination in water samples.

    PubMed

    Vidal, Lorena; Silva, Sidnei G; Canals, Antonio; Nóbrega, Joaquim A

    2016-02-01

    A novel and environment friendly analytical method is reported for total chromium determination and chromium speciation in water samples, whereby tungsten coil atomic emission spectrometry (WCAES) is combined with in situ ionic liquid formation dispersive liquid-liquid microextraction (in situ IL-DLLME). A two stage multivariate optimization approach has been developed employing a Plackett-Burman design for screening and selection of the significant factor involved in the in situ IL-DLLME procedure, which was later optimized by means of a circumscribed central composite design. The optimum conditions were complexant concentration: 0.5% (or 0.1%); complexant type: DDTC; IL anion: PF6(-); [Hmim][Cl] IL amount: 60 mg; ionic strength: 0% NaCl; pH: 5 (or 2); centrifugation time: 10 min; and centrifugation speed: 1000 rpm. Under the optimized experimental conditions the method was evaluated and proper linearity was obtained with a correlation coefficient of 0.991 (5 calibration standards). Limits of detection and quantification for both chromium species were 3 and 10 µg L(-1), respectively. This is a 233-fold improvement when compared with chromium determination by WCAES without using preconcentration. The repeatability of the proposed method was evaluated at two different spiking levels (10 and 50 µg L(-1)) obtaining coefficients of variation of 11.4% and 3.6% (n=3), respectively. A certified reference material (SRM-1643e NIST) was analyzed in order to determine the accuracy of the method for total chromium determination and 112.3% and 2.5 µg L(-1) were the recovery (trueness) and standard deviation values, respectively. Tap, bottled mineral and natural mineral water samples were analyzed at 60 µg L(-1) spiking level of total Cr content at two Cr(VI)/Cr(III) ratios, and relative recovery values ranged between 88% and 112% showing that the matrix has a negligible effect. To our knowledge, this is the first time that combines in situ IL-DLLME and WCAES.

  15. Selective Iron(III) ion uptake using CuO-TiO2 nanostructure by inductively coupled plasma-optical emission spectrometry

    PubMed Central

    2012-01-01

    Background CuO-TiO2 nanosheets (NSs), a kind of nanomaterials is one of the most attracting class of transition doped semiconductor materials due to its interesting and important optical, electrical, and structural properties and has many technical applications, such as in metal ions detection, photocatalysis, Chemi-sensors, bio-sensors, solar cells and so on. In this paper the synthesis of CuO-TiO2 nanosheets by the wet-chemically technique is reported. Methods CuO-TiO2 NSs were prepared by a wet-chemical process using reducing agents in alkaline medium and characterized by UV/vis., FT-IR spectroscopy, X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (XRD), and field-emission scanning electron microscopy (FE-SEM) etc. Results The structural and optical evaluation of synthesized NSs were measured by XRD pattern, Fourier transform infrared (FT-IR) and UV–vis spectroscopy, respectively which confirmed that the obtained NSs are well-crystalline CuO-TiO2 and possessing good optical properties. The morphological analysis of CuO-TiO2 NSs was executed by FE-SEM, which confirmed that the doped products were sheet-shaped and growth in large quantity. Here, the analytical efficiency of the NSs was applied for a selective adsorption of iron(III) ion prior to detection by inductively coupled plasma-optical emission spectrometry (ICP-OES). The selectivity of NSs towards various metal ions, including Au(III), Cd(II), Co(II), Cr(III), Fe(III), Pd(II), and Zn(II) was analyzed. Conclusions Based on the selectivity study, it was confirmed that the selectivity of doped NSs phase was the most towards Fe(III) ion. The static adsorption capacity for Fe(III) was calculated to be 110.06 mgg−1. Results from adsorption isotherm also verified that the adsorption process was mainly monolayer-adsorption onto a surface containing a finite number of CuO-TiO2 NSs adsorption sites. PMID:23244218

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

    PubMed

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

    2002-01-01

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

  17. Tungsten coil atomic emission spectrometry combined with dispersive liquid-liquid microextraction: A synergistic association for chromium determination in water samples.

    PubMed

    Vidal, Lorena; Silva, Sidnei G; Canals, Antonio; Nóbrega, Joaquim A

    2016-02-01

    A novel and environment friendly analytical method is reported for total chromium determination and chromium speciation in water samples, whereby tungsten coil atomic emission spectrometry (WCAES) is combined with in situ ionic liquid formation dispersive liquid-liquid microextraction (in situ IL-DLLME). A two stage multivariate optimization approach has been developed employing a Plackett-Burman design for screening and selection of the significant factor involved in the in situ IL-DLLME procedure, which was later optimized by means of a circumscribed central composite design. The optimum conditions were complexant concentration: 0.5% (or 0.1%); complexant type: DDTC; IL anion: PF6(-); [Hmim][Cl] IL amount: 60 mg; ionic strength: 0% NaCl; pH: 5 (or 2); centrifugation time: 10 min; and centrifugation speed: 1000 rpm. Under the optimized experimental conditions the method was evaluated and proper linearity was obtained with a correlation coefficient of 0.991 (5 calibration standards). Limits of detection and quantification for both chromium species were 3 and 10 µg L(-1), respectively. This is a 233-fold improvement when compared with chromium determination by WCAES without using preconcentration. The repeatability of the proposed method was evaluated at two different spiking levels (10 and 50 µg L(-1)) obtaining coefficients of variation of 11.4% and 3.6% (n=3), respectively. A certified reference material (SRM-1643e NIST) was analyzed in order to determine the accuracy of the method for total chromium determination and 112.3% and 2.5 µg L(-1) were the recovery (trueness) and standard deviation values, respectively. Tap, bottled mineral and natural mineral water samples were analyzed at 60 µg L(-1) spiking level of total Cr content at two Cr(VI)/Cr(III) ratios, and relative recovery values ranged between 88% and 112% showing that the matrix has a negligible effect. To our knowledge, this is the first time that combines in situ IL-DLLME and WCAES. PMID:26653490

  18. Ultrasound- and microwave-assisted extractions followed by hydride generation inductively coupled plasma optical emission spectrometry for lead determination in geological samples.

    PubMed

    Welna, Maja; Borkowska-Burnecka, Jolanta; Popko, Malgorzata

    2015-11-01

    Followed the current idea of simplified sample pretratmet before analysis we evaluated the procedure for the determination of Pb in calcium-rich materials such as dolomites after ultrasound- or microwave- assisted extraction with diluted acids using hydride generation inductively coupled plasma optical emission spectrometry (HG-ICP-OES). Corresponding Pb hydride was generated in the reaction of an acidified sample solution with NaBH4 after pre-oxidation of Pb(II) to Pb(IV) by K3[Fe(CN)6]. Several chemical (acidic media: HCl, HNO3 or CH3COOH, concentration of the reductant as well as type and concentration of oxidazing agents) and physical (reagents flow rates, reaction coil length) parameters affecting the efficiency of plumbane formation were optimized in order to improve the detectability of Pb using HG-ICP-OES. Limitation of the method derived from the matrix effects was pointed out. Employing Pb separation by HG technique allows the significant reduction of interferences caused by sample matrix constituents (mainly Ca and Mg), nevertheless they could not be overcame at all, hence calibration based on the standard addition method was recommended for Pb quantification in dolomites. Under the selected conditions, i.e. 0.3 mol L(-1) HCl, HNO3 or CH3COOH, 1.5% NaBH4 and 3.0% K3[Fe(CN)6] the limits of detection (LODs) between 2.3-5.6 μg L(-1) (3.4-6.8 μg L(-1) considering matrix effects) and the precision below 5% were achieved. The accuracy of the procedure was verified by analysis of certified reference materials (NCS DC70308 (Carbonate Rock) and NIST 14000 (Bone Ash)) and recovery test with satisfactory results of Pb recoveries ranging between 94-108% (CRMs analysis) and 92-114% (standard addition method). The applicability of the proposed method was demonstrated by the determination of Pb in dolomites used by different fertiliser factories. PMID:26452913

  19. A novel method for simultaneous determination of selected elements in dolomite and magnesia by Inductively Coupled Plasma Atomic Emission Spectroscopy with slurry sample introduction

    NASA Astrophysics Data System (ADS)

    Bok-Badura, Joanna; Jakóbik-Kolon, Agata; Turek, Marian; Szczerba, Jacek; Lemanowicz, Marcin; Karoń, Krzysztof

    2015-11-01

    The slurry nebulization ICP-AES method for simultaneous determination of selected elements in dolomite and magnesia was proposed. Based on the investigation results the optimal conditions for this analysis were as follows: particle size < 40 μm, the nitric acid concentration 10%, the RF power 1.0 kW, aqueous solutions (no dispersing agents) and mixing on magnetic stirrer, during the sample introduction into plasma, as homogenization method. The certified reference materials Dolomite CRM 782-1 and High Purity Magnesia BCS-CRM 389/1 were analyzed. Student's t-test proved that there were no statistically significant differences between determined values and the certified ones. This proves that the slurry sample introduction into plasma in ICP-AES technique can be applied for simultaneous determination of elements in dolomite and magnesia.

  20. Plants as biomarkers for monitoring heavy metal contaminants on landfill sites using sequential extraction and inductively coupled plasma atomic emission spectrophotometry (ICP-AES).

    PubMed

    Murphy, A P; Coudert, M; Barker, J

    2000-12-01

    There have been a number of studies investigating metal uptake in plants on contaminated landfill sites, but little on their role as biomarkers to identify metal mobility for continuous monitoring purposes. Vegetation can be used as a biomonitor of site pollution, by identifying the mobilisation of heavy metals and by providing an understanding of their bioavailability. Plants selected were the common nettle (Uritica Dioica), bramble (Rubus Fruticosa) and sycamore (Acer Pseudoplatanus). A study of the soil fractionation was made to investigate the soil properties that are likely to influence metal mobility and a correlation exercise was undertaken to investigate if variations in concentration of metals in vegetation can reflect variations in concentration of the metals in soil. The soil was digested using aqua regia in a microwave closed vessel. The vegetation was digested using both microwave and a hydrogen peroxide-nitric acid mixture, refluxed on a heating block and a comparison made. The certified reference materials (CRMs) used were Standard Reference Material (SRM) 1547, peach leaves for vegetation (NIST) and for soil CRM 143R, sewage sludge-amended soil (BCR). The relative standard deviations (RSDs) were 2-6% for the analyses. Our findings show evidence of phytoextraction by some plants, (especially bramble and nettle), with certain plants, (sycamore) exhibiting signs of phytostabilisation. The evidence suggests that there is a degree of selectivity in metal uptake and partitioning within the plant compartments. It was also possible to correlate mobility phases of certain metals (Pb, Cu and Zn) using the soil and plant record. Zn and Cu exhibited the greatest potential to migrate from the roots to the leaves, with Pb found principally in the roots of ground vegetation. Our results suggest that analysis of bramble leaves, nettle leaves and roots can be used to monitor the mobility of Pb in the soil with nettle, bramble and sycamore leaves to monitor Cu and Zn. PMID:11296751

  1. Feasibility of depth profiling of Zn-based coatings by laser ablation inductively coupled plasma optical emission and mass spectrometry using infrared Nd:YAG and ArF* lasers

    NASA Astrophysics Data System (ADS)

    Hrdlička, Aleš; Otruba, Vítĕzslav; Novotný, Karel; Günther, Detlef; Kanický, Viktor

    2005-03-01

    The feasibility of depth profiling of zinc-coated iron sheets by laser ablation (LA) was studied using an Nd:YAG laser (1064 nm) with inductively coupled plasma optical emission spectrometry (ICP-OES), and an excimer ArF* laser (193 nm) with a beam homogenizer. The latter was coupled to an ICP with mass spectrometry (ICP-MS). Fixed-spot ablation was applied. Both LA systems were capable of providing depth profiles that approach the profiles obtained by glow discharge optical emission spectroscopy (GD-OES) and electron probe X-ray microanalysis (EPXMA). For Nd:YAG laser an artefact consisting of zinc depth profile signal tailing appeared, enlarging thus erroneously diffusional coating-substrate interface profile. However, the ArF* system partially reduced but not suppressed that phenomenon. For both LA systems the Fe signal from the substrate increased with depth as expected and reached a plateau. The depth resolution (depth range corresponding to 84%-16% change in the full signal) achieved was several micrometers. Ablation rate was found to depend on ablation spot area at constant irradiance. Consequently, ablated volume per shot dependence on pulse energy exhibits deviation from linear course.

  2. REAL TIME, ON-LINE CHARACTERIZATION OF DIESEL GENERATOR AIR TOXIC EMISSIONS BY RESONANCE ENHANCED MULTI-PHOTON IONIZATION TIME OF FLIGHT MASS SPECTROMETRY

    EPA Science Inventory

    The laser based resonance, enhanced multi-photon ionization time-of-flight mass spectrometry (REMPI-TOFMS) technique has been applied to the exhaust gas stream of a diesel generator to measure, in real time, concentration levels of aromatic air toxics. Volatile organic compounds ...

  3. Odor and odorous chemical emissions from dairy and swine facilities: Part 5-Simultaneous chemical and sensory analysis with Gas Chromatography - Mass Spectrometry - Olfactometry

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Simultaneous chemical and sensory analyses using gas chromatography-mass spectrometry-olfactometry (GC-MS-O) for air samples collected at barn exhaust fans were used for quantification and ranking of odor impact of target odorous gases. Fifteen target odorous VOCs (odorants) were selected. Air sampl...

  4. Deposition of TiN and HfO{sub 2} in a commercial 200 mm remote plasma atomic layer deposition reactor

    SciTech Connect

    Heil, S. B. S.; Hemmen, J. L. van; Hodson, C. J.; Singh, N.; Klootwijk, J. H.; Roozeboom, F.; Sanden, M. C. M. van de; Kessels, W. M. M.

    2007-09-15

    The authors describe a remote plasma atomic layer deposition reactor (Oxford Instruments FlexAL trade mark sign ) that includes an inductively coupled plasma source and a load lock capable of handling substrates up to 200 mm in diameter. The deposition of titanium nitride (TiN) and hafnium oxide (HfO{sub 2}) is described for the combination of the metal-halide precursor TiCl{sub 4} and H{sub 2}-N{sub 2} plasma and the combination of the metallorganic precursor Hf[N(CH{sub 3})(C{sub 2}H{sub 5})]{sub 4} and O{sub 2} plasma, respectively. The influence of the plasma exposure time and substrate temperature has been studied and compositional, structural, and electrical properties are reported. TiN films with a low Cl impurity content were obtained at 350 deg. C at a growth rate of 0.35 A /cycle with an electrical resistivity as low as 150 {mu}{omega} cm. Carbon-free (detection limit <2 at. %) HfO{sub 2} films were obtained at a growth rate of 1.0 A /cycle at 290 deg. C. The thickness and resisitivity nonuniformity was <5% for the TiN and the thickness uniformality was <2% for the HfO{sub 2} films as determined over 200 mm wafers.

  5. 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.

  6. Tecnical Note: Analysis of non-regulated vehicular emissions by extractive FTIR spectrometry: tests on a hybrid car in Mexico City

    NASA Astrophysics Data System (ADS)

    Reyes, F.; Grutter, M.; Jazcilevich, A.; González-Oropeza, R.

    2006-11-01

    A methodology to acquire valuable information on the chemical composition and evolution of vehicular emissions is presented. The analysis of the gases is performed by passing a constant flow of a sample gas from the tail-pipe into a 10 L multi-pass cell. The absorption spectra within the cell are obtained using an FTIR spectrometer at 0.5 cm-1 resolution along a 13.1 m optical path. Additionally, the total flow from the exhaust is continuously measured from a differential pressure sensor on a textit{Pitot} tube installed at the exit of the exhaust. This configuration aims to obtain a good speciation capability by coadding spectra during 30 s and reporting the emission (in g/km) of both criteria and non-regulated pollutants, such as CO2, CO, NO, SO2, NH3, HCHO and some NMHC, during predetermined driving cycles. The advantages and disadvantages of increasing the measurement frequency, as well as the effect of other parameters such as spectral resolution, cell volume and flow rate, are discussed. To test and evaluate the proposed technique, experiments were performed on a dynamometer running FTP-75 and typical driving cycles for the Mexico City Metropolitan Area (MCMA) on a Toyota Prius hybrid vehicle. This car is an example of recent marketed automotive technology dedicated to reduced emissions, increasing the need for sensitive detection techniques. This study shows the potential of the proposed technique to measure and report in real time the emissions of a large variety of pollutants, even from a super ultra-low emission vehicle (SULEV). The emissions of HC's, NOx, CO and CO2 obtained here were compared to experiments performed in other locations with the same model vehicle. The proposed technique provides a tool for future studies comparing in detail the emissions of vehicles using alternative fuels and emission control systems.

  7. 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.

  8. [Identification of hashish samples with inductively coupled high-frequency plasma emission spectrometry and neutron activation analysis and data handling with neuronal networks. 1. Methods for the quantitative determination of characteristic trace elements].

    PubMed

    Lahl, H; Henke, G

    1997-11-01

    Neutron activation analysis (NAA) and inductively coupled plasma emission spectrometry (ICP-AES) were used to quantify the relative contents of Fe, Sc, Ce, Pa, Cr, Co, respectively the absolute contents of Cr, Zn, Mn, Fe, Mg, Al, Cu, Ti, Ca, Sr in hashish samples, seized in different countries. The samples were processed after dry ashing by means of instrumental NAA and after wet mineralization by means of ICP-AES. For determination of the sampling and measurement errors, one of the samples was analyzed repeatedly with both methods. Classifying hashish samples with regard to concentration of certain elements could be done by artificial neural networks with a modified backpropagation algorithm. By this way, identity and non identity of one unknown sample with one of many different samples as data pool can be ascertained, on principle. PMID:9446107

  9. 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. PMID:27374562

  10. Comparision of results of diferent instrumental methodics (MP-AES, UV-Vis spectrometry) for determination of available forms of soil phosphorus.

    NASA Astrophysics Data System (ADS)

    Tonutare, Tonu

    2016-04-01

    The content of easily extractable forms of phosphorus (P) in soils is important as on the environmental viewpoint and also from agronomical side. For determination of plant available P there is several extraction methods developed. Due to big variations in soil properties, it is very complicated to find the best method for P extractions from soil. For determination of P content in extracts during the years Vis-spectroscopy was used as simple and economic method. During the last decade the role of atomic emission spectroscopic (AES) methods started to grow rapidly. The advantage of this method is accuracy and shorter time of analysis. For the plant growth it is important that the content of P is in phosphate form. This can be determined by phosphate-molybdate method Vis spectrometrically. AES method measured total content of P, including P in organic compound and therefore give a overestimated results of plant available P. The aim of our work was to investigate the possibility of the use of MP-AES spectrometry for determination of plant avalable P in soil. In work more than 100 soil samples with very diferent properties were used. For extraction Mehlich 3, acetate-lactate (AL), double lactate (DL) and calcium lactate (CAL) extragents were used. The content of extracted P was determined by molybdatemethod using Vis spectrometer and microplate reader and also the MP-AES (microwave plasma atomic emission spectrometer). The detection limits and limits of quantification for P is calculated. Comparision of analysed by Vis spectroscopy and MP AES P content is provided. Also the influence of soil pH and organic matter content to the results of analysis was reported.

  11. Acquired acid resistance of human enamel treated with laser (Er:YAG laser and Co2 laser) and acidulated phosphate fluoride treatment: An in vitro atomic emission spectrometry analysis

    PubMed Central

    Mathew, Anju; Reddy, N. Venugopal; Sugumaran, D. K.; Peter, Joby; Shameer, M.; Dauravu, Liju Marcely

    2013-01-01

    Background: Dental caries is essentially a process of diffusion and dissolution. If the aspect of dissolution can be curtailed some degree of prevention can be achieved. Aims: The present study was carried out to evaluate and compare the effect of Er:YAG laser and Co2 laser irradiation combined with acidulated phosphate fluoride treatment on in vitro acid resistance of human enamel. Design: An in vitro study was carried out on 30 human premolars to evaluate the enamel's acid resistance using an atomic emission spectrometry analysis. Materials and Methods: A total of 60 enamel specimens were prepared from 30 human premolars and were randomly assigned to 6 groups: (1) Untreated (control); (2) 1.23% acidulated phosphate fluoride (APF) gel application alone for 4 min; (3) Er:YAG laser treatment alone; (4) Co2 laser treatment alone; (5) Er:YAG laser + APF gel application; (6) Co2 laser + APF gel application. The specimens were then individually immersed in 5 ml of acetate buffer solution (0.1 mol/L, pH 4.5) and incubated at 37°C for 24 h, and the acid resistance was evaluated by determining the calcium ion concentration using the atomic emission spectrometry. Statistical Analysis: An ANOVA model was constructed (P value of 0.05), followed by Tukey's test for multiple pair wise comparisons of mean values. Results: Significant differences were found between the control group and the test groups (P < 0.001). Conclusions: Combining acidulated phosphate fluoride with either Er:YAG or Co2 laser had a synergistic effect in decreasing the enamel demineralization more than either fluoride treatment or laser treatment alone. PMID:24015004

  12. 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. PMID:26969551

  13. 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.

  14. 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...

  15. Evaluation of the stability of a mixture of volatile organic compounds on sorbents for the determination of emissions from indoor materials and products using thermal desorption/gas chromatography/mass spectrometry.

    PubMed

    Brown, Veronica M; Crump, Derrick R; Plant, Neil T; Pengelly, Ian

    2014-07-11

    The standard method for the determination of volatile organic compounds (VOCs) in indoor and test chamber air (ISO 16000-6:2011) specifies sampling onto the sorbent Tenax TA followed by analysis using thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS). The informative Annex D to the standard suggests the use of multi-sorbent samplers to extend the volatility range of compounds which can be determined. The aim of this study was to investigate the storage performance of Tenax TA and two multi-sorbent tubes loaded with a mixture of nine VOCs of relevance for material emissions testing. The sorbent combinations tested were quartz wool/Tenax TA/Carbograph™ 5TD and quartz wool/Tenax TA/Carbopack™ X. A range of loading levels, loading conditions (humidities and air volume), storage times (1-4 weeks) and storage conditions (refrigerated and ambient) were investigated. Longer term storage trials (up to 1 year) were conducted with Tenax TA tubes to evaluate the stability of tubes used for proficiency testing (PT) of material emissions analyses. The storage performance of the multi-sorbent tubes tested was found to be equal to that for Tenax TA, with recoveries after 4 weeks storage of within about 10% of the amounts loaded. No consistent differences in recoveries were found for the different loading or storage conditions. The longer term storage trials also showed good recovery for these compounds, although two other compounds, hexanal and BHT, were found to be unstable when stored on Tenax TA. The results of this study provide confidence in the stability of nine analytes for up to 4 weeks on two multi-sorbent tubes for material emissions testing and the same compounds loaded on Tenax TA sorbent for a recently introduced PT scheme for material emissions testing.

  16. Characterization of biomass burning emissions from cooking fires, peat, crop residue, and other fuels with high-resolution proton-transfer-reaction time-of-flight mass spectrometry

    NASA Astrophysics Data System (ADS)

    Stockwell, C. E.; Veres, P. R.; Williams, J.; Yokelson, R. J.

    2015-01-01

    We deployed a high-resolution proton-transfer-reaction time-of-flight mass spectrometer (PTR-TOF-MS) to measure biomass-burning emissions from peat, crop residue, cooking fires, and many other fire types during the fourth Fire Lab at Missoula Experiment (FLAME-4) laboratory campaign. A combination of gas standard calibrations and composition sensitive, mass-dependent calibration curves was applied to quantify gas-phase non-methane organic compounds (NMOCs) observed in the complex mixture of fire emissions. We used several approaches to assign the best identities to most major "exact masses", including many high molecular mass species. Using these methods, approximately 80-96% of the total NMOC mass detected by the PTR-TOF-MS and Fourier transform infrared (FTIR) spectroscopy was positively or tentatively identified for major fuel types. We report data for many rarely measured or previously unmeasured emissions in several compound classes including aromatic hydrocarbons, phenolic compounds, and furans; many of these are suspected secondary organic aerosol precursors. A large set of new emission factors (EFs) for a range of globally significant biomass fuels is presented. Measurements show that oxygenated NMOCs accounted for the largest fraction of emissions of all compound classes. In a brief study of various traditional and advanced cooking methods, the EFs for these emissions groups were greatest for open three-stone cooking in comparison to their more advanced counterparts. Several little-studied nitrogen-containing organic compounds were detected from many fuel types, that together accounted for 0.1-8.7% of the fuel nitrogen, and some may play a role in new particle formation.

  17. Infrared Spectrometry.

    ERIC Educational Resources Information Center

    McDonald, Robert S.

    1984-01-01

    This review on infrared spectrometry covering the period from late 1981 to late 1983, is divided into nine sections. Topic areas include: books; reviews; analytical applications; biochemical applications; environmental applications; polymer applications; infrared instrumentation; sampling techniques; and software and algorithms. (JN)

  18. Laser sampling system for an inductively-coupled atomic emission spectrometer. Final report

    SciTech Connect

    1998-02-15

    A laser sampling system was attached to a Perkin Elmer Optima 3000 inductively-coupled plasma, atomic emission spectrometer that was already installed and operating in the Chemistry and Geochemistry Department at the Colorado School of Mines. The use of the spectrometer has been highly successful. Graduate students and faculty from at least four different departments across the CSM campus have used the instrument. The final report to NSF is appended to this final report. Appendices are included which summarize several projects utilizing this instrument: acquisition of an inductively-coupled plasma atomic emission spectrometer for the geochemistry program; hydrogen damage susceptibility assessment for high strength steel weldments through advanced hydrogen content analysis, 1996 and 1997 annual reports; and methods for determination of hydrogen distribution in high strength steel welds.

  19. NATURE OF UNRESOLVED COMPLEX MIXTURE IN SIZE-DISTRIBUTED EMISSIONS FROM RESIDENTIAL WOOD COMBUSTION AS MEASURED BY THERMAL DESORPTION-GAS CHROMATOGRAPHY-MASS SPECTROMETRY

    EPA Science Inventory

    In this study, the unresolved complex mixture (UCM) in size resolved fine aerosol emissions from residential wood combustion (RWC) is examined. The aerosols are sorted by size in an electrical low-pressure impactor (ELPI) and subsequently analyzed by thermal desorbtion/gas chroma...

  20. THE DETERMINATION OF MERCURY SPECIES AND MULTIPLE METALS IN COAL COMBUSTION EMISSIONS USING IODINE-BASED IMPINGERS AND DIRECT INJECTION NEBULIZATION - INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY ANALYSIS

    EPA Science Inventory

    Mercury (Hg) emissions from coal utilities are difficult to control. Hg eludes capture by most air pollution control devices (APCDs). To determine the gaseous Hg species in stack gases, U.S. EPA Method 5 type sampling is used. In this type of sampling a hole is drilled into th...

  1. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry. Progress report, January 1, 1994--December 31, 1994

    SciTech Connect

    Montaser, A.

    1994-09-01

    This research follows a multifaceted approach, from theory to practice, to the investigation and development of novel helium plasmas, sample introduction systems, and diagnostic techniques for atomic and mass spectrometries. During the period January 1994 - December 1994, four major sets of challenging research programs were addressed that each included a number of discrete but complementary projects: (1) The first program is concerned with fundamental and analytical investigations of novel atmospheric-pressure helium inductively coupled plasmas (He ICPS) that are suitable for the atomization-excitation-ionization of elements, especially those possessing high excitation and ionization energies, for the purpose of enhancing sensitivity and selectivity of analytical measurements. (2) The second program includes simulation and computer modeling of He ICPS. The aim is to ease the hunt for new helium plasmas by predicting their structure and fundamental and analytical properties, without incurring the enormous cost for extensive experimental studies. (3) The third program involves spectroscopic imaging and diagnostic studies of plasma discharges to instantly visualize their prevailing structures, to quantify key fundamental properties, and to verify predictions by mathematical models. (4) The fourth program entails investigation of new, low-cost sample introduction systems that consume micro- to nanoliter quantity of sample solution in plasma spectrometries. A portion of this research involves development and applications of novel diagnostic techniques suitable for probing key fundamental properties of aerosol prior to and after injection into high-temperature plasmas. These efforts, still in progress, collectively offer promise of solving singularly difficult analytical problems that either exist now or are likely to arise in the future in the various fields of energy generation, environmental pollution, material science, biomedicine and nutrition.

  2. Analysis of enantiomeric and non-enantiomeric monoterpenes in plant emissions using portable dynamic air sampling/solid-phase microextraction (PDAS-SPME) and chiral gas chromatography/mass spectrometry

    NASA Astrophysics Data System (ADS)

    Yassaa, Noureddine; Williams, Jonathan

    A portable dynamic air sampler (PDAS) using a porous polymer solid-phase microextraction (SPME) fibre has been validated for the determination of biogenic enantiomeric and non-enantiomeric monoterpenes in air. These compounds were adsorbed in the field, and then thermally desorbed at 250 °C in a gas chromatograph injector port connected via a β-cyclodextrin capillary separating column to a mass spectrometer. The optimized method has been applied for investigating the emissions of enantiomeric monoterpenes from Pseudotsuga menziesii (Douglas-fir), Rosmarinus officinalis (Rosemary) and Lavandula lanata (Lavender) which were selected as representative of coniferous trees and aromatic plants, respectively. The enantiomers of α-pinene, sabinene, camphene, δ-3-carene, β-pinene, limonene, β-phellandrene, 4-carene and camphor were successfully determined in the emissions from the three plants. While Douglas-fir showed a strong predominance toward (-)-enantiomers, Rosemary and Lavender demonstrated a large variation in enantiomeric distribution of monoterpenes. The simplicity, rapidity and sensitivity of dynamic sampling with porous polymer coated SPME fibres coupled to chiral capillary gas chromatography/mass spectrometry (GC/MS) makes this method potentially useful for in-field investigations of atmosphere-biosphere interactions and studies of optically explicit atmospheric chemistry.

  3. Fine-particle emissions from solid biofuel combustion studied with single-particle mass spectrometry: Identification of markers for organics, soot, and ash components

    NASA Astrophysics Data System (ADS)

    Pagels, Joakim; Dutcher, Dabrina D.; Stolzenburg, Mark R.; McMurry, Peter H.; GäLli, Markus E.; Gross, Deborah S.

    2013-01-01

    The effects of combustion phase and fuel on smoke particle emissions from a wood stove operated with three different wood fuels and from a corn stove were investigated. A single-particle mass spectrometer (aerosol time of flight mass spectrometer (ATOFMS)) was used for time- and size-resolved chemical signatures and a scanning mobility particle sizer (SMPS) was used for online mobility size distributions. Markers of particle phase organics and elemental carbon, PM1.5, and CO emissions were strongly reduced for the corn stove compared to the wood stove. This is because the more controlled fuel and air supply in the corn stove result in more complete combustion. NOx emissions and particle phase phosphates showed the opposite trend. Marker ions and particle types associated with soot and alkali salts such as potassium chloride and potassium sulfates dominated during flaming combustion and were correlated with increased exhaust temperatures and reduced CO emissions. Marker ions of hydrocarbons and oxidized organics as well as a particle cluster type with a strong organic signature were associated with reduced combustion temperature and increased CO levels, observed during start up from cold stove, addition of fuel, and combustion with reduced air supply. Two different particle types were identified in corn experiments when particles were classified according to mobility before they were measured with the ATOFMS. "Less massive" particles contained mostly ash and soot and had vacuum aerodynamic diameters that were nearly independent of mobility diameter. "More massive" particles had aerodynamic diameters that increased linearly with mobility diameter, indicating approximately spherical shapes, and were hypothesized to consist of organics.

