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Sample records for plasma-atomic emission spectrometry

  1. [Determination of total sulfur in coal by inductively coupled plasma atomic emission spectrometry].

    Science.gov (United States)

    Liu, Dong-yan; Zhang, Yuan-li

    2002-02-01

    A direct method was reported for the determination of total sulfur in coal by inductively coupled plasma atomic emission spectrometry (ICP-AES). The dissolution conditions of coal samples as well as interference conditions of hydrochloric acid and matrix were studied. The recommended method not only proved to be simple and rapid than traditional gravimetric method but show satisfying precision and accuracy as well. The results of samples are as same as gravimetry. The recoveries are more than 96%, and the relative standard deviation of six samples are less than 3%.

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

    Science.gov (United States)

    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.

  3. Analysis of tungsten carbide coatings by UV laser ablation inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Kanicky, V.; Otruba, V.; Mermet, J.-M.

    2000-06-01

    Tungsten carbide coatings (thickness 0.1-0.2 mm) containing 8.0, 12.2, 17.2 and 22.9% Co were studied with laser ablation inductively coupled plasma atomic emission spectrometry (LA-ICP-AES). Composition of these plasma sprayed deposits on steel disks was determined using X-ray fluorescence spectrometry and electron microprobe energy/wavelength dispersive X-ray spectrometry. The coatings were ablated by means of a Q-switched Nd:YAG laser at 266 nm (10 Hz, 10 mJ per shot) coupled to an ICP echelle-based spectrometer equipped with a segmented charge-coupled device detector. Non-linear dependences of cobalt lines intensities on the Co percentage were observed both at a single spot ablation and at a sample translation. This behaviour could be attributed to a complex phase composition of the system W-C-Co. However, employing tungsten as internal standard the linear calibration was obtained for studied analytical lines Co II 228.616 nm, Co II 230.786 nm, Co II 236.379 nm and Co II 238.892 nm.

  4. [Determination of chlorine in gasoline by inductively coupled plasma atomic emission spectrometry].

    Science.gov (United States)

    Zhao, Yan; Chen, Xiao-yan; Xu, Dong-yu; Zhang, Shi-yuan; Chen, Ze-yong

    2014-12-01

    A new method was studied for the analysis of chlorine in gasoline by inductively coupled plasma atomic emission spectrometry (ICP-AES). Samples werediluted 1+4(φ) with kerosene. The intense spectral line for chlorine (134.724 nm) was used. In order to eliminate carbon and maintain stable plasma, small amounts of oxygen (0.050 L · min(-1)) were added to the auxiliary gas. The instrumental main condition was optimized in terms of effects of generator power, nebulizer gas flow, auxiliary gas flow, and oxygen flow on SBR for chlorine. Standard addition method was used to compensate matrix effect and signal drift. The recovery for spiking gasoline samples and the limit of detection were in the range of 96.6%~103.9% and 0.27 mg · L(-1) respectively. The relative standard deviation (RSD) was between 1.57% and 4.49%. Compared with microcoulometry, the analysis results of organic chlorine were basically the same. Moreover, chlorine content, including organic chlorine and inorganic chloride was determined by ICP-AES. The proposed method had the advantages of simplicity, speediness and sensitivity, and expanded the ICP-AES application in non-metals especially halogen elements. It can be used for the analysis of chlorine in gasoline and provides technical support for quality evaluation.

  5. Determination of additives in PVC material by UV laser ablation inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Hemmerlin, M.; Mermet, J. M.; Bertucci, M.; Zydowicz, P.

    1997-04-01

    UV laser ablation inductively coupled plasma atomic emission spectrometry (LA-ICP-AES) has been applied to the direct determination of additives in solid poly(vinyl chloride) materials. A Nd:YAG laser, operating at its fourth harmonic (266 nm), was used with a beam masking device, in the most reproducible conditions, to introduce solid particles into the plasma torch of a simultaneous ICP-AES system. Emphasis was placed on both precision and accuracy in the analysis of PVC materials by LA-ICP-AES. A series of six in-house PVC reference materials was prepared by incorporating several additives in increasing concentrations. Three alternative methods were evaluated to certify the amount of incorporated elements: ICP-AES with sample dissolution, NAA and XRF. Satisfactory results and good agreement were obtained for seven elements (Al, Ca, Cd, Mg, Sb, Sn and Ti) among the ten incorporated. Sample homogeneity appeared to be satisfactory, and calibration graphs obtained by LA-ICP-AES for several elements are presented. Finally, the performance of the technique in terms of repeatability (1.6-5%), reproducibility (2-5%), and limits of detection was investigated.

  6. Determination of myo-inositol hexakisphosphate (phytate) in urine by inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grases, F.; Perello, J.; Isern, B.; Prieto, R.M

    2004-05-10

    Myo-inositol hexakisphosphate (phytate) is a substance present in urine with an important role in preventing calcium renal calculi development. In spite of this, the use of urinary phytate levels on stone-formers' evaluation and treatment is still notably restricted as a consequence of the enormous difficulty to analyze this substance in urine. In this paper, a simple procedure for routinary urinary phytate determination based on phosphorus determination through inductively coupled plasma atomic emission spectrometry is described. The method only requires a previous separation of phytate from other components by column anion exchange chromatography. The working linear range used was 0-2 mg l{sup -1} phosphorus (0-7 mg l{sup -1} phytate). The limit of detection was 64 {mu}g l{sup -1} of phytate and the limit of quantification was 213 {mu}g l{sup -1}. The relative standard deviation (R.S.D.) for 1.35 mg l{sup -1} phytate was 2.4%. Different urine samples were analyzed using an alternative analytical methodology based on gas chromatography (GC)/mass detection used for inositol determination (phytate was previously hydrolyzed), resulting both methods comparable using as criterion to assess statistical significance P<0.05.

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

    Science.gov (United States)

    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.

  8. Inductively coupled plasma--atomic emission spectrometry: trace elements in oil matrices

    Energy Technology Data Exchange (ETDEWEB)

    Peterson, C. A.

    1977-12-01

    The simultaneous determination of up to 20 trace elements in various oil matrices by inductively coupled plasma-atomic emission spectrometry is reported. The oil matrices investigated were lubricating oils (for wear metals), fuel oil, centrifuged coal liquefaction product, crude soybean oil, and commercial edible oils. The samples were diluted with appropriate organic solvents and injected into the plasma as an aerosol generated by a pneumatic nebulization technique. Detection limits of the 28 elements studied ranged from 0.0006 to 9 ..mu..g/g with the majority falling in the 0.01 to 0.1 ..mu..g/g range. Analytical calibration curves were linear over at least two orders of magnitude and for some elements this linearity extended over 4.5 orders of magnitude. Relevant data on precision and accuracy are included. Because metals often occur as particles in lubricating oil and coal liquefaction products, the effect of particles on the analytical results was examined. Wear metal particles in used oil did not appear to affect the analytical results. However, incomplete recovery relative to organometallic reference solutions was obtained for iron particles with a nominal mean diameter of 3.0 ..mu..m suspended in oil. It was shown that the following factors contributed to incomplete recovery for the particles: settling of the suspended particles in the flask, a difference in nebulization efficiency between particle suspensions and organometallic solutions, and indications of incomplete vaporization of the larger particles in the plasma.

  9. Elemental analysis using instrumental neutron activation analysis and inductively coupled plasma atomic emission spectrometry: a comparative study

    Energy Technology Data Exchange (ETDEWEB)

    Chung, Yong Sam; Choi, Kwang Soon; Moon, Jong Hwa; Kim, Sun Ha; Lim, Jong Myoung; Kim, Young Jin [KAERI, Taejon (Korea, Republic of); Quraishi, Shamshad Begum [Bangladesh Atomic Energy Commission, Dhaka (Bangladesh)

    2003-05-01

    Elemental analyses for certified reference materials were carried out using instrumental neutron activation analysis and inductively coupled plasma-atomic emission spectrometry. Five Certified Reference Materials (CRM) were selected for the study on comparative analysis of environmental samples. The CRM are Soil (NIST SRM 2709), Coal fly ash (NIST SRM 1633a), urban dust (NIST SRM 1649a) and air particulate on filter media (NIST SRM 2783 and human hair (GBW 09101)

  10. Gunshot residue testing in suicides: Part II: Analysis by inductive coupled plasma-atomic emission spectrometry.

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  12. Determination of trace elements in refined gold samples by inductively coupled plasma atomic emission spectrometry

    Directory of Open Access Journals (Sweden)

    Steharnik Mirjana

    2013-01-01

    Full Text Available This paper presents a method for determination the trace contents of silver, copper, iron, palladium, zinc and platinum in refined gold samples. Simultaneous inductively coupled plasma atomic emission spectrometer with radial torch position and cross flow nebulizer was used for determination. In order to compare the different calibration strategies, two sets of calibration standards were prepared. The first set was based on matrix matched calibration standards and the second was prepared without the addition of matrix material. Detection limits for matrix matching calibrations were higher for some elements than those without matrix matching. In addition, the internal standardization method was applied and experiments indicated that indium was the best option as internal standard. The obtained results for gold sample by matrix matching and matrix free calibrations were compared with the obtained results by standard addition method. The accuracy of the methods was tested performing recovery test. Recoveries for spiked sample were in the range of 90-115 %. The accuracy of the methods was also tested by analysis of certified reference material of high pure goldAuGHP1. The best results were achieved by matrix free calibration and standard addition method using indium as internal standard at wavelength of 230 nm. [Projekat Ministarstva nauke Republike Srbije, br. 34024: Development of Technologies for Recycling of Precious, Rare and Associated Metals from Solid Waste in Serbia to High Purity Products

  13. Evaluation of arsenic and selenium in Brazilian soluble coffee by inductively coupled plasma atomic emission spectrometry with hydride generation

    Directory of Open Access Journals (Sweden)

    Santos Éder José dos

    2001-01-01

    Full Text Available A method for the evaluation of arsenic and selenium in soluble coffee by inductively coupled plasma atomic emission spectrometry with continuous hydride generation to attend the Brazilian food legislation is described. Samples were digested with nitric acid and hydrogen peroxide in a focused microwave system. Slow heating eliminated nitric acid and selenium (VI was reduced to selenium (IV by addition of 6 mol/L hydrochloric acid and heating at 90° C under a reflux system. The influence of sample acidity on sensitivity was investigated. Hydrochloric acid 6 mol/L was the most suitable reaction medium. Practical detection limits of 2.0mug/L for As and 1.0mu g/L for Se were achieved and attended the Brazilian food legislation. The results of recoveries on spiked samples demonstrate the reliability and accuracy of the procedure.

  14. Determination of Uranium in Apatite Minerals by Solvent Extraction--Inductively Coupled Plasma Atomic Emission Spectrometry

    OpenAIRE

    1993-01-01

    [Abstract] Solvent, extraction-ICP atomic emission spectrometry was applied to the determination of uranium in apatite minerals. Apatite minerals were treated with nitric acid. After removing a small quantity of insoluble residue, uranium was extracted with 0.05 mol/dm^3 1-phonyl-3-mcthyl-4-trifluoroacetyl-5-pyrazolonc-diisobutyl kctone at pH 0.8. The uranium content in the apatite was found to be (20.3〜132.9)×10^%.

  15. Analysis of tree leaves, bark and wood by sequential inductively coupled argon plasma atomic emission spectrometry

    Science.gov (United States)

    Verbeek, A. A.

    The analysis of extracts from tree leaf, bark and wood samples for Ca, Mg, K, Na, P, Mn, Fe, Al, B, Cu and Zn by inductively coupled argon plasma sequential emission spectrometry is described. Recovery percentages for simulated tree extracts and for spiked tree samples are presented together with typical analysis values for a leaf and a wood sample. The choice of analytical line for each element is discussed and spectral interferences, not listed in the ICP tables of Boumans, of Cu on the 214.9 nm line of P and of Fe on the 249.7 nm line of B are noted.

  16. Analysis of tungsten carbide coatings by infrared laser-induced argon spark with inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Kanický, V.; Otruba, V.; Mermet, J.-M.

    2000-10-01

    Infrared laser ablation was studied for application to the analysis of plasma-sprayed tungsten carbide/cobalt coatings. The potential of the laser induced argon-spark (LINA-Spark™), as a sample introduction device in inductively coupled plasma atomic emission spectrometry was studied. The use of an IR laser along with defocusing led to laser-induced microplasma-based ablation. The mass ablation rate, represented by the ICP emission intensity per laser beam unit area, exhibited a flat increase in the irradiance range 2-250 GW/cm 2. A low slope (0.5) of this dependence in log-log scale gave evidence of plasma shielding. The steep increase in the measured acoustic signal when focused in front of the sample, i.e. in argon, indicated a breakdown of argon. Consequently, considerably lower ICP emissions were observed within the same range of irradiance. The cobalt/tungsten line intensity ratio in the ICP was practically constant from 1.5 up to at least 250 GW/cm 2. Acceptable precision (R.S.D.<5%) was obtained without internal standardization for irradiance between 2 and 8 GW/cm 2. Optimization of the laser pulse energy, repetition rate, beam focusing and sample displacement during interaction led to the linearization of dependences of signal vs. cobalt percentage, at least up to the highest studied value of 23% Co.

  17. Determination of micro yttrium in an ytterbium matrix by inductively coupled plasma atomic emission spectrometry and wavelet transform

    Institute of Scientific and Technical Information of China (English)

    MA Xiaoguo

    2005-01-01

    In the determination of trace yttrium (Y) in an ytterbium (Yb) matrix by inductively coupled plasma atomic emission spectrometry (ICP-AES), the most prominent line of yttrium, Y 371.030 nm line, suffers from strong interference due to an emission line of ytterbium. In this work, a method based on wavelet transform was proposed for the spectral interference correction. Haar wavelet was selected as the mother wavelet. The discrete detail after the third decomposition, D3,was chosen for quantitative analysis based on the consideration of both separation degree and peak height. The linear correlation coefficient between the height of the left positive peak in D3 and the concentration of Y was calculated to be 0.9926.Six synthetic samples were analyzed, and the recovery for yttrium varied from 96.3% to 110.0%. The amounts of yttrium in three ytterbium metal samples were determined by the proposed approach with an average relative standard deviation (RSD)of 2.5%, and the detection limit for yttrium was 0.016%. This novel correction technique is fast and convenient, since neither complicated model assumption nor time-consuming iteration is required. Furthermore, it is not affected by the wavelength drift inherent in monochromators that will severely reduce the accuracy of results obtained by some chemometric methods.

  18. Evaluation of vapor generation for the determination of nickel by inductively coupled plasma-atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Marrero, Julieta [Comision Nacional de Energia Atomica, Unidad de Actividad Quimica, Centro Atomico Constituyentes, Av. Gral. Paz 1499, 1650-San Martin, Pcia. de Buenos Aires (Argentina); Smichowski, Patricia [Comision Nacional de Energia Atomica, Unidad Proyectos Especiales de Suministros Nucleares, Av. Libertador 8250, 1429-Buenos Aires (Argentina)

    2002-09-01

    Volatile species of Ni were generated by merging acidified aqueous samples and sodium tetrahydroborate(III) in a continuous flow system. The gaseous analyte was subsequently introduced via a stream of Ar carrier into the inlet tube of the plasma torch. Inductively coupled plasma atomic emission spectrometry (ICP-AES) was used for detection. The operating conditions (chemical and physical parameters) and the concentrations of different acids were evaluated for the efficient generation of Ni vapor. The detection limit (3 {sigma}{sub blank}) was 1.8 ng mL{sup -1}. The precision (RSD) of the determination was 4.2% at a level of 500 ng mL{sup -1} and 7.3% for 20 ng mL{sup -1} (n=10). The efficiency of the generation process was estimated to be 51%. The possible interfering effect of transition metals (Cd, Co, Cu, Cr, Fe, Mn, Zn), hydride forming elements (As, Ge, Pb, Sb, Se, Sn, Te), and Hg on Ni signal was examined. This study has demonstrated that Ni vapor generation is markedly free of interferences. (orig.)

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

    Science.gov (United States)

    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.

  20. Volatile organo-selenium speciation in biological matter by solid phase microextraction–moderate temperature multicapillary gas chromatography with microwave induced plasma atomic emission spectrometry detection

    OpenAIRE

    Dietz, Christian; Sanz Landaluze, Jon; Ximenez Embun, Pilar; Madrid Albarrán, Yolanda; Cámara, Carmen

    2004-01-01

    Microwave induced plasma atomic emission spectrometry (MIP-AES) in combination with multicapillary (MC) gas chromatography could be proven to be useful for element specific detection of volatile species. Solid phase microextraction (SPME) was used for preconcentration and sample-matrix separation. The fiber desorption unit as well as the heating control for the MCcolumn were in-house developed and multicapillary column was operated at moderate temperatures (30–100 ◦C). The method was...