  4. Characterization of primary organic aerosol emissions from meat cooking, trash burning, and motor vehicles with high-resolution aerosol mass spectrometry and comparison with ambient and chamber observations.

    PubMed

    Mohr, Claudia; Huffman, Alex; Cubison, Michael J; Aiken, Allison C; Docherty, Kenneth S; Kimmel, Joel R; Ulbrich, Ingrid M; Hannigan, Michael; Jimenez, Jose L

    2009-04-01

    Organic aerosol (OA) emissions from motor vehicles, meat-cooking and trash burning are analyzed here using a high-resolution aerosol mass spectrometer (AMS). High resolution data show that aerosols emitted by combustion engines and plastic burning are dominated by hydrocarbon-like organic compounds. Meat cooking and especially paper burning emissions contain significant fractions of oxygenated organic compounds; however, their unit-resolution mass spectral signatures are very similar to those from ambient hydrocarbon-like OA, and very different from the mass spectra of ambient secondary or oxygenated OA (OOA). Thus, primary OA from these sources is unlikelyto be a significant direct source of ambient OOA. There are significant differences in high-resolution tracer m/zs that may be useful for differentiating some of these sources. Unlike in most ambient spectra, all of these sources have low total m/z 44 and this signal is not dominated by the CO2+ ion. All sources have high m/z 57, which is low during high OOA ambient periods. Spectra from paper burning are similar to some types of biomass burning OA, with elevated m/z 60. Meat cooking aerosols also have slightly elevated m/z 60, whereas motor vehicle emissions have very low signal at this m/z.

  5. Real-time analysis of organic compounds in ship engine aerosol emissions using resonance-enhanced multiphoton ionisation and proton transfer mass spectrometry.

    PubMed

    Radischat, Christian; Sippula, Olli; Stengel, Benjamin; Klingbeil, Sophie; Sklorz, Martin; Rabe, Rom; Streibel, Thorsten; Harndorf, Horst; Zimmermann, Ralf

    2015-08-01

    Organic combustion aerosols from a marine medium-speed diesel engine, capable to run on distillate (diesel fuel) and residual fuels (heavy fuel oil), were investigated under various operating conditions and engine parameters. The online chemical characterisation of the organic components was conducted using a resonance-enhanced multiphoton ionisation time-of-flight mass spectrometer (REMPI TOF MS) and a proton transfer reaction-quadrupole mass spectrometer (PTR-QMS). Oxygenated species, alkenes and aromatic hydrocarbons were characterised. Especially the aromatic hydrocarbons and their alkylated derivatives were very prominent in the exhaust of both fuels. Emission factors of known health-hazardous compounds (e.g. mono- and poly-aromatic hydrocarbons) were calculated and found in higher amounts for heavy fuel oil (HFO) at typical engine loadings. Lower engine loads lead in general to increasing emissions for both fuels for almost every compound, e.g. naphthalene emissions varied for diesel fuel exhaust between 0.7 mg/kWh (75 % engine load, late start of injection (SOI)) and 11.8 mg/kWh (10 % engine load, late SOI) and for HFO exhaust between 3.3 and 60.5 mg/kWh, respectively. Both used mass spectrometric techniques showed that they are particularly suitable methods for online monitoring of combustion compounds and very helpful for the characterisation of health-relevant substances. Graphical abstract Three-dimensional REMPI data of organic species in diesel fuel and heavy fuel oil exhaust.

  6. Chandra X-ray Grating Spectrometry of Eta Carinae near X-ray Minimum: I. Variability of the Sulfur and Silicon Emission Lines

    NASA Technical Reports Server (NTRS)

    Henley, D. B.; Corcoran, M. F.; Pittard, J. M.; Stevens, I. R.; Hamaguchi, K.; Gull, T. R.

    2008-01-01

    We report on variations in important X-ray emission lines in a series of Chandra grating spectra of the supermassive colliding wind binary star eta Car, including key phases around the X-ray minimum/periastron passage in 2003.5. The X-rays arise from the collision of the slow, dense wind of eta Car with the fast, low-density wind of an otherwise hidden companion star. The X-ray emission lines provide the only direct measure of the flow dynamics of the companion's wind along the wind-wind collision zone. We concentrate here on the silicon and sulfur lines, which are the strongest and best resolved lines in the X-ray spectra. Most of the line profiles can be adequately fit with symmetric Gaussians with little significant skewness. Both the silicon and sulfur lines show significant velocity shifts and correlated increases in line widths through the observations. The R = forbidden-to-intercombination ratio from the Si XIII and S XV triplets is near or above the low-density limit in all observations, suggesting that the line-forming region is > 1.6 stellar radii from the companion star, and that the emitting plasma may be in a non-equilibrium state. We show that simple geometrical models cannot simultaneously fit both the observed centroid variations and changes in line width as a function of phase. We show that the observed profiles can be fitted with synthetic profiles with a reasonable model of the emissivity along the wind-wind collision boundary. We use this analysis to help constrain the line formation region as a function of orbital phase, and the orbital geometry. Subject headings: X-rays: stars -stars: early-type-stars: individual (q Car)

  7. Chandra X-Ray Grating Spectrometry of η Carinae near X-Ray Minimum. I. Variability of the Sulfur and Silicon Emission Lines

    NASA Astrophysics Data System (ADS)

    Henley, D. B.; Corcoran, M. F.; Pittard, J. M.; Stevens, I. R.; Hamaguchi, K.; Gull, T. R.

    2008-06-01

    We report on variations in important X-ray emission lines in a series of Chandra grating spectra of the supermassive colliding wind binary star η Car, including key phases around the X-ray minimum/periastron passage in 2003.5. The X-rays arise from the collision of the slow, dense wind of η Car with the fast, low-density wind of an otherwise hidden companion star. The X-ray emission lines provide the only direct measure of the flow dynamics of the companion's wind along the wind-wind collision zone. We concentrate here on the silicon and sulfur lines, which are the strongest and best-resolved lines in the X-ray spectra. Most of the line profiles can be adequately fit with symmetric Gaussians with little significant skewness. Both the silicon and sulfur lines show significant velocity shifts and correlated increases in line widths through the observations. The Script R = forbidden-to-intercombination ratio from the Si XIII and S XV triplets is near or above the low-density limit in all observations, suggesting that the line-forming region is >1.6 stellar radii from the companion star. We show that simple geometrical models cannot simultaneously fit both the observed centroid variations and changes in line width as a function of phase. We show that the observed profiles can be fitted with synthetic profiles with a reasonable model of the emissivity along the wind-wind collision boundary. We use this analysis to help constrain the line formation region as a function of orbital phase, and the orbital geometry.

  8. Characterization of Primary Organic Aerosol Emissions from Meat Cooking, Trash Burning, and Combustion Engines with High-Resolution Aerosol Mass Spectrometry and Comparison with Ambient and Chamber Observations

    NASA Astrophysics Data System (ADS)

    Mohr, C.; Huffman, J. A.; Cubison, M. J.; Aiken, A. C.; Docherty, K. S.; Kimmel, J. R.; Ulbrich, I. M.; Hannigan, M.; Garcia, J.; Jimenez, J. L.

    2009-04-01

    Organic aerosol (OA) emissions from motor vehicles, meat-cooking and trash burning are analyzed here using a high-resolution aerosol mass spectrometer (AMS) and supporting instrumentation. A semi-quantitative comparison of emission factors highlights the potential importance of meat cooking as an OA source. GC-MS and AMS mass spectra are compared for the first time and show high similarity, but with more fragmentation in the AMS due to higher vaporization temperatures. High resolution data show that aerosols emitted by combustion engines and plastic burning are dominated by hydrocarbon-like organic compounds. Meat cooking and especially paper burning contain significant fractions of oxygenated organic compounds; however, their unit-resolution mass spectral signatures are very similar to mass spectral signatures from hydrocarbon-like OA or primary OA, and very different from the mass spectra of ambient secondary or oxygenated OA (OOA). Thus, primary OA from any of these sources is very unlikely to be a significant direct source of ambient OOA. There are significant differences in high-resolution tracer m/z's that may be useful for differentiating these sources from each other. Unlike in most ambient spectra, all of these sources have low total m/z 44 and this signal is not dominated by the CO2+ ion. All sources have high m/z 57, which is low during high OOA ambient periods. Spectra from paper burning are similar to some types of biomass burning OA, with elevated m/z 60. Meat cooking aerosols also have slightly elevated m/z 60, while motor vehicle emissions have very low signal at this m/z.

  9. Determination of rare-earth elements, yttrium and scandium in manganese nodules by inductively-coupled argon-plastma emission spectrometry

    USGS Publications Warehouse

    Fries, T.; Lamothe, P.J.; Pesek, J.J.

    1984-01-01

    A sequential-scanning, inductively-coupled argon plasma emission spectrometer is used for the determination of the rare-earth elements, plus yttrium and scandium, in manganese nodules. Wavelength selection is optimized to minimize spectral interferences from manganese nodule components. Samples are decomposed with mixed acids in a sealed polycarbonate vessel, and elements are quantified without further treatment. Results for U.S. Geological Survey manganese nodule standards A-1 and P-1 had average relative standard deviations of 6.8% and 8.1%, respectively, and results were in good agreement with those obtained by other methods. ?? 1984.

  10. Characterization of submicron particles influenced by mixed biogenic and anthropogenic emissions using high-resolution aerosol mass spectrometry: results from CARES

    SciTech Connect

    Setyan, Ari; Zhang, Qi; Merkel, M.; Knighton, Walter B.; Sun, Y.; Song, Chen; Shilling, John E.; Onasch, Timothy B.; Herndon, Scott C.; Worsnop, Douglas R.; Fast, Jerome D.; Zaveri, Rahul A.; Berg, Larry K.; Wiedensohler, A.; Flowers, B. A.; Dubey, Manvendra K.; Subramanian, R.

    2012-09-11

    The Carbonaceous Aerosols and Radiative Effects Study (CARES) took place in the Sacramento Valley of California in summer 2010. We present results obtained at Cool, CA, the T1 site of the project ({approx}40 km downwind of urban emissions from Sacramento), where we deployed an Aerodyne high resolution time-of-flight aerosol mass spectrometer (HR-ToF-AMS) in parallel with complementary instrumentation to characterize the sources and processes of submicron particles (PM1). Cool is located at the foothill of the Sierra Nevada Mountains, where intense biogenic emissions are periodically mixed with urban outflow transported by daytime southwesterly winds from the Sacramento metropolitan area. The particle mass loading was low (3.0 {micro}gm{sup -3} on average) and dominated by organics (80% of the PM1 mass) followed by sulfate (9.9 %). Organics and sulfate appeared to be externally mixed, as suggested by their different time series (r2 = 0.13) and size distributions. Sulfate showed a bimodal distribution with a droplet mode peaking at {approx}400nm in vacuum aerodynamic diameter (Dva), and a condensation mode at {approx}150 nm, while organics generally displayed a broad distribution in 60-600nm (Dva). New particle formation and growth events were observed almost every day, emphasizing the roles of organics and sulfate in new particle growth, especially that of organics. The organic aerosol (OA) had a nominal formula of C{sub 1}H{sub 1.38}N{sub 0.004}O{sub 0.44}, thus an average organic mass-to-carbon (OM/OC) ratio of 1.70. Two different oxygenated OA (OOA, 90% of total OA mass) and a hydrocarbon-like OA (HOA, 10 %) were identified by Positive matrix factorization (PMF) of the high resolution mass spectra. The more oxidized MO-OOA (O/C = 0.54) corresponded to secondary OA (SOA) primarily influenced by biogenic emissions, while the less oxidized LO-OOA (O/C = 0.42) corresponded to SOA associated with urban transport. The HOA factor corresponded to primary emissions mainly

  11. Design and performance of a new continuous-flow sample-introduction system for flame infrared-emission spectrometry: Applications in process analysis, flow injection analysis, and ion-exchange high-performance liquid chromatography.

    PubMed

    Lam, C K; Zhang, Y; Busch, M A; Busch, K W

    1993-06-01

    A new sample introduction system for the analysis of continuously flowing liquid streams by flame infrared-emission (FIRE) spectrometry has been developed. The system uses a specially designed purge cell to strip dissolved CO(2) from solution into a hydrogen gas stream that serves as the fuel for a hydrogen/air flame. Vibrationally excited CO(2) molecules present in the flame are monitored with a simple infrared filter (4.4 mum) photometer. The new system can be used to introduce analytes as a continuous liquid stream (process analysis mode) or on a discrete basis by sample injection (flow injection analysis mode). The key to the success of the method is the new purge-cell design. The small internal volume of the cell minimizes problems associated with purge-cell clean-out and produces sharp, reproducible signals. Spent analytical solution is continuously drained from the cell, making cell disconnection and cleaning between samples unnecessary. Under the conditions employed in this study, samples could be analyzed at a maximum rate of approximately 60/h. The new sample introduction system was successfully tested in both a process analysis- and a flow injection analysis mode for the determination of total inorganic carbon in Waco tap water. For the first time, flame infrared-emission spectrometry was successfully extended to non-volatile organic compounds by using chemical pretreatment with peroxydisulfate in the presence of silver ion to convert the analytes into dissolved carbon dioxide, prior to purging and detection by the FIRE radiometer. A test of the peroxydisulfate/Ag(+) reaction using six organic acids and five sugars indicated that all 11 compounds were oxidized to nearly the same extent. Finally, the new sample introduction system was used in conjunction with a simple filter FIRE radiometer as a detection system in ion-exchange high-performance liquid chromatography. Ion-exchange chromatograms are shown for two aqueous mixtures, one containing six organic

  12. Anthropogenic sources of aerosol particles in a football stadium: Real-time characterization of emissions from cigarette smoking, cooking, hand flares, and color smoke bombs by high-resolution aerosol mass spectrometry

    NASA Astrophysics Data System (ADS)

    Faber, Peter; Drewnick, Frank; Veres, Patrick R.; Williams, Jonathan; Borrmann, Stephan

    2013-10-01

    Aerosol particles from several anthropogenic sources associated with football stadia including cooking, cigarette smoking, burning of color smoke bombs and hand flares were analyzed by high-resolution aerosol mass spectrometry. The physical and chemical characteristics of these different aerosols, in particular the organic fraction, were explored in laboratory studies to obtain robust references. These data were compared with field campaign results from a Bundesliga (German football league) match in the Coface Arena (Mainz, Germany) on 20th April 2012. The field measurement revealed a strongly elevated mass concentration of organic aerosols (OA) compared to background levels showing a temporal structure clearly related to the match. PMF analysis established that during the football match event cigarette smoke was the predominant component of submicron organic aerosol (67% of total OA). Cooking emissions from food outlets within the stadium correlated well with the sales figures of the catering stations and were also found to be of relevance (24% of total OA) especially in the period before kickoff. Pyrotechnics were not observed during this football match and no signatures of these sources were found in the mass spectra from the stadium measurements. All species that were elevated during the football match returned to their initial background levels within one hour after the match had finished. This demonstrates a good ventilation capacity of the open-topped Coface Arena.

  13. Determination of calcium, copper, iron, magnesium, manganese, potassium, phosphorus, sodium, and zinc in fortified food products by microwave digestion and inductively coupled plasma-optical emission spectrometry: single-laboratory validation and ring trial.

    PubMed

    Poitevin, Eric

    2012-01-01

    A single-laboratory validation (SLV) and a ring trial (RT) were undertaken to determine nine nutritional elements in food products by inductively coupled plasma-optical emission spectrometry in order to modernize AOAC Official Method 984.27. The improvements involved extension of the scope to all food matrixes (including infant formula), optimized microwave digestion, selected analytical lines, internal standardization, and ion buffering. Simultaneous determination of nine elements (calcium, copper, iron, potassium, magnesium, manganese, sodium, phosphorus, and zinc) was made in food products. Sample digestion was performed through wet digestion of food samples by microwave technology with either closed- or open-vessel systems. Validation was performed to characterize the method for selectivity, sensitivity, linearity, accuracy, precision, recovery, ruggedness, and uncertainty. The robustness and efficiency of this method was proven through a successful RT using experienced independent food industry laboratories. Performance characteristics are reported for 13 certified and in-house reference materials, populating the AOAC triangle food sectors, which fulfilled AOAC criteria and recommendations for accuracy (trueness, recovery, and z-scores) and precision (repeatability and reproducibility RSD, and HorRat values) regarding SLVs and RTs. This multielemental method is cost-efficient, time-saving, accurate, and fit-for-purpose according to ISO 17025 Norm and AOAC acceptability criteria, and is proposed as an extended updated version of AOAC Official Method 984.27 for fortified food products, including infant formula. PMID:22468357

  14. Restricted accessed material-copper(II) ion imprinted polymer solid phase extraction combined with inductively coupled plasma-optical emission spectrometry for the determination of free Cu(II) in urine and serum samples.

    PubMed

    Cui, Chao; He, Man; Chen, Beibei; Hu, Bin

    2013-11-15

    A novel restricted accessed material (RAM)-Cu(II) ion imprinted polymer (IIP) was synthesized by the surface imprinted-emulsion method, and possessed a high selectivity to Cu(II) and good macromolecules exclusion property. And a novel method of RAM-IIP packed microcolumn solid phase extraction (SPE) combined with inductively coupled plasma-optical emission spectrometry (ICP-OES) was developed for the determination of trace free Cu(II) in human body fluids. Under the optimized conditions, the adsorption capacity of RAM-IIP for Cu(II) was 15.9 mg g(-1). With a preconcentration factor of 30, the limit of detection was 0.17 µg L(-1), and the relative standard deviation was 2.2% (n=7, c=1 µg L(-1)). The developed method was validated by the analysis of two Certified Reference Materials, and the determined values were in good agreement with the certified values. This method was also successfully applied for the direct analysis of free Cu(II) in human urine and serum samples. While the total Cu can be determined by the proposed method after microwave digestion. The concentrations of free Cu(II) were much lower than that of total Cu, indicating that Cu is mainly coordinated with macromolecules in these biological samples. From this point of view, the developed method exhibits application potential in speciation of free metal ions and metallic complex molecules in biological samples. PMID:24148513

  15. Determination of cadmium(II), cobalt(II), nickel(II), lead(II), zinc(II), and copper(II) in water samples using dual-cloud point extraction and inductively coupled plasma emission spectrometry.

    PubMed

    Zhao, Lingling; Zhong, Shuxian; Fang, Keming; Qian, Zhaosheng; Chen, Jianrong

    2012-11-15

    A dual-cloud point extraction (d-CPE) procedure has been developed for simultaneous pre-concentration and separation of heavy metal ions (Cd2+, Co2+, Ni2+, Pb2+, Zn2+, and Cu2+ ion) in water samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on forming complexes of metal ion with 8-hydroxyquinoline (8-HQ) into the as-formed Triton X-114 surfactant rich phase. Instead of direct injection or analysis, the surfactant rich phase containing the complexes was treated by nitric acid, and the detected ions were back extracted again into aqueous phase at the second cloud point extraction stage, and finally determined by ICP-OES. Under the optimum conditions (pH=7.0, Triton X-114=0.05% (w/v), 8-HQ=2.0×10(-4) mol L(-1), HNO3=0.8 mol L(-1)), the detection limits for Cd2+, Co2+, Ni2+, Pb2+, Zn2+, and Cu2+ ions were 0.01, 0.04, 0.01, 0.34, 0.05, and 0.04 μg L(-1), respectively. Relative standard deviation (RSD) values for 10 replicates at 100 μg L(-1) were lower than 6.0%. The proposed method could be successfully applied to the determination of Cd2+, Co2+, Ni2+, Pb2+, Zn2+, and Cu2+ ion in water samples.

  16. Internal standardization for the determination of cadmium, cobalt, chromium and manganese in saline produced water from petroleum industry by inductively coupled plasma optical emission spectrometry after cloud point extraction

    NASA Astrophysics Data System (ADS)

    Bezerra, Marcos Almeida; Mitihiro do Nascimento Maêda, Sérgio; Oliveira, Eliane Padua; de Fátima Batista de Carvalho, Maria; Santelli, Ricardo Erthal

    2007-09-01

    In the present paper a procedure is proposed for the determination of traces of Cd, Co, Mn and Cr in petroleum industry produced water by inductively coupled plasma optical emission spectrometry. The procedure is based on cloud point extraction of these metals, as their dithizonate complexes, into the surfactant-rich phase of octylphenoxypolyethoxyethanol surfactant (Triton X-114). Extractions were carried out in solutions with salinities between 10‰ and 70‰. Since residual salinity in the surfactant-rich phase caused differences in its transport to the plasma, yttrium was used as an internal standard to correct for this effect. The simultaneous metal extraction procedure was optimized by response surface methodology using a Doehlert design and desirability function. Enhancement factors of 21, 21, 9 and 19, along with limits of quantification of 0.093, 0.20, 0.73 and 1.2 μg L - 1 , and precision expressed as relative standard deviation ( n = 8, 20.0 μg L - 1 ) of 5.8, 1.2, 1.7 and 5.7% were obtained for Cd, Co, Mn and Cr, respectively. The accuracy was evaluated by spike recovery tests on the high salinity water samples with salinity of 40 and 63‰.

  17. CHAPTER 7. BERYLLIUM ANALYSIS BY NON-PLASMA BASED METHODS

    SciTech Connect

    Ekechukwu, A

    2009-04-20

    The most common method of analysis for beryllium is inductively coupled plasma atomic emission spectrometry (ICP-AES). This method, along with inductively coupled plasma mass spectrometry (ICP-MS), is discussed in Chapter 6. However, other methods exist and have been used for different applications. These methods include spectroscopic, chromatographic, colorimetric, and electrochemical. This chapter provides an overview of beryllium analysis methods other than plasma spectrometry (inductively coupled plasma atomic emission spectrometry or mass spectrometry). The basic methods, detection limits and interferences are described. Specific applications from the literature are also presented.

  18. Inductively coupled plasma optical emission spectrometry for trace multi-element determination in vegetable oils, margarine and butter after stabilization with propan-1-ol and water

    NASA Astrophysics Data System (ADS)

    de Souza, Roseli M.; Mathias, Bárbara M.; da Silveira, Carmem Lúcia P.; Aucélio, Ricardo Q.

    2005-06-01

    The quantitative evaluation of trace elements in foodstuffs is of considerable interest due to the potential toxicity of many elements, and because the presence of some metallic species might affect the overall quality (flavor and stability) of these products. In the present work, an inductively coupled plasma optical emission spectrometric method has been developed for the determination of six elements (Cd, Co, Cr, Cu, Ni and Mn) in olive oil, soy oil, margarine and butter. Organic samples (oils and fats) were stabilized using propan-1-ol and water, which enabled long-time sample dispersion in the solution. This simple sample preparation procedure, together with an efficient sample introduction strategy (using a Meinhard K3 nebulizer and a twister cyclonic spray chamber), facilitated the overall analytical procedure, allowing quantification using calibration curves prepared with inorganic standards. Internal standardization (Sc) was used for correction of matrix effects and signal fluctuations. Good sensitivities with limits of detection in the ng g -1 range were achieved for all six elements. These sensitivities were appropriate for the intended application. The method was tested through the analysis of laboratory-fortified samples with good recoveries (between 91.3% and 105.5%).

  19. Particulate-matter distribution and its flow from power plants using infrared spectrometry and thermodynamics for in situ continuous emissions monitoring

    NASA Astrophysics Data System (ADS)

    Shlifshteyn, Alex; Lang, Fred D.; Ayrapetian, Robert

    1996-01-01

    Spectroscopy measurements made through a continuum having suspended particulate matter are addressed. The applications presented permit correction of spectral transmissions as effected by particulate-producing fossil-fuel combustion. The research is especially applicable to large effluent flows from coal-fired power plants, whose effluents are studied with in situ (smokestack) radiometers. Methods involving fast calculation procedures based on measured irradiances in unabsorbed regions of the IR spectrum are presented. The methodology is based on wavelength-dependent extinction of radiation by small particles, considering both elastic scattering and absorbing effects. This extinction leads to an observed skeweness (or shift) of the blackbody spectral shape. Based on such skeweness, the particulate number distribution is determined with Mie theory. In order to simplify, and to speed up the routine for real-time application, a two-step procedure is presented. During preinstallation calibration with Mie theory, sets of integral tables are computed for all possible solution values and stored in computer memory. Based on instantaneous spectral measurements, the appropriate integral tables are retrieved, then used as inputs in a process leading to particulate number distribution. Because all time-consuming calculations associated with Mie theory are performed during preinstallation calibration, the technique is capable of monitoring particulate emission in real time. Furthermore, given resolution of the number distribution in combination with thermodynamic analysis of the system, determination of particulate apparent density and particulate mass flow rate is made. These values have importance for environmental reporting. Comparisons of calculated particulate distributions with in situ measurements are also presented. Confirmatory testing programs conducted at several power plants are discussed.

  20. Single event mass spectrometry

    DOEpatents

    Conzemius, Robert J.

    1990-01-16

    A means and method for single event time of flight mass spectrometry for analysis of specimen materials. The method of the invention includes pulsing an ion source imposing at least one pulsed ion onto the specimen to produce a corresponding emission of at least one electrically charged particle. The emitted particle is then dissociated into a charged ion component and an uncharged neutral component. The ion and neutral components are then detected. The time of flight of the components are recorded and can be used to analyze the predecessor of the components, and therefore the specimen material. When more than one ion particle is emitted from the specimen per single ion impact, the single event time of flight mass spectrometer described here furnis This invention was made with Government support under Contract No. W-7405-ENG82 awarded by the Department of Energy. The Government has certain rights in the invention.

  1. Evaluation of sample preparation methods for the detection of total metal content using inductively coupled plasma optical emission spectrometry (ICP-OES) in wastewater and sludge

    NASA Astrophysics Data System (ADS)

    Dimpe, K. M.; Ngila, J. C.; Mabuba, N.; Nomngongo, P. N.

    Heavy metal contamination exists in aqueous wastes and sludge of many industrial discharges and domestic wastewater, among other sources. Determination of metals in the wastewater and sludge requires sample pre-treatment prior to analysis because of certain challenges such as the complexity of the physical state of the sample, which may lead to wrong readings in the measurement. This is particularly the case with low analyte concentration to be detected by the instrument. The purpose of this work was to assess and validate the different sample preparation methods namely, hot plate and microwave-assisted digestion procedures for extraction of metal ions in wastewater and sludge samples prior to their inductively coupled plasma optical emission spectrometric (ICP-OES) determination. For the extraction of As, Al, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Zn, three acid mixtures, that is, HNO3/H2O2, HNO3/HClO4/H2O2 and aqua regia + H2O2, were evaluated. Influent wastewater spiked with the SRM (CWW-TM-B) was used for the optimization of acid mixtures affecting the extraction procedure. After sample digestion, the filtration capabilities of cellulose-acetate filter paper and the acrodisc syringe filter with the pore size of 0.45 μm were compared. In terms of performance, acrodisc syringe filter in terms of the improved recoveries obtained, was found to be the best filtration method compared to the filter paper. Based on the analytical results obtained, microwave-assisted digestion (MAD) using aqua regia + H2O2 mixture was found to be the most suitable method for extraction of heavy metals and major elements in all the sample matrices. Therefore, MAD using aqua regia + H2O2 mixture was used for further investigations. The precision of the developed MAD method expressed in terms of relative standard deviations (% RSD) for different metals was found to be <5%. The limits of detection (LOD) and limits of quantification (LOQ) ranged from 0.12% to 2.18 μg L-1 and 0.61% to 3.43 μg L-1

  2. Chitosan modified ordered mesoporous silica as micro-column packing materials for on-line flow injection-inductively coupled plasma optical emission spectrometry determination of trace heavy metals in environmental water samples.

    PubMed

    Chen, Dahui; Hu, Bin; Huang, Chaozhang

    2009-04-30

    A novel adsorbent of chitosan chemically modified ordered mesoporous silica was synthesized and employed as a solid phase extraction (SPE) material for flow injection (FI) micro-column preconcentration on-line coupled with inductively coupled plasma optical emission spectrometry (ICP-OES) determination of trace heavy metals V, Cu, Pb, Cd and Hg in environmental water samples. The factors affecting separation and preconcentration of target heavy metals such as pH, sample flow rate and volume, eluent concentration and volume, interfering ions were investigated. Under the optimized experimental conditions, an enrichment factor of 20 and sampling frequency of 10h(-1) were obtained. The detection limits of the method for V, Cu, Pb, Cd and Hg were 0.33, 0.30, 0.96, 0.05 and 0.93 ng mL(-1), and the relative standard deviations (RSDs) were 2.8%, 6.7%, 1.8%, 4.0% and 5.3% (n=7, C=10 ng mL(-1)), respectively. The adsorption capacities of chitosan modified ordered mesoporous silica for V, Cu, Pb, Cd, and Hg were found to be 16.3, 21.7, 22.9, 12.2 and 13.5 mg g(-1), respectively. In order to validate the developed method, a certified reference material of GSBZ50009-88 environmental water sample was analyzed and the determined values were in good agreement with the certified values. The proposed method has also been applied to the determination of trace heavy metals in natural water samples with satisfactory results.

  3. Solid Phase Extraction of Trace Elements in Waterand Tissue Samples on a Mini Column with Diphenylcarbazone Impregnated Nano-TiO2 and Their Determination by Inductively Coupled Plasma Optical Emission Spectrometry

    PubMed Central

    Baytak, Sıtkı; Arslan, Zikri

    2015-01-01

    This study presents a simple, robust and environmentally friendly solid phase preconcentration procedure for multielement determination by inductively coupled plasma optical emission spectrometry (ICP-OES) using diphenylcarbazone (DPC) impregnated TiO2 nanopowder (n-TiO2). DPC was successfully impregnated onto n-TiO2 in colloidal solution. A number of elements, including Co(II), Cr(III), Cu(II), Fe(III), Mn(II) and Zn(II) were quantitatively preconcentrated from aqueous solutions between pH 8 and 8.5 at a flow rate of 2 mL min−1, and then eluted with 2 mL of 5% (v/v) HNO3. A mini-column packed with 0.12 g DPC impregnated n-TiO2 retained all elements quantitatively from up to 250 mL multielement solution (2.5 μg per analyte) affording an enrichment factor of 125. The limits of detection (LOD) for preconcentration of 50 mL blank solutions (n = 12) were 0.28, 0.15, 0.25, 0.22, 0.12, and 0.10 μg L−1 for Co, Cr, Cu, Fe, Mn, and Zn, respectively. The relative standard deviation (RSD) for five replicate determinations was 0.8, 3.4, 2.6, 2.2, 1.2 and 3.3% for Co, Cr, Cu, Fe, Mn and Zn, respectively, at 5 μg L−1 level. The method was validated with analysis of Freshwater (SRM 1643e) and Lobster hepatopancreas (TORT-2) certified reference materials, and then applied to the determination of the elements from tap water and lake water samples by ICP-OES. PMID:26236403

  4. Charge trapping characteristics of Au nanocrystals embedded in remote plasma atomic layer-deposited Al{sub 2}O{sub 3} film as the tunnel and blocking oxides for nonvolatile memory applications

    SciTech Connect

    Lee, Jaesang; Kim, Hyungchul; Park, Taeyong; Ko, Youngbin; Ryu, Jaehun; Jeon, Heeyoung; Park, Jingyu; Jeon, Hyeongtag

    2012-01-15

    Remote plasma atomic layer deposited (RPALD) Al{sub 2}O{sub 3} films were investigated to apply as tunnel and blocking layers in the metal-oxide-semiconductor capacitor memory utilizing Au nanocrystals (NCs) for nonvolatile memory applications. The interface stability of an Al{sub 2}O{sub 3} film deposited by RPALD was studied to observe the effects of remote plasma on the interface. The interface formed during RPALD process has high oxidation states such as Si{sup +3} and Si{sup +4}, indicating that RPALD process can grow more stable interface which has a small amount of fixed oxide trap charge. The significant memory characteristics were also observed in this memory device through the electrical measurement. The memory device exhibited a relatively large memory window of 5.6 V under a 10/-10 V program/erase voltage and also showed the relatively fast programming/erasing speed and a competitive retention characteristic after 10{sup 4} s. These results indicate that Al{sub 2}O{sub 3} films deposited via RPALD can be applied as the tunnel and blocking oxides for next-generation flash memory devices.

  5. Trapping effect on a small molecular drug with vascular-disrupting agent CA4P in rodent H22 hepatic tumor model: in vivo magnetic resonance imaging and postmortem inductively coupled plasma atomic emission spectroscopy.

    PubMed

    Gao, Meng; Yao, Nan; Huang, Dejian; Jiang, Cuihua; Feng, Yuanbo; Li, Yue; Lou, Bin; Peng, Fei; Sun, Ziping; Ni, Yicheng; Zhang, Jian

    2015-06-01

    The aim of the present study is to verify the trapping effect of combretastatin A-4-phosphate (CA4P) on small molecular drugs in rodent tumors. Mice with H22 hepatocarcinoma were randomized into groups A and B. Magnetic resonance imaging (MRI) of T1WI, T2WI, and DWI was performed as baseline. Mice in group A were injected with Gd-DTPA and PBS. Mice in group B were injected with Gd-DTPA and CA4P. All mice undergo CE-T1WI at 0 h, 3 h, 6 h, 12 h, and 24 h. Enhancing efficacy of the two groups on CE-T1WI was compared with the signal-to-noise ratio (SNR) calculated. Concentrations of gadolinium measured by ICP-AES in the tumor were compared between groups. On the early CE-T1WI, tumors were equally enhanced in both groups. On the delayed CE-T1WI, the enhancing effect of group A was weaker than that of group B. The SNR and the concentration of gadolinium within the tumor of group A were lower than that of group B at 6 h, 12 h, and 24 h after administration. This study indicates that CA4P could improve the retention of Gd-DTPA in the tumor and MRI allowed dynamically monitoring trapping effects of CA4P on local retention of Gd-DTPA as a small molecular drug.

  6. The evaluation of the x-ray fluorescence (XRF) technique for process monitoring of vitreous slag from thermal waste treatment systems: A comparative study of the analysis of Plasma Hearth slag for Ce, Fe and Cr by XRF and inductively coupled plasma spectrometries

    SciTech Connect

    Sutton, M.A.H.; Crane, P.J.; Cummings, D.G.; Carney, K.P.

    1995-05-01

    Slag material produced by the Plasma Hearth Process (PHP) varies in chemical composition due to the heterogeneous nature of the input sample feed. X-ray fluorescence (XRF) is a spectroscopic technique which has been evaluated to perform elemental analyses on surrogate slag material for process control. Vitreous slag samples were ground to a fine powder in an impact ball mill and analyzed directly using laboratory prepared standards. The fluorescent intensities of Si, Al and Fe in the slag samples was utilized to determine the appropriate matrix standard set for the determination of Ce. The samples were analyzed for Cr, Ni, Fe and Ce using a wavelength dispersive XRF polychromator. Split samples were dissolved and analyzed by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES). The precision of the XRF technique was better than 5% RSD. The limit of detection for Ce varied with sample matrix and was typically below 0.01% by weight. The linear dynamic range for the technique was evaluated over two orders of magnitude. Typical calibration standards ranged from 0.01% Ce to 1% Ce. The Ce determinations performed directly on ground slag material by the XRF techniques were similar to ICP-AES analyses. Various chemical dissolution and sample preparation techniques were evaluated for the analysis of Ce in slag samples. A fusion procedure utilizing LiBO{sub 2} was found to provide reliable analyses for the actinide surrogate in a variety of slag matrices. The use of the XRF technique reduced the time of analysis for Ce and Cr from three days to one day for five samples. No additional waste streams were created from the analyses by the XRF technique, while the ICP technique generated several liters of liquid waste.

  7. Measurement of Iron in Egg Yolk: An Instrumental Analysis Experiment Using Biochemical Principles

    ERIC Educational Resources Information Center

    Maloney, Kevin M.; Quiazon, Emmanuel M.; Indralingam, Ramee

    2008-01-01

    The generally accepted method to determine iron content in food is by acid digestion or dry ashing and subsequent flame atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry. We have developed an experiment that chemically extracts the iron from an egg yolk and quantifies it using UV-vis absorption…

  8. Nuclear Magnetic Resonance Spectrometry.

    ERIC Educational Resources Information Center

    Wasson, John R.; Salinas, Jorge E.

    1980-01-01

    Reviews current research in NMR spectrometry, in the areas of apparatus and techniques, spectral analysis, computer applications, analytical applications, and selected organic and inorganic systems. Various aspects of NMR spectrometry are presented in tabular form, with 133 references. Listed also are 124 references from the discussions in the…

  9. Mass spectrometry in India.

    PubMed

    Vairamani, M; Prabhakar, S

    2012-01-01

    This review emphasizes the mass spectrometry research being performed at academic and established research institutions in India. It consists of three main parts covering the work done in organic, atomic and biological mass spectrometry. The review reveals that the use of mass spectrometry techniques started in the middle of the 20th century and was applied to research in the fields of organic, nuclear, geographical and atomic chemistry. Later, with the advent of soft and atmospheric ionization techniques it has been applied to pharmaceutical and biological research. In due course, several research centers with advanced mass spectrometry facilities have been established for specific areas of research such as gas-phase ion chemistry, ion-molecule reactions, proscribed chemicals, pesticide residues, pharmacokinetics, protein/peptide chemistry, nuclear chemistry, geochronological studies, archeology, petroleum industry, proteomics, lipidomics and metabolomics. Day-by-day the mass spectrometry centers/facilities in India have attracted young students for their doctoral research and other advanced research applications.

  10. Characteristics of WN{sub x}C{sub y} films deposited using remote plasma atomic layer deposition with ({sup Me}Cp)W(CO){sub 2}(NO) for Cu diffusion barrier

    SciTech Connect

    Kim, Hyunjung; Park, Jingyu; Jeon, Heeyoung; Jang, Woochool; Jeon, Hyeongtag; Yuh, Junhan

    2015-09-15

    Diffusion barrier characteristics of tungsten–nitride–carbide (WN{sub x}C{sub y}) thin films interposed between Cu and SiO{sub 2} layers were studied. The WN{sub x}C{sub y} films were deposited by remote plasma atomic layer deposition (RPALD) using a metal organic source, ({sup Me}Cp)W(CO){sub 2}(NO), and ammonia. Auger electron spectroscopy analysis indicated the WN{sub x}C{sub y} films consisted of tungsten, nitrogen, carbon, and oxygen. X-ray diffraction (XRD) analysis showed that the film deposited at 350 °C was nanocrystalline. The resistivity of WN{sub x}C{sub y} film deposited by RPALD was very low compared to that in previous research because of the lower nitrogen content and different crystal structures of the WN{sub x}C{sub y}. To verify the diffusion barrier characteristics of the WN{sub x}C{sub y} film, Cu films were deposited by physical vapor deposition after WN{sub x}C{sub y} film was formed by RPALD on Si substrate. The Cu/WN{sub x}C{sub y}/Si film stack was annealed in a vacuum by rapid thermal annealing at 500 °C. Cu diffusion through the barrier layer was verified by XRD. Stable film properties were observed up to 500 °C, confirming that WN{sub x}C{sub y} film is suitable as a Cu diffusion barrier in microelectronic circuits.

  11. Method of trivalent chromium concentration determination by atomic spectrometry

    DOEpatents

    Reheulishvili, Aleksandre N.; Tsibakhashvili, Neli Ya.

    2006-12-12

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

  12. Reactive plasma atomization of aluminum nitride powder

    SciTech Connect

    Prichard, P.; Besser, M.; Sordelet, D.; Anderson, I.

    1997-02-01

    Experiments were performed to synthesize AlN powders by reacting Al with N using a conventional dc arc plasma as heat source. Feeding Al powder into Ar/N plasma open to atmosphere produced mainly Al oxide. Experiments using a chamber backfilled with nitrogen suppressed the Al oxide, but little AlN was formed. A furnace and crucible assembly was designed to feed molten Al directly into a DeLaval nozzle attached to the face of the dc arc plasma gun. Resulting submicron powders show a significant increase in AlN formation. This was dependent on chamber pressure, plasma velocity, and molten liquid feed rate. Experimental parameters, equipment design, effects of atomization/vaporization/condensation are discussed.

  13. Forensic Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Hoffmann, William D.; Jackson, Glen P.

    2015-07-01

    Developments in forensic mass spectrometry tend to follow, rather than lead, the developments in other disciplines. Examples of techniques having forensic potential born independently of forensic applications include ambient ionization, imaging mass spectrometry, isotope ratio mass spectrometry, portable mass spectrometers, and hyphenated chromatography-mass spectrometry instruments, to name a few. Forensic science has the potential to benefit enormously from developments that are funded by other means, if only the infrastructure and personnel existed to adopt, validate, and implement the new technologies into casework. Perhaps one unique area in which forensic science is at the cutting edge is in the area of chemometrics and the determination of likelihood ratios for the evaluation of the weight of evidence. Such statistical techniques have been developed most extensively for ignitable-liquid residue analyses and isotope ratio analysis. This review attempts to capture the trends, motivating forces, and likely impact of developing areas of forensic mass spectrometry, with the caveat that none of this research is likely to have any real impact in the forensic community unless: (a) The instruments developed are turned into robust black boxes with red and green lights for positives and negatives, respectively, or (b) there are PhD graduates in the workforce who can help adopt these sophisticated techniques.

  14. Time-resolved analysis of the emission of sidestream smoke (SSS) from cigarettes during smoking by photo ionisation/time-of-flight mass spectrometry (PI-TOFMS): towards a better description of environmental tobacco smoke.

    PubMed

    Streibel, T; Mitschke, S; Adam, T; Zimmermann, R

    2013-09-01

    In this study, the chemical composition of sidestream smoke (SSS) emissions of cigarettes are characterised using a laser-based single-photon ionisation time-of-flight mass spectrometer. SSS is generated from various cigarette types (2R4F research cigarette; Burley, Oriental and Virginia single-tobacco-type cigarettes) smoked on a single-port smoking machine and collected using a so-called fishtail chimney device. Using this setup, a puff-resolved quantification of several SSS components was performed. Investigations of the dynamics of SSS emissions show that concentration profiles of various substances can be categorised into several groups, either depending on the occurrence of a puff or uninfluenced by the changes in the burning zone during puffing. The SSS emissions occurring directly after a puff strongly resemble the composition of mainstream smoke (MSS). In the smouldering phase, clear differences between MSS and SSS are observed. The changed chemical profiles of SSS and MSS might be also of importance on environmental tobacco smoke which is largely determined by SSS. Additionally, the chemical composition of the SSS is strongly affected by the tobacco type. Hence, the higher nitrogen content of Burley tobacco leads to the detection of increased amounts of nitrogen-containing substances in SSS.

  15. Fourier transform mass spectrometry.

    PubMed

    Scigelova, Michaela; Hornshaw, Martin; Giannakopulos, Anastassios; Makarov, Alexander

    2011-07-01

    This article provides an introduction to Fourier transform-based mass spectrometry. The key performance characteristics of Fourier transform-based mass spectrometry, mass accuracy and resolution, are presented in the view of how they impact the interpretation of measurements in proteomic applications. The theory and principles of operation of two types of mass analyzer, Fourier transform ion cyclotron resonance and Orbitrap, are described. Major benefits as well as limitations of Fourier transform-based mass spectrometry technology are discussed in the context of practical sample analysis, and illustrated with examples included as figures in this text and in the accompanying slide set. Comparisons highlighting the performance differences between the two mass analyzers are made where deemed useful in assisting the user with choosing the most appropriate technology for an application. Recent developments of these high-performing mass spectrometers are mentioned to provide a future outlook.

  16. Environmental Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Lebedev, Albert T.

    2013-06-01

    Environmental mass spectrometry is an important branch of science because it provides many of the data that underlie policy decisions that can directly influence the health of people and ecosystems. Environmental mass spectrometry is currently undergoing rapid development. Among the most relevant directions are a significant broadening of the lists of formally targeted compounds; a parallel interest in nontarget chemicals; an increase in the reliability of analyses involving accurate mass measurements, tandem mass spectrometry, and isotopically labeled standards; and a shift toward faster high-throughput analysis, with minimal sample preparation, involving various approaches, including ambient ionization techniques and miniature instruments. A real revolution in analytical chemistry could be triggered with the appearance of robust, simple, and sensitive portable mass spectrometers that can utilize ambient ionization techniques. If the cost of such instruments is reduced to a reasonable level, mass spectrometers could become valuable household devices.

  17. Fourier Transform Mass Spectrometry

    PubMed Central

    Scigelova, Michaela; Hornshaw, Martin; Giannakopulos, Anastassios; Makarov, Alexander

    2011-01-01

    This article provides an introduction to Fourier transform-based mass spectrometry. The key performance characteristics of Fourier transform-based mass spectrometry, mass accuracy and resolution, are presented in the view of how they impact the interpretation of measurements in proteomic applications. The theory and principles of operation of two types of mass analyzer, Fourier transform ion cyclotron resonance and Orbitrap, are described. Major benefits as well as limitations of Fourier transform-based mass spectrometry technology are discussed in the context of practical sample analysis, and illustrated with examples included as figures in this text and in the accompanying slide set. Comparisons highlighting the performance differences between the two mass analyzers are made where deemed useful in assisting the user with choosing the most appropriate technology for an application. Recent developments of these high-performing mass spectrometers are mentioned to provide a future outlook. PMID:21742802

  18. Ion Mobility Spectrometry (IMS) and Mass Spectrometry

    SciTech Connect

    Shvartsburg, Alexandre A.

    2010-04-20

    In a media of finite viscosity, the Coulomb force of external electric field moves ions with some terminal speed. This dynamics is controlled by “mobility” - a property of the interaction potential between ions and media molecules. This fact has been used to separate and characterize gas-phase ions in various modes of ion mobility spectrometry (IMS) developed since 1970. Commercial IMS devices were introduced in 1980-s for field detection of volatile traces such as explosives and chemical warfare agents. Coupling to soft-ionization sources, mass spectrometry (MS), and chromatographic methods in 1990-s had allowed IMS to handle complex samples, enabling new applications in biological and environmental analyses, nanoscience, and other areas. Since 2003, the introduction of commercial systems by major instrument vendors started bringing the IMS/MS capability to broad user community. The other major development of last decade has been the differential IMS or “field asymmetric waveform IMS” (FAIMS) that employs asymmetric time-dependent electric field to sort ions not by mobility itself, but by the difference between its values in strong and weak electric fields. Coupling of FAIMS to conventional IMS and stacking of conventional IMS stages have enabled two-dimensional separations that dramatically expand the power of ion mobility methods.

  19. Ambient ionization mass spectrometry

    NASA Astrophysics Data System (ADS)

    Lebedev, A. T.

    2015-07-01

    Ambient ionization mass spectrometry emerged as a new scientific discipline only about ten years ago. A considerable body of information has been reported since that time. Keeping the sensitivity, performance and informativity of classical mass spectrometry methods, the new approach made it possible to eliminate laborious sample preparation procedures and triggered the development of miniaturized instruments to work directly in the field. The review concerns the theoretical foundations and design of ambient ionization methods. Their advantages and drawbacks, as well as prospects for application in chemistry, biology, medicine, environmetal analysis, etc., are discussed. The bibliography includes 194 references.

  20. Analytical mass spectrometry

    SciTech Connect

    Not Available

    1990-01-01

    This 43rd Annual Summer Symposium on Analytical Chemistry was held July 24--27, 1990 at Oak Ridge, TN and contained sessions on the following topics: Fundamentals of Analytical Mass Spectrometry (MS), MS in the National Laboratories, Lasers and Fourier Transform Methods, Future of MS, New Ionization and LC/MS Methods, and an extra session. (WET)

  1. Analytical mass spectrometry. Abstracts

    SciTech Connect

    Not Available

    1990-12-31

    This 43rd Annual Summer Symposium on Analytical Chemistry was held July 24--27, 1990 at Oak Ridge, TN and contained sessions on the following topics: Fundamentals of Analytical Mass Spectrometry (MS), MS in the National Laboratories, Lasers and Fourier Transform Methods, Future of MS, New Ionization and LC/MS Methods, and an extra session. (WET)

  2. MASS SPECTROMETRY IN ENVIRONMENTAL SCIENCES

    EPA Science Inventory

    This review covers applications of mass spectrometry to the environmental sciences. From the early applications of mass spectrometry to environmental research in the 1960s and 1970s, mass spectrometry has played an important role in aiding our understanding of environmental poll...

  3. Development of a hydrophilic interaction liquid chromatography-mass spectrometry method for detection and quantification of urea thermal decomposition by-products in emission from diesel engine employing selective catalytic reduction technology.

    PubMed

    Yassine, Mahmoud M; Dabek-Zlotorzynska, Ewa; Celo, Valbona

    2012-03-16

    The use of urea based selective catalytic reduction (SCR) technology for the reduction of NOx from the exhaust of diesel-powered vehicles has the potential to emit at least six thermal decomposition by-products, ammonia, and unreacted urea from the tailpipe. These compounds may include: biuret, dicyandiamine, cyanuric acid, ammelide, ammeline and melamine. In the present study, a simple, sensitive and reliable hydrophilic interaction liquid chromatography (HILIC)-electrospray ionization (ESI)/mass spectrometry (MS) method without complex sample pre-treatment was developed for identification and determination of urea decomposition by-products in diesel exhaust. Gradient separation was performed on a SeQuant ZIC-HILIC column with a highly polar zwitterionic stationary phase, and using a mobile phase consisting of acetonitrile (eluent A) and 15 mM ammonium formate (pH 6; eluent B). Detection and quantification were performed using a quadrupole ESI/MS operated simultaneously in negative and positive mode. With 10 μL injection volume, LODs for all target analytes were in the range of 0.2-3 μg/L. The method showed a good inter-day precision of retention time (RSD<0.5%) and peak area (RSD<3%). Satisfactory extraction recoveries from spiked blanks ranged between 96 and 98%. Analyses of samples collected during transient chassis dynamometer tests of a bus engine equipped with a diesel particulate filter (DPF) and urea based SCR technology showed the presence of five target analytes with cyanuric acid and ammelide the most abundant compounds in the exhaust.

  4. Multielement plant tissue analysis using ICP spectrometry.

    PubMed

    Hansen, T H; de Bang, T C; Laursen, K H; Pedas, P; Husted, S; Schjoerring, J K

    2013-01-01

    Plant tissue analysis is a valuable tool for evaluating the nutritional status and quality of crops and is widely used for scientific and commercial purposes. The majority of plant analyzes are now performed by techniques based on ICP spectrometry such as inductively coupled plasma-optical emission spectroscopy (ICP-OES) or ICP-mass spectrometry (ICP-MS). These techniques enable fast and accurate measurements of multielement profiles when combined with appropriate methods for sample preparation and digestion. This chapter presents state-of-the-art methods for digestion of plant tissues and subsequent analysis of their multielement composition by ICP spectrometry. Details on upcoming techniques, expected to gain importance within the field of multielement plant tissue analysis over the coming years, are also provided. Finally, attention is given to laser ablation ICP-MS (LA-ICP-MS) for multielement bioimaging of plant tissues. The presentation of the methods covers instructions on all steps from sampling and sample preparation to data interpretation. PMID:23073880

  5. Hydrogen Exchange Mass Spectrometry.

    PubMed

    Mayne, Leland

    2016-01-01

    Hydrogen exchange (HX) methods can reveal much about the structure, energetics, and dynamics of proteins. The addition of mass spectrometry (MS) to an earlier fragmentation-separation HX analysis now extends HX studies to larger proteins at high structural resolution and can provide information not available before. This chapter discusses experimental aspects of HX labeling, especially with respect to the use of MS and the analysis of MS data.

  6. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; use of a modified ultrasonic nebulizer for the analysis of low ionic-strength water by inductively coupled optical emission spectrometry

    USGS Publications Warehouse

    Harris, Carl M.; Litteral, Charles J.; Damrau, Donna L.

    1997-01-01

    The U.S. Geological Survey National Water Quality Laboratory has developed a method for the determination of dissolved calcium, iron, magnesium, manganese, silica, and sodium using a modified ultrasonic nebulizer sample-introduction system to an inductively coupled plasma-optical emission spectrometer. The nebulizer's spray chamber has been modified to avoid carryover and memory effects common in some conventional ultrasonic designs. The modified ultrasonic nebulizer is equipped with a high-speed rinse cycle to remove previously analyzed samples from the spray chamber without excessive flush times. This new rinse cycle decreases sample washout times by reducing carryover and memory effects from salt or analytes in previously analyzed samples by as much as 45 percent. Plasma instability has been reduced by repositioning the argon carrier gas inlet on the spray chamber and by directly pumping waste from the chamber, instead of from open drain traps, thereby maintaining constant pressure to the plasma. The ultrasonic nebulizer improves signal intensities, which are 8 to 16 times greater than for a conventional cross-flow pneumatic nebulizer, without being sensitive to clogging from salt buildup as in cross-flow nebulizers. Detection limits for the ultrasonic nebulizer are 4 to 18 times less than detection limits achievable using a cross-flow pneumatic nebulizer, with equivalent sample analysis time.

  7. Mass spectrometry with accelerators.

    PubMed

    Litherland, A E; Zhao, X-L; Kieser, W E

    2011-01-01

    As one in a series of articles on Canadian contributions to mass spectrometry, this review begins with an outline of the history of accelerator mass spectrometry (AMS), noting roles played by researchers at three Canadian AMS laboratories. After a description of the unique features of AMS, three examples, (14)C, (10)Be, and (129)I are given to illustrate the methods. The capabilities of mass spectrometry have been extended by the addition of atomic isobar selection, molecular isobar attenuation, further ion acceleration, followed by ion detection and ion identification at essentially zero dark current or ion flux. This has been accomplished by exploiting the techniques and accelerators of atomic and nuclear physics. In 1939, the first principles of AMS were established using a cyclotron. In 1977 the selection of isobars in the ion source was established when it was shown that the (14)N(-) ion was very unstable, or extremely difficult to create, making a tandem electrostatic accelerator highly suitable for assisting the mass spectrometric measurement of the rare long-lived radioactive isotope (14)C in the environment. This observation, together with the large attenuation of the molecular isobars (13)CH(-) and (12)CH 2(-) during tandem acceleration and the observed very low background contamination from the ion source, was found to facilitate the mass spectrometry of (14)C to at least a level of (14)C/C ~ 6 × 10(-16), the equivalent of a radiocarbon age of 60,000 years. Tandem Accelerator Mass Spectrometry, or AMS, has now made possible the accurate radiocarbon dating of milligram-sized carbon samples by ion counting as well as dating and tracing with many other long-lived radioactive isotopes such as (10)Be, (26)Al, (36)Cl, and (129)I. The difficulty of obtaining large anion currents with low electron affinities and the difficulties of isobar separation, especially for the heavier mass ions, has prompted the use of molecular anions and the search for alternative

  8. Spectrometry of nebulae

    NASA Astrophysics Data System (ADS)

    Acker, A.

    2011-04-01

    Nebular emission lines are easy to observe, and their spectrum contains a lot of information. We explain the mechanisms of production of the emissions, and the relation between the intensity of the recombination and forbidden lines, and the physical parameters of the objects. A gallery of emission lines spectra is presented, and a rough analysis will clarify their differences. The case of Planetary Nebulae will be developed, in order to determine the extinction constant, the plasma parameters (electron density and temperature), the chemical abundances, and also the properties of the central star (temperature, mass, stellar wind velocity, age).

  9. 40 CFR Appendix C to Part 136 - Determination of Metals and Trace Elements in Water and Wastes by Inductively Coupled Plasma...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... Code of Federal Regulation (40 CFR Part 136 Table 1B for NPDES, and Part 141 § 141.23 for drinking... Safety and Health Standards, General Industry, (29 CFR 1910), Occupational Safety and Health... Elements in Water and Wastes by Inductively Coupled Plasma-Atomic Emission Spectrometry Method 200.7...

  10. 40 CFR Appendix C to Part 136 - Determination of Metals and Trace Elements in Water and Wastes by Inductively Coupled Plasma...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... Code of Federal Regulation (40 CFR Part 136 Table 1B for NPDES, and Part 141 § 141.23 for drinking... Safety and Health Standards, General Industry, (29 CFR 1910), Occupational Safety and Health... Elements in Water and Wastes by Inductively Coupled Plasma-Atomic Emission Spectrometry Method 200.7...

  11. Questa baseline and pre-mining ground water investigation; 11, Geochemistry of composited material from alteration scars and mine-waste piles

    USGS Publications Warehouse

    Briggs, P.H.; Sutley, S.J.; Livo, Keith Eric

    2003-01-01

    Composited, surficial material was collected from alteration scars, a less intensely altered site, and mine-waste piles. All samples were analyzed for forty elements by inductively coupled plasma-atomic emission spectrometry, total sulfur and quantitative X-ray diffraction. This work was performed in cooperation with the New Mexico Environment Department.

  12. "Magic" Ionization Mass Spectrometry.

    PubMed

    Trimpin, Sarah

    2016-01-01

    The systematic study of the temperature and pressure dependence of matrix-assisted ionization (MAI) led us to the discovery of the seemingly impossible, initially explained by some reviewers as either sleight of hand or the misinterpretation by an overzealous young scientist of results reported many years before and having little utility. The “magic” that we were attempting to report was that with matrix assistance, molecules, at least as large as bovine serum albumin (66 kDa), are lifted into the gas phase as multiply charged ions simply by exposure of the matrix:analyte sample to the vacuum of a mass spectrometer. Applied heat, a laser, or voltages are not necessary to achieve charge states and ion abundances only previously observed with electrospray ionization (ESI). The fundamentals of how solid phase volatile or nonvolatile compounds are converted to gas-phase ions without added energy currently involves speculation providing a great opportunity to rethink mechanistic understanding of ionization processes used in mass spectrometry. Improved understanding of the mechanism(s) of these processes and their connection to ESI and matrix-assisted laser desorption/ionization may provide opportunities to further develop new ionization strategies for traditional and yet unforeseen applications of mass spectrometry. This Critical Insights article covers developments leading to the discovery of a seemingly magic ionization process that is simple to use, fast, sensitive, robust, and can be directly applied to surface characterization using portable or high performance mass spectrometers. PMID:26486514

  13. "Magic" Ionization Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Trimpin, Sarah

    2016-01-01

    The systematic study of the temperature and pressure dependence of matrix-assisted ionization (MAI) led us to the discovery of the seemingly impossible, initially explained by some reviewers as either sleight of hand or the misinterpretation by an overzealous young scientist of results reported many years before and having little utility. The "magic" that we were attempting to report was that with matrix assistance, molecules, at least as large as bovine serum albumin (66 kDa), are lifted into the gas phase as multiply charged ions simply by exposure of the matrix:analyte sample to the vacuum of a mass spectrometer. Applied heat, a laser, or voltages are not necessary to achieve charge states and ion abundances only previously observed with electrospray ionization (ESI). The fundamentals of how solid phase volatile or nonvolatile compounds are converted to gas-phase ions without added energy currently involves speculation providing a great opportunity to rethink mechanistic understanding of ionization processes used in mass spectrometry. Improved understanding of the mechanism(s) of these processes and their connection to ESI and matrix-assisted laser desorption/ionization may provide opportunities to further develop new ionization strategies for traditional and yet unforeseen applications of mass spectrometry. This Critical Insights article covers developments leading to the discovery of a seemingly magic ionization process that is simple to use, fast, sensitive, robust, and can be directly applied to surface characterization using portable or high performance mass spectrometers.

  14. "Magic" Ionization Mass Spectrometry.

    PubMed

    Trimpin, Sarah

    2016-01-01

    The systematic study of the temperature and pressure dependence of matrix-assisted ionization (MAI) led us to the discovery of the seemingly impossible, initially explained by some reviewers as either sleight of hand or the misinterpretation by an overzealous young scientist of results reported many years before and having little utility. The “magic” that we were attempting to report was that with matrix assistance, molecules, at least as large as bovine serum albumin (66 kDa), are lifted into the gas phase as multiply charged ions simply by exposure of the matrix:analyte sample to the vacuum of a mass spectrometer. Applied heat, a laser, or voltages are not necessary to achieve charge states and ion abundances only previously observed with electrospray ionization (ESI). The fundamentals of how solid phase volatile or nonvolatile compounds are converted to gas-phase ions without added energy currently involves speculation providing a great opportunity to rethink mechanistic understanding of ionization processes used in mass spectrometry. Improved understanding of the mechanism(s) of these processes and their connection to ESI and matrix-assisted laser desorption/ionization may provide opportunities to further develop new ionization strategies for traditional and yet unforeseen applications of mass spectrometry. This Critical Insights article covers developments leading to the discovery of a seemingly magic ionization process that is simple to use, fast, sensitive, robust, and can be directly applied to surface characterization using portable or high performance mass spectrometers.

  15. Automated standardization technique for an inductively-coupled plasma emission spectrometer

    USGS Publications Warehouse

    Garbarino, J.R.; Taylor, H.E.

    1982-01-01

    The manifold assembly subsystem described permits real-time computer-controlled standardization and quality control of a commercial inductively-coupled plasma atomic emission spectrometer. The manifold assembly consists of a branch-structured glass manifold, a series of microcomputer-controlled solenoid valves, and a reservoir for each standard. Automated standardization involves selective actuation of each solenoid valve that permits a specific mixed standard solution to be pumped to the nebulizer of the spectrometer. Quality control is based on the evaluation of results obtained for a mixed standard containing 17 analytes, that is measured periodically with unknown samples. An inaccurate standard evaluation triggers restandardization of the instrument according to a predetermined protocol. Interaction of the computer-controlled manifold assembly hardware with the spectrometer system is outlined. Evaluation of the automated standardization system with respect to reliability, simplicity, flexibility, and efficiency is compared to the manual procedure. ?? 1982.