  1. Determination of {sup 233}U by inductively coupled argon plasma - atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Patwardhan, A.B.; Kulkarni, V.T.; Radhakrishnan, K.; Ramanujam, A.; Page, A.G. [Bhabha Atomic Research Centre, Bombay (India)

    1994-09-01

    The paper describes studies carried out for the determination of {sup 233}U at various stages during the recovery and purification of {sup 233}U from {sup 233}U-Al alloy scraps generated during the fabrication of {sup 233}U-Al alloy fuel. Employing a high resolution sequential spectrometer and Inductively Coupled argon Plasma (ICP) as the spectral excitation source, isotope shift for {sup 233}U with respect to {sup 238}U has been resolved and recorded. The shift for the 424.437 nm emission line of {sup 238}U is found to be of the order of 0.040 nm on the lower wavelength side for {sup 233}U and this isotopic effect has been utilised for the quantitative determination of {sup 233}U. The overall precision of the method is 5% RSD with the detection limit of 0.01 {mu}g/ml.

  2. Determination of nickel in biological materials after microwave dissolution using inductively coupled plasma atomic emission spectrometry with prior extraction into butan-1-ol.

    Science.gov (United States)

    Vereda Alonso, E; García de Torres, A; Cano Pavón, J M

    1992-07-01

    A sensitive procedure has been developed for the determination of ultratrace amounts of nickel in biological materials by inductively coupled plasma atomic emission spectrometry after extraction of the nickel ion into butan-1-ol by using 1,5-bis(di-2-pyridylmethylene)thiocarbonohydrazide as the extracting reagent. Fast, efficient and complete sample digestion is achieved by an HNO3-HCl poly(tetrafluoroethylene) bomb dissolution technique using microwave heating. Results obtained for eleven certified reference materials agreed with the certified values.

  3. Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis

    Energy Technology Data Exchange (ETDEWEB)

    Papadopoulou, D.N. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Zachariadis, G.A. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Anthemidis, A.N. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Tsirliganis, N.C. [Archaeometry Laboratory, Cultural and Educational Technology Institute, Tsimiski 58, GR-67100, Xanthi (Greece); Stratis, J.A. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece)]. E-mail: jstratis@chem.auth.gr

    2004-12-01

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

  4. Standard practice for analysis of aqueous leachates from nuclear waste materials using inductively coupled plasma-atomic emission spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 This practice is applicable to the determination of low concentration and trace elements in aqueous leachate solutions produced by the leaching of nuclear waste materials, using inductively coupled plasma-atomic emission spectroscopy (ICP-AES). 1.2 The nuclear waste material may be a simulated (non-radioactive) solid waste form or an actual solid radioactive waste material. 1.3 The leachate may be deionized water or any natural or simulated leachate solution containing less than 1 % total dissolved solids. 1.4 This practice should be used by analysts experienced in the use of ICP-AES, the interpretation of spectral and non-spectral interferences, and procedures for their correction. 1.5 No detailed operating instructions are provided because of differences among various makes and models of suitable ICP-AES instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This test method does not address comparative accuracy of different devices...

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  7. 电感耦合等离子体-原子发射光谱法的应用%Application of Inductively Coupled Plasma-Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    时亮; 隋欣

    2013-01-01

    The application of inductively coupled plasma-atomic emission spectrometry in animal and plant analysis, environmental analysis, metallurgical analysis, electric power production, food analysis, lithium niobate analysis, harmful heavy metals detection in toys, and the cultural relics protection, etc, were summarized.%  综述了利用电感耦合高频等离子体作为激发光源的原子发射光谱法在动植物分析、环境分析、冶金分析、电力生产、食品分析、铌酸锂分析、玩具中有害重金属测定及文物保护科学研究等方面中的应用。

  8. Calibration graphs for Ti, Ta and Nb in sintered tungsten carbide by infrared laser ablation inductively coupled plasma atomic emission spectrometry.

    Science.gov (United States)

    Kanický, V; Otruba, V; Mermet, J M

    2001-12-01

    Infrared laser ablation (IR-LA) has been studied as a sample introduction technique for the analysis of sintered cobalt-cemented tungsten carbide materials by inductively coupled plasma atomic emission spectrometry (ICP-AES). Fractionation of cobalt was observed. Linearity of calibration plots was verified at least up to 15% Ti, 8% Ta, and 3% Nb. Above 1% (m/m) Ti, Ta, and Nb, the repeatability of results was better than 3% R.S.D. The relative uncertainty at the centroid of the calibration line was in the range from +/- 3% to +/- 4% for Ti, Ta, and Nb with internal standardization by tungsten and up to +/- 5% without internal standardization. The limits of detection were 0.004% Ti, 0.001% Ta, and 0.004% Nb. Elimination of the cemented hardmetal dissolution procedure is the main advantage of this method.

  9. Investigations on the on-line determination of metals in air flows by capacitively coupled microwave plasma atomic emission spectrometry

    Science.gov (United States)

    Seelig, M.; Broekaert, J. A. C.

    2001-09-01

    Plasma optical emission spectrometry with a capacitively coupled microwave plasma (CMP) operated with air has been investigated with respect to its possibilities for real-time environmental monitoring of combustion processes. The unique feature is the possibility to operate the CMP with air as working gas, as is usually the case in exhaust gases of combustion processes. The CMP also is shown to be stable in the presence of large amounts of water and CO 2, which makes this source ideally suitable for this purpose. The detection limits obtained for the environmentally relevant elements Cd, Co, Cr, Fe, Mg, Ni and Pb show the possibility to monitor directly heavy metals in air in an on-line mode and down to the 2-160-μg m -3 level. These detection limits are generally lower than the threshold limit values of the 'Federal Law for Immission Protection' in Germany in the gaseous effluents of industrial plants. In order to investigate the influence of the water loading (32-222 g m -3) on the detection limits a comparison of results obtained with three different nebulizers (Légère nebulizer, hydraulic high-pressure nebulizer and ultrasonic nebulizer) was made, with which aerosols with different water loading are entered into the plasma. For the hydraulic high-pressure nebulizer and the ultrasonic nebulizer no desolvation unit was found to be necessary. It was shown that especially for elements with lines having high excitation energy (Cd) or for which ion lines are used (Mg II) the increase in water loading deteriorates the detection limits. The rotational temperatures ( Trot) and excitation temperatures ( Texe) in the case of different amounts of water are of the order of 3700-4900 K and 4700-7100 K, respectively. The temperatures show that changes in the geometry and temperature distribution in the case of Trot but also the values of Texe themselves are responsible for this increase in detection limits. Furthermore, different amounts of CO 2 mixed to the working gas (3

  10. Volatile organo-selenium speciation in biological matter by solid phase microextraction-moderate temperature multicapillary gas chromatography with microwave induced plasma atomic emission spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Dietz, C.; Sanz Landaluze, J.; Ximenez-Embun, P.; Madrid-Albarran, Y.; Camara, C

    2004-01-16

    Microwave induced plasma atomic emission spectrometry (MIP-AES) in combination with multicapillary (MC) gas chromatography could be proven to be useful for element specific detection of volatile species. Solid phase microextraction (SPME) was used for preconcentration and sample-matrix separation. The fiber desorption unit as well as the heating control for the MC column were in-house developed and multicapillary column was operated at moderate temperatures (30-100 deg. C). The method was optimized for organo-selenium species (dimethylselenide (DMSe), diethylselenide (DEtSe) and dimethyldiselenide (DMDSe)), using a chemometric approach. Stationary phases for the separation column were optimized using a conventional GC and contrasted with the results obtained with the MC. Application was focussed on selenium accumulating biological matter, such as lupine, yeast, Indian mustard and garlic. These samples were grown in hydroponic solution containing inorganic selenium (Na{sub 2}SeO{sub 3} and Na{sub 2}SeO{sub 4}). SPME sampling was carried out in fixed volume flow boxes in headspace above the living plants and in vials using treated samples. Results demonstrate inorganic selenium transformation into volatile organic species during metabolism. Separation is fast, a chromatogram can be obtained in less than 3 min and detection limits were at sub-ppb level for all investigated species. The system is independent from the use of a conventional gas chromatographic oven and can be used as a versatile alternative to highly cost intensive methods such as GC-ICP-MS.

  11. 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.

    Science.gov (United States)

    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.

  12. Slurry sampling fluorination assisted electrothermal vaporization-inductively coupled plasma-atomic emission spectrometry for the direct determination of metal impurities in aluminium oxide ceramic powders.

    Science.gov (United States)

    Peng, T; Chang, G; Wang, L; Jiang, Z; Hu, B

    2001-03-01

    A new analytical procedure for the direct determination of metal impurities (Cr, Cu, Fe and V) in aluminium oxide ceramic powders by slurry sampling fluorination assisted electrothermal vaporization-inductively coupled plasma-atomic emission spectrometry (ETV-ICP-AES) is reported. A polytetrafluoroethylene (PTFE) emulsion was used as a fluorinating reagent to promote the vaporization of impurity elements in aluminium oxide ceramic powders from the graphite tube. A vaporization stage with a long ramp time and a short hold time provided the possibility of temporal analyte-matrix separation. The experimental results indicated that a 10 microL 1% m/v slurry of aluminium oxide could be destroyed and vaporized completely with 600 micrograms PTFE under the selected conditions. Two aluminium oxide ceramic powder samples were used without any additional pretreatment. Analytical results obtained by using standard addition method with aqueous standard solution were checked by comparison of the results with pneumatic nebulization (PN)-ICP-AES based on the wet-chemical decomposition and analyte-matrix separation. The limits of detection (LODs) between 0.30 microgram g-1 (Fe) and 0.08 microgram g-1 (Cu) were achieved, and, the repeatability of measurements was mainly better than 10%.

  13. Microwave-assisted versus conventional decomposition procedures applied to a ceramic potsherd standard reference material by inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-03-03

    Inductively coupled plasma atomic emission spectrometry (ICP-AES) is a powerful, sensitive analytical technique with numerous applications in chemical characterization including that of ancient pottery, mainly due to its multi-element character, and the relatively short time required for the analysis. A critical step in characterization studies of ancient pottery is the selection of a suitable decomposition procedure for the ceramic matrix. The current work presents the results of a comparative study of six decomposition procedures applied on a standard ceramic potsherd reference material, SARM 69. The investigated decomposition procedures included three microwave-assisted decomposition procedures, one wet decomposition (WD) procedure by conventional heating, one combined microwave-assisted and conventional heating WD procedure, and one fusion procedure. Chemical analysis was carried out by ICP-AES. Five major (Si, Al, Fe, Ca, Mg), three minor (Mn, Ba, Ti) and two trace (Cu, Co) elements were determined and compared with their certified values. Quantitation was performed at two different spectral lines for each element and multi-element matrix-matched calibration standards were used. The recovery values for the six decomposition procedures ranged between 75 and 110% with a few notable exceptions. Data were processed statistically in order to evaluate the investigated decomposition procedures in terms of recovery, accuracy and precision, and eventually select the most appropriate one for ancient pottery analysis.

  14. Problems, possibilities and limitations of inductively coupled plasma atomic emission spectrometry in the determination of platinum, palladium and rhodium in samples with different matrix composition

    Science.gov (United States)

    Petrova, P.; Velichkov, S.; Velitchkova, N.; Havezov, I.; Daskalova, N.

    2010-02-01

    The economic and geological importance of platinum group of elements has led to the development of analytical methods to quantify them in different types of samples. In the present paper the quantitative information for spectral interference in radial viewing 40.68 MHz inductively coupled plasma atomic emission spectrometry in the determination of Pt, Pd and Rh in the presence of complex matrix, containing Al, Ca, Fe, Mg, Mn, P and Ti as matrix constituents was obtained. The database was used for optimum line selections. By using the selected analysis lines the following detection limits in ng g - 1 were obtained: Pt 1700, Pd-1440, Rh-900. The reached detection limits determine the possibilities and limitation of the direct ICP-AES method in the determination of Pt, Pd and Rh in geological and environmental materials. The database for spectral interferences in the presence of aluminum can be used for the determination of platinum group of elements in car catalysts. The accuracy of the analytical results was experimentally demonstrated by two certified reference materials that were analyzed: SARM 7, Pt ore and recycled auto-catalyst certified reference material SRM 2556.

  15. Problems, possibilities and limitations of inductively coupled plasma atomic emission spectrometry in the determination of platinum, palladium and rhodium in samples with different matrix composition

    Energy Technology Data Exchange (ETDEWEB)

    Petrova, P.; Velichkov, S. [Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bontchev Str. bl. 11, 1113 Sofia (Bulgaria); Velitchkova, N. [Geological Institute, Bulgarian Academy of Sciences, Acad. G. Bontchev Str., bl.24, 1113 Sofia (Bulgaria); Havezov, I. [Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bontchev Str. bl. 11, 1113 Sofia (Bulgaria); Daskalova, N., E-mail: das15482@svr.igic.bas.b [Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bontchev Str. bl. 11, 1113 Sofia (Bulgaria)

    2010-02-15

    The economic and geological importance of platinum group of elements has led to the development of analytical methods to quantify them in different types of samples. In the present paper the quantitative information for spectral interference in radial viewing 40.68 MHz inductively coupled plasma atomic emission spectrometry in the determination of Pt, Pd and Rh in the presence of complex matrix, containing Al, Ca, Fe, Mg, Mn, P and Ti as matrix constituents was obtained. The database was used for optimum line selections. By using the selected analysis lines the following detection limits in ng g{sup -1} were obtained: Pt 1700, Pd-1440, Rh-900. The reached detection limits determine the possibilities and limitation of the direct ICP-AES method in the determination of Pt, Pd and Rh in geological and environmental materials. The database for spectral interferences in the presence of aluminum can be used for the determination of platinum group of elements in car catalysts. The accuracy of the analytical results was experimentally demonstrated by two certified reference materials that were analyzed: SARM 7, Pt ore and recycled auto-catalyst certified reference material SRM 2556.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Jankowski, Krzysztof [Warsaw University of Technology, Faculty of Chemistry, Department of Analytical Chemistry, 00-664 Warsaw, ul. Noakowskiego 3 (Poland)]. E-mail: kj@ch.pw.edu.pl; Yao Jun [College of Chemistry and Chemical Engineering, Jishou University, 120 Renmin South Road, Jishou 416000 (China); Kasiura, Krzysztof [Warsaw University of Technology, Faculty of Chemistry, Department of Analytical Chemistry, 00-664 Warsaw, ul. Noakowskiego 3 (Poland); Jackowska, Adrianna [Warsaw University of Technology, Faculty of Chemistry, Department of Analytical Chemistry, 00-664 Warsaw, ul. Noakowskiego 3 (Poland); Sieradzka, Anna [Warsaw University of Technology, Faculty of Chemistry, Department of Analytical Chemistry, 00-664 Warsaw, ul. Noakowskiego 3 (Poland)

    2005-03-31

    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{sub 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{sup -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.

  18. 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.

    Science.gov (United States)

    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.

  19. 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

    Energy Technology Data Exchange (ETDEWEB)

    Beiraghi, Assadollah [Faculty of Chemistry, Tarbiat Moallem University, Mofatteh Avenue, No. 49, P.O. Box 15614, Tehran (Iran, Islamic Republic of)], E-mail: Beiraghi@Saba.tmu.ac.ir; Babaee, Saeed [Faculty of Chemistry, Tarbiat Moallem University, Mofatteh Avenue, No. 49, P.O. Box 15614, Tehran (Iran, Islamic Republic of)

    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 0.4 mL of a 60:40 methanol-water mixture containing 0.03 mL HNO{sub 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{sup -4} mol L{sup -1} 1,8-dihydroxyanthrone, 1.2 x 10{sup -4} mol L{sup -1} CPC, 0.15% (v/v) Triton X-114, 50 deg. C equilibrium temperature) the calibration graph was linear in the range of 0.006-80 ng mL{sup -1} with detection limit of 0.001 ng mL{sup -1} and the precision (R.S.D.%) for five replicate determinations at 18 ng mL{sup -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.

  20. Ultrasound bath-assisted enzymatic hydrolysis procedures as sample pretreatment for the multielement determination in mussels by inductively coupled plasma atomic emission spectrometry.

    Science.gov (United States)

    Peña-Farfal, Carlos; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Adela; Bermejo-Barrera, Pilar; Pinochet-Cancino, Hugo; de Gregori-Henríquez, Ida

    2004-07-01

    Ultrasound energy has been applied to speed up enzymatic hydrolysis processes of mussel tissue in order to determine trace and ultratrace elements (As, Al, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Zn). The element releases, by action of three proteases (pepsin, pancreatin, trypsin), lipase, and alpha-amylase, have been evaluated by inductively coupled plasma atomic emission spectrometry. Different variables such as pH, sonication temperature, ionic strength, hydrolysis time, ultrasound frequency, extracting volume, and enzyme mass were simultaneously studied by applying an experimental design approach (Plackett-Burman design and central composite design). Results showed that the hydrolysis time was statistically nonsignificant (confidence interval of 95%) for most of the elements and enzymes, meaning that the hydrolysis procedure can be finished within a 30-60-min range. These hydrolysis times are far shorter than those obtained when using thermostatic cameras, between 12 and 24 h. Statistically significant factors were the ultrasound frequency (the highest metals releasing at high-ultrasound frequency), pH, sonication temperature, and ionic strength. All metals can be extracted using the same operating conditions (pH of 1.0 and sodium chloride at 1.0% for pepsin; pH of 7.5, temperature at 37 degrees C, and 0.4 M potassium dihydrogen phosphate/potassium hydrogen phosphate buffer for amylase; pH of 8.0 and 0.5 M potassium dihydrogen phosphate/potassium hydrogen phosphate buffer for pancreatin; pH of 5.0 and 0.5 M potassium dihydrogen phosphate/potassium hydrogen phosphate buffer for lipase; pH of 8.0 and 0.2 M potassium dihydrogen phosphate/potassium hydrogen phosphate buffer for trypsin). Analytical performances, such as limits of detection and quantification, repeatability of the overall procedure, and accuracy, by analyzing DORM-1, DORM-2, and TORT-1 certified reference materials, were finally assessed for each enzyme.