  16. International Mass Spectrometry Society (IMSS).

    PubMed

    Cooks, R G; Gelpi, E; Nibbering, N M

    2001-02-01

    This paper gives a brief description of the recently formalized International Mass Spectrometry Society (IMSS). It is presented here in order to increase awareness of the opportunities for collaboration in mass spectrometry in an international context. It also describes the recent 15th International Mass Spectrometry Conference, held August/September 2000, in Barcelona. Each of the authors is associated with the IMSS. The 15th Conference, which covers all of mass spectrometry on a triennial basis, was chaired by Professor Emilio Gelpi of the Instituto de Investigaciones Biomedicas, Barcelona. The outgoing and founding President of the IMSS is Professor Graham Cooks, Purdue University, and the incoming President is Professor Nico Nibbering, University of Amsterdam. Similar material has been provided to the Editors of other journals that cover mass spectrometry.

  17. Apparatus for studying premixed laminar flames using mass spectrometry and fiber-optic spectrometry

    NASA Astrophysics Data System (ADS)

    Olsson, Jim O.; Andersson, Lars L.; Lenner, Magnus; Simonson, Margaret

    1990-03-01

    An integrated flat-flame/ microprobe sampling quadrupole mass spectrometer system, complemented by optical spectrometry based on optical fibers, is presented. The short microprobe sampling line (total 25 cm) is directly connected to an open ion source closely flanked by two nude cryopumps (900 l/s) yielding a background pressure of 10-9 Torr and a sampling pressure of about 10-5 Torr. Due to this improved microprobe system, mass spectrometry can be used for analysis of stable species (including fuel, O2, H2O, CO2, CO, and Ar) with less disturbance of the sample than with a conventional microprobe with a back pressure of about 1 Torr. Optical spectrometry is used for the study of emission from important radical species (such as C2, CH, and OH). The system is proposed as a complement to more conventional flat-flame/MBMS systems in which the sampling cone can effect the experimental system. Details are provided concerning the configuration of the whole system ranging from gas delivery to data evaluation. Test data are presented for a 16% methanol/68% oxygen/16% argon flame studied at a pressure of 40 Torr, to elucidate the special features of this system.

  18. Developments in ion mobility spectrometry-mass spectrometry.

    PubMed

    Collins, D C; Lee, M L

    2002-01-01

    Ion mobility spectrometry (IMS) has been used for over 30 years as a sensitive detector of organic compounds. The following is a brief review of IMS and its principles with an emphasis on its usage when coupled to mass spectrometry. Since its inception, IMS has been interfaced with quadrupole, time-of-flight, and Fourier-transform ion cyclotron resonance mass spectrometry. These hybrid instruments have been employed for the analysis of a variety of target analytes, including biomolecules, explosives, chemical warfare degradation products, and illicit drugs. PMID:11939214

  19. Observation of infrared emission spectra from silicon combustion products

    NASA Astrophysics Data System (ADS)

    Smit, Kenneth J.; De Yong, Leo V.; Gray, Rodney

    1996-05-01

    The combustion of silicon based pyrotechnic compositions is observed with time resolved infrared spectrometry. This revealed the build up of strong emission at 9.1 ± 0.1 μm, which is associated with condensed silicon dioxide particulates. Time averaged spectra for compositions containing different oxidants or binders illustrate the dependence of SiO 2 emission intensity on composition.

  20. Two new advanced forms of spectrometry for space and commercial applications

    NASA Technical Reports Server (NTRS)

    Schlager, Kenneth J.

    1991-01-01

    Reagentless ultraviolet absorption spectrometry (UVAS) and Liquid Atomic Emission Spectrometry (LAES) represent new forms of spectrometry with extensive potential in both space and commercial applications. Originally developed under KSC sponsorship for monitoring nutrient solutions for the Controlled Ecological Life Support System (CELSS), both UVAS and LAES have extensive analytical capabilities for both organic and inorganic chemical compounds. Both forms of instrumentation involve the use of remote fiber optic probes and real-time measurements for on-line process monitoring. Commercial applications exist primarily in environmental analysis and for process control in the chemical, pulp and paper, food processing, metal plating, and water/wastewater treatment industries.

  1. An inductively coupled plasma carbon emission detector for aqueous carbohydrate separations by liquid chromatography.

    PubMed

    Peters, H L; Levine, K E; Jones, B T

    2001-02-01

    An inductively coupled plasma atomic emission spectrometer is used to detect carbon-containing compounds following separation by high-performance liquid chromatography. A calcium form ligand exchange column with distilled and deionized water as the mobile phase is used to separate carbohydrates. The eluting species are detected by monitoring the carbon atomic emission line at 193.09 nm. The mass detection limits using a photomultiplier tube for sucrose and glucose are 50 ng, while that for fructose is 60 ng. The carbon emission detector should provide the same detection limit for any compound with a similar mass percent of carbon, whether or not the compound exhibits appreciable absorption characteristics. While the carbon emission detector will universally detect any organic compound, it will discriminate against species with high molar absorptivity that may be present at low concentration. Such species may act as interferences in chromatograms generated with conventional UV-visible absorption detectors. To demonstrate the utility of the carbon emission detector, three sugars (glucose, fructose, sucrose) are determined in apple, crangrape, and orange juice.

  2. Biomedical accelerator mass spectrometry

    NASA Astrophysics Data System (ADS)

    Freeman, Stewart P. H. T.; Vogel, John S.

    1995-05-01

    Ultrasensitive SIMS with accelerator based spectrometers has recently begun to be applied to biomedical problems. Certain very long-lived radioisotopes of very low natural abundances can be used to trace metabolism at environmental dose levels ( [greater-or-equal, slanted] z mol in mg samples). 14C in particular can be employed to label a myriad of compounds. Competing technologies typically require super environmental doses that can perturb the system under investigation, followed by uncertain extrapolation to the low dose regime. 41Ca and 26Al are also used as elemental tracers. Given the sensitivity of the accelerator method, care must be taken to avoid contamination of the mass spectrometer and the apparatus employed in prior sample handling including chemical separation. This infant field comprises the efforts of a dozen accelerator laboratories. The Center for Accelerator Mass Spectrometry has been particularly active. In addition to collaborating with groups further afield, we are researching the kinematics and binding of genotoxins in-house, and we support innovative uses of our capability in the disciplines of chemistry, pharmacology, nutrition and physiology within the University of California. The field can be expected to grow further given the numerous potential applications and the efforts of several groups and companies to integrate more the accelerator technology into biomedical research programs; the development of miniaturized accelerator systems and ion sources capable of interfacing to conventional HPLC and GMC, etc. apparatus for complementary chemical analysis is anticipated for biomedical laboratories.

  3. Clinical protein mass spectrometry.

    PubMed

    Scherl, Alexander

    2015-06-15

    Quantitative protein analysis is routinely performed in clinical chemistry laboratories for diagnosis, therapeutic monitoring, and prognosis. Today, protein assays are mostly performed either with non-specific detection methods or immunoassays. Mass spectrometry (MS) is a very specific analytical method potentially very well suited for clinical laboratories. Its unique advantage relies in the high specificity of the detection. Any protein sequence variant, the presence of a post-translational modification or degradation will differ in mass and structure, and these differences will appear in the mass spectrum of the protein. On the other hand, protein MS is a relatively young technique, demanding specialized personnel and expensive instrumentation. Many scientists and opinion leaders predict MS to replace immunoassays for routine protein analysis, but there are only few protein MS applications routinely used in clinical chemistry laboratories today. The present review consists of a didactical introduction summarizing the pros and cons of MS assays compared to immunoassays, the different instrumentations, and various MS protein assays that have been proposed and/or are used in clinical laboratories. An important distinction is made between full length protein analysis (top-down method) and peptide analysis after enzymatic digestion of the proteins (bottom-up method) and its implication for the protein assay. The document ends with an outlook on what type of analyses could be used in the future, and for what type of applications MS has a clear advantage compared to immunoassays.

  4. Accelerator mass spectrometry.

    PubMed

    Hellborg, Ragnar; Skog, Göran

    2008-01-01

    In this overview the technique of accelerator mass spectrometry (AMS) and its use are described. AMS is a highly sensitive method of counting atoms. It is used to detect very low concentrations of natural isotopic abundances (typically in the range between 10(-12) and 10(-16)) of both radionuclides and stable nuclides. The main advantages of AMS compared to conventional radiometric methods are the use of smaller samples (mg and even sub-mg size) and shorter measuring times (less than 1 hr). The equipment used for AMS is almost exclusively based on the electrostatic tandem accelerator, although some of the newest systems are based on a slightly different principle. Dedicated accelerators as well as older "nuclear physics machines" can be found in the 80 or so AMS laboratories in existence today. The most widely used isotope studied with AMS is 14C. Besides radiocarbon dating this isotope is used in climate studies, biomedicine applications and many other fields. More than 100,000 14C samples are measured per year. Other isotopes studied include 10Be, 26Al, 36Cl, 41Ca, 59Ni, 129I, U, and Pu. Although these measurements are important, the number of samples of these other isotopes measured each year is estimated to be less than 10% of the number of 14C samples.

  5. Methods for Neutron Spectrometry

    DOE R&D Accomplishments Database

    Brockhouse, Bertram N.

    1961-01-09

    The appropriate theories and the general philosophy of methods of measurement and treatment of data neutron spectrometry are discussed. Methods of analysis of results for liquids using the Van Hove formulation, and for crystals using the Born-von Karman theory, are reviewed. The most useful of the available methods of measurement are considered to be the crystal spectrometer methods and the pulsed monoenergetic beam/time-of-flight method. Pulsed-beam spectrometers have the advantage of higher counting rates than crystal spectrometers, especially in view of the fact that simultaneous measurements in several counters at different angles of scattering are possible in pulsed-beam spectrometers. The crystal spectrometer permits several valuable new types of specialized experiments to be performed, especially energy distribution measurements at constant momentum transfer. The Chalk River triple-axis crystal-spectrometer is discussed, with reference to its use in making the specialized experiments. The Chalk River rotating crystal (pulsed-beam) spectrometer is described, and a comparison of this type instrument with other pulsed-beam spectrometers is made. A partial outline of the theory of operation of rotating-crystal spectrometers is presented. The use of quartz-crystal filters for fast neutron elimination and for order elimination is discussed. (auth)

  6. Field-Domain Ion Spectrometry

    NASA Technical Reports Server (NTRS)

    Bowers, W. D.; Chuan, R. L.

    1992-01-01

    Field-domain ion spectrometry (FDIS) is variant of established technique known as ion-mobility spectrometry. Operates at atmospheric pressure and only requires small pump to draw air sample into instrument. Strength of retarding electric field varied to distinguish among ions of different mobilities. New concept offers potential for development of small, (hand-held), low-power, portable devices detecting airborne chemical substances in real-time at concentrations at parts-per-billion level.

  7. Fraunhofer effect atomic absorption spectrometry.

    PubMed

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

    2005-02-15

    The dark lines in the solar spectrum were discovered by Wollaston and cataloged by Fraunhofer in the early days of the 19th century. Some years later, Kirchhoff explained the appearance of the dark lines: the sun was acting as a continuum light source and metals in the ground state in its atmosphere were absorbing characteristic narrow regions of the spectrum. This discovery eventually spawned atomic absorption spectrometry, which became a routine technique for chemical analysis in the mid-20th century. Laboratory-based atomic absorption spectrometers differ from the original observation of the Fraunhofer lines because they have always employed a separate light source and atomizer. This article describes a novel atomic absorption device that employs a single source, the tungsten coil, as both the generator of continuum radiation and the atomizer of the analytes. A 25-microL aliquot of sample is placed on the tungsten filament removed from a commercially available 150-W light bulb. The solution is dried and ashed by applying low currents to the coil in a three-step procedure. Full power is then applied to the coil for a brief period. During this time, the coil produces white light, which may be absorbed by any metals present in the atomization cloud produced by the sample. A high-resolution spectrometer with a charge-coupled device detector monitors the emission spectrum of the coil, which includes the dark lines from the metals. Detection limits are reported for seven elements: 5 pg of Ca (422.7 nm); 2 ng of Co (352.7 nm); 200 pg of Cr (425.4 nm); 7 pg of Sr (460.7 nm); 100 pg of Yb (398.8 nm); 500 pg of Mn (403.1 nm); and 500 pg of K (404.4 nm). Simultaneous multielement analyses are possible within a 4-nm spectral window. The relative standard deviations for the seven metals are below 8% for all metals except for Ca (10.7%), which was present in the blank at measurable levels. Analysis of a standard reference material (drinking water) resulted in a mean percent

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

    NASA Astrophysics Data System (ADS)

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

    2000-07-01

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

  9. Mass spectrometry. [in organic chemistry

    NASA Technical Reports Server (NTRS)

    Burlingame, A. L.; Shackleton, C. H. L.; Howe, I.; Chizhov, O. S.

    1978-01-01

    A review of mass spectrometry in organic chemistry is given, dealing with advances in instrumentation and computer techniques, selected topics in gas-phase ion chemistry, and applications in such fields as biomedicine, natural-product studies, and environmental pollution analysis. Innovative techniques and instrumentation are discussed, along with chromatographic-mass spectrometric on-line computer techniques, mass spectral interpretation and management techniques, and such topics in gas-phase ion chemistry as electron-impact ionization and decomposition, photoionization, field ionization and desorption, high-pressure mass spectrometry, ion cyclotron resonance, and isomerization reactions of organic ions. Applications of mass spectrometry are examined with respect to bio-oligomers and their constituents, biomedically important substances, microbiology, environmental organic analysis, and organic geochemistry.

  10. Symposium on accelerator mass spectrometry

    SciTech Connect

    1981-01-01

    The area of accelerator mass spectrometry has expanded considerably over the past few years and established itself as an independent and interdisciplinary research field. Three years have passed since the first meeting was held at Rochester. A Symposium on Accelerator Mass Spectrometry was held at Argonne on May 11-13, 1981. In attendance were 96 scientists of whom 26 were from outside the United States. The present proceedings document the program and excitement of the field. Papers are arranged according to the original program. A few papers not presented at the meeting have been added to complete the information on the status of accelerator mass spectrometry. Individual papers were prepared separately for the data base.

  11. Imaging mass spectrometry in microbiology

    PubMed Central

    Watrous, Jeramie D.; Dorrestein, Pieter C.

    2013-01-01

    Mass spectrometry tools which allow for the 2-D visualization of the distribution of trace metals, metabolites, surface lipids, peptides and proteins directly from biological samples without the need for chemical tagging or antibodies are becoming increasingly useful for microbiology applications. These tools, comprised of different imaging mass spectrometry techniques, are ushering in an exciting new era of discovery by allowing for the generation of chemical hypotheses based on of the spatial mapping of atoms and molecules that can correlate to or transcend observed phenotypes. In this review, we explore the wide range of imaging mass spectrometry techniques available to microbiologists and describe their unique applications to microbiology with respect to the types of microbiology samples to be investigated. PMID:21822293

  12. Purification of silicon powder by the formation of thin porous layer followed byphoto-thermal annealing.

    PubMed

    Khalifa, Marouan; Hajji, Messaoud; Ezzaouia, Hatem

    2012-08-08

    Porous silicon has been prepared using a vapor-etching based technique on a commercial silicon powder. Strong visible emission was observed in all samples. Obtained silicon powder with a thin porous layer at the surface was subjected to a photo-thermal annealing at different temperatures under oxygen atmosphere followed by a chemical treatment. Inductively coupled plasma atomic emission spectrometry results indicate that silicon purity is improved from 99.1% to 99.994% after annealing at 900°C.

  13. Mass spectrometry for biomarker development

    SciTech Connect

    Wu, Chaochao; Liu, Tao; Baker, Erin Shammel; Rodland, Karin D.; Smith, Richard D.

    2015-06-19

    Biomarkers potentially play a crucial role in early disease diagnosis, prognosis and targeted therapy. In the past decade, mass spectrometry based proteomics has become increasingly important in biomarker development due to large advances in technology and associated methods. This chapter mainly focuses on the application of broad (e.g. shotgun) proteomics in biomarker discovery and the utility of targeted proteomics in biomarker verification and validation. A range of mass spectrometry methodologies are discussed emphasizing their efficacy in the different stages in biomarker development, with a particular emphasis on blood biomarker development.

  14. Determination of metal content in valerian root phytopharmaceutical derivatives by atomic spectrometry.

    PubMed

    Arce, Silvia; Cerutti, Soledad; Olsina, Roberto; Gomez, María R; Martínez, Luis D

    2005-01-01

    Phytopharmaceuticals containing Valerian are used as mild sleep-inducing agents. The elemental composition of 3 different marks of Valeriana officinalis roots commercially available in the Argentinian market, their teas, and a commercial tincture have been studied. The content of Al, Ca, Cd, Co, Cr, Cu, Fe, Li, Mn, Ni, Pb, V, and Zn was determined in phytopharmaceuticals by flame atomic emission/absorption spectrometry, electrothermal atomic absorption spectrometry, and ultrasonic nebulization coupled to inductively coupled plasma-optical emission spectrometry. Prior to analyses of the samples, a digestion procedure was optimized. The analytical results obtained for Fe, Al, Ca, and V in the solid sample study were within the range 100-1000 mg/kg, and for Mn, Zn, and Pb within the range 10-100 mg/kg. Cadmium was found at levels up to 0.0125 mg/kg. PMID:15759744

  15. Innovating spectrometry studies at undergraduate level using a linear CCD array

    NASA Astrophysics Data System (ADS)

    Garg, Amit; Sharma, Reena; Dhingra, Vishal

    2011-10-01

    Students are less enthused in performing various spectrometry experiments in a conventional optics laboratory at the undergraduate level. In order to motivate students towards spectrometry, the present development focuses on innovating spectrometry experiments in undergraduate optics laboratory by integrating a linear CCD (Charge Coupled Device) for optical intensity capture using LabVIEW based application and a Digital Storage Oscilloscope with NI LabVIEW Signal Express. In the first step, students have calibrated wavelength in terms of x- position using a standard Mercury light source. Then this calibration has been used to display and measure the emission spectra of various light sources. Various measurements performed include characterizing various LEDs in terms of wavelengths emitted for use in measurement of Planck's constant, measuring characteristic wavelengths in emission spectra of hydrogen lamp (for calculating Rydberg's constant).

  16. [Research Progress in Analytical Technology for Heavy Metals in Atmospheric Particles].

    PubMed

    Wang, Yu-jie; Tu, Zhen-quan; Zhou, Li; Chi, Yong-jie; Luo, Qin

    2015-04-01

    Atmospheric particles have become the primary atmospheric pollutions, of which the heavy metals, owing to non-degradability and hysteresis, a serious threat to human life and natural environment, have become a hot research issue currently. The analytical methods of heavy metals in atmospheric particles are summarized in the present review, including atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry, inductively coupled plasma mass spectrometry, neutron activation analysis, fluorescence spectrometry, glow discharge atomic emission spectrometry, microwave plasma atomic emission spectrometry, and laser induced breakdown spectroscopy, and some proposals are tried to make for improving the shortcomings of these technologies: continuum source Atomic absorption spectrometry for simultaneously measuring multi-elements, atomic emission spectrometry for direct determination of particulates, high resolution laser ablation inductively coupled plasma mass spectrometry for determination of solid samples, low scattering synchrotron fluorescence spectrum for determination of atmospheric particulate matter and k0 neutron activation analysis for determination of radioactive elements in the troposphere Analysis techniques of heavy metals in atmospheric particulate matter are promoted to develop toward being real-time, fast, low- detection-limit, direct-measurement and simple-operation due to the spatial and temporal distribution difference of the heavy metals in atmospheric particles and human requirement for improvement of ambient air quality as well as rapid development of modern instrument science and technology. PMID:26197596

  17. Ultraviolet and Light Absorption Spectrometry.

    ERIC Educational Resources Information Center

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

    1984-01-01

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

  18. Linear electric field mass spectrometry

    DOEpatents

    McComas, D.J.; Nordholt, J.E.

    1992-12-01

    A mass spectrometer and methods for mass spectrometry are described. The apparatus is compact and of low weight and has a low power requirement, making it suitable for use on a space satellite and as a portable detector for the presence of substances. High mass resolution measurements are made by timing ions moving through a gridless cylindrically symmetric linear electric field. 8 figs.

  19. Linear electric field mass spectrometry

    DOEpatents

    McComas, David J.; Nordholt, Jane E.

    1992-01-01

    A mass spectrometer and methods for mass spectrometry. The apparatus is compact and of low weight and has a low power requirement, making it suitable for use on a space satellite and as a portable detector for the presence of substances. High mass resolution measurements are made by timing ions moving through a gridless cylindrically symmetric linear electric field.

  20. Mass Spectrometry for the Masses

    ERIC Educational Resources Information Center

    Persinger, Jared D.; Hoops, Geoffrey, C.; Samide, Michael J.

    2004-01-01

    A simple, qualitative experiment is developed for implementation, where the gas chromatography-mass spectrometry (GC-MS) plays an important role, into the laboratory curriculum of a chemistry course designed for nonscience majors. This laboratory experiment is well suited for the students as it helps them to determine the validity of their…

  1. Molecular secondary ion mass spectrometry: New dimensions in chemical characterization

    NASA Astrophysics Data System (ADS)

    Colton, Richard J.; Campana, Joseph E.; Kidwell, David A.; Ross, Mark M.; Wyatt, Jeffrey R.

    1985-04-01

    Secondary ion mass spectrometry (SIMS) has become a diverse tool for the study of many substances other than metals and semiconductors. This paper discusses the emission of polyatomic and molecular ions from surfaces that contain various inorganic and organic compounds including polymers and biomolecules. The mass and abundance distribution of cluster ions emitted from various solids — Van der Waals, metallic, ionic and covalent — are compared. Trends in the emission patterns are discussed in terms of a recombination or direct emission mechanism. The emission of molecular ions is also discussed with respect to the method of ionization and the various sample preparation and matrix-assisted procedures used. The matrices include various solid-state and liquid matrices such as ammonium chloride, charcoal, glycerol and gallium. Various chemical derivatization procedures have been developed to enhance the sensitivity of molecular SIMS and to detect selectively components in mixtures. The procedures are demonstrated for the low-level detection of airborne contaminants from paints, for the analysis of drugs in biological fluids, and for the sequencing of biomolecules such as peptides and sugars. The emission of characteristic fragment ions from the surfaces of polymers is also described for thick, insulating films.

  2. Differential mobility spectrometry-mass spectrometry for atomic analysis.

    PubMed

    Sinatra, Francy L; Wu, Tianpeng; Manolakos, Spiros; Wang, Jing; Evans-Nguyen, Theresa G

    2015-02-01

    Analysis and separation of atomic ions within a portable setting are studied in forensic applications of radiological debris analysis. Ion mobility spectrometry (IMS) may be used to show separation of atomic ions, while the related method of differential mobility spectrometry (DMS) has focused on fractionation of primarily molecular components. We set out to investigate DMS as a means for separating atomic ions. We initially derived the differential ion mobility parameter, alpha, from classic empirical IMS data of atomic ions, cesium and potassium, each showing its own distinct form of alpha. These alpha functions were applied to DMS simulations and supported by analytical treatment that suggested a means for a rapid disambiguation of atomic ions using DMS. We validated this hypothesis through the prototype cesium-potassium system investigated experimentally by DMS coupled to mass spectrometry (MS). Such a feature would be advantageous in a field portable instrument for rapid atomic analyses especially in the case of isobaric ions that cannot be distinguished by MS. Herein, we first report this novel method for the derivation of alpha from existing field dependent drift tube ion mobility data. Further, we translate experimental DMS data into alpha parameters by expanding upon existing methods. Refining the alpha parameter in this manner helps convey the interpretation of the alpha parameter particularly for those new to the DMS field.

  3. Biogenic emissions from Citrus species in California

    NASA Astrophysics Data System (ADS)

    Fares, Silvano; Gentner, Drew R.; Park, Jeong-Hoo; Ormeno, Elena; Karlik, John; Goldstein, Allen H.

    2011-09-01

    Biogenic Volatile Organic Compounds (BVOC) emitted from plants are the dominant source of reduced carbon chemicals to the atmosphere and are important precursors to the photochemical production of ozone and secondary organic aerosols. Considering the extensive land used for agriculture, cultivated Citrus plantations may play an important role in the chemistry of the atmosphere especially in regions such as the Central Valley of California. Moreover, the BVOC emissions from Citrus species have not been characterized in detail and more species-specific inputs for regional models of BVOC emissions are needed. In this study, we measured the physiological parameters and emissions of the most relevant BVOC (oxygenated compounds, monoterpenes, and sesquiterpenes) for four predominant Citrus species planted in California ( Citrus sinensis var. 'Parent Navel', Citrus limon var. 'Meyer', Citrus reticulata var. 'W. Murcott' and 'Clementine'). We used two analytical techniques to measure a full range of BVOC emitted: Proton Transfer Reaction Mass Spectrometry (PTR-MS) and gas chromatography with mass spectrometry. Methanol, followed by acetone and acetaldehyde, were the dominant BVOC emitted from lemon and mandarin trees (basal emission rates up to 300 ng(C) g(DW) -1 h -1), while oxygenated monoterpenes, monoterpenes, and sesquiterpenes were the main BVOC emitted from orange trees (basal emission rates up to = 2500 ng(C) g(DW) -1 h -1). Light and temperature-dependent algorithms were better predictors of methanol, acetaldehyde, acetone, isoprene and monoterpenes for all the Citrus species. Whereas, temperature-dependent algorithms were better predictors of oxygenated monoterpenes, and sesquiterpenes. We observed that flowering increased emissions from orange trees by an order of magnitude with the bulk of BVOC emissions being comprised of monoterpenes, sesquiterpenes, and oxygenated monoterpenes. Chemical speciation of BVOC emissions show that the various classes of terpene

  4. MASS SPECTROMETRY-BASED METABOLOMICS

    PubMed Central

    Dettmer, Katja; Aronov, Pavel A.; Hammock, Bruce D.

    2007-01-01

    This review presents an overview of the dynamically developing field of mass spectrometry-based metabolomics. Metabolomics aims at the comprehensive and quantitative analysis of wide arrays of metabolites in biological samples. These numerous analytes have very diverse physico-chemical properties and occur at different abundance levels. Consequently, comprehensive metabolomics investigations are primarily a challenge for analytical chemistry and specifically mass spectrometry has vast potential as a tool for this type of investigation. Metabolomics require special approaches for sample preparation, separation, and mass spectrometric analysis. Current examples of those approaches are described in this review. It primarily focuses on metabolic fingerprinting, a technique that analyzes all detectable analytes in a given sample with subsequent classification of samples and identification of differentially expressed metabolites, which define the sample classes. To perform this complex task, data analysis tools, metabolite libraries, and databases are required. Therefore, recent advances in metabolomics bioinformatics are also discussed. PMID:16921475

  5. Imaging Mass Spectrometry in Neuroscience

    PubMed Central

    2013-01-01

    Imaging mass spectrometry is an emerging technique of great potential for investigating the chemical architecture in biological matrices. Although the potential for studying neurobiological systems is evident, the relevance of the technique for application in neuroscience is still in its infancy. In the present Review, a principal overview of the different approaches, including matrix assisted laser desorption ionization and secondary ion mass spectrometry, is provided with particular focus on their strengths and limitations for studying different neurochemical species in situ and in vitro. The potential of the various approaches is discussed based on both fundamental and biomedical neuroscience research. This Review aims to serve as a general guide to familiarize the neuroscience community and other biomedical researchers with the technique, highlighting its great potential and suitability for comprehensive and specific chemical imaging. PMID:23530951

  6. Instrumentation for mass spectrometry: 1997

    SciTech Connect

    McLuckey, S.A.

    1997-08-01

    All mass spectrometry experiments involve the manipulation of material, an interface with the mass spectrometer, ionization, ion manipulation/analysis, detection and data collection/reduction. Each of these elements involve instrumentation. The wide range of species now amenable to mass spectrometry and the diverse areas of physical science in which it plays a role have led to a seemingly unlimited array of instrumental combinations. However, only a limited number of mass analyzers, and their combinations, dominate. The dominant analyzers include time-of-flight, Fourier transform ion cyclotron resonance, the Paul trap, the mass filter, and the sector mass spectrometer. Why there are so few (or so many, depending upon one`s point of view) can be understood upon consideration of a set of mass analyzer figures of merit. These include mass resolution, mass accuracy, mass range, dynamic range, abundance sensitivity, precision, efficiency, speed, MS{sup n} capability, compatibility with the ionizer, cost, and size. The most appropriate form of mass spectrometry is determined by the priorities of the particular measurement placed on the various mass analyzer characteristics and the relative strengths of the analyzers in meeting the requirements. Each of the analyzer types has a unique set of figures of merit that makes it optimally suited for particular applications. This paper discusses these figures of merit, provides data illustrating recent developments for each analyzer type, and gives the figures of merit of each type of analyzer as they stand in 1997. 101 refs., 24 figs.

  7. 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.

  8. 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. PMID:18351436

  9. Speciation of mercury in human whole blood by capillary gas chromatography with a microwave-induced plasma emission detector system following complexometric extraction and butylation.

    PubMed

    Bulska, E; Emteborg, H; Baxter, D C; Frech, W; Ellingsen, D; Thomassen, Y

    1992-03-01

    Methyl- and inorganic mercury were extracted from human whole blood samples, as their diethyldithiocarbamate complexes, into toluene and butylated by using a Grignard reagent. The mercury species were then separated by gas chromatography (on a 12 m non-polar DB-1 capillary column) and detected by a microwave-induced plasma atomic emission spectrometric (GC-MPD) system. The accuracy and precision of the proposed method were established by the analysis of Seronorm lyophilized human whole blood standards for methyl- and inorganic mercury. No statistical difference (t-test) between the sum of these two species determined by the GC-MPD based method and the recommended total mercury concentrations in the Seronorm samples was observed. Results for the determination of methyl- and inorganic mercury in 60 controls and 90 previously occupationally exposed (to inorganic mercury) workers are presented to illustrate the practical utility of the proposed method. No significantly elevated inorganic mercury concentrations between the two groups were evident.

  10. Laminar-flow torch for helium inductively coupled plasma spectrometry

    SciTech Connect

    Tan, H.; Chan, S.K.; Montaser, A.

    1988-11-15

    Helium inductively coupled plasmas (He ICPs) operated at atmospheric pressure, possess two advantages compared to Ar ICPs for atomic emission spectrometry (AES) and mass spectrometry (MS). First, for the elements tested so far, the detection powers for the He ICPs are superior to those for an Ar discharge. Second, the emission background spectra of the He ICPs are quite simple in the red and the near-infrared regions, thus reducing the spectral interference problems encountered with the determination of halogens and other nonmetals. Relatedly, certain mass spectral interferences noted in the detection of monoisotopic elements are eliminated when helium is used as the plasma gas instead of argon. For the most recent studies of He ICPs, the authors used a tangential-flow torch to form an annular plasma at forward power of 1500 W with a total helium gas flow of 8 L/min. The present study is concerned with the formation and preliminary characterization of a He ICP using a laminar-flow torch. The total helium gas flow for this torch is less than 2 L/min. Studies of plasmas formed in laminar-flow torches are important because of the possibility to reduce one major source of noise resulting from the rotation of the plasma gas in tangential-flow torches.

  11. A mass spectrometry primer for mass spectrometry imaging

    PubMed Central

    Rubakhin, Stanislav S.; Sweedler, Jonathan V.

    2011-01-01

    Mass spectrometry imaging (MSI), a rapidly growing subfield of chemical imaging, employs mass spectrometry (MS) technologies to create single- and multi-dimensional localization maps for a variety of atoms and molecules. Complimentary to other imaging approaches, MSI provides high chemical specificity and broad analyte coverage. This powerful analytical toolset is capable of measuring the distribution of many classes of inorganics, metabolites, proteins and pharmaceuticals in chemically and structurally complex biological specimens in vivo, in vitro, and in situ. The MSI approaches highlighted in this Methods in Molecular Biology volume provide flexibility of detection, characterization, and identification of multiple known and unknown analytes. The goal of this chapter is to introduce investigators who may be unfamiliar with MS to the basic principles of the mass spectrometric approaches as used in MSI. In addition to guidelines for choosing the most suitable MSI method for specific investigations, cross-references are provided to the chapters in this volume that describe the appropriate experimental protocols. PMID:20680583

  12. Mass spectrometry of aerospace materials

    NASA Technical Reports Server (NTRS)

    Colony, J. A.

    1976-01-01

    Mass spectrometry is used for chemical analysis of aerospace materials and contaminants. Years of analytical aerospace experience have resulted in the development of specialized techniques of sampling and analysis which are required in order to optimize results. This work has resulted in the evolution of a hybrid method of indexing mass spectra which include both the largest peaks and the structurally significant peaks in a concise format. With this system, a library of mass spectra of aerospace materials was assembled, including the materials responsible for 80 to 90 percent of the contamination problems at Goddard Space Flight Center during the past several years.

  13. Mass spectrometry. [review of techniques

    NASA Technical Reports Server (NTRS)

    Burlingame, A. L.; Kimble, B. J.; Derrick, P. J.

    1976-01-01

    Advances in mass spectrometry (MS) and its applications over the past decade are reviewed in depth, with annotated literature references. New instrumentation and techniques surveyed include: modulated-beam MS, chromatographic MS on-line computer techniques, digital computer-compatible quadrupole MS, selected ion monitoring (mass fragmentography), and computer-aided management of MS data and interpretation. Areas of application surveyed include: organic MS and electron impact MS, field ionization kinetics, appearance potentials, translational energy release, studies of metastable species, photoionization, calculations of molecular orbitals, chemical kinetics, field desorption MS, high pressure MS, ion cyclotron resonance, biochemistry, medical/clinical chemistry, pharmacology, and environmental chemistry and pollution studies.

  14. Counting Molecules by Desorption Ionization and Mass Spectrometry/Mass Spectrometry.

    ERIC Educational Resources Information Center

    Cooks, R. G.; Busch, K. L.

    1982-01-01

    Discusses two newer methods in mass spectrometry and shows how they can increase signal and signal-to-noise ratios, respectively. The first method, desorption ionization (DI), increases sensitivity while the second method, mass spectrometry/mass spectrometry (MS/MS), increases specificity. Together, the two methods offer improved analytical…

  15. Chemical analysis of trace elements for air pollution detection. August 1973-May 1990 (A Bibliography from the NTIS data base). Report for August 1973-May 1990

    SciTech Connect

    Not Available

    1990-06-01

    This bibliography contains citations concerning the identification and analysis of trace elements and compounds occurring in air and airborne particulate samples. The citations present methods of analysis and the equipment required for the determinations. Analytical techniques include spectrometry, inductively-coupled plasma, atomic absorption and atomic emission, Fourier transform infrared analysis, and ion chromatography. A separate Published Search covers analysis of trace elements in water pollution detection. (Contains 103 citations fully indexed and including a title list.)

  16. Quantitative mass spectrometry: an overview.

    PubMed

    Urban, Pawel L

    2016-10-28

    Mass spectrometry (MS) is a mainstream chemical analysis technique in the twenty-first century. It has contributed to numerous discoveries in chemistry, physics and biochemistry. Hundreds of research laboratories scattered all over the world use MS every day to investigate fundamental phenomena on the molecular level. MS is also widely used by industry-especially in drug discovery, quality control and food safety protocols. In some cases, mass spectrometers are indispensable and irreplaceable by any other metrological tools. The uniqueness of MS is due to the fact that it enables direct identification of molecules based on the mass-to-charge ratios as well as fragmentation patterns. Thus, for several decades now, MS has been used in qualitative chemical analysis. To address the pressing need for quantitative molecular measurements, a number of laboratories focused on technological and methodological improvements that could render MS a fully quantitative metrological platform. In this theme issue, the experts working for some of those laboratories share their knowledge and enthusiasm about quantitative MS. I hope this theme issue will benefit readers, and foster fundamental and applied research based on quantitative MS measurements.This article is part of the themed issue 'Quantitative mass spectrometry'. PMID:27644965

  17. Quantitative mass spectrometry: an overview

    NASA Astrophysics Data System (ADS)

    Urban, Pawel L.

    2016-10-01

    Mass spectrometry (MS) is a mainstream chemical analysis technique in the twenty-first century. It has contributed to numerous discoveries in chemistry, physics and biochemistry. Hundreds of research laboratories scattered all over the world use MS every day to investigate fundamental phenomena on the molecular level. MS is also widely used by industry-especially in drug discovery, quality control and food safety protocols. In some cases, mass spectrometers are indispensable and irreplaceable by any other metrological tools. The uniqueness of MS is due to the fact that it enables direct identification of molecules based on the mass-to-charge ratios as well as fragmentation patterns. Thus, for several decades now, MS has been used in qualitative chemical analysis. To address the pressing need for quantitative molecular measurements, a number of laboratories focused on technological and methodological improvements that could render MS a fully quantitative metrological platform. In this theme issue, the experts working for some of those laboratories share their knowledge and enthusiasm about quantitative MS. I hope this theme issue will benefit readers, and foster fundamental and applied research based on quantitative MS measurements. This article is part of the themed issue 'Quantitative mass spectrometry'.

  18. Quantitative mass spectrometry: an overview.

    PubMed

    Urban, Pawel L

    2016-10-28

    Mass spectrometry (MS) is a mainstream chemical analysis technique in the twenty-first century. It has contributed to numerous discoveries in chemistry, physics and biochemistry. Hundreds of research laboratories scattered all over the world use MS every day to investigate fundamental phenomena on the molecular level. MS is also widely used by industry-especially in drug discovery, quality control and food safety protocols. In some cases, mass spectrometers are indispensable and irreplaceable by any other metrological tools. The uniqueness of MS is due to the fact that it enables direct identification of molecules based on the mass-to-charge ratios as well as fragmentation patterns. Thus, for several decades now, MS has been used in qualitative chemical analysis. To address the pressing need for quantitative molecular measurements, a number of laboratories focused on technological and methodological improvements that could render MS a fully quantitative metrological platform. In this theme issue, the experts working for some of those laboratories share their knowledge and enthusiasm about quantitative MS. I hope this theme issue will benefit readers, and foster fundamental and applied research based on quantitative MS measurements.This article is part of the themed issue 'Quantitative mass spectrometry'.

  19. Glass frit nebulizer for atomic spectrometry

    USGS Publications Warehouse

    Layman, L.R.

    1982-01-01

    The nebuilizatlon of sample solutions Is a critical step In most flame or plasma atomic spectrometrlc methods. A novel nebulzatlon technique, based on a porous glass frit, has been Investigated. Basic operating parameters and characteristics have been studied to determine how thte new nebulizer may be applied to atomic spectrometrlc methods. The results of preliminary comparisons with pneumatic nebulizers Indicate several notable differences. The frit nebulizer produces a smaller droplet size distribution and has a higher sample transport efficiency. The mean droplet size te approximately 0.1 ??m, and up to 94% of the sample te converted to usable aerosol. The most significant limitations In the performance of the frit nebulizer are the stow sample equMbratton time and the requirement for wash cycles between samples. Loss of solute by surface adsorption and contamination of samples by leaching from the glass were both found to be limitations only In unusual cases. This nebulizer shows great promise where sample volume te limited or where measurements require long nebullzatlon times.

  20. Triacylglycerol profiling of marine microalgae by mass spectrometry[S

    PubMed Central

    Danielewicz, Megan A.; Anderson, Lisa A.; Franz, Annaliese K.

    2011-01-01

    We present a method for the determination of triacylglycerol (TAG) profiles of oleaginous saltwater microalgae relevant for the production of biofuels, bioactive lipids, and high-value lipid-based chemical precursors. We describe a technique to remove chlorophyll using quick, simple solid phase extraction (SPE) and directly compare the intact TAG composition of four microalgae species (Phaeodactylum tricornutum, Nannochloropsis salina, Nannochloropsis oculata, and Tetraselmis suecica) using MALDI time-of-flight (TOF) mass spectrometry (MS), ESI linear ion trap-orbitrap (LTQ Orbitrap) MS, and 1H NMR spectroscopy. Direct MS analysis is particularly effective to compare the polyunsaturated fatty acid (PUFA) composition for triacylglycerols because oxidation can often degrade samples upon derivatization. Using these methods, we observed that T. suecica contains significant PUFA levels with respect to other microalgae. This method is applicable for high-throughput MS screening of microalgae TAG profiles and may aid in the commercial development of biofuels. PMID:21840867

  1. Mercaptans emissions in diesel and biodiesel exhaust

    NASA Astrophysics Data System (ADS)

    Corrêa, Sérgio Machado; Arbilla, Graciela

    Biodiesel and ethanol are fuels in clear growth and evidence, basically due to its relation with the greenhouse effect reduction. There are several works regarding regulated pollutants emissions, but there is a lack of reports in non-regulated emissions. In a previous paper (Corrêa and Arbilla, 2006) the emissions of aromatic hydrocarbons were reported and in 2007 another paper was published in 2008 focusing carbonyls emissions (Corrêa and Arbilla, 2008). In this work four mercaptans (methyl, ethyl, n-propyl and n-butyl mercaptans) were evaluated for a heavy-duty diesel engine, fueled with pure diesel (D) and biodiesel blends (v/v) of 2% (B2), 5% (B5), 10% (B10), and 20% (B20). The tests were carried using a six cylinder heavy-duty engine, typical of the Brazilian fleet of urban buses, during a real use across the city. The exhaust gases were diluted near 20 times and the mercaptans were sampled with glass fiber filters impregnated with mercuric acetate. The chemical analyses were performed by gas chromatography with mass spectrometry detection. The results indicated that the mercaptans emissions exhibit a reduction with the increase of biodiesel content, but this reduction is lower as the mercaptan molar mass increases. For B20 results the emission reduction was 18.4% for methyl mercaptan, 18.1% for ethyl mercaptan, 16.3% for n-propyl mercaptan, and 9.6% for n-butyl mercaptan.

  2. High-resolution alpha-particle spectrometry of ²³⁸U.

    PubMed

    Pommé, S; García-Toraño, E; Marouli, M; Crespo, M T; Jobbágy, V; Van Ammel, R; Paepen, J; Stroh, H

    2014-05-01

    The alpha-particle emission probabilities associated with the three main alpha transitions of (238)U were measured by high-resolution alpha-particle spectrometry. Highly enriched (238)U material was used and its isotopic composition characterised by mass spectrometry. Source production through electrodeposition was optimised to reconcile conflicting demands for good spectral resolution and statistical precision. Measurements were performed at IRMM and CIEMAT for 1-2 years in three different set-ups. A new magnet system was put into use to largely eliminate true coincidence effects with low-energy conversion electrons. Finally the accuracy and precision of the relative emission probabilities for the three transitions - 77.01 (10)%, 22.92 (10)% and 0.068 (10)%, respectively - have been improved significantly.

  3. High-resolution alpha-particle spectrometry of ²³⁸U.

    PubMed

    Pommé, S; García-Toraño, E; Marouli, M; Crespo, M T; Jobbágy, V; Van Ammel, R; Paepen, J; Stroh, H

    2014-05-01

    The alpha-particle emission probabilities associated with the three main alpha transitions of (238)U were measured by high-resolution alpha-particle spectrometry. Highly enriched (238)U material was used and its isotopic composition characterised by mass spectrometry. Source production through electrodeposition was optimised to reconcile conflicting demands for good spectral resolution and statistical precision. Measurements were performed at IRMM and CIEMAT for 1-2 years in three different set-ups. A new magnet system was put into use to largely eliminate true coincidence effects with low-energy conversion electrons. Finally the accuracy and precision of the relative emission probabilities for the three transitions - 77.01 (10)%, 22.92 (10)% and 0.068 (10)%, respectively - have been improved significantly. PMID:24355304

  4. Silicon oxynitride: A field emission suppression coating

    NASA Astrophysics Data System (ADS)

    Theodore, Nimel D.

    We have studied coatings deposited using our inductively-coupled RF plasma ion implantation and desposition system to suppress field emission from large, 3-D electrode structures used in high voltage applications, like those used by Thomas Jefferson National Accelerator Facility in their DC-field photoelectron gun. Currently time and labor-intensive hand-polishing procedures are used to minimize field emission from these structures. Previous work had shown that the field emission from polished stainless steel (27 muA of field-emitted current at 15 MV/m) could be drastically reduced with simultaneous deposition of sputtered silicon dioxide during nitrogen implantation (167 pA of field-emitted current at 30 MV/m). We have determined that this unique implantation and deposition procedure produces high-purity silicon oxynitride films that can suppress field emission from stainless steel regardless of their initial surface polish. However, when this implantation procedure was applied to large, 3-D substrates, arcs occurred, damaging the coating and causing unreliable and unrepeatable field emission suppression. We have developed a novel reactive sputtering procedure to deposit high-purity silicon oxynitride coatings without nitrogen ion implantation. We can control the stoichometry and deposition rate of these coatings by adjusting the nitrogen pressure and incident RF-power. Using profilometry, Auger electron spectroscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, Rutherford backscattering spectrometry, elastic recoil detection analysis, and current-voltage measurements, we have determined that the elemental composition, chemical bonding, density, and electrical properties of the reactively-sputtered silicon oxynitride coatings are similar to those produced by nitrogen implantation during silicon dioxide deposition. Furthermore, high voltage tests determined that both coatings similarly suppress field emission from 6" diameter, polished

  5. Neuroscience and Accelerator Mass Spectrometry

    SciTech Connect

    Palmblad, M N; Buchholz, B A; Hillegonds, D J; Vogel, J S

    2004-08-02

    Accelerator mass spectrometry (AMS) is a mass spectrometric method for quantifying rare isotopes. It has had great impact in geochronology and archaeology and is now being applied in biomedicine. AMS measures radioisotopes such as {sup 3}H, {sup 14}C, {sup 26}Al, {sup 36}Cl and {sup 41}Ca, with zepto- or attomole sensitivity and high precision and throughput, enabling safe human pharmacokinetic studies involving: microgram doses, agents having low bioavailability, or toxicology studies where administered doses must be kept low (<1 {micro}g/kg). It is used to study long-term pharmacokinetics, to identify biomolecular interactions, to determine chronic and low-dose effects or molecular targets of neurotoxic substances, to quantify transport across the blood-brain barrier and to resolve molecular turnover rates in the human brain on the timescale of decades. We will here review how AMS is applied in neurotoxicology and neuroscience.

  6. Electrophoresis-mass spectrometry probe

    DOEpatents

    Andresen, Brian D.; Fought, Eric R.

    1987-01-01

    The invention involves a new technique for the separation of complex mixtures of chemicals, which utilizes a unique interface probe for conventional mass spectrometers which allows the electrophoretically separated compounds to be analyzed in real-time by a mass spectrometer. This new chemical analysis interface, which couples electrophoresis with mass spectrometry, allows complex mixtures to be analyzed very rapidly, with much greater specificity, and with greater sensitivity. The interface or probe provides a means whereby large and/or polar molecules in complex mixtures to be completely characterized. The preferred embodiment of the probe utilizes a double capillary tip which allows the probe tip to be continually wetted by the buffer, which provides for increased heat dissipation, and results in a continually operating interface which is more durable and electronically stable than the illustrated single capillary tip probe interface.

  7. Hadamard transform visible Raman spectrometry

    SciTech Connect

    Tilotta, D.C.; Freeman, R.D.; Fateley, W.G.

    1987-11-01

    The successful application of LC-SLM Hadamard transform spectrometry as a simultaneous multiwavelength detection system to Raman spectroscopy is presented. Multiplexed Raman data are obtained with the use of an Ar/sup +/ laser lasing at 514.5 nm and a room-temperature silicon photodiode. A conventional 90/sup 0/ scattering geometry is employed for measurements. It is demonstrated that the LC-SLM Hadamard transform Raman spectrometer possesses the capability of performing spectral subtraction and the ability to obtain depolarization ratios of Raman bands, and can function as a selectively tunable optical filter for both Rayleigh line rejection and optical band notching. It is also demonstrated that, for the Hadamard transform Raman experiment, the silicon photodiode used as the detector produces spectra with slightly better signal-to-noise ratios than those obtained with the photomultiplier tube (PMT) used as the detector, although the PMT shows an increase in sensitivity.

  8. Electrophoresis-mass spectrometry probe

    DOEpatents

    Andresen, B.D.; Fought, E.R.

    1987-11-10

    The invention involves a new technique for the separation of complex mixtures of chemicals, which utilizes a unique interface probe for conventional mass spectrometers which allows the electrophoretically separated compounds to be analyzed in real-time by a mass spectrometer. This new chemical analysis interface, which couples electrophoresis with mass spectrometry, allows complex mixtures to be analyzed very rapidly, with much greater specificity, and with greater sensitivity. The interface or probe provides a means whereby large and/or polar molecules in complex mixtures to be completely characterized. The preferred embodiment of the probe utilizes a double capillary tip which allows the probe tip to be continually wetted by the buffer, which provides for increased heat dissipation, and results in a continually operating interface which is more durable and electronically stable than the illustrated single capillary tip probe interface. 8 figs.

  9. Comprehensive laboratory measurements of biomass-burning emissions: 1. Emissions from Indonesian, African, and other fuels

    NASA Astrophysics Data System (ADS)

    Christian, T. J.; Kleiss, B.; Yokelson, R. J.; Holzinger, R.; Crutzen, P. J.; Hao, W. M.; Saharjo, B. H.; Ward, D. E.

    2003-12-01

    Trace gas and particle emissions were measured from 47 laboratory fires burning 16 regionally to globally significant fuel types. Instrumentation included the following: open-path Fourier transform infrared spectroscopy; proton transfer reaction mass spectrometry; filter sampling with subsequent analysis of particles with diameter <2.5 μm for organic and elemental carbon and other elements; and canister sampling with subsequent analysis by gas chromatography (GC)/flame ionization detector, GC/electron capture detector, and GC/mass spectrometry. The emissions of 26 compounds are reported by fuel type. The results include the first detailed measurements of the emissions from Indonesian fuels. Carbon dioxide, CO, CH4, NH3, HCN, methanol, and acetic acid were the seven most abundant emissions (in order) from burning Indonesian peat. Acetol (hydroxyacetone) was a major, previously unobserved emission from burning rice straw (21-34 g/kg). The emission factors for our simulated African fires are consistent with field data for African fires for compounds measured in both the laboratory and the field. However, the higher concentrations and more extensive instrumentation in this work allowed quantification of at least 10 species not previously quantified for African field fires (in order of abundance): acetaldehyde, phenol, acetol, glycolaldehyde, methylvinylether, furan, acetone, acetonitrile, propenenitrile, and propanenitrile. Most of these new compounds are oxygenated organic compounds, which further reinforces the importance of these reactive compounds as initial emissions from global biomass burning. A few high-combustion-efficiency fires emitted very high levels of elemental (black) carbon, suggesting that biomass burning may produce more elemental carbon than previously estimated.

  10. Mid-IR enhanced laser ablation molecular isotopic spectrometry

    NASA Astrophysics Data System (ADS)

    Brown, Staci; Ford, Alan; Akpovo, Codjo A.; Johnson, Lewis

    2016-08-01

    A double-pulsed laser-induced breakdown spectroscopy (DP-LIBS) technique utilizing wavelengths in the mid-infrared (MIR) for the second pulse, referred to as double-pulse LAMIS (DP-LAMIS), was examined for its effect on detection limits compared to single-pulse laser ablation molecular isotopic spectrometry (LAMIS). A MIR carbon dioxide (CO2) laser pulse at 10.6 μm was employed to enhance spectral emissions from nanosecond-laser-induced plasma via mid-IR reheating and in turn, improve the determination of the relative abundance of isotopes in a sample. This technique was demonstrated on a collection of 10BO and 11BO molecular spectra created from enriched boric acid (H3BO3) isotopologues in varying concentrations. Effects on the overall ability of both LAMIS and DP-LAMIS to detect the relative abundance of boron isotopes in a starting sample were considered. Least-squares fitting to theoretical models was used to deduce plasma parameters and understand reproducibility of results. Furthermore, some optimization for conditions of the enhanced emission was achieved, along with a comparison of the overall emission intensity, plasma density, and plasma temperature generated by the two techniques.

  11. Laser ablation molecular isotopic spectrometry of carbon isotopes

    NASA Astrophysics Data System (ADS)

    Bol‧shakov, Alexander A.; Mao, Xianglei; Jain, Jinesh; McIntyre, Dustin L.; Russo, Richard E.

    2015-11-01

    Quantitative determination of carbon isotopes using Laser Ablation Molecular Isotopic Spectrometry (LAMIS) is described. Optical emission of diatomic molecules CN and C2 is used in these measurements. Two quantification approaches are presented: empirical calibration of spectra using a set of reference standards and numerical fitting of a simulated spectrum to the experimental one. Formation mechanisms of C2 and CN in laser ablation plasma are briefly reviewed to provide insights for implementation of LAMIS measurements. A simulated spectrum of the 12C2 Swan system was synthesized using four constituents within 473.5-476.5 nm. Simulation included three branches of 12C2 (1-0), branches R(0-0) and R(1-1), and branch P(9-8) of 12C2. Spectral positions of the tail lines in R(0-0) and R(1-1) were experimentally measured, since they were not accurately known before. The Swan band (1-0) of the isotopologue 13C12C was also simulated. Fitting to the experimental spectrum yielded the ratio 13C/12C = 1.08% in a good agreement with measurements by isotope ratio mass spectrometry. LAMIS promises to be useful in coal, oil and shale exploration, carbon sequestration monitoring, and agronomy studies.

  12. Thomson parabola spectrometry for gold laser-generated plasmas

    SciTech Connect

    Torrisi, L.; Cutroneo, M.; Ando, L.; Ullschmied, J.

    2013-02-15

    The plasma generated from thin gold films irradiated in high vacuum at high intensity ({approx}10{sup 15} W/cm{sup 2}) laser shot is characterized in terms of ion generation through time-of-flight techniques and Thomson parabola spectrometry. Gold ions and protons, accelerated in forward direction by the electric field developed in non-equilibrium plasma, have been investigated. Measurements, performed at PALS laboratory, give information about the gold charge states distributions, the ion energy distributions and the proton acceleration driven as a function of film thickness, laser parameters, and angular emission. The ion diagnostics of produced plasma in forward direction permits to understand some mechanisms developed during its expansion kinetics. The role of the focal position of a laser beam with respect to the target surface, plasma properties, and the possibility to accelerate protons up to energies above 3 MeV has been presented and discussed.

  13. Attomole quantitation of protein separations with accelerator mass spectrometry

    SciTech Connect

    Vogel, J S; Grant, P G; Buccholz, B A; Dingley, K; Turteltaub, K W

    2000-12-15

    Quantification of specific proteins depends on separation by chromatography or electrophoresis followed by chemical detection schemes such as staining and fluorophore adhesion. Chemical exchange of short-lived isotopes, particularly sulfur, is also prevalent despite the inconveniences of counting radioactivity. Physical methods based on isotopic and elemental analyses offer highly sensitive protein quantitation that has linear response over wide dynamic ranges and is independent of protein conformation. Accelerator mass spectrometry quantifies long-lived isotopes such as 14C to sub-attomole sensitivity. We quantified protein interactions with small molecules such as toxins, vitamins, and natural biochemicals at precisions of 1-5% . Micro-proton-induced-xray-emission quantifies elemental abundances in separated metalloprotein samples to nanogram amounts and is capable of quantifying phosphorylated loci in gels. Accelerator-based quantitation is a possible tool for quantifying the genome translation into proteome.

  14. Rapid discrimination of bacteria by paper spray mass spectrometry.

    PubMed

    Hamid, Ahmed M; Jarmusch, Alan K; Pirro, Valentina; Pincus, David H; Clay, Bradford G; Gervasi, Gaspard; Cooks, R Graham

    2014-08-01

    Paper spray mass spectrometry ambient ionization is utilized for rapid discrimination of bacteria without sample preparation. Bacterial colonies were smeared onto filter paper precut to a sharp point, then wetted with solvent and held at a high potential. Charged droplets released by field emission were sucked into the mass spectrometer inlet and mass spectra were recorded. Sixteen different species representing eight different genera from Gram-positive and Gram-negative bacteria were investigated. Phospholipids were the predominant species observed in the mass spectra in both the negative and positive ion modes. Multivariate data analysis based on principal component analysis, followed by linear discriminant analysis, allowed bacterial discrimination. The lipid information in the negative ion mass spectra proved useful for species level differentiation of the investigated Gram-positive bacteria. Gram-negative bacteria were differentiated at the species level by using a numerical data fusion strategy of positive and negative ion mass spectra. PMID:25014713

  15. Evaluation of field-portable X-ray fluorescence spectrometry for the determination of lead contamination on small-arms firing ranges

    SciTech Connect

    Schneider, J.F.; Taylor, J.D.; Bass, D.A.; Zellmer, D.; Rieck, M.

    1995-02-01

    Field analytical methods for the characterization of lead contamination in soil are being developed. In this study, the usefulness of a commercially available, field-portable energy-dispersive X-ray fluorescence spectrometer (XRF) is evaluated for determining the extent of lead contamination in soils on small-arms firing ranges at a military installation. This field screening technique provides significant time and cost savings for the study of sites with lead-contaminated soil. Data obtained with the XRF unit in the field are compared with data obtained from soil samples analyzed in an analytical laboratory by inductively coupled plasma atomic emission spectroscopy. Results indicate that the field-portable XRF unit evaluated in this study provides data that are useful in determining the extent and relative magnitude of lead contamination. For the commercial unit used in this study, improvements in the spectral resolution and in the limit of detection would be required to make the unit more than just a screening tool.

  16. Wireless Data Acquisition of Transient Signals for Mobile Spectrometry Applications.

    PubMed

    Trzcinski, Peter; Weagant, Scott; Karanassios, Vassili

    2016-05-01

    Wireless data acquisition using smartphones or handhelds offers increased mobility, it provides reduced size and weight, it has low electrical power requirements, and (in some cases) it has an ability to access the internet. Thus, it is well suited for mobile spectrometry applications using miniaturized, field-portable spectrometers, or detectors for chemical analysis in the field (i.e., on-site). There are four main wireless communications standards that can be used for wireless data acquisition, namely ZigBee, Bluetooth, Wi-Fi, and UWB (ultra-wide band). These are briefly reviewed and are evaluated for applicability to data acquisition of transient signals (i.e., time-domain) in the field (i.e., on-site) from a miniaturized, field-portable photomultiplier tube detector and from a photodiode array detector installed in a miniaturized, field-portable fiber optic spectrometer. These are two of the most widely used detectors for optical measurements in the ultraviolet-visible range of the spectrum. A miniaturized, 3D-printed, battery-operated microplasma-on-a-chip was used for generation of transient optical emission signals. Elemental analysis from liquid microsamples, a microplasma, and a handheld or a smartphone will be used as examples. Development and potential applicability of wireless data acquisition of transient optical emission signals for taking part of the lab to the sample types of mobile, field-portable spectrometry applications will be discussed. The examples presented are drawn from past and ongoing work in the authors' laboratory. A handheld or a smartphone were used as the mobile computing devices of choice.

  17. Wireless Data Acquisition of Transient Signals for Mobile Spectrometry Applications.

    PubMed

    Trzcinski, Peter; Weagant, Scott; Karanassios, Vassili

    2016-05-01

    Wireless data acquisition using smartphones or handhelds offers increased mobility, it provides reduced size and weight, it has low electrical power requirements, and (in some cases) it has an ability to access the internet. Thus, it is well suited for mobile spectrometry applications using miniaturized, field-portable spectrometers, or detectors for chemical analysis in the field (i.e., on-site). There are four main wireless communications standards that can be used for wireless data acquisition, namely ZigBee, Bluetooth, Wi-Fi, and UWB (ultra-wide band). These are briefly reviewed and are evaluated for applicability to data acquisition of transient signals (i.e., time-domain) in the field (i.e., on-site) from a miniaturized, field-portable photomultiplier tube detector and from a photodiode array detector installed in a miniaturized, field-portable fiber optic spectrometer. These are two of the most widely used detectors for optical measurements in the ultraviolet-visible range of the spectrum. A miniaturized, 3D-printed, battery-operated microplasma-on-a-chip was used for generation of transient optical emission signals. Elemental analysis from liquid microsamples, a microplasma, and a handheld or a smartphone will be used as examples. Development and potential applicability of wireless data acquisition of transient optical emission signals for taking part of the lab to the sample types of mobile, field-portable spectrometry applications will be discussed. The examples presented are drawn from past and ongoing work in the authors' laboratory. A handheld or a smartphone were used as the mobile computing devices of choice. PMID:27006023

  18. Characterization of emissions from conversion varnishes

    SciTech Connect

    McCrillis, R.C.; Howard, E.M.; Fortmann, R.

    1996-12-31

    Three commercially available conversion varnish coating {open_quotes}systems{close_quotes} (stain, sealer, and topcoat) were selected for an initial scoping study. Total volatile content of the catalyzed varnishes, as determined by EPA Method 24, ranged from 64 to 73% (w/w). Uncombined (free) formaldehyde concentrations, determined by a sodium sulfite titration method, ranged from 0.15 to 0.58% (w/w) of the resin. Each resin was also analyzed by gas chromatography/mass spectrometry (EPA Method 311) to identify the volatile components that may be emitted. The primary volatile organic constituents identified in the resin formulations included 2-butanone, n-butanol, 4-methyl-2-pentanone, toluene, ethylbenzene, 1,2,4-trimethylbenzene, and the xylenes. Dynamic small chamber (53L stainless steel) tests were performed to identify and quantify emissions following application to coupons of typical kitchen cabinet wood substrates and during curing and aging. One of the objectives is to determine the relationship between the concentration of hazardous air pollutants (HAPs), volatile organic compounds (VOCs), and formaldehyde in the resins and emissions from the catalyzed varnish. The results to date show good mass balance for the HAPs and VOCs. Formaldehyde emissions show 6-7 times the emission compared to the free formaldehyde content, indicating that formaldehyde is formed during the curing process. Results of the formulation analyses and emission tests completed to date are described in this paper.