  1. On-line cloud point extraction combined with electrothermal vaporization inductively coupled plasma atomic emission spectrometry for the speciation of inorganic antimony in environmental and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Li Yingjie [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)]. E-mail: binhu@whu.edu.cn; Jiang Zucheng [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2006-08-25

    A new method for the determination of inorganic Sb species by on-line cloud point extraction combined with electrothermal vaporization inductively coupled plasma atomic emission spectrometry (ETV-ICP-AES) is presented and evaluated. The method is based on the complexation of Sb(III) with pyrrolidine dithiocarbamate (PDC) which form an hydrophobic complex at pH 5.5 and subsequently enter surfactant-rich phase at pH 5.5, whereas Sb(V) remained in aqueous solutions. The preconcentration step is mediated by micelles of the non-ionic surfactant Triton X-114 with ammonium pyrrolidine dithiocarbamate (APDC). The micellar system containing the complex was loaded into the FIA manifold at a flow rate of 2.5 mL min{sup -1}, and the surfactant-rich phase was retained in a microcolumn packed with absorbent cotton, at pH 5.5. After the surfactant-rich phase was eluted with 100 {mu}L acetonitrile, it was determined by ETV-ICP-AES. Sb(V) is reduced to Sb(III) by L-cysteine prior to determined total Sb, and its assay is based on subtracting Sb(III) from total antimony. The main factors affecting separation/preconcentration and the vaporization behavior of analyte in graphite tube were investigated in detail. Under the optimized conditions, the precision relative standard deviation (R.S.D.) for eight replicate measurements of 0.2 {mu}g mL{sup -1} Sb(III) was 4.3%. The apparent concentration factor, which is defined as the concentration ratio of the analyte in the final diluted surfactant-rich extract ready for ETV-ICP-AES detection and in the initial solution, was 872 for Sb(III). The limit of detection (LOD) for Sb(III) was 0.09 {mu}g L{sup -1}. The proposed method was successfully applied for the speciation of inorganic antimony in different water samples and urine sample with satisfactory results.

  2. Determination of the mineral compositions of some selected oil-bearing seeds and kernels using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES

    Directory of Open Access Journals (Sweden)

    Musa Özcan, M.

    2006-06-01

    Full Text Available The aim of this paper was to establish the mineral contents of oil-bearing seeds and kernels such as peanut, turpentine, walnut, hazelnut, sesame, corn, poppy, almond, sunflower etc., using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES. Significant differences in mineral composition were observed among crops. All seeds and kernels contained high amounts of Al, Ca, Fe, K, Mg, Na, P and Zn. B, Cr, Cu, Li, Ni, Sr, Ti while V contents of the crops were found to be very low. The levels of K and P of all crops in this study were found to be higher than those of other seeds and kernels. The results obtained from analyses of the crops showed that the mean levels of potassiumcontent ranged from 1701.08 mg/kg (corn to 20895.8 mg/kg (soybean, the average content of phosphorus ranged from 3076.9 mg/kg (turpentine to 12006,5 mg/kg to 2617.4 mg/kg (cotton seed, and Ca from 68.4 mg/kg (corn to 13195.7 mg/kg (poppy seed. The results show that these values may  be useful for the evaluation of dietary information. Particularly the obtained results provide evidence that soybean, pinestone and poppy seed are a good source of K, P and Ca, respectively. Whereas pinestone is a good source of zinc.La finalidad del trabajo es establecer el contenido en elementos minerales de semillas oleaginosas tales como cacahuetes, trementina, avellana, sesamo, maiz, almendras, girasol, utilizando ICP-AES. Se han observado diferencias significativas en la composición de minerales entre cosechas. Todas las semillas contienen cantidades elevadas de Al, Ca, Fe, K, Mg, Na, P y Zn. Los contenidos de B, Cr, Cu, Li, Ni, Sr, Ti y V, sin embargo, fueron bajos. Los contenidos de K y P en todas las semillas estudiadas fueron superiores a las de otras semillas. El contenido medio de K osciló entre 1.701,1 mg/kg (maiz a 20.895,8 mg/kg (soja, el P entre 3.076.9 mg/kg (trementina a 12.006.5 mg/kg o 2.617,4 mg/kg (semilla de algodón, y Ca de 68,4 mg/kg (maiz a 13.195,7 mg

  3. 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.

    Science.gov (United States)

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

    2016-11-01

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

  4. 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.

    Science.gov (United States)

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

    2014-01-02

    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. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. 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

    Directory of Open Access Journals (Sweden)

    Yajing Lou

    2014-01-01

    Full Text Available 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.

  6. 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

    Science.gov (United States)

    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

  7. Simultaneous determination of some trace metal impurities in high-purity sodium tungstate using coprecipitation and inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    MA Xiaoguo; KUANG Tongchun; LIU Qianjun

    2004-01-01

    A method based on the combination of coprecipitation with inductively coupled plasma atomic emission spec trometry (ICP-AES) was developed for the determination of impurities in high-purity sodium tungstate. Six elements (Co,Cu, Fe, Mn, Ni, and Pb) were coprecipitated by lanthanum hydroxide so as to be concentrated and separated from the tungsten matrix. Effects of some factors on the recoveries of the analytes and on the residual amount of sodium tungstate were investigated, and the optimum conditions for the coprecipitation were proposed. Matrix-matching calibration curve method was used for the analysis. It is shown that the elements mentioned above can be quantitatively recovered. The detection limits for Co, Cu, Fe, Mn, Ni, and Pb are 0.07, 0.4, 0.2, 0.1, 0.6, and 1.3 μg.g-1, respectively. The recoveries vary from 92.5% to 108%, and the relative standard deviations (RSDs) are in the range of 3.1%-5.5%.

  8. Use of stirred tanks for studying matrix effects caused by inorganic acids, easily ionized elements and organic solvents in inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Paredes, Eduardo [Departamento de Quimica Analitica, Nutricion y Bromatologia, University of Alicante, 03080 Alicante (Spain); Maestre, Salvador E. [Departamento de Quimica Analitica, Nutricion y Bromatologia, University of Alicante, 03080 Alicante (Spain); Todoli, Jose L. [Departamento de Quimica Analitica, Nutricion y Bromatologia, University of Alicante, 03080 Alicante (Spain)]. E-mail: jose.todoli@ua.es

    2006-03-15

    A stirred tank was used for the first time to elucidate the mechanism responsible for inductively coupled plasma atomic emission spectroscopy (ICP-AES) matrix effects caused by inorganic, acids and easily ionized elements (EIEs), as well as organic, ethanol and acetic acid, compounds. In order to gradually increase the matrix concentration, a matrix solution was introduced inside a stirred container (tank) initially filled with an aqueous multielement standard. PolyTetraFluoroEthylene (PTFE) tubing was used to deliver the resulting solution to the liquid sample introduction system. Matrix concentration ranged from 0 to 2 mol l{sup -1} in the case of inorganic acids (i.e., nitric, sulfuric, hydrochloric and a mixture of them), from 0 to about 2500 mg l{sup -1} for EIEs (i.e., sodium, calcium and mixtures of both) and from 0% to 15%, w/w for organic compounds. Up to 40-50 different solutions were prepared and measured in a period of time shorter than 6-7 min. This investigation was carried out in terms of emission intensity and tertiary aerosols characteristics. The experimental setup used in the present work allowed to thoroughly study the effect of matrix concentration on analytical signal. Generally speaking, the experiments concerning tertiary aerosol characterization revealed that, in the case of inorganic acids and EIEs, the mechanism responsible for changes in aerosol characteristics was the droplet fission. In contrast, for organic matrices it was found that the interference was caused by a change in both aerosol transport and plasma thermal characteristics. The extent of the interferences caused by organic as well as inorganic compounds was compared for a set of 14 emission lines through a wide range of matrix concentrations. With a stirred tank, it is possible to choose an efficient internal standard for any given matrix composition. The time required to complete this procedure was shorter than 7 min.

  9. 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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Science.gov (United States)

    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

  11. An analytical method for hydrogeochemical surveys: Inductively coupled plasma-atomic emission spectrometry after using enrichment coprecipitation with cobalt and ammonium pyrrolidine dithiocarbamate

    Science.gov (United States)

    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

  12. 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

    Energy Technology Data Exchange (ETDEWEB)

    Rosende, María [FI-TRACE group, Department of Chemistry, University of the Balearic Islands, Carretera de Valldemossa, km 7.5, Palma de Mallorca, Illes Balears E-07122 (Spain); Magalhães, Luis M.; Segundo, Marcela A. [REQUIMTE, Department of Chemistry, Faculty of Pharmacy, University of Porto, R. de Jorge Viterbo Ferreira, 228, Porto 4050-313 (Portugal); Miró, Manuel, E-mail: manuel.miro@uib.es [FI-TRACE group, Department of Chemistry, University of the Balearic Islands, Carretera de Valldemossa, km 7.5, Palma de Mallorca, Illes Balears E-07122 (Spain)

    2014-09-09

    Highlights: • Automatic oral bioaccessibility tests of trace metals under worst-case scenarios. • Use of intricate and realistic digestive fluids (UBM method). • Analysis of large amounts of soils (≥400 mg) in a flow-based configuration. • Smart interface to inductively coupled plasma atomic emission spectrometry. • Comparison of distinct flow systems mimicking physiological conditions. - Abstract: 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{sup −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

  13. Influence of binders on infrared laser ablation of powdered tungsten carbide pressed pellets in comparison with sintered tungsten carbide hardmetals studied by inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hola, Marketa [Research Centre for Environmental Chemistry and Ecotoxicology and Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University in Brno, Kotlarska 2, CZ 611 37 Brno (Czech Republic); Otruba, Vitezslav [Research Centre for Environmental Chemistry and Ecotoxicology and Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University in Brno, Kotlarska 2, CZ 611 37 Brno (Czech Republic); Kanicky, Viktor [Research Centre for Environmental Chemistry and Ecotoxicology and Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University in Brno, Kotlarska 2, CZ 611 37 Brno (Czech Republic)]. E-mail: viktork@chemi.muni.cz

    2006-05-15

    Laser ablation (LA) was studied as a sample introduction technique for the analysis of powdered and sintered tungsten carbides (WC/Co) by inductively coupled plasma optical emission spectrometry (ICP-OES). The possibility to work with powdered and compact materials with close chemical composition provided the opportunity to compare LA sampling of similar substances in different forms that require different preparation procedures. Powdered WC/Co precursors of sintered hardmetals were prepared for the ablation as pressed pellets with and without powdered silver as a binder, while sintered hardmetal blocks were embedded into a resin to obtain discs, which were then smoothed and polished. A Q-switched Nd:YAG laser operated at its fundamental wavelength of 1064 nm with a pulse frequency of 10 Hz and maximum pulse energy of 220 mJ was used. A single lens was used for the laser beam focusing. An ablation cell (14 cm{sup 3}) mounted on a PC-controlled XY-translator was connected to an ICP spectrometer Jobin Yvon 170 Ultrace (laterally viewed ICP, mono- and polychromator) using a 1.5-m tubing (4 mm i.d.). Ablation was performed in a circular motion (2 mm diameter). Close attention was paid to the study of the crater parametres depending on hardness, cohesion and Ag binder presence in WC/Co samples. The influence of the Co content on the depth and structure of the ablation craters of the binderless pellets was also studied. Linear calibration plots of Nb, Ta and Ti were obtained for cemented WC/Co samples, binderless and binder-containing pellets. Relative widths of uncertainty intervals about the centroids vary between {+-} 3% and {+-} 7%, and exceptionally reach a value above 10%. The lowest determinable quantities (LDQ) of Nb, Ta and Ti calculated from the calibration lines were less than 0.5% (m/m). To evaluate the possibility of quantitative elemental analysis by LA-ICP-OES, two real sintered WC/Co samples and two real samples of powdered WC/Co materials were analysed

  14. Influence of binders on infrared laser ablation of powdered tungsten carbide pressed pellets in comparison with sintered tungsten carbide hardmetals studied by inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Holá, Markéta; Otruba, Vítězslav; Kanický, Viktor

    2006-05-01

    Laser ablation (LA) was studied as a sample introduction technique for the analysis of powdered and sintered tungsten carbides (WC/Co) by inductively coupled plasma optical emission spectrometry (ICP-OES). The possibility to work with powdered and compact materials with close chemical composition provided the opportunity to compare LA sampling of similar substances in different forms that require different preparation procedures. Powdered WC/Co precursors of sintered hardmetals were prepared for the ablation as pressed pellets with and without powdered silver as a binder, while sintered hardmetal blocks were embedded into a resin to obtain discs, which were then smoothed and polished. A Q-switched Nd:YAG laser operated at its fundamental wavelength of 1064 nm with a pulse frequency of 10 Hz and maximum pulse energy of 220 mJ was used. A single lens was used for the laser beam focusing. An ablation cell (14 cm 3) mounted on a PC-controlled XY-translator was connected to an ICP spectrometer Jobin Yvon 170 Ultrace (laterally viewed ICP, mono- and polychromator) using a 1.5-m tubing (4 mm i.d.). Ablation was performed in a circular motion (2 mm diameter). Close attention was paid to the study of the crater parametres depending on hardness, cohesion and Ag binder presence in WC/Co samples. The influence of the Co content on the depth and structure of the ablation craters of the binderless pellets was also studied. Linear calibration plots of Nb, Ta and Ti were obtained for cemented WC/Co samples, binderless and binder-containing pellets. Relative widths of uncertainty intervals about the centroids vary between ± 3% and ± 7%, and exceptionally reach a value above 10%. The lowest determinable quantities (LDQ) of Nb, Ta and Ti calculated from the calibration lines were less than 0.5% (m/m). To evaluate the possibility of quantitative elemental analysis by LA-ICP-OES, two real sintered WC/Co samples and two real samples of powdered WC/Co materials were analysed. The

  15. ICP-AES法测定土壤中的钾、锌、钒和钴%Determination of Potassium,Zinc,Vanadium,and Cobalt in Soil by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES)

    Institute of Scientific and Technical Information of China (English)

    张继华; 张加萍

    2014-01-01

    Hydrochloric acid,nitric acid,hydrofluoric acid,and perchloric acid were applied to digest heavy met-als in soil sample.Inductively coupled plasma-atomic emission spectrometry (ICP-AES)method was employed to determine the contents of potassium,zinc,vanadium,and cobalt.The precision of this method to these four heavy metals was 3.09%for potassium,4.14%for zinc,3.76%for vanadium,and 3.85%for cobalt respective-ly.Generally,this method is simple and quick with wide linear range and few distractions.%采用盐酸-硝酸-氢氟酸-高氯酸全分解的方法消解,在选定的条件下以ICP-AES测定溶液中的K、Zn 、V 和Co含量,对国家标准物进行测定,方法精密度(RSD,n=16)为K 3.09%、Zn 4.14%、V 3.76%、Co3.85%。该方法具有线性范围宽、干扰少、快速、简便等优点,用于实样分析,结果令人满意。

  16. Determination of borax in yuba by inductively coupled plasma atomic emission spectrometry with microwave digestion%微波消解-等离子体发射光谱法测定腐竹中硼砂

    Institute of Scientific and Technical Information of China (English)

    黄子伟; 王世平; 汤大鹏

    2012-01-01

    The dielectric assisted microwave digestion conditions were selected by orthogonal design, the experimental design was used to investigate the effect of four parameters: microwave power, mixed acid ratio, mixed acid volume and digestion time. And the borax in Yuba was determination with Inductively Coupled Plasma Atomic Emission Spectrometry after microwave digestion. The detection limit of the method was 0.4 mg/kg, the recoveries were in the rang of 91.2%~103.9%, and relative standard deviations were less than 2%.%采用正交试验设计优化介质辅助微波消解样品的条件,以电感耦合等离子体发射光谱法(ICP-AES)测定腐竹中硼砂。考察了微波消解功率、混合酸的比例、混合酸用量、试样消解时间4个因素在不同水平条件下对仪器响应值的影响。在优化了微波消解条件下测定实际样品,方法检出限为0.4mg/kg,加标回收率为91.2%~103.9%,相对标准偏差〈2%。

  17. Purge-and-trap isothermal multicapillary gas chromatographic sample introduction accessory for speciation of mercury by microwave-induced plasma atomic emission spectrometry.

    Science.gov (United States)

    Rodriguez Pereiro, I; Wasik, A; Lobiński, R

    1998-10-01

    A compact device based on purge-and-trap multicapillary gas chromatography was developed for sensitive species-selective analysis of methylmercury and Hg2+ by atomic spectrometry. The operating mode includes in situ conversion of the analyte species to MeEtHg and HgEt2 and cryotrapping of the derivatives formed in a 0.53-mm-i.d. capillary, followed by their flash ( 60 mL min-1) compatible with an MIP AES detector (no dilution with a makeup gas is required). Developments regarding each of the steps of the analytical procedure and effects of operational variables (sample volume, purge flow, trap temperature, separation conditions) are discussed. The device allows speciation of MeHg+ and Hg2+ down to 5 pg g-1 in urine and, after a rapid microwave-assisted hydrolysis, down to 0.1 ng g-1 in solid biological samples with a throughput of 6 samples/h. The analytical protocols developed were validated by the analysis of DORM-1 (dogfish muscle), TORT-1 (lobster hepatopancreas), and Seronorm urine certified reference materials.

  18. Sequential-injection on-line preconcentration using chitosan resin functionalized with 2-amino-5-hydroxy benzoic acid for the determination of trace elements in environmental water samples by inductively coupled plasma-atomic emission spectrometry.

    Science.gov (United States)

    Sabarudin, Akhmad; Lenghor, Narong; Oshima, Mitsuko; Hakim, Lukman; Takayanagi, Toshio; Gao, Yun-Hua; Motomizu, Shoji

    2007-07-31

    A new chelating resin using chitosan as a base material was synthesized. Functional moiety of 2-amino-5-hydroxy benzoic acid (AHBA) was chemically bonded to the amino group of cross-linked chitosan (CCTS) through the arm of chloromethyloxirane (CCTS-AHBA resin). Several elements, such as Ag, Be, Cd, Co, Cu, Ni, Pb, U, V, and rare earth elements (REEs), could be adsorbed on the resin. To use the resin for on-line pretreatment, the resin was packed in a mini-column and installed into a sequential-injection/automated pretreatment system (Auto-Pret System) coupled with inductively coupled plasma-atomic emission spectrometry (ICP-AES). The sequential-injection/automated pretreatment system was a laboratory-assembled, and the program was written using Visual Basic software. This system can provide easy operation procedures, less reagent consumption, as well as less waste production. Experimental variables considered as effective factors in the improvement sensitivity, such as an eluent concentration, a sample and an eluent flow rate, pH of samples, and air-sandwiched eluent were carefully optimized. The proposed system provides excellent on-line collection efficiency, as well as high concentration factors of analytes in water samples, which results in highly sensitive detection of ultra-trace and trace analysis. Under the optimal conditions, the detection limits of 24 elements examined are in the range from ppt to sub-ppb levels. The proposed method was validated by using the standard reference material of a river water, SLRS-4, and the applicability was further demonstrated to the on-line collection/concentration of trace elements, such as Ag, Be, Cd, Co, Cu, Ni, Pb, U, V, and REEs in water samples.

  19. 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.

    Science.gov (United States)

    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.

  20. Determination of La,Mg in Co-based alloys by inductively coupled plasma atomic emission spectrometry%ICP-AES法测定钴基合金中La、Mg元素的含量

    Institute of Scientific and Technical Information of China (English)

    高颂; 庞晓辉; 许维兵

    2014-01-01

    A method for determination of principal elements lanthanum and magnesium in Co-based al-loys by inductively coupled plasma atomic emission spectrometry is proposed .In this method ,the micro-wave digestion is used to reduce the background .Matrix-matching method is used to eliminated spectral interference .The experiments of instrument parameters ,sample dissolution ,selection of analysis lines , and the effect of matrix on the determination ,and the comparison of reference materials and the analytical results are carried out .T he recovery rate is at the range of 90%-99% ,RSD≤4% .%研究了钴基合金样品的溶解方法,采用盐酸、硝酸、氢氟酸溶解,使用微波消解溶解方法,控制试剂用量,降低了空白;考察了基体和主量元素对待测元素的影响,选择待测元素灵敏度高、光谱干扰少的谱线 La 408.672nm、Mg 279.553nm为分析线,校准曲线溶液采用基体匹配消除了基体效应影响,实现了用电感耦合等离子体原子发射光谱法测定钴基合金中La、Mg元素含量,方法的检出限可达0.002μg/mL ,进行了标准物质对照试验,与标准值相符,进行了加入回收试验,回收率90~99%,RSD<4%。

  1. Ultra-trace monitoring of copper in environmental and biological samples by inductively coupled plasma atomic emission spectrometry after separation and preconcentration by using octadecyl silica membrane disks modified by a new schiff's base

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Ganjali

    2004-04-01

    Full Text Available Ultra-trace amounts of Cu(II were separated and preconcentrated by solid phase extraction on octadecyl-bonded silica membrane disks modified with a new Schiff,s base (Bis- (2-Hydroxyacetophenone -2,2-dimethyl-1,3-propanediimine (SBTD followed by elution and inductively coupled plasma atomic emission spectrometric detection. The method was applied as a separation and detection method for copper(II in environmental and biological samples. Extraction efficiency and the influence of sample matrix, flow rate, pH, and type and minimum amount of stripping acid were investigated. The concentration factor and detection limit of the proposed method are 500 and 12.5 pg mL-1, respectively.

  2. 电感耦合等离子体原子发射光谱法测定炼锑泡渣中碲%Determination of tellurium in refined antimony slag by inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    张忠亭; 邓飞跃; 蒋苏琼; 刘逸群; 李彪

    2011-01-01

    建立了用电感耦合等离子体原子发射光谱法(ICP-AES)测定炼锑泡渣中碲的方法.选择波长为214.281 nm的谱线作为碲的分析线,只有La 214.281 nm,V 214.274 nm,Pt214.250 nm,Nb 214.291 nm和Re 214.297 nm线有干扰,但炼锑泡渣中La、V、Pt、Nb、Re含量都很低,其影响可以忽略,因此不需要进行预分离,样品用王水溶解后可直接进行ICP-AES测定.考察了仪器工作参数对测定结果的影响,并确定了最佳工作条件:观测高度为15 mm,雾化气流速为0.8 L/min,射频功率为1 300 W.方法线性范围为0.01~100 mg/L,线性相关系数为1.000 0,检出限(3σ)为0.007 2 mg/L,样品测定结果的相对标准偏差(RSD)为0.16%,加标回收率为97%~102%.%The determination method of tellurium in refined antimony slag by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The spectral line of 214. 281 nm was used as the analytical line of tellurium. Only La 214. 281 nm, V 214. 274 nm, Pt 214. 250 nm, Nb 214. 291 nm and Re 214. 297 nm lines had interference. However, the content of La, V, Pt, Nb and Re in refined antimony slag were very low, so their influence could be ignored and the pre-separation was not necessary. After dissolving with aqua regia, the sample solution was directly determined by ICP-AES. The effect of instrumental working parameters on determination results was investigated. The optimal working conditions were as follows: observation height, 15 mm; flow rate of atomizing gas, 0.8 L/min; radio frequency power, 1 300 W. The linear range of method was 0. 01-100 mg/L with correlation coefficient of 1. 000 0. The detection limit (3a) was 0. 007 2 mg/L. The relative standard deviation (RSD) was 0. 16 %, and the recoveries of standard addition were 97 %-102 %.

  3. 电感耦合等离子体发射光谱法测定油田水中的硼%Determination of Boron in Oil Field Water by Inductively Coupled Plasma-Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    宋继芳

    2012-01-01

    样品经硝酸酸化、滤膜过滤处理后,用电感耦合等离子体发射光谱法直接测定其中硼的含量.通过正交实验优选仪器参数和分析谱线,在选定的波长208.959nm下,对样品稀释倍数和介质酸种类进行选择,结果表明,硼含量低于10mg/L的样品不用稀释,高于10mg/L的样品一般稀释20倍,介质选用硝酸可使测定结果更加准确.对油田水中共存的7种主要金属元素进行了干扰试验,样品中存在20mg/L的Sr、Ba、Fe,50mg/L的Mg、Ca,100mg/L的K,200mg/L的Na对待测元素的测定没有影响.选取油田水样品进行加标回收试验,方法平均回收率为95.3%~102.0%,精密度(RSD,n=11)为0.43%~0.92%,检出限为0.0020mg/L.方法简便、快速,结果令人满意,与姜黄素分光光度法比较,克服了分析流程长、使用试剂较多且不易操作的不足.%Boron in oil field water has been directly determined by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) after sample were treated with nitric acid and filtrated. This method overcomes the problems of spectrophotometry such as long analysis flow, more reagent and difficulty in controlling the chemical procedure. The working parameters and the spectral line were optimized by orthogonal tests. The dilute multiple and acid medium were analyzed using the selected 208.959 nm frequency. The results show that it is not necessary to dilute the sample when the content of B is less than 10 mg/L, and the dilution factor is 20 when B is greater than 10 mg/L. The selected HNO3 as the acid medium, improved the accuracy of the results. The interference tests were carried out for 7 major metals in oil field water. 20 mg/L Sr, Ba and Fe, 50 mg/L Mg and Ca, 100 mg/L K and 200 mg/L Na have no interference for the measurements of the target element. The detection limit of boron was 0.0020 mg/L and the recoveries ranged from 95.3% to 102.0% with a precision in the range of 0.43% - 0.92% ( RSD, n = 11

  4. 电感耦合等离子体原子发射光谱法测定银合金中的铂钯%Determination of Platinum and Palladium in Silver Alloy by Inductively Coupled Plasma Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    佡云; 褚晓君

    2016-01-01

    采用硝酸溶解样品,盐酸沉淀分离银,过滤洗涤后,在5%(体积分数)硝酸介质中,用电感耦合等离子体原子发射光谱法(ICP-AES)测定银合金样品中的铂、钯,该方法用于多个银合金中铂钯的测定,加标回收率在96%~101%,相对标准偏差(RSD,n=10)小于5%。%The sample was dissolved with nitric acidhydrochloric acid was added to the sample to produce precipitation of silver chloridethen filter and wash it.Platinum and palladium in silver alloy samples are determinated by inductively coupled plasma atomic emission spectrometryICP-AES in a 5% volume fraction nitric acid .The method was applied to the determination of platinum and palladium in silver al-lay samples.The recovery rate was in the range of 96%~101% and the relative standard deviationRSDn=10 was less than 5%.

  5. Determination of Trace Elements in Pomegranate Peel and Pomegranate Seed by Inductively Coupled Plasma-Atomic Emission Spectrometry with Microwave Digestion%微波消解-等离子体原子发射光谱法测定石榴皮和石榴籽中微量元素

    Institute of Scientific and Technical Information of China (English)

    吴佳; 解成喜

    2012-01-01

    采用微波消解样品,电感耦合等离子体原子发射光谱法(ICP-AES)测定了石榴皮和石榴籽中K、Ca、Mg、Fe、A1、Cu、Zn、Mn、Na、Li、P、S12种微量元素的含量.在最佳仪器工作条件下,各元素的加标回收率为91.8%~103.1%,相对标准偏差(RSD)为0.70%~2.68%.实验结果可为石榴皮和石榴籽中微量元素与其药效的相关性提供科学依据.%The trace elements of K,Ca,Mg,Fe, Al,Cu,Zn,Mn,Na,Li,P and S in the pomegranate peel and pomegranate seed were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) with microwave digestion. Under the optimal working conditions of the equipment, the element recoveries of standard addition are 91. 8% ~ 103. l%,and the relative standard deviations (RSDs) are 0. 70%~2. 68%.

  6. Determination of Twelve Trace Elements in Children`s hair by Inductively Coupled Plasma Atomic Emission Spectrometry%电感耦合等离子体发射光谱法测定儿童发样中十二种微量元素

    Institute of Scientific and Technical Information of China (English)

    代建强; 杨诗佳

    2013-01-01

    This paper uses the nitric acid and hydrogen peroxide sample digestionarticle, Determination of aluminum, calcium, chromium, copper, iron, potassium, magnesium, sodium, manganese, lead, nickel, zinc and other trace elements in children's hair by inductively coupled plasma atomic emission spectrometry.The recovery rate of 95%~105%,The detection limit of element (ug/ml) in 0.0010-0.011,The relative standard deviation (RSD, n=9) is less than 4%,After verification of human hair in national standard reference samples, The measured value had no significant difference with standard value.%采用硝酸-过氧化氢消解试样,电感耦合等离子体发射光谱法测定儿童发样中铝、钙、铬、铜、铁、钾、镁、锰、钠、铅、镍、锌等十二种微量元素。方法回收率95%~105%,各元素检出限(ug/mL)在0.0010~0.011之间,相对标准偏差(RSD,n=9)小于4%,经人发国家一级标准物质验证,测定值与标准认定值无明显差异。

  7. 电感耦合等离子体发射光谱法测定镍矿石中镍铜铅锌%Determination of Ni,Cu,Pb and Zn in nickel ores by inductive coupling plasma-atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    郭爽; 金震宇; 杨婷; 于微

    2012-01-01

    The authors dissolved the sample of the nickle ore with hydrofluoric acid,nitric acid,hydrochloric acid and high chloride acid.Dissolved the salt with aqua regia.To determine the elements of nickel,copper,lead and zinc in the solution by inductive coupling plasma-atomic emission spectrometry,to interfere survey the target elements in spectrum lines,and to select the suitable analytical spectral lines.The result of the experiment proves that the nickel can increase the spectrum line background and overlapping peak of the target elements,In addition,the recovery rate ranges from 98% to 103%,and the relative deviation less than 3.%选用氢氟酸、硝酸、盐酸、高氯酸对镍矿石样品进行溶样,用王水溶解盐类,电感耦合等离子体发射光谱法测定溶液中镍、铜、铅、锌元素,对目标元素进行谱线干扰考察,选择合适的分析谱线,结果表明镍会使目标元素谱线背景和叠加峰轻度增高,回收率都在98%~103%,相对偏差小于3。

  8. Separation and preconcentration of Cd(II), Cu(II), Ni(II), and Pb(II) in water and food samples using Amberlite XAD-2 functionalized with 3-(2-nitrophenyl)-1H-1,2,4-triazole-5(4H)-thione and determination by inductively coupled plasma-atomic emission spectrometry.

    Science.gov (United States)

    Kumar, Bommana Naresh; Ramana, D K Venkata; Harinath, Yapati; Seshaiah, Kalluru; Wang, M C

    2011-10-26

    A separation and preconcentration procedure was developed for the determination of trace amounts of Cd(II), Cu(II), Ni(II), and Pb(II) in water and food samples using Amberlite XAD-2 fuctionalized with a new chelating ligand, 3-(2-nitrophenyl)-1H-1,2,4-triazole-5(4H)-thione (Amberlite XAD-2-NPTT). The chelating resin was characterized by Fourier transform infrared spectroscopy (FT-IR) and used as a solid sorbent for enrichment of analytes from samples. The sorbed elements were subsequently eluted with 10 mL of 1.0 M HNO(3), and the eluates were analyzed by inductively coupled plasma-atomic emission spectrometry. The influences of the analytical parameters including pH, amount of adsorbent, eluent type and volume, flow rate of the sample solution, volume of the sample solution, and effect of matrix on the preconcentration of metal ions have been studied. The optimum pH for the sorption of four metal ions was about 6.0. The limits of detection were found to be 0.22, 0.18, 0.20, and 0.16 μg L(-1) for Cd(II), Cu(II), Ni(II), and Pb(II), respectively, with a preconcentration factor 60. The proposed method was applied successfully for the determination of metal ions in water and food samples.

  9. Determination of Heavy Metals in Electroplating Sludge Leaching Liquid by Inductively Coupled Plasma Atomic Emission Spectrometry%电感耦合等离子体原子发射光谱法测定电镀污泥浸出液中的重金属

    Institute of Scientific and Technical Information of China (English)

    徐国津; 樊颖果; 赵倩

    2014-01-01

    Heavy metals in electroplating sludge leaching liquid such as Cu,Zn,Ni,Cr,Pb,Cd and Ba were determined by inductively coupled plasma atomic emission spectrometry with sulfuric acid-nitric acid extraction. The working conditions of the instrument and interference factors and elimination method were studied. Under the selected conditions,the linear correlation coefficients were all 0.999 9,the detection limits were between 0.002 mg/L and 0.01 mg/L,recoveries ranged from 93.5%to 106.0%,and the relative standard deviations of determination results were less than 10%(n=6). The method could quickly and accurately detect some heavy metals in electroplating sludge leaching liquid.%采用硫酸-硝酸溶液浸提电镀污泥中的重金属,建立电感耦合等离子体原子发射光谱法(ICP-AES)测定电镀污泥浸出液中铜、锌、镍、铬、铅、镉、钡元素的分析方法。研究了仪器的工作条件及影响检测方法的干扰因素和消除。在选定的条件下,线性相关系数均为0.9999,检出限为0.002~0.01 mg/L,加标回收率为93.5%~106.0%,测定结果的相对标准偏差小于10%(n=6)。该方法准确快速,可用于电镀污泥浸出液中多种重金属的含量测定。

  10. 电感耦合等离子体原子发射光谱法测定新疆洋葱籽中常量/微量元素%Determination of Major/Trace Elements in the Xinjiang Allium cepa L.Seeds by Inductively Coupled Plasma Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    孙凤; 邓丽霜; 童红; 王强

    2013-01-01

    Six samples were pretreated by microwave digestion method and analyzed by inductively coupled plasma atomic emission spectrometry (ICP-AES). And 18 kinds of major/trace elements in Xinjiang Allium cepa L. seeds were determined including Co, Cr, Ca, K, Mg, P, Fe, Mn, Na, Ni, Sn, Zn, Cd, As,Se, Cu, Mo and V. Results indicated that Allium cepa L. seeds were riched in major elements such as K,Mg,P,Ca and Na, besides, the trace elements Fe, Mn,Zn,Cr,Ni,and Cu were also relatively abundant. Allium cepa L. seeds contain a lot of major and trace elements which are beneficial to human body and have high medicinal value.%采用微波消解法处理样品,以电感耦合等离子体原子发射光谱法(ICP AES)测定新疆洋葱籽样品中Co、Cr、Ca、K、Mg、P、Fe、Mn、Na、Ni、Sn、Zn、Cd、As、Se、Cu、Mo和V 18种常量/微量元素.结果显示,新疆洋葱籽中含有丰富的K、Mg、P、Ca和Na等常量元素,此外微量元素Fe、Mn、Zn、Cr、Ni、Cu的含量也较丰富.新疆洋葱籽中含有很多对人体有益的常量及微量元素,有较高的药用价值.