  19. Effect of fuel aromaticity on diesel emissions

    SciTech Connect

    Barbella, R.; Ciajolo, A.; D'Anna, A. ); Bertoli, C. )

    1989-09-01

    The effect of the fuel aromatic content on soot and heavy hydrocarbon emissions from a single-cylinder direct-injection diesel engine has been investigated burning a pure paraffinic fuel (n-tetradecane), a tetradecane-toluene mixture (70-30 vol%) and two diesel oils with different aromatic content. All experiments were at various air-fuel ratios with constant engine speed and injection timing advance. The detailed chemical analysis of exhaust heavy hydrocarbons in terms of mass percentage of paraffins, monoaromatics, polyaromatics and polar compounds, and the gas chromatography-mass spectrometry of each hydrocarbon class have been compared with the original fuel analyses in order to discriminate the unburned fuel compounds from the combustion-formed products. The soot emission rate has been found to be independent of the fuel aromatic content, but the fuel affects the quality and quantity of heavy hydrocarbon emission. Low amounts of heavy hydrocarbons, mainly partially oxidized compounds, are emitted from tetradecane combustion, whereas diesel fuel oils produced high emissions of heavy hydrocarbons, mainly unburned fuel compounds. The emission of polynuclear aromatic hydrocarbons (PAH) from tetradecane and tetradecane-toluene diesel combustion indicates that these compounds are combustion-formed products, but unburned fuel PAH are the main components of PAH emitted by the diesel fuel oils.

  20. Airborne Gamma-Spectrometry in Switzerland

    SciTech Connect

    Butterweck, Gernot; Bucher, Benno; Rybach, Ladislaus

    2008-08-07

    Airborne gamma-spectrometry is able to obtain fast radiological information over large areas. The airborne gamma-spectrometry unit deployed in Switzerland by the Swiss National Emergency Operations Centre (NEOC) consists of a Swiss army Super Puma helicopter equipped with four NaI-Detectors with a total volume of 17 liters, associated electronics and a real-time data evaluation and mapping unit developed by the Swiss Federal Institute of Technology (ETH) and the Paul Scherrer Institut (PSI). The operational readiness of the airborne gamma-spectrometry system is validated in annual exercises of one week duration. Data from 2005 and 2006 exercises are represented in maps of {sup 137}Cs activity concentration for two towns located in southern and western Switzerland. An indicator of man-made radioactivity (MMGC ratio) is demonstrated for an area with four different types of nuclear installations. The intercomparison between airborne gamma-spectrometry and ground measurements showed good agreement between both methods.

  1. Plasma Desorption Mass Spectrometry: Coming of Age.

    ERIC Educational Resources Information Center

    Cotter, Robert J.

    1988-01-01

    Discusses the history and development of Plasma Desorption Mass Spectrometry to determine molecular weights and structures of proteins and polymers. Outlines theory, instrumentation, and sample preparation commonly used. Gives several examples of resulting spectra. (ML)

  2. Nonaqueous Capillary Electrophoresis Mass Spectrometry.

    PubMed

    Klampfl, Christian W; Himmelsbach, Markus

    2016-01-01

    The term nonaqueous capillary electrophoresis (NACE) commonly refers to capillary electrophoresis with purely nonaqueous background electrolytes (BGE). Main advantages of NACE are the possibility to analyze substances with very low solubility in aqueous media as well as separation selectivity that can be quite different in organic solvents (compared to water)-a property that can be employed for manipulation of separation selectivities. Mass spectrometry (MS) has become more and more popular as a detector in CE a fact that applies also for NACE. In the present chapter, the development of NACE-MS since 2004 is reviewed. Relevant parameters like composition of BGE and its influence on separation and detection in NACE as well as sheath liquid for NACE-MS are discussed. Finally, an overview of the papers published in the field of NACE-MS between 2004 and 2014 is given. Applications are grouped according to the field (analysis of natural products, biomedical analysis, food analysis, analysis of industrial products, and fundamental investigations). PMID:27645734

  3. Quantitative mass spectrometry: an overview

    PubMed Central

    2016-01-01

    Mass spectrometry (MS) is a mainstream chemical analysis technique in the twenty-first century. It has contributed to numerous discoveries in chemistry, physics and biochemistry. Hundreds of research laboratories scattered all over the world use MS every day to investigate fundamental phenomena on the molecular level. MS is also widely used by industry—especially in drug discovery, quality control and food safety protocols. In some cases, mass spectrometers are indispensable and irreplaceable by any other metrological tools. The uniqueness of MS is due to the fact that it enables direct identification of molecules based on the mass-to-charge ratios as well as fragmentation patterns. Thus, for several decades now, MS has been used in qualitative chemical analysis. To address the pressing need for quantitative molecular measurements, a number of laboratories focused on technological and methodological improvements that could render MS a fully quantitative metrological platform. In this theme issue, the experts working for some of those laboratories share their knowledge and enthusiasm about quantitative MS. I hope this theme issue will benefit readers, and foster fundamental and applied research based on quantitative MS measurements. This article is part of the themed issue ‘Quantitative mass spectrometry’. PMID:27644965

  4. Nanotip Ambient Ionization Mass Spectrometry.

    PubMed

    Zhou, Zhenpeng; Lee, Jae Kyoo; Kim, Samuel C; Zare, Richard N

    2016-05-17

    A method called nanotip ambient ionization mass spectrometry (NAIMS) is described, which applies high voltage between a tungsten nanotip and a metal plate to generate a plasma in which ionized analytes on the surface of the metal plate are directed to the inlet and analyzed by a mass spectrometer. The dependence of signal intensity is investigated as a function of the tip-to-plate distance, the tip size, the voltage applied at the tip, and the current. These parameters are separately optimized to achieve sensitivity or high spatial resolution. A partially observable Markov decision process is used to achieve a stabilized plasma as well as high ionization efficiency. As a proof of concept, the NAIMS technique has been applied to phenanthrene and caffeine samples for which the limits of detection were determined to be 0.14 fmol for phenanthrene and 4 amol for caffeine and to a printed caffeine pattern for which a spatial resolution of 8 ± 2 μm, and the best resolution of 5 μm, was demonstrated. The limitations of NAIMS are also discussed. PMID:27087600

  5. Mass Spectrometry Imaging Quick View

    SciTech Connect

    2013-01-24

    MSI QuickView is a software designed to provide a graphical user interface (GUI) for greatly speeding up experimental feedback (visualization and analysis) of mass spectrometry imaging (MSI or IMS) data during data acquisition. Often different software loads the entire data set, i.e., all lines of data into computer memory (RAM). This causes out of memory errors for larger datasets. We solved this in MSI QuickView by reading in the data one line at a time. Only the required information (e.g. the final pixel values for that line of heat map) is maintained in RAM. Interim analysis options include the mean intensity vs. m/z spectrum, intensity vs. time spectrums for up to 6 different m/z values or ranges chosen by the user and heat maps for each line. This assists in validating the usefulness of the particular experiment after scanning the first few lines. In addition, the tool facilitates further processing and analysis of the massive datasets. The user can manually pick different m/z values, time ranges, scroll through the spectra for any line in the data without having to load it in manually, save multiple images, change aspect ratios for the heat maps, and process the heat maps in multiple ways including overlaying images at different m/z values, displaying up to 9 different heat maps, alignment of scans along each line etc. There is no manipulation of the data required by the user to visualize the data.

  6. Inorganic trace analysis by mass spectrometry

    NASA Astrophysics Data System (ADS)

    Becker, Johanna Sabine; Dietze, Hans-Joachim

    1998-10-01

    Mass spectrometric methods for the trace analysis of inorganic materials with their ability to provide a very sensitive multielemental analysis have been established for the determination of trace and ultratrace elements in high-purity materials (metals, semiconductors and insulators), in different technical samples (e.g. alloys, pure chemicals, ceramics, thin films, ion-implanted semiconductors), in environmental samples (waters, soils, biological and medical materials) and geological samples. Whereas such techniques as spark source mass spectrometry (SSMS), laser ionization mass spectrometry (LIMS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), glow discharge mass spectrometry (GDMS), secondary ion mass spectrometry (SIMS) and inductively coupled plasma mass spectrometry (ICP-MS) have multielemental capability, other methods such as thermal ionization mass spectrometry (TIMS), accelerator mass spectrometry (AMS) and resonance ionization mass spectrometry (RIMS) have been used for sensitive mono- or oligoelemental ultratrace analysis (and precise determination of isotopic ratios) in solid samples. The limits of detection for chemical elements using these mass spectrometric techniques are in the low ng g -1 concentration range. The quantification of the analytical results of mass spectrometric methods is sometimes difficult due to a lack of matrix-fitted multielement standard reference materials (SRMs) for many solid samples. Therefore, owing to the simple quantification procedure of the aqueous solution, inductively coupled plasma mass spectrometry (ICP-MS) is being increasingly used for the characterization of solid samples after sample dissolution. ICP-MS is often combined with special sample introduction equipment (e.g. flow injection, hydride generation, high performance liquid chromatography (HPLC) or electrothermal vaporization) or an off-line matrix separation and enrichment of trace impurities (especially for characterization of

  7. Mass spectrometry in systems biology an introduction.

    PubMed

    Dunn, Warwick B

    2011-01-01

    The qualitative detection, quantification, and structural characterization of analytes in biological systems are important requirements for objectives to be fulfilled in systems biology research. One analytical tool applied to a multitude of systems biology studies is mass spectrometry, particularly for the study of proteins and metabolites. Here, the role of mass spectrometry in systems biology will be assessed, the advantages and disadvantages discussed, and the instrument configurations available described. Finally, general applications will be briefly reviewed.

  8. Broadband Analysis of Bioagents by Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Fenselau, Catherine; Wynne, Colin; Edwards, Nathan

    Mass spectrometry was first reported to provide analysis of intact metabolite biomarkers from whole cells in 1975.1 Since then advances in ionization techniques have extended our capabilities to polar lipids and, eventually, to proteins.2, 3 Mass spectrometry provides a broadband detection system, which, however, has great specificity. Bioinformatics plays an important role in providing flexible and rapid characterization of species, based on protein and peptide mass spectra collected in the field.

  9. Mass Spectrometry Imaging Quick View

    2013-01-24

    MSI QuickView is a software designed to provide a graphical user interface (GUI) for greatly speeding up experimental feedback (visualization and analysis) of mass spectrometry imaging (MSI or IMS) data during data acquisition. Often different software loads the entire data set, i.e., all lines of data into computer memory (RAM). This causes out of memory errors for larger datasets. We solved this in MSI QuickView by reading in the data one line at a time.more » Only the required information (e.g. the final pixel values for that line of heat map) is maintained in RAM. Interim analysis options include the mean intensity vs. m/z spectrum, intensity vs. time spectrums for up to 6 different m/z values or ranges chosen by the user and heat maps for each line. This assists in validating the usefulness of the particular experiment after scanning the first few lines. In addition, the tool facilitates further processing and analysis of the massive datasets. The user can manually pick different m/z values, time ranges, scroll through the spectra for any line in the data without having to load it in manually, save multiple images, change aspect ratios for the heat maps, and process the heat maps in multiple ways including overlaying images at different m/z values, displaying up to 9 different heat maps, alignment of scans along each line etc. There is no manipulation of the data required by the user to visualize the data.« less

  10. Acoustic emission descriptors

    NASA Astrophysics Data System (ADS)

    Witos, Franciszek; Malecki, Ignacy

    The authors present selected problems associated with acoustic emission interpreted as a physical phenomenon and as a measurement technique. The authors examine point sources of acoustic emission in isotropic, homogeneous linearly elastic media of different shapes. In the case of an unbounded medium the authors give the analytical form of the stress field and the wave shift field of the acoustic emission. In the case of a medium which is unbounded plate the authors give a form for the equations which is suitable for numerical calculation of the changes over time of selected acoustic emission values. For acoustic emission as a measurement technique, the authors represent the output signal as the resultant of a mechanical input value which describes the source, the transient function of the medium, and the transient function of specific components of the measurement loop. As an effect of this notation, the authors introduce the distinction between an acoustic measurement signal and an acoustic measurement impulse. The authors define the basic parameters of an arbitrary impulse. The authors extensively discuss the signal functions of acoustic emission impulses and acoustic emission signals defined in this article as acoustic emission descriptors (or signal functions of acoustic emission impulses) and advanced acoustic emission descriptors (which are either descriptors associated with acoustic emission applications or the signal functions of acoustic emission signals). The article also contains the results of experimental research on three different problems in which acoustic emission descriptors associated with acoustic emission pulses, acoustic emission applications, and acoustic emission signals are used. These problems are respectively: a problem of the amplitude-load characteristics of acoustic emission pulses in carbon samples subjected to compound uniaxial compression, the use of acoustic emission to predict the durability characteristics of conveyor belts, and

  11. Volatile organic compound emissions from elephant grass and bamboo cultivars used as potential bioethanol crop

    NASA Astrophysics Data System (ADS)

    Crespo, E.; Graus, M.; Gilman, J. B.; Lerner, B. M.; Fall, R.; Harren, F. J. M.; Warneke, C.

    2013-02-01

    Volatile organic compound (VOC) emissions from elephant grass (Miscanthus gigantus) and black bamboo (Phyllostachys nigra) were measured online in semi-field chamber and plant enclosure experiments during growth and harvest using proton-transfer reaction mass spectrometry (PTR-MS), proton-transfer reaction ion-trap mass spectrometry (PIT-MS) and gas chromatography-mass spectrometry (GC-MS). Both cultivars are being considered for second-generation biofuel production. Before this study, no information was available on their yearly VOC emissions. This exploratory investigation shows that black bamboo is a strong isoprene emitter (daytime 28,516 ng gdwt-1 h-1) and has larger VOC emissions, especially for wound compounds from the hexanal and hexenal families, than elephant grass. Daytime emissions of methanol, acetaldehyde, acetone + propanal and acetic acid of black bamboo were 618, 249, 351, and 1034 ng gdwt-1 h-1, respectively. In addition, it is observed that elephant grass VOC emissions after harvesting strongly depend on the seasonal stage. Not taking VOC emission variations throughout the season for annual and perennial species into account, may lead to an overestimation of the impact on local air quality in dry periods. In addition, our data suggest that the use of perennial grasses for extensive growing for biofuel production have lower emissions than woody species, which might be important for regional atmospheric chemistry.

  12. Molecular hydrogen emission from the Cepheus A star-formation region

    SciTech Connect

    Doyon, R.; Nadeau, D.

    1988-11-01

    Fabry-Perot spectrometry of H2 emission lines in the Cepheus A star-formation region is presented. It is found that the H2 emission in Cep A(E) is associated with dense condensations of NH3 and CS, while the emission in Cep A(W) is associated with Herbig-Haro objects and reflection nebulae. The data support the hypothesis that the two lobes of emission are produced by a single outflow originating from the region of maser and compact H II regions at the western edge of Cep A(E). 49 references.

  13. Tropospheric Emission Spectrometer and Airborne Emission Spectrometer

    NASA Technical Reports Server (NTRS)

    Glavich, T.; Beer, R.

    1996-01-01

    The Tropospheric Emission Spectrometer (TES) is an instrument being developed for the NASA Earth Observing System Chemistry Platform. TES will measure the distribution of ozone and its precursors in the lower atmosphere. The Airborne Emission Spectrometer (AES) is an aircraft precursor to TES. Applicable descriptions are given of instrument design, technology challenges, implementation and operations for both.

  14. [Multivariate analysis of heavy metal element concentrations in atmospheric deposition in Harbin City, northeast China].

    PubMed

    Tang, Jie; Han, Wei-Zheng; Li, Na; Li, Zhao-Yang; Bian, Jian-Min; Li, Hai-Yi

    2011-11-01

    In order to understand the characteristics of atmospheric heavy metal deposition in Harbin City, 46 deposition samples were collected which were taken using bulk deposition samplers during the period of 2008-2009 (about 365 days). The samples were analyzed for heavy metal concentration by atomic fluorescence spectrometry (AFS) and inductively coupled plasma-atomic spectrometry (ICP-AES). The deposition flux was calculated. Sources analysis was made by the method of principal component analysis (PCA), Pearsons and enrichment factor (EF). The following points can be gained through multivariate analysis. Mn and Co are mostly from natural sources while the others may be brought by coal dust, vehicle emissions and metal smelting.

  15. Mass Spectrometry of Intact Membrane Protein Complexes

    PubMed Central

    Laganowsky, Arthur; Reading, Eamonn; Hopper, Jonathan T.S.; Robinson, Carol V.

    2014-01-01

    Mass spectrometry of intact soluble protein complexes has emerged as a powerful technique to study the stoichiometry, structure-function and dynamics of protein assemblies. Recent developments have extended this technique to the study of membrane protein complexes where it has already revealed subunit stoichiometries and specific phospholipid interactions. Here, we describe a protocol for mass spectrometry of membrane protein complexes. The protocol begins with preparation of the membrane protein complex enabling not only the direct assessment of stoichiometry, delipidation, and quality of the target complex, but also evaluation of the purification strategy. A detailed list of compatible non-ionic detergents is included, along with a protocol for screening detergents to find an optimal one for mass spectrometry, biochemical and structural studies. This protocol also covers the preparation of lipids for protein-lipid binding studies and includes detailed settings for a Q-ToF mass spectrometer after introduction of complexes from gold-coated nanoflow capillaries. PMID:23471109

  16. Sequencing Cyclic Peptides by Multistage Mass Spectrometry

    PubMed Central

    Mohimani, Hosein; Yang, Yu-Liang; Liu, Wei-Ting; Hsieh, Pei-Wen; Dorrestein, Pieter C.; Pevzner, Pavel A.

    2012-01-01

    Some of the most effective antibiotics (e.g., Vancomycin and Daptomycin) are cyclic peptides produced by non-ribosomal biosynthetic pathways. While hundreds of biomedically important cyclic peptides have been sequenced, the computational techniques for sequencing cyclic peptides are still in their infancy. Previous methods for sequencing peptide antibiotics and other cyclic peptides are based on Nuclear Magnetic Resonance spectroscopy, and require large amount (miligrams) of purified materials that, for most compounds, are not possible to obtain. Recently, development of mass spectrometry based methods has provided some hope for accurate sequencing of cyclic peptides using picograms of materials. In this paper we develop a method for sequencing of cyclic peptides by multistage mass spectrometry, and show its advantages over single stage mass spectrometry. The method is tested on known and new cyclic peptides from Bacillus brevis, Dianthus superbus and Streptomyces griseus, as well as a new family of cyclic peptides produced by marine bacteria. PMID:21751357

  17. Mass spectrometry: a revolution in clinical microbiology?

    PubMed

    Lavigne, Jean-Philippe; Espinal, Paula; Dunyach-Remy, Catherine; Messad, Nourredine; Pantel, Alix; Sotto, Albert

    2013-02-01

    Recently, different bacteriological laboratory interventions that decrease reporting time have been developed. These promising new broad-based techniques have merit, based on their ability to identify rapidly many bacteria, organisms difficult to grow or newly emerging strains, as well as their capacity to track disease transmission. The benefit of rapid reporting of identification and/or resistance of bacteria can greatly impact patient outcomes, with an improvement in the use of antibiotics, in the reduction of the emergence of multidrug resistant bacteria and in mortality rates. Different techniques revolve around mass spectrometry (MS) technology: matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS), PCR combined with electrospray ionization-mass spectrometry (PCR/ESIMS), iPLEX MassArray system and other new evolutions combining different techniques. This report emphasizes the (r)evolution of these technologies in clinical microbiology.

  18. [Imaging Mass Spectrometry in Histopathologic Analysis].

    PubMed

    Yamazaki, Fumiyoshi; Seto, Mitsutoshi

    2015-04-01

    Matrix-assisted laser desorption/ionization (MALDI)-imaging mass spectrometry (IMS) enables visualization of the distribution of a range of biomolecules by integrating biochemical information from mass spectrometry with positional information from microscopy. IMS identifies a target molecule. In addition, IMS enables global analysis of biomolecules containing unknown molecules by detecting the ratio of the molecular weight to electric charge without any target, which makes it possible to identify novel molecules. IMS generates data on the distribution of lipids and small molecules in tissues, which is difficult to visualize with either conventional counter-staining or immunohistochemistry. In this review, we firstly introduce the principle of imaging mass spectrometry and recent advances in the sample preparation method. Secondly, we present findings regarding biological samples, especially pathological ones. Finally, we discuss the limitations and problems of the IMS technique and clinical application, such as in drug development. PMID:26536781

  19. Capillary electrophoresis electrospray ionization mass spectrometry interface

    DOEpatents

    Smith, Richard D.; Severs, Joanne C.

    1999-01-01

    The present invention is an interface between a capillary electrophoresis separation capillary end and an electrospray ionization mass spectrometry emitter capillary end, for transporting an anolyte sample from a capillary electrophoresis separation capillary to a electrospray ionization mass spectrometry emitter capillary. The interface of the present invention has: (a) a charge transfer fitting enclosing both of the capillary electrophoresis capillary end and the electrospray ionization mass spectrometry emitter capillary end; (b) a reservoir containing an electrolyte surrounding the charge transfer fitting; and (c) an electrode immersed into the electrolyte, the electrode closing a capillary electrophoresis circuit and providing charge transfer across the charge transfer fitting while avoiding substantial bulk fluid transfer across the charge transfer fitting. Advantages of the present invention have been demonstrated as effective in providing high sensitivity and efficient analyses.

  20. NARSTO EMISSION INVENTORY ASSESSMENT

    EPA Science Inventory

    The NARSTO Ozone and Particulate Matter Assessments emphasized that emission inventories are critical to the success of air quality management programs and that emissions inventories in Canada, Mexico, and the United States need improvement to meet expectations for quality, timel...

  1. Control of Emissions

    NASA Technical Reports Server (NTRS)

    Parrish, Clyde F. (Inventor); Chung, Landy (Inventor)

    2013-01-01

    Methods and apparatus utilizing chlorine dioxide and hydrogen peroxide are useful to reduce NOx emissions, as well as SOx and mercury (or other heavy metal) emissions, from combustion flue gas streams.

  2. High-resolution alpha-particle spectrometry of the 230U decay series.

    PubMed

    Marouli, M; Pommé, S; Paepen, J; Van Ammel, R; Jobbágy, V; Dirican, A; Suliman, G; Stroh, H; Apostolidis, C; Abbas, K; Morgenstern, A

    2012-09-01

    High-resolution alpha-particle spectrometry was performed on the (230)U decay series. A (230)U source was prepared on a stainless steel disc by electrodeposition in an ammonium nitrate solution. Spectrometry of the alpha-particle energy spectrum was performed with ion-implanted planar silicon detectors in vacuum. A set of alpha emission probabilities is presented for (230)U and (226)Th. The measured peak intensities were corrected mathematically for coincidental detection of alpha-particles and conversion electrons emitted in the same decay. A good agreement with literature data was observed. The uncertainty budget and the correlation matrix are presented. The validity of the alpha-particle energies was tested and could be confirmed for most peaks within a few keV, but discrepancies were found for the 2nd peak of (226)Th and the main peak of (218)Rn.

  3. Determination of elements by atomic absorption spectrometry in medicinal plants employed to alleviate common cold symptoms.

    PubMed

    Küçükbay, F Zehra; Kuyumcu, Ebru

    2014-09-01

    Eleven important medicinal plants generally used by the people of Turkey for the treatment of common cold have been studied for their mineral contents. Eleven minor and major elements (essential, non-essential and toxic) were identified in the Asplenium adiantum-nigrum L. , Althaea officinalis L. , Verbascum phlomoides L., Euphorbia chamaesyce L., Zizyphus jujube Miller, Peganum harmala L., Arum dioscoridis Sm., Sambucus nigra L., Piperlongum L., Tussilago farfara L. and Elettaria cardamomum Maton by employing flame atomic absorption and emission spectrometry and electro-thermal atomic absorption spectrometry. Microwave digestion procedure for total concentration was applied under optimized conditions for dissolution of medicinal plants. Plant based biological certified reference materials (CRMs) served as standards for quantification. These elements are found to be present in varying concentrations in the studied plants. The baseline data presented in this work can be used in understanding the role of essential, non-essential and toxic elements in nutritive, preventive and therapeutic properties of medicinal plants.

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

    NASA Technical Reports Server (NTRS)

    Wittmann, A.; Willay, G.

    1986-01-01

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

  5. Acoustic emission frequency discrimination

    NASA Technical Reports Server (NTRS)

    Sugg, Frank E. (Inventor); Graham, Lloyd J. (Inventor)

    1988-01-01

    In acoustic emission nondestructive testing, broadband frequency noise is distinguished from narrow banded acoustic emission signals, since the latter are valid events indicative of structural flaws in the material being examined. This is accomplished by separating out those signals which contain frequency components both within and beyond (either above or below) the range of valid acoustic emission events. Application to acoustic emission monitoring during nondestructive bond verification and proof loading of undensified tiles on the Space Shuttle Orbiter is considered.

  6. Mass Spectrometry in the Home and Garden

    NASA Astrophysics Data System (ADS)

    Pulliam, Christopher J.; Bain, Ryan M.; Wiley, Joshua S.; Ouyang, Zheng; Cooks, R. Graham

    2015-02-01

    Identification of active components in a variety of chemical products used directly by consumers is described at both trace and bulk levels using mass spectrometry. The combination of external ambient ionization with a portable mass spectrometer capable of tandem mass spectrometry provides high chemical specificity and sensitivity as well as allowing on-site monitoring. These experiments were done using a custom-built portable ion trap mass spectrometer in combination with the ambient ionization methods of paper spray, leaf spray, and low temperature plasma ionization. Bactericides, garden chemicals, air fresheners, and other products were examined. Herbicide applied to suburban lawns was detected in situ on single leaves 5 d after application.

  7. Analysis of Electroblotted Proteins by Mass Spectrometry

    PubMed Central

    Luque-Garcia, Jose L.; Neubert, Thomas A.

    2015-01-01

    Summary Identification of proteins by mass spectrometry is crucial for better understanding of many biological, biochemical, and biomedical processes. Here we describe two methods for the identification of electroblotted proteins by on-membrane digestion prior to analysis by mass spectrometry. These on-membrane methods take approximately half the time of in-gel digestion and provide better digestion efficiency, due to the better accessibility of the protease to the proteins adsorbed onto the nitrocellulose, and better protein sequence coverage, especially for membrane proteins where large and hydrophobic peptides are commonly present. PMID:26139272

  8. Mass spectrometry for pectin structure analysis.

    PubMed

    Ralet, Marie-Christine; Lerouge, Patrice; Quéméner, Bernard

    2009-09-28

    Pectin are extremely complex biopolymers made up of different structural domains. Enzymatic degradation followed by purification and structural analysis of the degradation products proved to be efficient tools for the understanding of pectin fine structure, including covalent interactions between pectic structural domains or with other cell wall polysaccharides. Due to its high sensitivity, high throughput and capacity to analyze mixtures, mass spectrometry has gained more and more importance as a tool for oligosaccharides structural characterization in the past 10 years. This review will focus on the combined use of mass spectrometry and enzymatic digestion for pectins structural characterization. PMID:19058795

  9. Third International Workshop on Ion Mobility Spectrometry

    NASA Technical Reports Server (NTRS)

    Cross, John H. (Editor)

    1995-01-01

    Basic research in ion mobility spectrometry has given rise to rapid advancement in hardware development and applications. The Third International Workshop on Ion Mobility Spectrometry (IMS) was held October 16-19, 1994, at Johnson Space Center to provide a forum for investigators to present the most recent results of both basic and applied IMS research. Presenters included manufacturers and various users, including military research organizations and drug enforcement agencies. Thirty papers were given in the following five sessions: Fundamental IMS Studies, Instrument Development, Hyphenated IMS Techniques, Applications, and Data Reduction and Signal Processing. Advances in hardware development, software development, and user applications are described.

  10. Simultaneous determination of arsenic, cadmium, calcium, chromium, cobalt, copper, iron, lead, magnesium, manganese, molybdenum, nickel, selenium, and zinc in fertilizers by microwave acid digestion and inductively coupled plasma-optical emission spectrometry detection: single-laboratory validation of a modification and extension of AOAC 2006.03.

    PubMed

    Webb, Sharon; Bartos, James; Boles, Rhonda; Hasty, Elaine; Thuotte, Ethel; Thiex, Nancy J

    2014-01-01

    A single-laboratory validation study was conducted for the simultaneous determination of arsenic, cadmium, calcium, cobalt, copper, chromium, iron, lead, magnesium, manganese, molybdenum, nickel, selenium, and zinc in all major types of commercial fertilizer products by microwave digestion and inductively coupled plasma-optical emission spectroscopy analysis. This validation study proposes an extension and modification of AOAC 2006.03. The extension is the inclusion of calcium, copper, iron, magnesium, manganese, and zinc, and the modification is incorporation of hydrochloric acid in the digestion system. This dual acid digestion utilizes both hydrochloric and nitric acids in a 3 to 9 mL volume ratio/100 mL. In addition to 15 of the 30 original validation materials used in the 2006.03 collaborative study, National Institute of Standards and Technology Standard Reference Material 695 and Magruder 2009-06 were incorporated as accuracy materials. The main benefits of this proposed method are a significant increase in laboratory efficiency when compared to the use of both AOAC Methods 965.09 and 2006.03 to achieve the same objective and an enhanced recovery of several metals.

  11. Emissions from cooking microwave popcorn.

    PubMed

    Rosati, Jacky A; Krebs, Kenneth A; Liu, Xiaoyu

    2007-01-01

    This study characterized chemicals released into a chamber in the process of cooking microwave popcorn. Seventeen types of microwave popcorn from eight different brands were studied. The work proceeded in two phases: phase one investigated chemicals emitted during popping and opening, phase two investigated chemicals emitted at discrete intervals from 0-40 minutes post-pop opening. The research was performed using a microwave oven enclosed in a chamber with ports for air sampling of particulate matter (PM) and volatile organic compounds (VOCs). VOCs in the air samples were identified and quantified using gas chromatography/mass spectrometry (GC/MS). PM was characterized using both an aerodynamic particle sizer (APS) and a scanning mobility particle sizer (SMPS) to cover a full range of emitted sizes. The compounds measured during popping and opening included butter flavoring components such as diacetyl, butyric acid, acetoin, propylene glycol, 2-nonanone, and triacetin and bag components such as p-xylene and perfluorinated alcohol 8:2 telomer. The greatest chemical quantity is emitted when the bag is opened post-popping; more than 80% of the total chemical emissions occur at this time. PMID:17987444

  12. Linking Mass Spectrometry with Toxicology for Emerging Water Contaminants

    EPA Science Inventory

    This overview presentation will discuss the benefits of combining mass spectrometry with toxicology. These benefits will be described for 3 main areas: (1) Toxicity assays used to test new environmental contaminants previously identified using mass spectrometry, such that furth...