  11. Determination of eight impurity elements in industrial silicon by inductively coupled plasma atomic emission spectrometry%电感耦合等离子体原子发射光谱法测定工业硅中8种杂质元素

    Institute of Scientific and Technical Information of China (English)

    张云晖; 杨晓静; 亢若谷; 赵建为; 金波

    2013-01-01

    The inert sample injection system resistant hydrofluoric acid of inductively coupled plasma atomic emission spectrometer was used. The sample solution was injected directly without removing hydrofluoric acid and silicon matrix after sample was dissolved in hydrofluoric acid, nitric acid and perchloric acid. Eight impurities including iron, aluminum, calcium, titanium, manganese, nickel, boron and phosphorus in industrial silicon powder were simultaneously determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Most of matrix silicon had been volatilized and removed in sample dissolution process, so the matrix effect had no influence on the determination of i-ron, aluminum, calcium, titanium, manganese and nickel. However, the determination of boron and phosphorus was still affected, which could be eliminated by vertical observation method. The detection limit of the method was calculated by three times of standard deviation of blank. The detection limits (w/%) for iron, aluminum, calcium, titanium, manganese, nickel, boron and phosphorus were 0. 004, 0. 001, 0. 004, 0. 001, 0. 0001, 0. 0001, 0. 000 04 and 0. 000 06, respectively. The proposed method was applied to the determination of eight impurities in industrial silicon. The found results were consistent with the certified values or those obtained by standard method (GB/T 14849. 4-2008).%采用电感耦合等离子体原子发射光谱仪的耐氢氟酸惰性进样系统,在样品用氢氟酸、硝酸、高氯酸溶解完全后无需赶尽氢氟酸和硅基体,直接进样,电感耦合等离子体原子发射光谱法同时测定了工业硅粉中铁、铝、钙、钛、锰、镍、硼和磷8种杂质元素.因为在溶样过程中大部分基体硅已挥发除去,基体效应对铁、铝、钙、钛、锰、镍的测定没有影响,但是对硼和磷的测定仍有影响,这种影响可以采用垂直观测方式克服.按照空白值的3倍标准偏差计算方法的检测限,得到

  12. 电感耦合等离子体原子发射光谱法同时测定饮用水的硬度和碱度%Simultaneous determination of the hardness and alkalinity in drinking water by inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    霍建中; 段旭川

    2013-01-01

    The feasibility of simultaneous determination of hardness and alkalinity of drinking water by inductively coupled plasma atomic emission spectrometry (ICP-AES) was studied.the water sample was acidified off-line with diluted hydrochloric acid.The bicarbonates in water sample were in-situ converted into carbon dioxide,which was also dissolved in original water.Then,the solution was sampled by conventional single tube of inductively coupled plasma atomic emission spectrometer.The simultaneous sampling of CO2,Ca and Mg was realized at relatively low atomizer pressure.Among them,CO2 was sampled in gas state,while Ca and Mg were sampled in atomizing state.In this study,the bicarbonates with low sampling efficiency in atomizing method were converted into gas carbon dioxide,which had high sampling efficiency,thus the determination sensitivity of carbon was increased,realizing the accurate determination.The measured content of inorganic carbon was converted to the content of bicarbonates,so the alkalinity of drinking water was obtained.Meanwhile,the content of Ca and Mg was converted to the content of calcium carbonate to calculate the hardness of water.Under the optimal experimental conditions,i.e.,atomizer pressure of 241.3 kPa and dilution ratio of 5for water sample,the hardness and alkalinity of drinking water were simultaneously determined by this method.The found results were consistent with those obtained by titration method.%研究了使用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定饮用水的硬度和碱度可行性.通过用稀盐酸离线酸化水样,使水样中的碳酸氢根原位转化为二氧化碳并继续溶解在原水中,然后使用ICP-AES仪器上常规的单管吸取溶液,在比较低的雾化器压力下实现了CO2、Ca、Mg的同时进样.其中CO2属于气态进样,而钙、镁属于雾化进样.由于方法将雾化法进样效率低的碳酸氢根转化成进样效率高的二氧化碳气态,因此碳的测定灵敏

  13. Determination of Chromium,Zirconium,Vanadium and Hafnium in Polyethylene and Polypropylene by Inductively Coupled Plasma Atomic Emission Spectrometry%电感耦合等离子体原子发射光谱法测定聚乙烯、聚丙烯中铬、锆、钒和铪

    Institute of Scientific and Technical Information of China (English)

    陈金凤; 陈章捷; 钟坚海; 郑宗展

    2011-01-01

    采用微波消解技术对以聚乙烯、聚丙烯为原料制作的食品容器、食品包装薄膜进行预处理,确定了溶样酸介质及其用量、微波消解温度、时间等关键因素,建立了一种快速测定聚乙烯、聚丙烯材料中铬、锆、钒和铪含量的电感耦合等离子体原子发射光谱法。实验结果表明,5mL硝酸和1mL过氧化氢的混合溶液即可实现样品的完全消解,同时通过优化光谱分析条件,得到铬、锆、钒和铪的检测限分别为1.0 mg/kg,0.7mg/kg,0.7 mg/kg,1.4 mg/kg。该法加标回收率在88%-103%之间,相对标准偏差(n=3)为0.84-6.4%。用于实际样品的测定,所得结果与标准样品的参考值相符。%A method for the rapid determination of chromium,zirconium,vanadium and hafnium in polyethylene and polypropylene by inductively coupled plasma atomic emission spectrometry was established.The samples made of polyethylene and polypropylene used as food container or food wrapper was pretreated by microwave digestion.The effects of digestion media and it's use amount,digestion temperature and holding time on digestion results were investigated.It was experimentally indicated that the samples could be thoroughly digested in a mixture of 5 mL of nitric acid and 2 mL of hydrogen peroxide.Under the optimal conditions,the detection limits of chromium,zirconium,vanadium and hafnium were 1.0 mg/kg,0.7 mg/kg,0.7 mg/kg and 1.4 mg/kg respectively.The recoveries of standards in polyethylene and polypropylene samples were from 88% to 103%,with the RSDs of 0.84%-6.4%(n=3).This method was employed in the determination of real samples,the analytical results was accorded with the certified results.

  14. 碱熔融电感耦合等离子体原子发射光谱法测定生铁中硅锰磷含量%Determination of Silicon Manganese and Phosphorus in Pig Iron with Inductively Coupled Plasma Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    吴金龙; 金献忠

    2014-01-01

    A method was proposed for the determination of silicon, manganese, and phosphorus in pig iron with inductively coupled plasma atomic emission spectrometry . Samples were fused with sodium hydroxide and sodium peroxide in zirconium crucibles and leached out with hydrochloric acid solution. The matrix effect were investigated, no effect on the measured elements by sodium between 5.0 mg/mL and 6.0 mg/mL, zirconium in 20μg/mL and other elements in pig iron was found. Acidity effect was discussed and the effect of the volume of hydrochloric acid between 8 percent and 12 percent was able to be ignored. CRMs of pig iron were analyzed, and good agreements were achieved on the detected levels and the certified values with RSDs (n=5) being in the range of 0.3%-1.0%.%提出了一种电感耦合等离子体原子发射光谱法测定生铁中硅、锰、磷含量的方法。生铁样品采用氢氧化钠和过氧化钠在锆坩埚内熔融,盐酸浸取;研究了共存元素的影响,浓度在5.0 mg/mL-6.0 mg/mL之间的钠元素、20μg/mL的锆元素以及样品中其他共存元素对各元素的测定结果无影响;考察了酸度效应,盐酸用量在体积分数8%-12%时,对各元素测定的影响可以忽略。以生铁标准物质作为样品进行分析,测定值和认定值相吻合,RSD(n=5)为0.3%-1.0%。

  15. 碱熔—电感耦合等离子体原子发射光谱法测定红土镍矿中硅钙镁铝锰钛铬镍钴%Determination of silicon, calcium, magnesium, aluminium, manganese,titanium, chromium, nickel and cobalt in laterite nickel ore by alkali fusion-inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    高亮

    2013-01-01

    The determination method of nine elements (silicon, calcium, magnesium, aluminium, manganese, titanium, chromium, nickel and cobalt) in laterite nickel ore by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The laterite nickel ore sample was fused by anhydrous Na2CO3-H3BO3 mixed flux, then acidified and leached by hydrochloric acid. The high salt atomizer and cyclone chamber were used. Under the selected measurement conditions, the content of nine elements in sample solution was determined by ICP-AES. The influence of salts introduced by matrix iron and sample treatment could be eliminated by matrix matching method. The precision test results showed that, the relative standard deviations (RSD) of elements were smaller than 5 %. The proposed method was applied to the determination of reference material, and the determination results of nine elements were basically consistent with the certified values.%建立了红土镍矿中Si、Ca、Mg、Al、Mn、Ti、Cr、Ni、Co 9种元素的电感耦合等离子体原子发射光谱测定方法.红土镍矿样品用无水Na2CO3-H3BO3混合熔剂熔融,盐酸浸取、酸化,选用高盐雾化器和旋流雾室,在选定的测量条件下,用电感耦合等离子体原子发射光谱法测定试液中9种元素含量.基体铁和处理样品时引入试液中的盐分对测定的影响可以通过基体匹配的方法消除.精密度试验结果表明,样品中各元素测定结果的相对标准偏差小于5%.用本法测定标准样品,9种元素的测定值与认定值基本一致.

  16. Affirmation of the Method that Simultaneous Determination of Copper, Lead, Zinc, Cobalt and Nickel in Copper, Lead and Zinc Ores by Inductively Coupled Plasma-Atomic Emission Spectrometry%电感耦合等离子体发射光谱法同时测定铜铅锌矿石中铜铅锌钴镍等元素方法确认

    Institute of Scientific and Technical Information of China (English)

    熊英; 王晓雁; 胡建平

    2011-01-01

    文章在修订GB/T 14353-1993研究工作中,建立了电感耦合等离子体发射光谱同时测定铜铅锌矿石中铜铅锌钴镍等元素的标准分析方法.通过控制试样量和制备试样溶液的体积,可实现主量元素铜、铅、锌与次量元素钴、镍的同时测定.测定范围为铜0.002%~8.5%,铅0.01%~5%,锌0.005%~3%,钴0.001 5%~0.5%,镍0.003%~0.5%.按照相关国家标准对测量方法与结果的准确度进行8个实验室协同参加的准确度试验,统计参数结果表明在限定水平范围内方法偏倚不显著;利用方法重复性限参数,计算可能产生的最大相对偏差.分析方法精密度满足的要求.%A standard analysis method for simultaneous detecting copper, lead, zinc, cobalt, nickel and other elements by inductively coupled plasma-atomic emission spectrometry (ICP-AES) was developed when improving GB/T 14353-1993 , the method for chemical analysis of copper ore, lead ore and zinc ore. The major elements such as copper, lead, zinc and the minor elements of cobalt and nickel can be simultaneous detected by adjusting the test portion amounts and reagent solution volumes. The determination ranges of copper, lead, zinc, cobalt and nickel are respectively 0.002% -8.5% , 0. 01% - 5% , 0. 005% - 3% , 0. 001 5% - 0. 5% and 0. 003% - 0. 5%. According to relevant national standards, this method was tested by eight cooperation laboratories. Statistical results indicated that the method is impartial within a definitive range. The repeatability limit parameter was used to calculate the possible maximum deviations. The precision of the method satisfied the requirement of "The specification of testing quality management for geological laboratoris".

  17. 电感耦合等离子体发射光谱法测定红土镍矿中镍钻铜%Determination of Ni, Co and Cu in Laterite-Nickel Ores by Inductively Coupled Plasma-Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    王国新; 许玉宇; 王慧; 刘烽; 吴骋; 胡清

    2011-01-01

    A method for the determination of Ni, Co and Cu contents in laterite is presented in this paper. Laterite samples were fused with a mixed flux of Na2CO3-Na2B4O7, then the analytes were extracted by HC1 acid. The sample solution was measured by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The internal standard method was used to avoid matrix interference based on choosing Y 371. 030 nm as the internal calibration line for Cu (324.754 nm) and Y 224.306 nm for Ni (231.604 nm) and Co (228.616 nm). The detection limits for Ni, Co and Cu were 0. 5 μg/g, 1.0 μg/g and 1.0 μg/g, respectively. The relative standard deviations (RSD) of the test result were 1. 2% -2. 0% (n =7) , and the recoveries ranged from 95% to 103.6%, which met the requirements of analysis for laterite.%红土镍矿样品用无水Na2 CO3 - Na2 B4 O7混合熔剂熔融,HCl浸出酸化,电感耦合等离子体发射光谱法直接测定样品中镍、钴、铜的含量.Cu 324.754 nm使用Y 371.030 nm作为内标线,Ni 231.604 nm、Co 228.616 nm使用Y 224.306 nm作为内标线校正基体干扰,方法检出限镍为0.5μg/g、钴为1.0 μg/g、铜为1.0μg/g,相对标准偏差( RSD,n=7)为1.2% ~2.0%,加标回收率为95.0% ~ 103.6%,能满足红土镍矿的分析要求.

  18. Methods of Cold Soaking, Foam Plastics Enrichment and Inductive Coupling Plasma Atomic Emission Spectrometry%冷浸取--泡塑富集-电感耦合等离子体发射光谱法测定化探样品中的超痕量金铂钯研究

    Institute of Scientific and Technical Information of China (English)

    闵慧英; 袁蕙霞; 郭玉翠

    2015-01-01

    建立了冷浸--泡沫塑料富集,采用 ICP-AES 测定地球化学勘探样品中超痕量金、铂、钯的方法,并试验了冷浸取、泡沫塑料富集时各种因素的影响;确定了采用氯化钠、盐酸和高锰酸钾冷浸取分解试样,以泡沫塑料富集、灰化,残渣用王水溶解,用电感耦合等离子体发射光谱法测定的条件。该方法检出限分别为:Au 0.039ng/g,Pt 0.040ng/g,Pd 0.058ng/g;回收率为95.6%~102.5%之间;测量精密度( RSD%)为:Au 4.85%,Pt 5.76%,Pd 6.45%。采用该方法测定了国家一级地球化学标准物质中的痕量 Au,Pt,Pd,测定值与标准值符合规范要求。%In this paper, we set up the enrichment of cold soaking foam plastics by adopting the method of ICP-AES to test the ultra-trace of gold, platinum and palladium from the geochemical exploration sample and studied all kinds of effective factors in cold soaking foam plastics enrichment. And we confirmed the requirements of using sodi-um chloride, hydrochloric acid and potassium permanganate cold soak-ing to decompose the sample, using foam plastics to enrich and ash, aqua regia to dissolve residue, and measuring by inductive coupling Plasma Atomic Emission Spectrometry. The detection limits of this method are as follows: detection limit: Au 0.039ng/g, Pt 0.040ng/g, Pd 0.058ng/g; recovery rate: between 95.9% and 102.2%; relative stan-dard deviation (RSD%): Au 4.85%,Pt 5.76%,Pd 6.45%.We tested the trace amount of Au, Pt and Pd in the country-level geochemistry stan-dard substance. The measured value is consistent with the normalized value.

  19. 电感耦合等离子体原子发射光谱法测定镍基钎焊料中铬和硅%Determination of chromium and silicon in nickel-based brazing material by inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    杨丽; 王金阳; 张庸

    2013-01-01

    The analysis conditions of chromium and silicon in nickel-based brazing material by inductively coupled plasma atomic emission spectrometry (ICP-AES) were discussed.After the nickelbased brazing material was dissolved with aqua regia-hydrofluoric acid mixed acid,and matrix effect was reduced by matrix matching,chromium and silicon in the sample were determined by ICP-AES with spectral line of 267.716(125) nm and 251.612(133) nm as the analytical lines for chromium and silicon respectively.This proposed method was applied to the determination of chromium and silicon in actual samples and the results were consistent with those obtained by ammonium persulfate oxidization titration method and perchloric acid dehydration method.The relative standard deviation (RSD,n =6) of chromium and silicon was 0.55%-0.73% and 0.71%-1.0%,respectively.The recoveries were 100%-101% and 99%-100%,respectively.%探讨了电感耦合等离子体原子发射光谱法(ICP-AES)测定镍基钎焊料中铬和硅的分析条件.试样经王水和氢氟酸混合酸溶解,选择267.716(125) nm和251.612(133) nm的光谱线分别作为铬和硅的分析线,并采用基体匹配法降低了基体效应,ICP-AES测定了镍基钎焊料中铬和硅含量.实际样品中铬和硅的测定结果与过硫酸铵氧化滴定法和高氯酸脱水法相符,铬和硅的相对标准偏差(n=6)分别为0.55%~0.73%和0.71%~1.0%,加标回收率分别为100%~101%和99%~100%.