  13. Warming increases isoprene emissions from an arctic fen.

    PubMed

    Lindwall, Frida; Svendsen, Sophie Sylvest; Nielsen, Cecilie Skov; Michelsen, Anders; Rinnan, Riikka

    2016-05-15

    Emissions of biogenic volatile organic compounds (BVOCs) from dry ecosystems at high latitudes respond strongly to small increases in temperature, and warm canopy surface temperatures drive emissions to higher levels than expected. However, it is not known whether emissions from wetlands, cooled by through-flowing water and higher evapotranspiration show similar response to warming as in drier ecosystems. Climate change will cause parts of the Arctic to experience increased snow fall, which delays the start of the growing season, insulates soil from low temperatures in winter, and increases soil moisture and possibly nutrient availability. Currently the effects of increasing snow depth on BVOC emissions are unknown. BVOC emissions were measured in situ across the growing season in a climate experiment, which used open top chambers to increase temperature and snow fences to increase winter snow depth. The treatments were arranged in a full factorial design. Measurements took place during two growing seasons in a fen ecosystem in west Greenland. BVOC samples collected by an enclosure technique in adsorbent cartridges were analysed using gas chromatography-mass spectrometry. Gross ecosystem production (GEP) was measured with a closed chamber technique, to reveal any immediate effect of treatments on photosynthesis, which could further influence BVOC emissions. Isoprene made up 84-92% of the emitted BVOCs. Isoprene emission increased 240 and 340% due to an increase in temperature of 1.3 and 1.6°C in 2014 and 2015, respectively. Isoprene emissions were 25 times higher in 2015 than in 2014 most likely due to a 2.4°C higher canopy air temperature during sampling in 2015. Snow addition had no significant effect on isoprene emissions even though GEP was increased by 24%. Arctic BVOC emissions respond strongly to rising temperatures in wet ecosystems, suggesting a large increase in arctic emissions in a future warmer climate.

  14. Galactic Diffuse Emissions

    SciTech Connect

    Digel, Seth W.; /SLAC

    2007-10-25

    Interactions of cosmic rays with interstellar nucleons and photons make the Milky Way a bright, diffuse source of high-energy {gamma}-rays. Observationally, the results from EGRET, COMPTEL, and OSSE have now been extended to higher energies by ground-based experiments, with detections of diffuse emission in the Galactic center reported by H.E.S.S. in the range above 100 GeV and of diffuse emission in Cygnus by MILAGRO in the TeV range. In the range above 100 keV, INTEGRAL SPI has found that diffuse emission remains after point sources are accounted for. I will summarize current knowledge of diffuse {gamma}-ray emission from the Milky Way and review some open issues related to the diffuse emission -- some old, like the distribution of cosmic-ray sources and the origin of the 'excess' of GeV emission observed by EGRET, and some recently recognized, like the amount and distribution of molecular hydrogen not traced by CO emission -- and anticipate some of the advances that will be possible with the Large Area Telescope on GLAST. We plan to develop an accurate physical model for the diffuse emission, which will be useful for detecting and accurately characterizing emission from Galactic point sources as well as any Galactic diffuse emission from exotic processes, and for studying the unresolved extragalactic emission.

  15. Temporal and modal characterization of DoD source air toxic emission factors: final report

    EPA Science Inventory

    This project tested three, real-/near real-time monitoring techniques to develop air toxic emission factors for Department of Defense (DoD) platform sources. These techniques included: resonance enhanced multi photon ionization time of flight mass spectrometry (REMPI-TOFMS) for o...

  16. Introduction to mass spectrometry-based proteomics.

    PubMed

    Matthiesen, Rune; Bunkenborg, Jakob

    2013-01-01

    Mass spectrometry has been widely applied to study biomolecules and one rapidly developing field is the global analysis of proteins, proteomics. Understanding and handling mass spectrometry data is a multifaceted task that requires many decisions to be made to get the most comprehensive information from an experiment. Later chapters in this book deal in-depth with various aspects of the process and how different tools can be applied to the many analytical challenges. This introductory chapter is intended as a basic introduction to mass spectrometry (MS)-based proteomics to set the scene for newcomers and give pointers to reference material. There are many applications of mass spectrometry in proteomics and each application is associated with some analytical choices, instrumental limitations and data processing steps that depend on the aim of the study and means of conducting it. Different aspects of the proteome can be explored by choosing the right combination of sample preparation, MS instrumentation and data processing. This chapter gives an outline for some of these commonly used setups and some of the key concepts, many of which are explored in greater depth in later chapters. PMID:23666720

  17. Nanostructure-initiator mass spectrometry biometrics

    DOEpatents

    Leclerc, Marion; Bowen, Benjamin; Northen, Trent

    2015-09-08

    Several embodiments described herein are drawn to methods of identifying an analyte on a subject's skin, methods of generating a fingerprint, methods of determining a physiological change in a subject, methods of diagnosing health status of a subject, and assay systems for detecting an analyte and generating a fingerprint, by nanostructure-initiator mass spectrometry (NIMS).

  18. Pyrolysis Mass Spectrometry of Complex Organic Materials.

    ERIC Educational Resources Information Center

    Meuzelaar, Henk L. C.; And Others

    1984-01-01

    Illustrates the state of the art in pyrolysis mass spectrometry techniques through applications in: (1) structural determination and quality control of synthetic polymers; (2) quantitative analysis of polymer mixtures; (3) classification and structural characterization of fossil organic matter; and (4) nonsupervised numerical extraction of…

  19. Atmospheric pressure femtosecond laser imaging mass spectrometry

    NASA Astrophysics Data System (ADS)

    Coello, Yves; Gunaratne, Tissa C.; Dantus, Marcos

    2009-02-01

    We present a novel imaging mass spectrometry technique that uses femtosecond laser pulses to directly ionize the sample. The method offers significant advantages over current techniques by eliminating the need of a laser-absorbing sample matrix, being suitable for atmospheric pressure sampling, and by providing 10μm resolution, as demonstrated here with a chemical image of vegetable cell walls.

  20. Introduction to mass spectrometry-based proteomics.

    PubMed

    Matthiesen, Rune; Bunkenborg, Jakob

    2013-01-01

    Mass spectrometry has been widely applied to study biomolecules and one rapidly developing field is the global analysis of proteins, proteomics. Understanding and handling mass spectrometry data is a multifaceted task that requires many decisions to be made to get the most comprehensive information from an experiment. Later chapters in this book deal in-depth with various aspects of the process and how different tools can be applied to the many analytical challenges. This introductory chapter is intended as a basic introduction to mass spectrometry (MS)-based proteomics to set the scene for newcomers and give pointers to reference material. There are many applications of mass spectrometry in proteomics and each application is associated with some analytical choices, instrumental limitations and data processing steps that depend on the aim of the study and means of conducting it. Different aspects of the proteome can be explored by choosing the right combination of sample preparation, MS instrumentation and data processing. This chapter gives an outline for some of these commonly used setups and some of the key concepts, many of which are explored in greater depth in later chapters.

  1. Decimetric radio dot emissions

    NASA Astrophysics Data System (ADS)

    Mészárosová, H.; Karlický, M.; Sawant, H. S.; Fernandes, F. C. R.; Cecatto, J. R.; de Andrade, M. C.

    2008-11-01

    Context: We study a rare type of solar radio bursts called decimetric dot emissions. Aims: In the period 1999-2001, 20 events of decimetric dot emissions observed by the Brazilian Solar Spectroscope (BSS) in the frequency range 950-2640 MHz are investigated statistically and compared with radio fine structures of zebras and fibers. Methods: For the study of the spectral characteristics of the dot emissions we use specially developed Interactive Data Language (IDL) software called BSSView and basic statistical methods. Results: We have found that the dm dot emissions, contrary to the fine structures of the type IV bursts (i.e. zebras, fibers, lace bursts, spikes), are not superimposed on any background burst emission. In the radio spectrum, in most cases the dot emissions form chains that appear to be arranged in zebra patterns or fibers. Because some zebras and fibers, especially those observed with high time and high spectral resolutions, also show emission dots (but superimposed on the background burst emission), we compared the spectral parameters of the dot emissions with the dots being the fine structure of zebras and fibers. For both these dots, similar spectral characteristics were found. Some similarities of the dot emissions can be found also with the lace bursts and spikes. For some events the dot emissions show structural evolution from patterns resembling fibers to patterns resembling zebras and vice versa, or they evolve into fully chaotic patterns. Conclusions: For the first time, we present decimetric dot emissions that appear to be arranged in zebra patterns or fibers. We propose that these emissions are generated by the plasma emission mechanism at the locations in the solar atmosphere where the double resonance condition is fulfilled.

  2. Low Emissions Aftertreatment and Diesel Emissions Reduction

    SciTech Connect

    2005-05-27

    Detroit Diesel Corporation (DDC) has successfully completed a five-year Low Emissions Aftertreatment and Diesel Emissions Reduction (LEADER) program under a DOE project entitled: ''Research and Development for Compression-Ignition Direct-Injection Engines (CIDI) and Aftertreatment Sub-Systems''. The objectives of the LEADER Program were to: Demonstrate technologies that will achieve future federal Tier 2 emissions targets; and Demonstrate production-viable technical targets for engine out emissions, efficiency, power density, noise, durability, production cost, aftertreatment volume and weight. These objectives were successfully met during the course of the LEADER program The most noteworthy achievements in this program are listed below: (1) Demonstrated Tier 2 Bin 3 emissions target over the FTP75 cycle on a PNGV-mule Neon passenger car, utilizing a CSF + SCR system These aggressive emissions were obtained with no ammonia (NH{sub 3}) slip and a combined fuel economy of 63 miles per gallon, integrating FTP75 and highway fuel economy transient cycle test results. Demonstrated feasibility to achieve Tier 2 Bin 8 emissions levels without active NOx aftertreatment. (2) Demonstrated Tier 2 Bin 3 emissions target over the FTP75 cycle on a light-duty truck utilizing a CSF + SCR system, synergizing efforts with the DOE-DDC DELTA program. This aggressive reduction in tailpipe out emissions was achieved with no ammonia slip and a 41% fuel economy improvement, compared to the equivalent gasoline engine-equipped vehicle. (3) Demonstrated Tier 2 near-Bin 9 emissions compliance on a light-duty truck, without active NOx aftertreatment devices, in synergy with the DOE-DDC DELTA program. (4) Developed and applied advanced combustion technologies such as ''CLEAN Combustion{copyright}'', which yields simultaneous reduction in engine out NOx and PM emissions while also improving engine and aftertreatment integration by providing favorable exhaust species and temperature

  3. Optical emission spectroscopy studies of the influence of laser ablated mass on dry inductively coupled plasma conditions

    NASA Astrophysics Data System (ADS)

    Ciocan, A. C.; Mao, X. L.; Borisov, Oleg V.; Russo, R. E.

    1998-03-01

    The amount of ablated mass can influence the temperature and excitation characteristics of the inductively coupled plasma (ICP) and must be taken into account to ensure accurate chemical analysis. The ICP electron number density was investigated by using measurements of the Mg ionic to atomic resonant-line ratios during laser ablation of an aluminum matrix. The ICP excitation temperature was measured by using selected Fe lines during laser ablation of an iron matrix. A Nd:YAG laser (3 ns pulse duration) at 266 nm was used for these ablation-sampling studies. Laser energy, power density, and repetition rate were varied in order to change the quantity of ablated mass into the ICP. Over the range of laser operating conditions studied herein, the ICP was not significantly influenced by the quantity of solid sample. Therefore, analytical measurements can be performed accurately and fundamental studies of laser ablation processes (such as ablation mass roll-off, fractional vaporization) can be investigated using inductively coupled plasma-atomic emission spectroscopy (ICP-AES).

  4. REAL-TIME EMISSION CHARACTERIZATION OF ORGANIC AIR TOXIC POLLUTANTS DURING STEADY STATE AND TRANSIENT OPERATION OF A MEDIUM DUTY DIESEL ENGINE

    EPA Science Inventory

    An on-line monitoring method, jet resonance-enhanced multi-photon ionization (REMPI) with time-of-flight mass spectrometry (TOFMS) was used to measure emissions of organic air toxics from a medium-duty (60 kW)diesel generator during transient and steady state operations. Emission...

  5. High-sensitivity mass spectrometry with a tandem accelerator

    SciTech Connect

    Henning, W.

    1983-01-01

    The characteristic features of accelerator mass spectrometry are discussed. A short overview is given of the current status of mass spectrometry with high-energy (MeV/nucleon) heavy-ion accelerators. Emphasis is placed on studies with tandem accelerators and on future mass spectrometry of heavier isotopes with the new generation of higher-voltage tandems.

  6. Properties, performance and emissions of biofuels in blends with gasoline

    NASA Astrophysics Data System (ADS)

    Eslami, Farshad

    The emission performance of fuels and their blends in modern combustion systems have been studied with the purpose of reducing regulated and unregulated emissions, understanding of exhaust products of fuels such as gasoline, ethanol and 2,5-dimethylfuran and comparison of results. A quantitative analysis of individual hydrocarbon species from exhaust emissions of these three fuels were carried out with direct injects spark ignition (DISI) single cylinder engine. The analysis of hydrocarbon species were obtained using gas chromatography-mass spectrometry (GCMS) connected on-line to SI engine. During this project, novel works have been done including the set up of on-line exhaust emission measurement device for detection and quantification of individual volatile hydrocarbons. Setting of a reliable gas chromatography mass spectrometry measurement system required definition and development of a precise method. Lubricity characteristics of biofuels and gasoline were investigated using High Frequency Reciprocating Rig (HFRR). Results showed great enhancing lubricity characteristics of biofuels when added to conventional gasoline. 2,5-dimenthylfuran was found to be the best among the fuels used, addition of this fuel to gasoline also showed better result compared with ethanol addition.

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

    NASA Astrophysics Data System (ADS)

    Betti, Maria

    2005-04-01

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

  8. A history of mass spectrometry in Australia.

    PubMed

    Downard, Kevin M; de Laeter, John R

    2005-09-01

    An interest in mass spectrometry in Australia can be traced back to the 1920s with an early correspondence with Francis Aston who first visited these shores a decade earlier. The region has a rich tradition in both the development of the field and its application, from early measurements of ionization and appearance potentials by Jim Morrison at the Council for Scientific and Industrial Research (CSIR) around 1950 to the design and construction of instrumentation including the first use of a triple quadrupole mass spectrometer for tandem mass spectrometry, the first suite of programs to simulate ion optics (SIMION), the development of early TOF/TOF instruments and orthogonal acceleration and the local design and construction of several generations of a sensitive high-resolution ion microprobe (SHRIMP) instrument. Mass spectrometry has been exploited in the study and characterization of the constituents of this nation's unique flora and fauna from Australian apples, honey, tea plant and eucalyptus oil, snake, spider, fish and frog venoms, coal, oil, sediments and shale, environmental studies of groundwater to geochronological dating of limestone and granite, other terrestrial and meteoritic rocks and coral from the Great Barrier Reef. Peter Jeffery's establishment of geochronological dating techniques in Western Australia in the early 1950s led to the establishment of geochronology research both at the Australian National University and at what is now the Curtin Institute of Technology in the 1960s. This article traces the history of mass spectrometry in its many guises and applications in the island continent of Australia. An article such as this can never be complete. It instead focuses on contributions of scientists who played a major role in the early establishment of mass spectrometry in Australia. In general, those who are presently active in the field, and whose histories are incomplete, have been mentioned at best only briefly despite their important

  9. New Cs sputter ion source with polyatomic ion beams for secondary ion mass spectrometry applications

    NASA Astrophysics Data System (ADS)

    Belykh, S. F.; Palitsin, V. V.; Veryovkin, I. V.; Kovarsky, A. P.; Chang, R. J. H.; Adriaens, A.; Dowsett, M. G.; Adams, F.

    2007-08-01

    A simple design for a cesium sputter ion source compatible with vacuum and ion-optical systems as well as with electronics of the commercially available Cameca IMS-4f instrument is reported. This ion source has been tested with the cluster primary ions of Sin- and Cun-. Our experiments with surface characterization and depth profiling conducted to date demonstrate improvements of the analytical capabilities of the secondary ion mass spectrometry instrument due to the nonadditive enhancement of secondary ion emission and shorter ion ranges of polyatomic projectiles compared to atomic ones with the same impact energy.

  10. Emissions of metals associated with motor vehicle roadways.

    PubMed

    Lough, Glynis C; Schauer, James J; Park, June-Soo; Shafer, Martin M; Deminter, Jeffrey T; Weinstein, Jason P

    2005-02-01

    Emissions of metals and other particle-phase species from on-road motor vehicles were measured in two tunnels in Milwaukee, WI during the summer of 2000 and winter of 2001. Emission factors were calculated from measurements of fine (PM2.5) and coarse (PM10) particulate matter at tunnel entrances and exits, and effects of fleet composition and season were investigated. Cascade impactors (MOUDI) were used to obtain size-resolved metal emission rates. Metals were quantified with inductively-coupled plasma mass spectrometry (ICP-MS) and X-ray fluorescence (XRF). PM10 emission rates ranged from 38.7 to 201 mg km(-1) and were composed mainly of organic carbon (OC, 30%), inorganic ions (sulfate, chloride, nitrate, ammonium, 20%), metals (19%), and elemental carbon (EC, 9.3%). PM10 metal emissions were dominated by crustal elements Si, Fe, Ca, Na, Mg, Al, and K, and elements associated with tailpipe emissions and brake and tire wear, including Cu, Zn, Sb, Ba, Pb, and S. Metals emitted in PM2.5 were lower (11.6% of mass). Resuspension of roadway dust was dependent on weather and road surface conditions, and increased emissions were related to higher traffic volumes and fractions of heavy trucks. Emission of noble metals from catalytic converters appeared to be impacted by the presence of older vehicles. Elements related to brake wear were impacted by enriched road dust resuspension, but correlations between these elements in PM2.5 indicate that direct brake wear emissions are also important. A submicrometer particle mode was observed in the emissions of Pb, Ca, Fe, and Cu.

  11. Global Seabird Ammonia Emissions

    NASA Astrophysics Data System (ADS)

    Riddick, S. N.; Blackall, T. D.; Dragosits, U.; Daunt, F. H.; Braban, C. F.; Tang, Y. S.; Trathan, P.; Wanless, S.; Sutton, M. A.

    2010-12-01

    Seabird colonies represent a major source of atmospheric ammonia (NH3) in remote coastal and marine systems in temperate, tropical and polar regions. Previous studies have shown that NH3 emissions from Scottish seabird colonies were substantial - of similar magnitude to the most intensive agricultural point source emissions. The UK data were used to model global seabird NH3 emissions and suggested that penguins are a major source of emissions on and around the Antarctic continent. The largest seabird colonies are in the order of millions of seabirds. Due to the isolation of these colonies from anthropogenic nitrogen sources, they may play a major role in the nitrogen cycle within these ecosystems. A global seabird database was constructed and used in conjunction with a species-specific seabird bioenergetics model to map the locations of NH3 emissions from seabird colonies. The accuracy of the modelled emissions was validated with field data of NH3 emissions measured at key seabird colonies in different climatic regions of the world: temperate (Isle of May, Scotland), tropical (Ascension Island) and polar (Signy Island, South Georgia). The field data indicated good agreement between modelled and measured NH3 emissions. The measured NH3 emissions also showed the variability of emission with climate. Climate dependence of seabird NH3 emissions may have further implications under a changing global climate. Seabird colonies represent NH3 emission ‘hotspots’, often far from anthropogenic sources, and are likely to be the major source of nitrogen input to these remote coastal ecosystems. The direct manuring by seabirds at colony locations may strongly influence species richness and biodiversity. The subsequent volatilisation and deposition of NH3 increases the spatial extent of seabird influence on nitrogen cycling in their local ecosystem. As many seabird populations are fluctuating due to changing food supply, climate change or anthropogenic pressures, these factors

  12. Purification of silicon powder by the formation of thin porous layer followed byphoto-thermal annealing

    PubMed Central

    2012-01-01

    Porous silicon has been prepared using a vapor-etching based technique on a commercial silicon powder. Strong visible emission was observed in all samples. Obtained silicon powder with a thin porous layer at the surface was subjected to a photo-thermal annealing at different temperatures under oxygen atmosphere followed by a chemical treatment. Inductively coupled plasma atomic emission spectrometry results indicate that silicon purity is improved from 99.1% to 99.994% after annealing at 900°C. PMID:22873706

  13. Toluene emissions from plants

    NASA Astrophysics Data System (ADS)

    Heiden, A. C.; Kobel, K.; Komenda, M.; Koppmann, R.; Shao, M.; Wildt, J.

    The emission of toluene from different plants was observed in continuously stirred tank reactors and in field measurements. For plants growing without stress, emission rates were low and ranged from the detection limit up to 2·10-16 mol·cm-2·s-1. Under conditions of stress, the emission rates exceeded 10-14 mol·cm-2·s-1. Exposure of sunflower (Helianthus annuus L. cv. Gigantheus) to 13CO2 resulted in 13C-labeling of the emitted toluene on a time scale of hours. Although no biochemical pathway for the production of toluene is known, these results indicate that toluene is synthesized by the plants. The emission rates of toluene from sunflower are dependent on nutrient supply and wounding. Since α-pinene emission rates are also influenced by these factors, toluene and α-pinene emissions show a high correlation. During pathogen attack on Scots pines (Pinus sylvestris L.) significant toluene emissions were observed. In this case emissions of toluene and α-pinene also show a good correlation. Toluene emissions were also found in field experiments with pines using branch enclosures.

  14. Field emission chemical sensor

    DOEpatents

    Panitz, J.A.

    1983-11-22

    A field emission chemical sensor for specific detection of a chemical entity in a sample includes a closed chamber enclosing two field emission electrode sets, each field emission electrode set comprising (a) an electron emitter electrode from which field emission electrons can be emitted when an effective voltage is connected to the electrode set; and (b) a collector electrode which will capture said electrons emitted from said emitter electrode. One of the electrode sets is passive to the chemical entity and the other is active thereto and has an active emitter electrode which will bind the chemical entity when contacted therewith.

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

    SciTech Connect

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

    2015-01-14

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

  16. Monitoring Trace Contaminants in Air Via Ion Trap Mass Spectrometry

    NASA Technical Reports Server (NTRS)

    Palmer, Peter T.; Karr, Dane; Pearson, Richard; Valero, Gustavo; Wong, Carla

    1995-01-01

    Recent passage of the Clean Air Act with its stricter regulation of toxic gas emissions, and the ever-growing number of applications which require faster turnaround times between sampling and analysis are two major factors which are helping to drive the development of new instrument technologies for in-situ, on-line, real-time monitoring. The ion trap, with its small size, excellent sensitivity, and tandem mass spectrometry capability is a rapidly evolving technology which is well-suited for these applications. In this paper, we describe the use of a commercial ion trap instrument for monitoring trace levels of chlorofluorocarbons (CFCs) and volatile organic compounds (VOCs) in air. A number of sample introduction devices including a direct transfer line interface, short column GC, and a cryotrapping interface are employed to achieve increasing levels of sensitivity. MS, MS/MS, and MS/MS/MS methods are compared to illustrate trade-offs between sensitivity and selectivity. Filtered Noise Field (FNF) technology is found to be an excellent means for achieving lower detection limits through selective storage of the ion(s) of interest during ionization. Figures of merit including typical sample sizes, detection limits, and response times are provided. The results indicate the potential of these techniques for atmospheric assessments, the High Speed Research Program, and advanced life support monitoring applications for NASA.

  17. [Combustion temperature measurement of pyrotechnic composition using remote sensing Fourier transform infrared spectrometry].

    PubMed

    Zhou, Xin-li; Li, Yan; Liu, Zu-liang; Zhu, Chang-jiang; Wang, Jun-de; Lu, Chun-xu

    2002-10-01

    In this paper, combustion characterization of pyrotechnic composition is investigated using a remote sensing Fourier transform infrared spectrometry. The emission spectra have been recorded between 4,700 and 740 cm-1 with a spectral resolution of 4 cm-1. The combustion temperature can be determined remotely from spectral line intensity distribution of the fine structure of the emission fundamental band of gaseous products such as HF. The relationship between combustion temperature and combustion time has been given. Results show that there is a violent mutative temperature field with bigger temperature gradient near combustion surface. It reveals that the method of temperature measurement using remote sensing FTIR for flame temperature of unstable, violent and short time combustion on real time is a rapid, accurate and sensitive technique without interference the flame temperature field. Potential prospects of temperature measurement, gas product concentration measurement and combustion mechanism are also revealed.

  18. Emissions of oxygenated volatile organic compounds from open crop burning in Yangtze River Delta region, China

    NASA Astrophysics Data System (ADS)

    Tanimoto, H.; Kudo, S.; Pan, X.; Inomata, S.; Saito, S.; Kanaya, Y.; Wang, Z.

    2013-12-01

    Measurements of volatile organic compounds (VOCs) were made by gas chromatography/flame ionization detection/mass spectrometry (GC/FID/MS) and proton transfer reaction-mass spectrometry (PTR-MS) at Rudong, a rural area of Central East China in June 2010. During the campaign we identified several plumes originated from open biomass burning by the simultaneous enhancements of carbon monoxide and acetonitrile. Based on positive matrix factorization (PMF) analysis, the contribution of biomass burning was in the range from 60 to 80% for the plumes. We found that oxygenated VOCs were predominant for these events. The emission ratios of OVOCs to CO for open crop burnings derived in this work were found to be high. Combined with the updated CO emissions of 12.7 Tg per year from crop burning, we estimated OVOC emissions from crop burning can be about 1.2 Tg per year, accounting for substantial amount of VOCs emitted from crop burning.

  19. Analytical Aspects of Hydrogen Exchange Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Engen, John R.; Wales, Thomas E.

    2015-07-01

    This article reviews the analytical aspects of measuring hydrogen exchange by mass spectrometry (HX MS). We describe the nature of analytical selectivity in hydrogen exchange, then review the analytical tools required to accomplish fragmentation, separation, and the mass spectrometry measurements under restrictive exchange quench conditions. In contrast to analytical quantitation that relies on measurements of peak intensity or area, quantitation in HX MS depends on measuring a mass change with respect to an undeuterated or deuterated control, resulting in a value between zero and the maximum amount of deuterium that can be incorporated. Reliable quantitation is a function of experimental fidelity and to achieve high measurement reproducibility, a large number of experimental variables must be controlled during sample preparation and analysis. The method also reports on important qualitative aspects of the sample, including conformational heterogeneity and population dynamics.

  20. Impact of automation on mass spectrometry.

    PubMed

    Zhang, Yan Victoria; Rockwood, Alan

    2015-10-23

    Mass spectrometry coupled to liquid chromatography (LC-MS and LC-MS/MS) is an analytical technique that has rapidly grown in popularity in clinical practice. In contrast to traditional technology, mass spectrometry is superior in many respects including resolution, specificity, multiplex capability and has the ability to measure analytes in various matrices. Despite these advantages, LC-MS/MS remains high cost, labor intensive and has limited throughput. This specialized technology requires highly trained personnel and therefore has largely been limited to large institutions, academic organizations and reference laboratories. Advances in automation will be paramount to break through this bottleneck and increase its appeal for routine use. This article reviews these challenges, shares perspectives on essential features for LC-MS/MS total automation and proposes a step-wise and incremental approach to achieve total automation through reducing human intervention, increasing throughput and eventually integrating the LC-MS/MS system into the automated clinical laboratory operations.

  1. Mass spectrometry imaging for biomedical applications

    PubMed Central

    Liu, Jiangjiang; Ouyang, Zheng

    2013-01-01

    The development of mass spectrometry imaging technologies is of significant current research interest. Mass spectrometry potentially is capable of providing highly specific information about the distribution of chemical compounds on tissues at highly sensitive levels. The required in-situ analysis for the tissue imaging forced MS analysis being performed off the traditional conditions optimized in pharmaceutical applications with intense sample preparation. This critical review seeks to present an overview of the current status of the MS imaging with different sampling ionization methods and to discuss the 3D imaging and quantitative imaging capabilities needed to be further developed, the importance of the multi-modal imaging, and a balance between the pursuit of the high imaging resolution and the practical application of MS imaging in biomedicine. PMID:23539099

  2. Continuous Simultaneous Detection in Mass Spectrometry

    SciTech Connect

    Schilling, G. D.; Andrade, Francisco J.; Barnes IV., James H.; Sperline, Roger P.; Denton, M. Bonner; Barinaga, Charles J.; Koppenaal, David W.; Hieftje, Gary M.

    2007-10-15

    In mass spectrometry, several advantages can be derived when multiple mass-to-charge values are detected simultaneously. One such advantage is an improved duty cycle, which leads to superior limits of detection, better precision, shorter analysis times, and reduced sample sizes. A second advantage is the ability to reduce correlated noise by taking the ratio of two or more simultaneously collected signals, enabling greatly enhanced isotope ratio data. A final advantage is the elimination of spectral skew, leading to more accurate transient signal analysis. Here, these advantages are demonstrated by means of a novel Faraday-strip array detector coupled to a Mattauch-Herzog mass spectrograph. The same system is used to monitor elemental fractionation phenomena in laser ablation inductively coupled plasma mass spectrometry.

  3. Outsourcing CO2 Emissions

    NASA Astrophysics Data System (ADS)

    Davis, S. J.; Caldeira, K. G.

    2009-12-01

    CO2 emissions from the burning of fossil fuels are the primary cause of global warming. Much attention has been focused on the CO2 directly emitted by each country, but relatively little attention has been paid to the amount of emissions associated with consumption of goods and services in each country. This consumption-based emissions inventory differs from the production-based inventory because of imports and exports of goods and services that, either directly or indirectly, involved CO2 emissions. Using the latest available data and reasonable assumptions regarding trans-shipment of embodied carbon through third-party countries, we developed a global consumption-based CO2 emissions inventory and have calculated associated consumption-based energy and carbon intensities. We find that, in 2004, 24% of CO2 emissions are effectively outsourced to other countries, with much of the developed world outsourcing CO2 emissions to emerging markets, principally China. Some wealthy countries, including Switzerland and Sweden, outsource over half of their consumption-based emissions, with many northern Europeans outsourcing more than three tons of emissions per person per year. The United States is both a big importer and exporter of emissions embodied in trade, outsourcing >2.6 tons of CO2 per person and at the same time as >2.0 tons of CO2 per person are outsourced to the United States. These large flows indicate that CO2 emissions embodied in trade must be taken into consideration when considering responsibility for increasing atmospheric greenhouse gas concentrations.

  4. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry.

    PubMed

    Bentlin, Fabrina R S; Pozebon, Dirce; Mello, Paola A; Flores, Erico M M

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO3)2 was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 microg g(-1) of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES).

  5. Time-resolved inductively coupled plasma mass spectrometry measurements with individual, monodisperse drop sample introduction.