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

    Energy Technology Data Exchange (ETDEWEB)

    Perring, Loic; Basic-Dvorzak, Marija [Department of Quality and Safety Assurance, Nestle Research Centre, P.O. Box 44, Vers chez-les-Blanc, 1000, Lausanne (Switzerland)

    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. (orig.)

  1. 碱熔-电感耦合等离子体发射光谱法测定大气颗粒物样品中无机元素%Quantification of Inorganic Elements in Aerosol Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry with Alkali Melting

    Institute of Scientific and Technical Information of China (English)

    付爱瑞; 陈庆芝; 罗治定; 姜云军; 金倩; 王芸

    2011-01-01

    大气颗粒物(TSP和PM10)中Si、Al、Ca、Mg、K、Fe、Na等元素含量较高,是颗粒物源分析的指示性元素.目前分析大气颗粒物样品中无机元素的方法有中子活化分析法、X射线荧光光谱法、微波消解(或高压釜消解)电感耦合等离子体发射光谱法和电感耦合等离子体质谱法.本文建立了碱熔-电感耦合等离子体发射光谱法测定大气颗粒物样品中Si、Al、Ca、Mg、Fe、Ti、Ba、Sr、Zr等无机元素的分析方法,样品于镍坩埚中530~550℃灰化60 min后用NaOH融熔,水提取,再用2 mL 50%的HCl酸化,钠基体匹配消除干扰,解决了大气颗粒物滤膜样品中Si易产生的溶解不完全等问题,提高了Ti、Ba、Sr、Zr等主、次量元素测定的精密度和准确度.讨论了坩埚和熔剂的选择、灰化温度、灰化时间、酸度、干扰等影响因素.在选定条件下,测定结果相对误差(RE)﹤4%,相对标准偏差(RSD,n=12)﹤5%,检出限为0.0047~1.2 ng/g.方法所需设备简单,分析成本低,快速简便,精密度好,准确度高,适宜批量样品的测定.%In atmospheric particles ( TSP and PM10 ), the high contents of some inorganic elements including Si, Al, Ca, Mg, K, Fe and Na are the proxy elements for the particles source analysis. At present, there are several methods to analyze inorganic elements for atmospheric particles such as neutron activation analysis, X-ray Fluorescence Spectrometry ( XRF ), Inductively Coupled Plasma-Atomic Emission Spectrometry ( ICP-AES ) and Inductively Coupled Plasma-Mass Spectrometry ( ICP-MS ) after dissolving by microwave ( or high-pressured cauldron ). The established method for determining Si, Al, Ca, Mg, Fe, Ti, Sr, Ba and Zr in aerosols by ICP-AES with alkali melting solved the problems of incomplete dissolving for Si caught in an atmospheric particles filter diaphragm, and improved the precision and accuracy of the determinations of major and trace elements such as Ti, Ba, Sr, Zr. In

  2. Separation of gold, palladium and platinum in chromite by anion exchange chromatography for inductively coupled plasma atomic emission spectrometric analysis

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Kwang Soon; Lee, Chang Heon; Park, Yeong Jae; Joe, Kih Soo; Kim, Won Ho [KAERI, Taejon (Korea, Republic of)

    2001-08-01

    A study has been carried out on the separation of gold, iridium, palladium, rhodium, ruthenium and platinum in chromite samples and their quantitative determination using inductively coupled plasma atomic emission spectrometry (ICP-AES). The dissolution condition of the minerals by fusion with sodium peroxide was optimized and chromatographic elution behavior of the rare metals was investigated by anion exchange chromatography. Spectral interference of chromium, a matrix of the minerals, was investigated on determination of gold. Chromium interfered on determination of gold at the concentration of 500 mg/L and higher. Gold plus trace amounts of iridium, palladium, rhodium and ruthenium, which must be preconcentrated before ICP-AES was separated by anion exchange chromatography after reducing Cr(VI) to Cr(III) by H{sub 2}O{sub 2}. AuCl{sup -}{sub 4} retained on the resin column was selectively eluted with acetone- HNO{sub 3}-H{sub 2}O as an eluent. In addition, iridium, palladium, rhodium and ruthenium remaining on the resin column were eluted as a group with concentrated HCl. However, platinum was eluted with concentrated HNO{sub 3}. The recovery yield of gold with acetone-HNO{sub 3}-H{sub 2}O was 100.7 {+-} 2.0 % , and the yields of palladium and platinum with concentrated HCl and HNO{sub 3} were 96.1 {+-} 1.8% and 96.6 {+-} 1.3%, respectively. The contents of gold and platinum in a Mongolian chromite sample were 32.6 {+-} 2.2 {mu}g/g and 1.6 {+-} 0.14 {mu}g/g, respectively. Palladium was not detected.

  3. Determination of elements in tea seeds by inductively coupled plasma atomic emission spectrometry%电感耦合等离子体发射光谱(ICP-OES)法快速测定茶叶籽中多种元素

    Institute of Scientific and Technical Information of China (English)

    董海胜; 臧鹏; 王妮; 黄贱英

    2014-01-01

    Objective To analyze the etal elements in tea seed, so as to provide a reference for tea seed utilization. Methods Rapid quantitative analysis for elements As, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Pb, Se and Zn in tea seeds was carried out by the high-pressure sealed microwave digestion combined with inductively coupled plasma atomic emission spectrometry. Results The content of each element in tea seed were as fol-lowing:Mg (1652.23 mg/kg), Ca (1 026.36 mg/kg), Mn (122.44 mg/kg), Na (37.77 mg/kg) , Cr (7.58 mg/kg), Cu (9.11 mg/kg), Fe (58.17 mg/kg), Zn (17.59 mg/kg) and K (9191.29 mg/kg), while, As, Cd, Pb and Se were not detected. Method recoveries for all the elements used in this research were between 89%and 113%. Con-clusion The method established in this research satisfies the analysis requirements of element in tea seed. Contents of potassium, magnesium and calcium are of high lever in tea seed, while sodium content is relatively low. Tea seed is rich in minor elements such as manganese, iron, zinc and chromium.%目的:对茶叶籽中金属元素进行分析,为茶叶籽综合利用提供参考。方法采用高压密闭微波消解结合电感耦合等离子体发射光谱法对茶叶籽中As、Ca、Cd、Cr、Cu、Fe、K、Mg、Mn、Na、Pb、Se及Zn等元素进行了同时快速定量分析。结果茶叶籽中各元素含量: Mg(1652.23 mg/kg)、Ca(1026.36 mg/kg)、Mn(122.44 mg/kg)、Na(37.77 mg/kg)、Cr(7.58 mg/kg)、Cu(9.11 mg/kg)、Fe(58.17 mg/kg)、Zn(17.59 mg/kg)、K (9191.29 mg/kg)。As、Cd、Pb及Se未检出。方法加标回收率89%~113%。结论此方法满足茶叶籽样品中所述元素的分析要求。茶叶籽中钾、镁及钙含量较高,钠含量相对较低;锰、铁、锌及铬元素含量丰富。

  4. Determination of platinum and palladium in copper leaching residue by inductively coupled plasma atomic emission spectrometry with lead fire assaying%铅试金-电感耦合等离子体原子发射光谱法测定铜浸出渣中铂钯

    Institute of Scientific and Technical Information of China (English)

    魏巍; 柴徐彬

    2015-01-01

    Platinum and palladium in copper leaching residue were captured into gold-silver composite granule by lead fire assaying method. Then, the gold-silver composite granule was dissolved with nitric acid (1+7). After the solution was pouring out, the residues were dissolved with aqua regia(1+1). Merging the solutions above, the hy-drochloric acid (1+1) was added to precipitate the silver. After filtration, the content of platinum and palladium in filtrate was determined. Thus, a method was established for determination of platinum and palladium in copper leaching residue by inductively coupled plasma atomic emission spectrometry ( ICP-AES) . The interference tests of gold and silver in gold-silver composite granule indicated that the absorption of platinum and palladium by silver chloride precipitate could be eliminated through continuous stirring in precipitation process. Meanwhile, gold in so-lution had no interference with the determination. The proposed method was applied to the determination of copper leaching residue actual samples. The relative standard deviations of the results (RSD, n=11) were 5. 6%-9. 7%, and the recoveries were between 94% and 104%. The content of platinum and palladium in control samples of cop-per leaching residue was determined by proposed method. The results were consistent with the reference values.%采用铅试金法将铜浸出渣中的铂和钯捕集于金银合粒中,用硝酸(1+7)溶解金银合粒,倾出硝酸溶解液,用王水(1+1)溶解剩余的残渣,合并两次溶解液,加入盐酸(1+1)沉淀银,过滤,对溶液中铂和钯进行测定,建立了电感耦合等离子体原子发射光谱法( ICP-AES )测定铜浸出渣中铂和钯的分析方法。金银合粒中金和银的干扰试验表明:在沉淀过程中不断搅拌可消除氯化银沉淀对铂和钯吸附的影响,同时溶液中的金对测定不产生干扰。方法用于铜浸出渣实际样品分析,测得结果的相对标准偏差(RSD,n=11)为5.6%~9.7%,

  5. 电感耦合等离子体发射光谱法测定镍矿石中镍铝磷镁钙%Determination of Ni, AI, P, Mg and Ca in Nickel Ores by Inductively Coupled Plasma-Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    张超; 李享

    2011-01-01

    The simultaneous determination of Ni, Al, P, Mg, and Ca in nickel ores by inductively coupled plasma atomic emission spectrometry (ICP-AES) has been developed and is described in this paper. The sample was dissolved in nitric acid with hydrofluoric acid as flux. Perchloric acid was added and heated in order to remove hydrofluoric acid. After dissolving the salts with hydrochloric, Ni, Al, P, Mg and Ca were determined by ICP-AES. The selected spectral lines forNi, Al, P, Mg and Ca were 221. 6 nm, 396.1 nm, 178. 2 nm, 285. 2 nm and 393. 3 nm, respectively. The matrix effect was corrected by adding the same amount of Fe as the measured sample into the standard curve. The recoveries were 98. 00% -100.50%. The precisions of Ni, Al, P, Mg and Ca were all less than 1 % and the detection limits were 0. 0054 μg/mL, 0. 0028 μg/mL, 0. 0060 μg/mL, 0. 0030 μg/mL and 0. 0013 μg/mL, respectively. Compared with other methods, this method increased sensitivity and decreased the detection limit. It was applied to the determination of nickel ores from Indonesia, and the measured results were consistent with the standard values and RSD was below 1 % ( n = 6 ).%样品用硝酸溶解,氢氟酸助溶,高氯酸冒烟除去氢氟酸,盐酸溶解盐类后,在选定的测量条件下用电感耦合等离子体发射光谱法( ICP - AES)测定镍矿中镍、铝、磷、镁、钙.选择Ni 221.6 nm、Al 396.1nm、P 178.2 nm、Mg 285.2 nm、Ca 393.3 nm分别作为镍、铝、磷、镁、钙的分析线;通过在标准曲线中加入与待测样品等量的铁,消除基体干扰的影响.方法回收率为98.0% ~ 100.5%,镍、铝、磷、镁、钙的精密度均小于1%,检出限分别为0.0054、0.0028、0.0060、0.0030、0.0013 μg/mL.与同类ICP - AES方法比较,本法灵敏度提高,检出限降低.方法用于测定印度尼西亚的两批次镍矿石样品,结果与化学法的测定值基本一致,相对标准偏差小于1%(n=6).

  6. Determination of Cr, V and P in Ilmenite by Inductively Coupled Plasma-Atomic Emission Spectrometry with Sodium Peroxide Fusion%过氧化钠碱熔-电感耦合等离子体发射光谱法测定钛铁矿中铬磷钒

    Institute of Scientific and Technical Information of China (English)

    王卿; 赵伟; 张会堂; 周长祥; 回寒星

    2012-01-01

    An analytical method for the determination of trace elements of Cr, P and V in ilmenite with sodium peroxide by Inductively Coupled Plasma-Atomic Emission Spectrometry ( ICP-AES ) is proposed. The sample was digested by sodium peroxide fusion following which, the clear top solution was acidized to measure Cr, P and V by ICP-AES. The optimum instrumental conditions and selection of spectral lines for the elemental analysis were studied. The large dilution of 1000 and calibration standard solution by adding sodium as the matrix were conducted to eliminate the matrix effect. 2 mL HC1 was loaded to acidize the sample solution in order to avoid eroding the machines sampling system by the strong basicity of the solution by sodium peroxide fusion. The detection limit of this method was 4.46 -23.55 fig/g. According to the validation by national standard materials, the accuracy of the method (relative error) was less than 10% , and precision (RSD, n = 12) was 0.68% to 9. 90%. Compared with the spectrophotometer method for single element determination, this method showed many advantages, such as a low detection limit, high sensitivity, a wide measuring range, convenient operation, and was suitable for batch samples.%样品经过氧化钠碱熔,溶解后的上层清液直接酸化,用电感耦合等离子体发射光谱测定钛铁矿中铬、磷、钒的含量.确定了钛铁矿石中Cr、P、V的分析谱线、光谱级次;为了消除钠盐基体的影响,确定稀释因子为1000,标准曲线基体与样品基体保持一致;为避免过氧化钠熔矿后溶液碱性较大对选样系统造成腐蚀,加入2.00 mL盐酸对溶液进行酸化.方法检出限为4.46 ~23.55μg/g,采用国家一级标准物质进行验证,方法准确度小于10%,精密度为0.68%~9.90%.本法与分光光度法单一元素测定相比较,具有测量范围宽、结果准确、操作简便、省时省力、适合大批量样品测定等突出的优点.

  7. Determination of Fe_2O_3,TiO_2 and SiO_2 in bauxite by inductivelycoupled plasma-atomic emission spectrometry%ICP-AES法测定矾土中Fe2O3、TiO2和SiO2

    Institute of Scientific and Technical Information of China (English)

    郝荷芳; 苑利

    2011-01-01

    采用四硼酸锂熔融试样,电感耦合等离子体原子发射光谱法(ICP-AES法)测定矾土中Fe2 O3、TiO2和SiO2。通过对熔样方法选择、铝基体以及背景的研究,确定了分析条件。结果表明,该法具有良好的精密度和准确性,回收率在94%~108%。%A method based on inductively coupled plasma-atomic emission spectrometry(ICP-AES) was established for the determination of Fe2O3,TiO2 and SiO2 in bauxite.The sample was melted into lithium tetraborate.The analysis conditions were obtained by studying the melted methods,Al matrix and background.The recommended method showed satisfying precision and accuracy as well.The recovery percents detected by standard addition method were in range of 94%~108%.

  8. Determination of cobalt, nickel, iron, niobium, tantalum, vanadium and chrome in tungsten-based hard alloy by microwave digestion-inductively coupled plasma atomic emission spectrometry%微波消解-电感耦合等离子体原子发射光谱法测定钨基硬质合金中钴镍铁铌钽钒铬

    Institute of Scientific and Technical Information of China (English)

    成勇; 彭慧仙; 袁金红; 胡金荣

    2013-01-01

    以硝酸和磷酸(V(HNO3)∶V(H3PO4)=5∶1)作为消解试剂,采取高压密闭微波加热方法对钨钴或钨镍类钨基硬质合金样品进行消解,消解液用水定容后直接以电感耦合等离子体原子发射光谱法(ICP-AES)测定0.005%~10% Co、Ni和0.005%~1% Fe、Nb、Ta、V、Cr、Mo的含量.考察了消解试剂中的硝酸和磷酸量对试样消解的影响以及微波控制参数等最佳消解条件,建立了微波消解-无机试剂络合基体钨的样品消解方法,从而避免了因钨酸沉淀析出而导致部分待测元素损失和使用有机络合剂对光谱测定的干扰影响.实验结果表明:采用以5 min升温至130℃并保持5 min,再以5 min升温至190℃并保持15 min的消解程序,样品的消解效果较好.试验通过优选元素分析谱线,基体匹配和同步背景校正法消除了高钨基体的影响和光谱干扰,确保了方法的可靠性.背景等效浓度值从5 μg/L (Nb)至18 μg/L(Fc),元素检出限从4 μg/L (Nb)至13 μg/L (Fe).方法用于钨基硬质合金样品中上述合金或杂质元素的测定,RSD<3%,加标回收率在97%~104%之间,测定结果与国家标准方法检测结果对照一致.%The tungsten-based hard alloy samples (such as tungsten-cobalt and tungsten-nickel) were digested by high pressure closed microwave heating method using nitric acid-phosphoric acid (V(HNO3) : V(H3PO4)=5 :1) as digestion reagent. After dilution with water, the content of Co, Ni (0.005%-10%), Fe, Nb, Ta, V, Cr and Mo (0. 005%-l%) in digestion solution was directly determined by microwave digestion-inductively coupled plasma atomic emission spectrometry (ICP-AES). The effect of nitric acid and phosphoric acid concentration on sample digestion was investigated. The optimal digestion conditions such as microwave control parameters were studied. The sample digestion method by microwave digestion was established. The matrix tungsten was complexed with inorganic reagents

  9. 超声辅助萃取-电感耦合等离子体原子发射光谱仪联用同时测定水样中多种金属离子%Simultaneous determination of metal ions in water samples by ultrasound-assisted extraction coupled with inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    宋杨; 孟楚桥; 朱田; 高庆历; 聂红霞; 谭彩云; 祁艳霞; 赵前程

    2015-01-01

    目的:优化超声辅助乳化萃取结合电感耦合等离子体(inductively coupled plasma, ICP)原子发射法,同时测定水样中镉、钴、镍、锌4种金属离子。方法采用吡咯烷二硫代氨基甲酸铵(APDC)溶液作为螯合剂,超声条件下采用二氯甲烷对重金属螯合物进行萃取。优化了缓冲液的 pH 值,测定了不同加标浓度下方法的回收率。并对自来水、矿泉水、海水等水样进行了测定。结果该方法对Cd、Co、Ni、Zn 4种金属离子在200μg/L加标条件下绝对回收率为27.0%~91.0%,检出限为Cd为0.81μg/L, Co为1.03μg/L, Ni为1.28μg/L, Zn为0.14μg/L。检测实际自来水样,镉、钴、镍、锌4种金属离子相对回收率分别为96.4%、77.4%、120.2%、85.6%,所测自来水中镉、钴、镍、锌4种金属含量分别为1μg/L、0μg/L、2μg/L和146μg/L,均符合国标要求。对矿泉水中镉、钴、镍的相对回收率分别为77.8%,89.9%和74.2%。矿泉水中没有检测到镉、钴两种金属离子,镍含量为1μg/L。结论该方法适合于自来水和矿泉水中部分金属离子的测定,不适合于对海水中金属离子的测定。%Objective To optimize the ultrasonic-assisted emulsification extraction combined with inductively coupled plasma atomic emission spectrometry (ICP-OES) in order to determinate the concentration of cadmium, cobalt, nickel and zinc in water simultaneously.MethodsAmmonium pyrrolidinedithio carbamate (APDC) was used as a chelating agent, and dichloromethane was used as the extraction reagent of the heavy metal chelating ultrasonic extraction. The pH of the buffer was optimized, and the recovery of every metal ion was measured at different spiked concentration. And the concentration of metal ions in tap water, mineral water and sea water were determined. Results The absolute recovery of Cd, Co, Ni, Zn 4 kinds of metal ions in 200 μg/L spiked conditions were between 27.0%~91.0%, and the detection limits of method were Cd 0

  10. Zinc, lead and copper in human teeth measured by induced coupled argon plasma atomic emission spectroscopy (ICP-AES)

    Energy Technology Data Exchange (ETDEWEB)

    Chew, L.T.; Bradley, D.A. E-mail: D.A.Bradley@exeter.ac.uk; Mohd, Y.; Jamil, M

    2000-11-15

    Inductively Coupled Argon Plasma Atomic Emission Spectroscopy (ICP-AES) has been used to determine Pb, Zn and Cu levels in 47 exfoliated human teeth (all of which required extraction for orthodontic reasons). Lead concentrations for the group were 1.7 {mu}g (g tooth mass){sup -1} to 40.5 {mu}g (g tooth mass){sup -1}, with a median of 9.8 {mu}g (g tooth mass){sup -1}. A median lead level in excess of the group value was found for the teeth of six lorry drivers who were included in the study. A more significant enhancement was found for the seven subjects whose age was in excess of 60 years. The median values for Zn and Cu were 123.0 and 0.6 {mu}g (g tooth mass){sup -1} respectively. Present values for tooth-Zn are lower than published data for other ethnic groups.

  11. Determination of some inorganic metals in edible vegetable oils by inductively coupled plasma atomic emission spectroscopy (ICP-AES

    Directory of Open Access Journals (Sweden)

    Musa Özcan, M.

    2008-09-01

    Full Text Available Seventeen edible vegetable oils were analyzed spectrometrically for their metal (Cu, Fe, Mn, Co, Cr, Pb, Cd, Ni, and Zn contents. Toxic metals in edible vegetable oils were determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES. The highest metal concentrations were measured as 0.0850, 0.0352, 0.0220, 0.0040, 0.0010, 0.0074, 0.0045, 0.0254 and 0.2870 mg/kg for copper in almond oil, for iron in corn oil-(c, for manganese in soybean oil, for cobalt in sunflower oil-(b and almond oil, for chromium in almond oil, for lead in virgin olive oil, for cadmium in sunflower oil-(e, for nickel almond oil and for zinc in almond oil respectively. The method for determining toxic metals in edible vegetable oils by using ICP-AES is discussed. The metals were extracted from low quantities of oil (2-3 g with a 10% nitric acid solution. The extracted metal in acid solution can be injected into the ICPAES. The proposed method is simple and allows the metals to be determined in edible vegetable oils with a precision estimated below 10% relative standard deviation (RSD for Cu, 5% for Fe, 15% for Mn, 8% for Co, 10% for Cr, 20% for Pb, 5% for Cd, 16% for Ni and 11% for Zn.En este estudio se analizó espectrométricamente el contenido en metales (Cu, Fe, Mn, Co, Cr, Pb, Cd, Ni, and Zn de 17 aceites vegetales comestibles mediante ICP-AES. Las concentaciones más elevadas se encontraron para el cobre en el aceite de almendra (0.0850 mg/kg, para el hierro en el aceite de maiz(c,(0.0352 mg/kg, para el manganeso en el aceite de soja (0.0220 mg/kg, para el cobalto en el aceite de girasol (b (0.0040 mg/kg, para el cromo en el aceite de almendra (0.0010 mg/kg, para el plomo en el aceite de oliva virgen (0.0074 mg/kg, para el cadmio en el aceite de girasol (e (0.0045 mg/kg, para el niquel en el aceite de almendra (0.0254 mg/kg y para el zincen el aceite de almendra (0.2870 mg/kg. Los metales se extrajeron a partir de bajas cantidades de aceite (2-3 g, con

  12. Comparative measurements of mineral elements in milk powders with laser-induced breakdown spectroscopy and inductively coupled plasma atomic emission spectroscopy.

    Science.gov (United States)

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

    2011-07-01

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

  13. Fingerprinting of complex mixtures with the use of high performance liquid chromatography, inductively coupled plasma atomic emission spectroscopy and chemometrics

    Energy Technology Data Exchange (ETDEWEB)

    Ni Yongnian [Department of Chemistry, Nanchang University, Nanchang, Jiangxi 330047 (China)], E-mail: ynni@ncu.edu.cn; Peng Yunyan [Department of Chemistry, Nanchang University, Nanchang, Jiangxi 330047 (China); Kokot, Serge [Inorganic Materials Program, School of Physical and Chemical Sciences, Queensland University of Technology, Brisbane, Queensland 4001 (Australia)

    2008-05-26

    The molecular and metal profile fingerprints were obtained from a complex substance, Atractylis chinensis DC-a traditional Chinese medicine (TCM), with the use of the high performance liquid chromatography (HPLC) and inductively coupled plasma atomic emission spectroscopy (ICP-AES) techniques. This substance was used in this work as an example of a complex biological material, which has found application as a TCM. Such TCM samples are traditionally processed by the Bran, Cut, Fried and Swill methods, and were collected from five provinces in China. The data matrices obtained from the two types of analysis produced two principal component biplots, which showed that the HPLC fingerprint data were discriminated on the basis of the methods for processing the raw TCM, while the metal analysis grouped according to the geographical origin. When the two data matrices were combined into a one two-way matrix, the resulting biplot showed a clear separation on the basis of the HPLC fingerprints. Importantly, within each different grouping the objects separated according to their geographical origin, and they ranked approximately in the same order in each group. This result suggested that by using such an approach, it is possible to derive improved characterisation of the complex TCM materials on the basis of the two kinds of analytical data. In addition, two supervised pattern recognition methods, K-nearest neighbors (KNNs) method, and linear discriminant analysis (LDA), were successfully applied to the individual data matrices-thus, supporting the PCA approach.

  14. Elemental Content in Brown Rice by Inductively Coupled Plasma Atomic Emission Spectroscopy Reveals the Evolution of Asian Cultivated Rice

    Institute of Scientific and Technical Information of China (English)

    Yawen Zeng; Luxiang Wang; Juan Du; Jiafu Liu; Shuming Yang; Xiaoying Pu; Fenghui Xiao

    2009-01-01

    The phylogenetic relationship for classification traits and eight mineral elements in brown rice (Oryza sativa L.) from Yunnan Province in China was carried out using microwave assisted digestion followed by inductively coupled plasma atomic emission spectroscopy, and the analytical procedures were carefully controlled and validated. In general, the results show that the mean levels of K, Ca, Mg, Fe and Cu in brown rice for 789 accessions of rice landraces was distinctly lower than that of improved cultivars. They further demonstrate that Ca plays an important role in the differentiation of subspecies indica-japonica, especially to enhance adaptation of cold stress, and that five mineral elements in brown rice enhance the eurytopicity from landrace to improved cultivar. Hierarchical cluster analysis, using average linkage from SPSS software based on eight mineral elements in brown rice, showed that Yunnan rice could be grouped into rice landrace and improved cultivar, with the rice landrace being further clustered into five subgroups, and that, interestingly, purple rice does not cluster with either of the groups. Our present data confirm that indica is the closest relative of late rice and white rice, and that they constitute rice landraces together, whereas japonica is the closest relatives of non-nuda, early-mid and glutinous rice. It is further shown that japonica, non-nuda, early-mid, glutinous, white and red rice might be more primitive than indica, nuda, late, non-glutinous and purple rice, respectively.

  15. Standard test method for determining elements in waste Streams by inductively coupled plasma-atomic emission spectroscopy

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 This test method covers the determination of trace, minor, and major elements in waste streams by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) following an acid digestion of the sample. Waste streams from manufacturing processes of nuclear and non-nuclear materials can be analyzed. This test method is applicable to the determination of total metals. Results from this test method can be used to characterize waste received by treatment facilities and to formulate appropriate treatment recipes. The results are also usable in process control within waste treatment facilities. 1.2 This test method is applicable only to waste streams that contain radioactivity levels that do not require special personnel or environmental protection. 1.3 A list of the elements determined in waste streams and the corresponding lower reporting limit is found in Table 1. 1.4 This test method has been used successfully for treatment of a large variety of waste solutions and industrial process liquids. The com...

  16. 40 CFR Table 4 to Subpart Uuu of... - Requirements for Performance Tests for Metal HAP Emissions From Catalytic Cracking Units Not...

    Science.gov (United States)

    2010-07-01

    ... Plasma-Atomic Emission Spectrometry, EPA Method 6020, Inductively Coupled Plasma-Mass Spectrometry, EPA Method 7520, Nickel Atomic Absorption, Direct Aspiration, and EPA Method 7521, Nickel Atomic...

  17. 微波消解-耐氢氟酸系统进样电感耦合等离子体发射光谱法测定锰矿中铝磷镁铁锌镍%Determination of aluminum, phosphorus, magnesium, iron, zinc and nickel in manganese ore by inductively coupled plasma atomic emission spectrometry with hydrofluoric add resistant sampling system after microwave digestion

    Institute of Scientific and Technical Information of China (English)

    邓全道; 许光; 林冠春; 刘建发; 刘灵芝

    2011-01-01

    采用混合酸作溶剂微波消解试样,样液定客后,直接用耐氢氟酸进样系统(Duo HF KIT)进样,电感耦合等离子体发射光谱法(ICP-AES)测定锰矿石试液中的铝、磷、镁、铁、锌、镍,避免因为引入硼酸掩蔽氟离子而带来的基体干扰,缩短了检测时间.测定时选择波长为369.152 nm{85}、186.942 nm{481}、280.270 nm{120}、240.488 nm{140}、213.856 nm{457}和341.476 nm{99}光谱线分别作为Al、P、Mg、Fe、Zn、Ni分析线,采用基体匹配方法来消除锰的基体效应.本法已测定国家锰矿标准物质中铝、磷、镁、铁、锌、镍,并与国标方法测定结果相比对,分析结果与认定值及国标方法的测定值相符,且重复性好.各元素的加标回收率为94%~107%,测定结果的相对标准偏差(RSD,n=12)小于1.1%.%The samples were dissolved by microwave digestion using mixed acid as solvent. After dilution, the aluminum, phosphorus, magnesium, iron, zinc and nickel in manganese ore were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) using hydrofluoric acid resistant sampling system (Duo HF KIT). The matrix effect of boric acid introduced for masking fluorine ion was prevented , and the detection time was shortened. The spectral lines for Al, P, Mg, Fe, Zn and Ni were 369. 152 nm{ 85 } , 186. 942 nm{ 481 } , 280. 270 nm{120} , 240. 488 nm {140} , 213. 856 nm {457} and 341. 476 nm {99}, respectively. The matrix effect of manganese was eliminated by matrix matching method. The proposed method had been applied to the determination of aluminum, phosphorus, magnesium, iron, zinc and nickel in certified reference materials of manganese ore. The determination results were compared with those obtained by national standard method. It was found that the analytical results were consistent with the certified values and those obtained by national standard method. Moreover, the repeatability was good. The recoveries of elements were 94%-107

  18. 电感耦合等离子体光谱法测定童鞋中的铬含量%Inductively Coupled Plasma-Atomic Emission Spectrometric (ICP-AES) Determination of Chromium in Children's Leather Shoes

    Institute of Scientific and Technical Information of China (English)

    刘贵深; 李婷; 侯晓东

    2012-01-01

    采用微波消解-电感耦合等离子体光谱法测定市场上不同厂家生产的童鞋中铬含量,对结果进行分析研究,找出重金属铬超标的原因并提出解决的对策,为降低健康安全风险,提高产品质量提供一定的参考依据。%Chromium content in children's leather shoes from different manufacturer was determined using microwave digestion and inductively coupled plasma-atomic emission spectrometry. This monitoring provides some references to reduce the health and safety risks, and improve the quality of products.

  19. 溴-甲醇提取-电感耦合等离子体原子发射光谱法测定红土镍矿还原产物中金属镍%Determination of metallic nickel in reducing products of nickel laterite ore by inductively coupled plasma atomic emission spectrometry after bromine-methanol extraction

    Institute of Scientific and Technical Information of China (English)

    李博; 王华; 魏永刚

    2011-01-01

    The metallic nickel in reducing products of nickel laterite ore was extracted by bromine-methanol. After filtering and separating the insoluble residue, the filtrate was evaporated to dryness. The residual was then dissolved in hydrochloric acid. The 231. 604 nm was selected as analytical spectral line of nickel. The content of nickel in solution was determined by inductively coupled plasma a-tomic emission spectrometry under optimal instrumental conditions. Hence, the content of metallic nickel could be calculated. The influence of sample size, extraction time, bromine concentration, dosage of bromine-methanol and interference elements on determination results was studied. Moreover, the sample analysis and recovery test were performed. The results showed that, when the sample size was smaller than 0.1 mm, and the metallic nickel was extracted with 100 mL of 5 % (V/V) bromine-methanol for 90 min, the determination results were best. Under this condition, some other active metal elements such as magnesium, aluminum and iron could be also extracted. Since their spectral lines would be overlapped with that of nickel, the determination of nickel would be affected. However, the interference could be eliminated by background correction method. The proposed method was applied to the determination of metallic nickel in reducing products of nickel laterite ore. The relative standard deviations (RSD) of determination results were in the range of 0. 96 % -5. 9 %. The recoveries of standard addition were 97. 8% -103. 8%.%采用溴-甲醇提取红土镍矿还原产物中金属镍,过滤分离不溶残渣,滤液蒸干后用盐酸溶解,选择231.604nm作为镍的分析谱线,在最佳的仪器条件下用电感耦合等离子体原子发射光谱法测定溶液中镍的含量,然后通过计算得出金属镍的含量.研究了样品粒度、提取时间、溴浓度、溴-甲醇用量、干扰元素对测定结果的影响,并进行了样品分析和回收率实验.结

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  1. Investigation of biodistribution behavior of platinum particles in mice: Correlation between inductively coupled plasma-atomic emission spectroscopy and X-ray scanning analytical microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Abe, Shigeaki, E-mail: sabe@den.hokudai.ac.jp [Graduate School of Dental Medicine, Hokkaido University, Sapporo (Japan); Koyama, Chika; Mutoh, Mami [Faculty of Dental Medicine, Hokkaido University, Sapporo (Japan); Akasaka, Tsukasa [Graduate School of Dental Medicine, Hokkaido University, Sapporo (Japan); Uo, Motohiro [Graduate School of Medical and Dental Sciences, Tokyo Medical and Dental University, Tokyo (Japan); Watari, Fumio [Graduate School of Dental Medicine, Hokkaido University, Sapporo (Japan)

    2012-12-01

    Highlights: Black-Right-Pointing-Pointer We investigated the biodistribution of platinum microparticles in mice. Black-Right-Pointing-Pointer The biodistribution behavior was observed using inductively coupled plasma-atomic emission spectroscopy (ICP) and scanning X-ray analytical microscopy (XSAM). Black-Right-Pointing-Pointer The administered particles quickly reached in spleen, liver and lung with constant ration. Black-Right-Pointing-Pointer We also estimated the correlation ship between XSAM and ICP measurement. Black-Right-Pointing-Pointer The relative ratio of XSAM intensity showed highly correlation with the relative ratio of Pt concentration in organs. - Abstract: In this study, we investigated the biodistribution of platinum (Pt) microparticles in mice. The particles were administered through the tail vein, and then the biodistribution behavior was observed using inductively coupled plasma-atomic emission spectroscopy (ICP) and scanning X-ray analytical microscopy (XSAM). The administered particles quickly reached the spleen, liver, and lung at a constant ratio, and the ratio remained constant for four weeks. We also estimated the correlation between XSAM and ICP measurement. The relative ratio of XSAM intensity showed strong correlation with the relative ratio of Pt concentration in organs.