    PubMed

    Dziewatkoski, M P; Daniels, L B; Olesik, J W

    1996-04-01

    Individual ion clouds, each produced in the ICP from a single drop of sample, were monitored using time-resolved mass spectrometry and optical emission spectrometry simultaneously. The widths of the ion clouds in the plasma as a function of distance from the point of initial desolvated particle vaporization in the ICP were estimated. The Li(+) cloud width (full width at halfmaximum) varied from 85 to 272 μs at 3 and 10 mm from the apparent vaporization point, respectively. The Sr(+) cloud width varied from 97 to 142 μs at 5 and 10 mm from the apparent vaporization point, respectively. The delays between optical and mass spectrometry signals were used to measure gas velocities in the ICP. The velocity data could then be used to convert ion cloud peak widths in time to cloud sizes in the ICP. Li(+) clouds varied from 2.1 to 6.6 mm (full width at half-maximum) and Sr(+) clouds varied from 2.4 to 3.5 mm at the locations specified above. Diffusion coefficients were estimated from experimental data to be 88, 44, and 24 cm(2)/s for Li(+), Mg(+), and Sr(+), respectively. The flight time of ions from the sampling orifice of the mass spectrometer to the detector were mass dependent and varied from 13 to 21 μs for Mg(+) to 93 to 115 μs for Pb(+).

  6. Translating metabolic exchange with imaging mass spectrometry

    PubMed Central

    Yang, Yu-Liang; Xu, Yuquan; Straight, Paul; Dorrestein, Pieter C.

    2009-01-01

    Metabolic exchange between an organism and the environment, including interactions with neighboring organisms, is important for processes of organismal development. Here we develop and use thin-layer agar natural product MALDI-TOF imaging mass spectrometry of intact bacterial colonies grown on top of the MALDI target plate to study an interaction between two species of bacteria and provide direct evidence that a Bacillus subtilis silences the defensive arsenal of Streptomyces coelicolor. PMID:19915536

  7. Dielectric barrier discharges applied for optical spectrometry

    NASA Astrophysics Data System (ADS)

    Brandt, S.; Schütz, A.; Klute, F. D.; Kratzer, J.; Franzke, J.

    2016-09-01

    The present review reflects the importance of dielectric barrier discharges for optical spectrometric detection in analytical chemistry. In contrast to usual discharges with a direct current the electrodes are separated by at least one dielectric barrier. There are two main features of the dielectric barrier discharges: they can serve as dissociation and excitation devices as well as ionization sources, respectively. This article portrays various application fields of dielectric barrier discharges in analytical chemistry used for elemental and molecular detection with optical spectrometry.

  8. Diamond detector for alpha-particle spectrometry.

    PubMed

    Dueñas, J A; de la Torre Pérez, J; Martín Sánchez, A; Martel, I

    2014-08-01

    An artificially grown high purity diamond was used as a detector for alpha-particle spectrometry. Diamond detectors can match the performance of silicon detectors employed in standard continuous air monitoring systems. Its radiation hardness and electronic properties make them ideal to work under extreme condition such as high temperature and ambient lights. A 50 μm thickness single-crystal diamond detector has been compared with a 300 μm passivated implanted planar silicon detector, under ambient conditions.

  9. Optimization Of A Mass Spectrometry Process

    SciTech Connect

    Lopes, Jose; Alegria, F. Correa; Redondo, Luis; Barradas, N. P.; Alves, E.; Rocha, Jorge

    2011-06-01

    In this paper we present and discuss a system developed in order to optimize the mass spectrometry process of an ion implanter. The system uses a PC to control and display the mass spectrum. The operator interacts with the I/O board, that interfaces with the computer and the ion implanter by a LabVIEW code. Experimental results are shown and the capabilities of the system are discussed.

  10. Mass Spectrometry Imaging under Ambient Conditions

    PubMed Central

    Wu, Chunping; Dill, Allison L.; Eberlin, Livia S.; Cooks, R. Graham; Ifa, Demian R.

    2012-01-01

    Mass spectrometry imaging (MSI) has emerged as an important tool in the last decade and it is beginning to show potential to provide new information in many fields owing to its unique ability to acquire molecularly specific images and to provide multiplexed information, without the need for labeling or staining. In MSI, the chemical identity of molecules present on a surface is investigated as a function of spatial distribution. In addition to now standard methods involving MSI in vacuum, recently developed ambient ionization techniques allow MSI to be performed under atmospheric pressure on untreated samples outside the mass spectrometer. Here we review recent developments and applications of MSI emphasizing the ambient ionization techniques of desorption electrospray ionization (DESI), laser ablation electrospray ionization (LAESI), probe electrospray ionization (PESI), desorption atmospheric pressure photoionization (DAPPI), femtosecond laser desorption ionization (fs-LDI), laser electrospray mass spectrometry (LEMS), infrared laser ablation metastable-induced chemical ionization (IR-LAMICI), liquid microjunction surface sampling probe mass spectrometry (LMJ-SSP MS), nanospray desorption electrospray ionization (nano-DESI), and plasma sources such as the low temperature plasma (LTP) probe and laser ablation coupled to flowing atmospheric-pressure afterglow (LA-FAPA). Included are discussions of some of the features of ambient MSI including the ability to implement chemical reactions with the goal of providing high abundance ions characteristic of specific compounds of interest and the use of tandem mass spectrometry to either map the distribution of targeted molecules with high specificity or to provide additional MS information in the structural identification of compounds. We also describe the role of bioinformatics in acquiring and interpreting the chemical and spatial information obtained through MSI, especially in biological applications for tissue

  11. Dissecting SUMO Dynamics by Mass Spectrometry.

    PubMed

    Drabikowski, Krzysztof; Dadlez, Michał

    2016-01-01

    Protein modification by SUMO proteins is one of the key posttranslational modifications in eukaryotes. Here, we describe a workflow to analyze SUMO dynamics in response to different stimuli, purify SUMO conjugates, and analyze the changes in SUMOylation level in organisms, tissues, or cell culture. We present a protocol for lysis in denaturing conditions that is compatible with downstream IMAC and antibody affinity purification, followed by mass spectrometry and data analysis. PMID:27613044

  12. Monolithic multinozzle emitters for nanoelectrospray mass spectrometry

    DOEpatents

    Wang, Daojing; Yang, Peidong; Kim, Woong; Fan, Rong

    2011-09-20

    Novel and significantly simplified procedures for fabrication of fully integrated nanoelectrospray emitters have been described. For nanofabricated monolithic multinozzle emitters (NM.sup.2 emitters), a bottom up approach using silicon nanowires on a silicon sliver is used. For microfabricated monolithic multinozzle emitters (M.sup.3 emitters), a top down approach using MEMS techniques on silicon wafers is used. The emitters have performance comparable to that of commercially-available silica capillary emitters for nanoelectrospray mass spectrometry.

  13. High resolution alpha particle spectrometry through collimation

    NASA Astrophysics Data System (ADS)

    Park, Seunghoon; Kwak, Sung-Woo; Kang, Han-Byeol

    2015-06-01

    Alpha particle spectrometry with collimation is a useful method for identifying nuclear materials among various nuclides. A mesh type collimator reduces the low energy tail and broadened energy distribution by cutting off particles with a low incidence angle. The relation between the resolution and the counting efficiency can be investigated by changing a ratio of the mesh hole diameter and the collimator thickness. Through collimation, a target particle can be distinguished by a PIPS® detector under a mixture of various nuclides.

  14. Air Emission Inventory for the INEEL -- 1999 Emission Report

    SciTech Connect

    Zohner, Steven K

    2000-05-01

    This report presents the 1999 calendar year update of the Air Emission Inventory for the Idaho National Engineering and Environmental Laboratory (INEEL). The INEEL Air Emission Inventory documents sources and emissions of nonradionuclide pollutants from operations at the INEEL. The report describes the emission inventory process and all of the sources at the INEEL, and provides nonradionuclide emissions estimates for stationary sources.

  15. Application of mass spectrometry for metabolite identification.

    PubMed

    Ma, Shuguang; Chowdhury, Swapan K; Alton, Kevin B

    2006-06-01

    Metabolism studies play a pivotal role in drug discovery and development. Characterization of metabolic "hot-spots" as well as reactive and pharmacologically active metabolites is critical to designing new drug candidates with improved metabolic stability, toxicological profile and efficacy. Metabolite identification in the preclinical species used for safety evaluation is required in order to determine whether human metabolites have been adequately tested during non-clinical safety assessment. From an instrumental standpoint, high performance liquid chromatography (HPLC) coupled with mass spectrometry (MS) dominates all analytical tools used for metabolite identification. The general strategies employed for metabolite identification in both drug discovery and drug development settings together with sample preparation techniques are reviewed herein. These include a discussion of the various ionization methods, mass analyzers, and tandem mass spectrometry (MS/MS) techniques that are used for structural characterization in a modern drug metabolism laboratory. Mass spectrometry-based techniques, such as stable isotope labeling, on-line H/D exchange, accurate mass measurement to enhance metabolite identification and recent improvements in data acquisition and processing for accelerating metabolite identification are also described. Rounding out this review, we offer additional thoughts about the potential of alternative and less frequently used techniques such as LC-NMR/MS, CRIMS and ICPMS. PMID:16787159

  16. DNA sequence analysis by MALDI mass spectrometry.

    PubMed Central

    Kirpekar, F; Nordhoff, E; Larsen, L K; Kristiansen, K; Roepstorff, P; Hillenkamp, F

    1998-01-01

    Conventional DNA sequencing is based on gel electrophoretic separation of the sequencing products. Gel casting and electrophoresis are the time limiting steps, and the gel separation is occasionally imperfect due to aberrant mobility of certain fragments, leading to erroneous sequence determination. Furthermore, illegitimately terminated products frequently cannot be distinguished from correctly terminated ones, a phenomenon that also obscures data interpretation. In the present work the use of MALDI mass spectrometry for sequencing of DNA amplified from clinical samples is implemented. The unambiguous and fast identification of deletions and substitutions in DNA amplified from heterozygous carriers realistically suggest MALDI mass spectrometry as a future alternative to conventional sequencing procedures for high throughput screening for mutations. Unique features of the method are demonstrated by sequencing a DNA fragment that could not be sequenced conventionally because of gel electrophoretic band compression and the presence of multiple non-specific termination products. Taking advantage of the accurate mass information provided by MALDI mass spectrometry, the sequence was deduced, and the nature of the non-specific termination could be determined. The method described here increases the fidelity in DNA sequencing, is fast, compatible with standard DNA sequencing procedures, and amenable to automation. PMID:9592136

  17. Emission properties of explosive field emission cathodes

    SciTech Connect

    Roy, Amitava; Patel, Ankur; Menon, Rakhee; Sharma, Archana; Chakravarthy, D. P.; Patil, D. S.

    2011-10-15

    The research results of the explosive field emission cathode plasma expansion velocity and the initial emission area in the planar diode configuration with cathodes made of graphite, stainless steel, polymer velvet, carbon coated, and carbon fiber (needle type) cathodes are presented. The experiments have been performed at the electron accelerator LIA-200 (200 kV, 100 ns, and 4 kA). The diode voltage has been varied from 28-225 kV, whereas the current density has been varied from 86-928 A/cm{sup 2} with 100 ns pulse duration. The experimentally obtained electron beam diode perveance has been compared with the 1 dimensional Child-Langmuir- law. It was found that initially only a part of the cathode take part in the emission process. The plasma expands at 1.7-5.2 cm/{mu}s for 4 mm anode-cathode gap for various cathode materials. It was found that the plasma expansion velocity increases with the decrease in the cathode diameter. At the beginning of the accelerating pulse, the entire cathode area participates in the electron emission process only for the multiple needle type carbon fiber cathode.

  18. Emission Standards for Particulates

    ERIC Educational Resources Information Center

    Walsh, George W.

    1974-01-01

    Promulgation of standards of performance under Section 111 and national emission standards for hazardous pollutants under Section 112 of the Clean Air Act is the responsibility of the Emission Standards and Engineering Division of the Environmental Protection Agency. The problems encountered and the bases used are examined. (Author/BT)

  19. NARSTO EMISSION INVENTORY ASSESSMENT

    EPA Science Inventory

    The NARSTO Emission Inventory Committee has been pursuing enhancement of the emission inventory program for North American countries--Canada, Mexico, and the United States. With the completion of the NARSTO Ozone and Particulate Matter Assessments, it was recognized that emissio...

  20. Database of emission lines

    NASA Astrophysics Data System (ADS)

    Binette, L.; Ortiz, P.; Joguet, B.; Rola, C.

    1998-11-01

    A widely accessible data bank (available through Netscape) and consiting of all (or most) of the emission lines reported in the litterature is being built. It will comprise objects as diverse as HII regions, PN, AGN, HHO. One of its use will be to define/refine existing diagnostic emission line diagrams.

  1. Microplasma-based atomic emission detectors for gas chromatography.

    PubMed

    Miclea, M; Okruss, M; Kunze, K; Ahlman, N; Franzke, J

    2007-08-01

    This paper is an update on the development of microplasmas as detectors for gas chromatography. Direct current (dc), alternating current (ac), and radio frequency (rf) microplasmas developed in recent years will be described with their significant analytical results, which mostly concern the detection of halogens and sulfur. New results will be added which employ a microhollow cathode discharge (MHCD) as excitation source. Emphasis will be given to this microplasma which has already been implemented as an element-selective detector for emission spectrometry and as ionization source for mass spectrometry. The possibility to use it as a multielement-selective detector for gas chromatography will be presented. A discussion of the published detection limits of all these microplasmas is given.

  2. Observed Barium Emission Rates

    NASA Technical Reports Server (NTRS)

    Stenbaek-Nielsen, H. C.; Wescott, E. M.; Hallinan, T. J.

    1993-01-01

    The barium releases from the CRRES satellite have provided an opportunity for verifying theoretically calculated barium ion and neutral emission rates. Spectra of the five Caribbean releases in the summer of 1991 were taken with a spectrograph on board a U.S. Air Force jet aircraft. Because the line of sight release densities are not known, only relative rates could be obtained. The observed relative rates agree well with the theoretically calculated rates and, together with other observations, confirm the earlier detailed theoretical emission rates. The calculated emission rates can thus with good accuracy be used with photometric observations. It has been postulated that charge exchange between neutral barium and oxygen ions represents a significant source for ionization. If so. it should be associated with emissions at 4957.15 A and 5013.00 A, but these emissions were not detected.

  3. Graphene field emission devices

    SciTech Connect

    Kumar, S. Raghavan, S.; Duesberg, G. S.; Pratap, R.

    2014-09-08

    Graphene field emission devices are fabricated using a scalable process. The field enhancement factors, determined from the Fowler-Nordheim plots, are within few hundreds and match the theoretical predictions. The devices show high emission current density of ∼10 nA μm{sup −1} at modest voltages of tens of volts. The emission is stable with time and repeatable over long term, whereas the noise in the emission current is comparable to that from individual carbon nanotubes emitting under similar conditions. We demonstrate a power law dependence of emission current on pressure which can be utilized for sensing. The excellent characteristics and relative ease of making the devices promise their great potential for sensing and electronic applications.

  4. Interactions between boreal wildfire and urban emissions

    NASA Astrophysics Data System (ADS)

    Bein, Keith J.; Zhao, Yongjing; Johnston, Murray V.; Wexler, Anthony S.

    2008-04-01

    A suite of particulate, gaseous and meteorological measurements during the Pittsburgh Supersite experiment were used to characterize the impact of the 2002 Quebec wildfires on pollutant concentrations and physical and chemical processes dominant in the region. Temporal trends in the number distribution of wildfire particles (isolated using Rapid Single-ultrafine-particle Mass Spectrometry data) combined with CO, NOx and O3 mixing ratios identified two separate periods (Periods I and II) when the measurement site was directly impacted by plumes of relatively unprocessed wildfire emissions; i.e., increases in primary ultrafine wildfire particles, CO and NOx concomitant with a decrease in O3 from intraplume NOx titration. Carbonaceous particle number distributions predominantly associated with vehicular emissions, PM2.5 sulfate mass concentration and SO2 mixing ratio resolved individual components of local and regional sources. Single particle signatures indicated a period of intense atmospheric processing following Period II that caused rapid growth of the ultrafine mode due to simultaneous sulfate and secondary organic mass accumulation, resulting in significant changes to particle physical and chemical properties. Particle growth was concurrent with large increases in O3 and maxima in incoming solar radiation and ambient temperature and is posited to have occurred in situ as the air mass, containing a mixture of urban and wildfire emissions, was advected past the site. In total, the current work demonstrates significant added severity for pollution episodes in an area already burdened by large anthropogenic emission rates due to the impact of the 2002 Quebec wildfires. High levels of atmospheric processing increased sulfate accumulation and SOA formation and brought PM2.5 mass concentrations close to, and O3 mixing ratios in excess of, the National Ambient Air Quality Standards. Projections of increasing wildfire activity under a warming climate may increase the

  5. Characterizing exposures to airborne metals and nanoparticle emissions in a refinery.

    PubMed

    Miller, Arthur; Drake, Pamela L; Hintz, Patrick; Habjan, Matt

    2010-07-01

    An air quality survey was conducted at a precious metals refinery in order to evaluate worker exposures to airborne metals and to provide detailed characterization of the aerosols. Two areas within the refinery were characterized: a furnace room and an electro-refining area. In line with standard survey practices, both personal and area air filter samples were collected on 37-mm filters and analyzed for metals by inductively coupled plasma-atomic emission spectroscopy. In addition to the standard sampling, measurements were conducted using other tools, designed to provide enhanced characterization of the workplace aerosols. The number concentration and number-weighted particle size distribution of airborne particles were measured with a fast mobility particle sizer (FMPS). Custom-designed software was used to correlate particle concentration data with spatial location data to generate contour maps of particle number concentrations in the work areas. Short-term samples were collected in areas of localized high concentrations and analyzed using transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) to determine particle morphology and elemental chemistry. Analysis of filter samples indicated that all of the workers were exposed to levels of silver above the Occupational Safety and Health Administration permissible exposure limit of 0.01 mg m(-3) even though the localized ventilation was functioning. Measurements with the FMPS indicated that particle number concentrations near the furnace increased up to 1000-fold above the baseline during the pouring of molten metal. Spatial mapping revealed localized elevated particle concentrations near the furnaces and plumes of particles rising into the stairwells and traveling to the upper work areas. Results of TEM/EDS analyses confirmed the high number of nanoparticles measured by the FMPS and indicated the aerosols were rich in metals including silver, lead, antimony, selenium, and zinc. Results of

  6. India Co2 Emissions

    NASA Astrophysics Data System (ADS)

    Sharan, S.; Diffenbaugh, N. S.

    2010-12-01

    Is there a way to find a balance between improving living conditions for the people on the margins and also reducing emissions while limiting our negative impacts on the climate? This is a critical question today because there are many arguments between developed and developing countries about who is responsible for global warming. Developed countries believe that it is the poor countries because they are not educated enough to know about how they are affecting the climate. While the developing countries hold wealthy nations responsible because they are using the most resources. However it is important to acknowledge the fact that if there was no gap in between the developed and developing countries our emissions total would be much higher. This “gap” has been a natural controlling factor in climate change. This is why I wanted to see if I could plot what it would look like if a developing country such as India were to produce emissions that the US or Switzerland or Norway are producing as developed countries. India has a population total of 1.1 billion compared to the US with only 298 million, Switzerland with 7.5 million, and Norway with 4.6 million people. When the population is compared to the emissions output in metric tons, per capita, India produced the least emissions out of these countries, 1.4 tons per person while having the second largest population in the world, while the US produced 19 tons per capita, Switzerland produced 5.6 and Norway produced 8.7 tons per capita in 2006. The emissions rate is growing every year and increases widely and globally. If India was producing emissions that equal Norway, Switzerland and the US the total emissions it would be producing annually would be 9 billion for Norway, 6 billion for Switzerland and 20 billion emissions for the US, all in the year 2006 alone. This shows how the balance between countries with huge populations and very little emission output and average population and high emission out put has

  7. The role of ion mobility spectrometry-mass spectrometry in the analysis of protein reference standards.

    PubMed

    Pritchard, Caroline; O'Connor, Gavin; Ashcroft, Alison E

    2013-08-01

    To achieve comparability of measurement results of protein amount of substance content between clinical laboratories, suitable reference materials are required. The impact on measurement comparability of potential differences in the tertiary and quaternary structure of protein reference standards is as yet not well understood. With the use of human growth hormone as a model protein, the potential of ion mobility spectrometry-mass spectrometry as a tool to assess differences in the structure of protein reference materials and their interactions with antibodies has been investigated here.

  8. Applications of new mass spectrometry techniques in pesticide chemistry

    SciTech Connect

    Rosen, J.

    1987-01-01

    The partial contents are: New Instruments, New Methods and the Search for Selectivity. Chemical Ionization Mass Spectrometry in Pesticide Metabolite Indentification. Negative Ion Electron Capture Chemical Ionization Mass Spectrometry of Fluorinated Pesticide Derivatives. Negative Ion Chemical Ionization Mass Spectrometry of Toxaphene. Methane-enhanced Negative Ion Mass Spectra of Hexachlorocyclopentadiene Derivatives. Isomer Specific Analysis of Dioxins and Dibenzofurnas by HRGC/SIM-MS. Determination of Double-bond Position in Conjugated Dienes by Chemical Ionization Mass Spectrometry with Isobutane. Application of Desorption Chemical Ionization Techniques for Analysis of Biologically Active Compounds Isolated from Insects. FD and FAB Mass Spectrometry of Sulfate Conjugants and of Conjugated Metabolites of Pyroquilon. Application of Fast Atom Bombardment Mass Spectrometry to Polar Pesticides. Thermospray HPLC/MS as a Problem-solving Tool for the Analysis of Thermally Labile Herbicides.

  9. Combustion and emissions technology

    NASA Technical Reports Server (NTRS)

    Grobman, J.; Anderson, D. N.; Diehl, L. A.; Niedzwiecki, R. W.

    1975-01-01

    Combustor development is discussed as it relates to emissions reduction. The nature of the aircraft pollution problem is examined along with the aircraft pollution standards that have been established by the Environmental Protection Agency. The effect of engine operating conditions on pollutant formation levels is shown, as well as how close present-day engines are to meeting the established standards. The magnitude of the emissions reductions required to meet these standards is indicated. The progress that has been made in evolving the needed emissions reduction technology is the main topic.

  10. Emission Abatement System

    DOEpatents

    Bromberg, Leslie; Cohn, Daniel R.; Rabinovich, Alexander

    2003-05-13

    Emission abatement system. The system includes a source of emissions and a catalyst for receiving the emissions. Suitable catalysts are absorber catalysts and selective catalytic reduction catalysts. A plasma fuel converter generates a reducing gas from a fuel source and is connected to deliver the reducing gas into contact with the absorber catalyst for regenerating the catalyst. A preferred reducing gas is a hydrogen rich gas and a preferred plasma fuel converter is a plasmatron. It is also preferred that the absorber catalyst be adapted for absorbing NO.sub.x.

  11. Emissivity of microstructured silicon.

    PubMed

    Maloney, Patrick G; Smith, Peter; King, Vernon; Billman, Curtis; Winkler, Mark; Mazur, Eric

    2010-03-01

    Infrared transmittance and hemispherical-directional reflectance data from 2.5 to 25 microm on microstructured silicon surfaces have been measured, and spectral emissivity has been calculated for this wavelength range. Hemispherical-total emissivity is calculated for the samples and found to be 0.84 before a measurement-induced annealing and 0.65 after the measurement for the sulfur-doped sample. Secondary samples lack a measurement-induced anneal, and reasons for this discrepancy are presented. Emissivity numbers are plotted and compared with a silicon substrate, and Aeroglaze Z306 black paint. Use of microstructured silicon as a blackbody or microbolometer surface is modeled and presented, respectively.

  12. MOVES2014: Evaporative Emissions Report

    EPA Science Inventory

    Vehicle evaporative emissions are now modeled in EPA’s MOVES according to physical processes, permeation, tank vapor venting, liquid leaks, and refueling emissions. With this update, the following improvements are being incorporated into MOVES evaporative emissions methodology, a...

  13. Determination of trace elements in lithium niobate crystals by solid sampling and solution-based spectrometry methods.

    PubMed

    Bencs, László; György, Krisztina; Kardos, Márta; Osán, János; Alföldy, Bálint; Varga, Imre; Ajtony, Zsolt; Szoboszlai, Norbert; Stefánka, Zsolt; Széles, Eva; Kovács, László

    2012-05-13

    Solid sampling (SS) graphite furnace atomic absorption spectrometry (GFAAS) and solution-based (SB) methods of GFAAS, flame atomic absorption spectrometry (FAAS), inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) were elaborated and/or optimized for the determination of Cr, Fe and Mn trace elements used as dopants in lithium niobate optical crystals. The calibration of the SS-GFAAS analysis was possible with the application of the three-point-estimation standard addition method, while the SB methods were mostly calibrated against matrix-matched and/or acidic standards. Spectral and non-spectral interferences were studied in SB-GFAAS after digestion of the samples. The SS-GFAAS method required the use of less sensitive spectral lines of the analytes and a higher internal furnace gas (Ar) flow rate to decrease the sensitivity for crystal samples of higher (doped) analyte content. The chemical forms of the matrix produced at various stages of the graphite furnace heating cycle, dispensed either as a solid sample or a solution (after digestion), were studied by means of the X-ray near-edge absorption structure (XANES). These results revealed that the solid matrix vaporized/deposited in the graphite furnace is mostly present in the metallic form, while the dry residue from the solution form mostly vaporized/deposited as the oxide of niobium. PMID:22541007

  14. Gaseous Emissions from Wastewater Facilities.

    PubMed

    Koh, Sock-Hoon; Shaw, Andrew R

    2016-10-01

    A review of the literature published in 2015 on topics relating to gaseous emissions from wastewater facilities is presented. This review is divided into the following sections: odorant emissions from wastewater treatment plants (WWTPs); greenhouse gas (GHG) emissions from WWTPs; gaseous emissions from wastewater collection systems; physiochemical odor/emissions control methods; biological odor/emissions control methods; odor characterization/monitoring; and odor impacts/ risk assessments. PMID:27620089

  15. Crux: rapid open source protein tandem mass spectrometry analysis.

    PubMed

    McIlwain, Sean; Tamura, Kaipo; Kertesz-Farkas, Attila; Grant, Charles E; Diament, Benjamin; Frewen, Barbara; Howbert, J Jeffry; Hoopmann, Michael R; Käll, Lukas; Eng, Jimmy K; MacCoss, Michael J; Noble, William Stafford

    2014-10-01

    Efficiently and accurately analyzing big protein tandem mass spectrometry data sets requires robust software that incorporates state-of-the-art computational, machine learning, and statistical methods. The Crux mass spectrometry analysis software toolkit ( http://cruxtoolkit.sourceforge.net ) is an open source project that aims to provide users with a cross-platform suite of analysis tools for interpreting protein mass spectrometry data. PMID:25182276

  16. Nuclear applications of inorganic mass spectrometry.

    PubMed

    De Laeter, John

    2010-01-01

    There are several basic characteristics of mass spectrometry that are not always fully appreciated by the science community. These characteristics include the distinction between relative and absolute isotope abundances, and the influence of isotope fractionation on the accuracy of isotopic measurements. These characteristics can be illustrated in the field of nuclear physics with reference to the measurement of nuclear parameters, which involve the use of enriched isotopes, and to test models of s-, r-, and p-process nucleosynthesis. The power of isotope-dilution mass spectrometry (IDMS) to measure trace elements in primitive meteorites to produce accurate Solar System abundances has been essential to the development of nuclear astrophysics. The variety of mass spectrometric instrumentation used to measure the isotopic composition of elements has sometimes been accompanied by a lack of implementation of basic mass spectrometric protocols which are applicable to all instruments. These metrological protocols are especially important in atomic weight determinations, but must also be carefully observed in cases where the anomalies might be very small, such as in studies of the daughter products of extinct radionuclides to decipher events in the early history of the Solar System. There are occasions in which misleading conclusions have been drawn from isotopic data derived from mass spectrometers where such protocols have been ignored. It is important to choose the mass spectrometer instrument most appropriate to the proposed experiment. The importance of the integrative nature of mass spectrometric measurements has been demonstrated by experiments in which long, double beta decay and geochronological decay half-lives have been measured as an alternative to costly radioactive-counting experiments. This characteristic is also illustrated in the measurement of spontaneous fission yields, which have accumulated over long periods of time. Mass spectrometry is also a

  17. Emissions of hydrogen cyanide from on-road gasoline and diesel vehicles

    NASA Astrophysics Data System (ADS)

    Moussa, Samar G.; Leithead, Amy; Li, Shao-Meng; Chan, Tak W.; Wentzell, Jeremy J. B.; Stroud, Craig; Zhang, Junhua; Lee, Patrick; Lu, Gang; Brook, Jeffery R.; Hayden, Katherine; Narayan, Julie; Liggio, John

    2016-04-01

    Hydrogen cyanide (HCN) is considered a marker for biomass burning emissions and is a component of vehicle exhaust. Despite its potential health impacts, vehicular HCN emissions estimates and their contribution to regional budgets are highly uncertain. In the current study, Proton Transfer Reaction-Time of Flight-Mass Spectrometry (PTR-ToF-MS) was used to measure HCN emission factors from the exhaust of individual diesel, biodiesel and gasoline vehicles. Laboratory emissions data as a function of fuel type and driving mode were combined with ambient measurement data and model predictions. The results indicate that gasoline vehicles have the highest emissions of HCN (relative to diesel fuel) and that biodiesel fuel has the potential to significantly reduce HCN emissions even at realistic 5% blend levels. The data further demonstrate that gasoline direct injection (GDI) engines emit more HCN than their port fuel injection (PFI) counterparts, suggesting that the expected full transition of vehicle fleets to GDI will increase HCN emissions. Ambient measurements of HCN in a traffic dominated area of Toronto, Canada were strongly correlated to vehicle emission markers and consistent with regional air quality model predictions of ambient air HCN, indicating that vehicle emissions of HCN are the dominant source of exposure in urban areas. The results further indicate that additional work is required to quantify HCN emissions from the modern vehicle fleet, particularly in light of continuously changing engine, fuel and after-treatment technologies.

  18. Laser Microprobe Mass Spectrometry 1: Basic Principles and Performance Characteristics.

    ERIC Educational Resources Information Center

    Denoyer, Eric; And Others

    1982-01-01

    Describes the historical development, performance characteristics (sample requirements, analysis time, ionization characteristics, speciation capabilities, and figures of merit), and applications of laser microprobe mass spectrometry. (JN)

  19. Fugitive emissions monitoring trends

    SciTech Connect

    Brown, K.H.

    1997-02-01

    New Clean Air Act requirements are pushing facilities to reevaluate their monitoring programs. A description of the fugitive emission guidelines is included in this article, along with ideas about monitoring.

  20. Photon enhanced thermionic emission

    SciTech Connect

    Schwede, Jared; Melosh, Nicholas; Shen, Zhixun

    2014-10-07

    Photon Enhanced Thermionic Emission (PETE) is exploited to provide improved efficiency for radiant energy conversion. A hot (greater than 200.degree. C.) semiconductor cathode is illuminated such that it emits electrons. Because the cathode is hot, significantly more electrons are emitted than would be emitted from a room temperature (or colder) cathode under the same illumination conditions. As a result of this increased electron emission, the energy conversion efficiency can be significantly increased relative to a conventional photovoltaic device. In PETE, the cathode electrons can be (and typically are) thermalized with respect to the cathode. As a result, PETE does not rely on emission of non-thermalized electrons, and is significantly easier to implement than hot-carrier emission approaches.