  2. Application of inductively coupled plasma atomic emission spectroscopy analysis with a polychromator/monochromator combination the byproducts of coal-fired power stations

    Science.gov (United States)

    Weers, C. A.

    The by-products of coal-fired power plants may be hazardous for the environment. Good analysis methods are therefore required in order to establish either a possible usage of the by-products or their possible storage. Preliminary experiments performed with inductively coupled plasma atomic emission spectroscopy have proven very successful. Moreover, the method is cost-effective. A short description is given of the optimized system for routine analysis. The system consists of a 2- and a 15-channel polychromator in combination with a monochromator. The opportunities is provides are also described. Use of the monochromator to analyze coal and run-off water from the flue-gases desulphurization, and of the polychromators to analyze coal fly-ash is described separately.

  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.

    Science.gov (United States)

    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. Infrared laser ablation study of pressed soil pellets with inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mikolas, J.; Musil, P.; Stuchlikova, V.; Novotny, K.; Otruba, V.; Kanicky, V. [Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University Brno, Kotlarska 2, 61137 Brno (Czech Republic)

    2002-09-01

    Potential of infrared laser ablation (LA) coupled with ICP-AES as a technique suitable for the determination of trace elements (Zn, Cu, Ni, Cr, and V) in agricultural soils was studied. Operating parameters such as laser beam energy, laser beam focusing with respect to the sample surface, and velocity of the sample translation in the plane perpendicular to the laser beam were optimized. Soil samples were mixed with powdered Ag as a binder, and an internal standard (GeO{sub 2}), and pressed into pellets. Calibration samples were prepared by adding known amounts of oxides of elements of interest into soils of known elemental composition and then processed in the same way as the analyzed samples. Calibration curves were found to be linear at least up to several hundreds of mg kg{sup -1} for the elements of interest. The elemental contents obtained by using LA-ICP-AES were compared with those obtained by analysis using wet chemistry followed by ICP-AES with pneumatic nebulization (PN). The results were in good agreement. Accuracy was also tested using certified reference soils with a bias not exceeding 10% relative. (orig.)

  5. Determination of trace elements in heroin by inductively coupled plasma atomic emission spectrometry using ultrasonic nebulization

    Science.gov (United States)

    Budič, Bojan; Klemenc, Sonja

    2000-06-01

    A method for the determination of Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Ni, P, S, Sr and Zn in heroin samples by ICP-AES using ultrasonic nebulization is described. The samples were microwave digested with HNO 3. To improve the detection limits and minimise the matrix interferences the experimental parameters were optimised by variation of the operating power, carrier gas flow rate and observation height above the load coil. Optimum operating conditions for most of the analytes were at operating power 1550 W, carrier gas flow rate between 0.8 and 1.0 l min -1 and observation height between 10 and 12 mm above load coil. The limits of detection were below 0.5 μg g -1 (dry mass) for most of the elements investigated. The analytical recoveries of spiked samples were in the range between 94 and 103% and precision was on average better than 6%. The analysis of heroin samples shows that the method is simple, rapid and capable of providing accurate results for all the analytes investigated with the exception of nickel which was below the limit of detection in the analyzed samples.

  6. Determination of Metals Present in Textile Dyes Using Laser-Induced Breakdown Spectroscopy and Cross-Validation Using Inductively Coupled Plasma/Atomic Emission Spectroscopy

    Directory of Open Access Journals (Sweden)

    K. Rehan

    2017-01-01

    Full Text Available Laser-induced breakdown spectroscopy (LIBS was used for the quantitative analysis of elements present in textile dyes at ambient pressure via the fundamental mode (1064 nm of a Nd:YAG pulsed laser. Three samples were collected for this purpose. Spectra of textile dyes were acquired using an HR spectrometer (LIBS2000+, Ocean Optics, Inc. having an optical resolution of 0.06 nm in the spectral range of 200 to 720 nm. Toxic metals like Cr, Cu, Fe, Ni, and Zn along with other elements like Al, Mg, Ca, and Na were revealed to exist in the samples. The %-age concentrations of the detected elements were measured by means of standard calibration curve method, intensities of every emission from every species, and calibration-free (CF LIBS approach. Only Sample 3 was found to contain heavy metals like Cr, Cu, and Ni above the prescribed limit. The results using LIBS were found to be in good agreement when compared to outcomes of inductively coupled plasma/atomic emission spectroscopy (ICP/AES.

  7. Development of novel and sensitive methods for the determination of sulfide in aqueous samples by hydrogen sulfide generation-inductively coupled plasma-atomic emission spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Colon, M. [Department of Chemistry, University of Girona, Campus Montilivi, 17071 Girona (Spain); Departamento de Quimica Analitica, Nutricion y Bromatologia, University of Alicante, 03080 Alicante (Spain); Todoli, J.L. [Departamento de Quimica Analitica, Nutricion y Bromatologia, University of Alicante, 03080 Alicante (Spain); Hidalgo, M. [Department of Chemistry, University of Girona, Campus Montilivi, 17071 Girona (Spain); Iglesias, M. [Department of Chemistry, University of Girona, Campus Montilivi, 17071 Girona (Spain)], E-mail: monica.iglesias@udg.es

    2008-02-25

    Two new, simple and accurate methods for the determination of sulfide (S{sup 2-}) at low levels ({mu}g L{sup -1}) in aqueous samples were developed. The generation of hydrogen sulfide (H{sub 2}S) took place in a coil where sulfide reacted with hydrochloric acid. The resulting H{sub 2}S was then introduced as a vapor into an inductively coupled plasma-atomic emission spectrometer (ICP-AES) and sulfur emission intensity was measured at 180.669 nm. In comparison to when aqueous sulfide was introduced, the introduction of sulfur as H{sub 2}S enhanced the sulfur signal emission. By setting a gas separator at the end of the reaction coil, reduced sulfur species in the form of H{sub 2}S were removed from the water matrix, thus, interferences could be avoided. Alternatively, the gas separator was replaced by a nebulizer/spray chamber combination to introduce the sample matrix and reagents into the plasma. This methodology allowed the determination of both sulfide and sulfate in aqueous samples. For both methods the linear response was found to range from 5 {mu}g L{sup -1} to 25 mg L{sup -1} of sulfide. Detection limits of 5 {mu}g L{sup -1} and 6 {mu}g L{sup -1} were obtained with and without the gas separator, respectively. These new methods were evaluated by comparison to the standard potentiometric method and were successfully applied to the analysis of reduced sulfur species in environmental waters.

  8. Particle transport in a He-microchip plasma atomic emission system with an ultrasonic nebulizer for aqueous sample introduction

    Science.gov (United States)

    Oh, Joosuck; Lim, H. B.

    2008-11-01

    The transport efficiency of dried particles generated from an ultrasonic nebulizer (USN) was studied to improve the analytical performance of a lab-made, He-microchip plasma system, in which a quartz tube (~ 1 mm i.d.) was positioned inside the central channel of a poly(dimethylsiloxane) (PDMS) polymer chip. The polymer microchip plasma has the advantages of low cost, small size, easy handling and design, and self-ignition with long stabilization (> 24 h). However, direct introduction of aqueous solution into the microplasma for the detection of metals remains problematic due to plasma instability. In addition, the much smaller size of the system can cause signal suppression due to low transport efficiency. Therefore, knowledge of particle transport efficiency in this microplasma system is required to enhance the sensitivity and stability. The weight of transported particles in the range of 0.02 to 10 mg m - 3 was measured using a piezobalance with a precision of 0.4-17.8%, depending on the operating conditions. The significant effects of the USN operating conditions and the physical properties of the tubing, namely, length, inner diameter and surface characteristics, on the number of particles transported from the nebulizer to the microplasma were studied. When selected metals, such as Na, Mg and Pb, at a concentration of 5 mg L - 1 were nebulized, transported particles were obtained with a mass range of 0.5-5 mg m - 3 , depending on atomic weights. For application of the He-rf-microplasma, the atomic emission system was optimized by changing both the radio frequency (rf) power (60-200 W) and cooling temperature of the USN (- 12-9 °C). The limits of detection obtained for K, Na and Cu were 0.26, 0.22, and 0.28 mg L - 1 , respectively. These results confirmed the suitable stability and sensitivity of the He-rf-PDMS microchip plasma for application as an atomization source.

  9. Particle transport in a He-microchip plasma atomic emission system with an ultrasonic nebulizer for aqueous sample introduction

    Energy Technology Data Exchange (ETDEWEB)

    Oh, Joosuck [Department of Chemistry, Dankook University, 126 Jukjeon-dong, Suji-gu, Yongin-si, Gyeonggi-do, 448-701 (Korea, Republic of); Lim, H.B. [Department of Chemistry, Dankook University, 126 Jukjeon-dong, Suji-gu, Yongin-si, Gyeonggi-do, 448-701 (Korea, Republic of)], E-mail: plasma@dankook.ac.kr

    2008-11-15

    The transport efficiency of dried particles generated from an ultrasonic nebulizer (USN) was studied to improve the analytical performance of a lab-made, He-microchip plasma system, in which a quartz tube ({approx} 1 mm i.d.) was positioned inside the central channel of a poly(dimethylsiloxane) (PDMS) polymer chip. The polymer microchip plasma has the advantages of low cost, small size, easy handling and design, and self-ignition with long stabilization (> 24 h). However, direct introduction of aqueous solution into the microplasma for the detection of metals remains problematic due to plasma instability. In addition, the much smaller size of the system can cause signal suppression due to low transport efficiency. Therefore, knowledge of particle transport efficiency in this microplasma system is required to enhance the sensitivity and stability. The weight of transported particles in the range of 0.02 to 10 mg m{sup -3} was measured using a piezobalance with a precision of 0.4-17.8%, depending on the operating conditions. The significant effects of the USN operating conditions and the physical properties of the tubing, namely, length, inner diameter and surface characteristics, on the number of particles transported from the nebulizer to the microplasma were studied. When selected metals, such as Na, Mg and Pb, at a concentration of 5 mg L{sup -1} were nebulized, transported particles were obtained with a mass range of 0.5-5 mg m{sup -3}, depending on atomic weights. For application of the He-rf-microplasma, the atomic emission system was optimized by changing both the radio frequency (rf) power (60-200 W) and cooling temperature of the USN (- 12-9 deg. C). The limits of detection obtained for K, Na and Cu were 0.26, 0.22, and 0.28 mg L{sup -1}, respectively. These results confirmed the suitable stability and sensitivity of the He-rf-PDMS microchip plasma for application as an atomization source.

  10. Simultaneous Cu-, Fe-, and Zn-specific detection of metalloproteins contained in rabbit plasma by size-exclusion chromatography-inductively coupled plasma atomic emission spectroscopy.

    Science.gov (United States)

    Manley, Shawn A; Byrns, Simon; Lyon, Andrew W; Brown, Peter; Gailer, Jürgen

    2009-01-01

    Analytical methods which are capable of determining the plasma or serum metalloproteome have inherent diagnostic value for human diseases associated with increased or decreased concentrations of specific plasma metalloproteins. We have therefore systematically developed a method to rapidly determine the major Cu-, Fe-, and Zn-containing metalloproteins in rabbit plasma (0.5 mL) based on size-exclusion chromatography (SEC; stationary phase Superdex 200, mobile phase phosphate-buffered saline pH 7.4) and the simultaneous online detection of Cu, Fe, and Zn in the column effluent by an inductively coupled plasma atomic emission spectrometer (ICP-AES). Whereas most previous studies reported on the analysis of serum, our investigations clearly demonstrated that the analysis of plasma within 30 min of collection results in the detection of one more Cu peak (blood coagulation factor V) than has been previously reported (transcuprein, ceruloplasmin, albumin-bound Cu, and small molecular weight Cu). The average amount of Cu associated with these five proteins corresponded to 21, 18, 21, 30 and 10% of total plasma Cu, respectively. In contrast, only two Fe metalloproteins (ferritin and transferrin, corresponding to an average of 9 and 91% of total plasma Fe) and approximately five Zn metalloproteins (alpha(2)-macroglobulin and albumin-bound Zn, which corresponded to an average of 10 and 57% of total [corrected] plasma Zn) were detected. Metalloproteins were assigned on the basis of the coelution of the corresponding metal and protein identified by immunoassays or activity-based enzyme assays. The SEC-ICP-AES approach developed allowed the determination of approximately 12 Cu, Fe, and Zn metalloproteins in rabbit plasma within approximately 24 min and can be applied to analyze human plasma, which is potentially useful for diagnosing Cu-, Fe-, and Zn-related diseases.

  11. Speciation analysis of organomercurial compounds in Fish Tissue by capillary gas chromatography coupled to microwave-induced plasma atomic emission detection

    Directory of Open Access Journals (Sweden)

    Dorfe Díaz

    Full Text Available This paper describes a novel approach for analysis of mercury speciation in fish using gas chromatography coupled with microwave-induced plasma optical emission spectrometry (GC-MIP-OES in surfatron resonant cavity. Sample treatment was based on quantitative leaching of mercury species from fish tissue with ultrasound-assisted acid-toluene extraction. The extracted mercury species analyzed with GC-MIP-OES attained detection limits of 5 and 9 pg for methylmercury (MeHg and ethylmercury (EtHg, respectively. A complete chromatogram could be completed in 1.5 min. MeHg values obtained with GC-MIP-OES were matched with organic mercury values obtained with selective reduction cold vapour- atomic absorption spectrometry (CV-AAS.

  12. Building and analyzing models from data by stirred tank experiments for investigation of matrix effects caused by inorganic matrices and selection of internal standards in Inductively Coupled Plasma-Atomic Emission Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Grotti, Marco [Dipartimento di Chimica e Chimica Industriale, Via Dodecaneso 31, 16146 Genova (Italy)], E-mail: grotti@chimica.unige.it; Paredes, Eduardo; Maestre, Salvador; Todoli, Jose Luis [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, 03080, Alicante (Spain)

    2008-05-15

    Interfering effects caused by inorganic matrices (inorganic acids as well as easily ionized elements) in inductively coupled plasma-atomic emission spectroscopy have been modeled by regression analysis of experimental data obtained using the 'stirred tank method'. The main components of the experimental set-up were a magnetically-stirred container and two peristaltic pumps. In this way the matrix composition was gradually and automatically varied, while the analyte concentration remained unchanged throughout the experiment. An inductively coupled plasma spectrometer with multichannel detection based on coupled charge device was used to simultaneously measure the emission signal at several wavelengths when the matrix concentration was modified. Up to 50 different concentrations were evaluated in a period of time of 10 min. Both single interfering species (nitric, hydrochloric and sulphuric acids, sodium and calcium) and different mixtures (aqua regia, sulfonitric mixture, sodium-calcium mixture and sodium-nitric acid mixture) were investigated. The dependence of the emission signal on acid concentration was well-fitted by logarithmic models. Conversely, for the easily ionized elements, 3-order polynomial models were more suitable to describe the trends. Then, the coefficients of these models were used as 'signatures' of the matrix-related signal variations and analyzed by principal component analysis. Similarities and differences among the emission lines were highlighted and discussed, providing a new insight into the interference phenomena, mainly with regards to the combined effect of concomitants. The combination of the huge amount of data obtained by the stirred tank method in a short period of time and the speed of analysis of principal component analysis provided a judicious means for the selection of the optimal internal standard in inductively coupled plasma-atomic emission spectroscopy.

  13. Elemental speciation analysis by multicapillary gas chromatography with microwave-induced plasma atomic spectrometric detection.

    Science.gov (United States)

    Rodriguez Pereiro, I; Schmitt, V O; Lobiński, R

    1997-12-01

    Multicapillary column gas chromatography (MC-GC)/microwave-induced plasma atomic emission spectrometry (MIP AES) was developed for fast speciation analysis of organotin compounds in the environment. Ethylated butyltin compounds could be separated isothermally within less than 30 s (instead of ∼5-10 min) without sacrificing either the resolution or the sample capacity of conventional capillary GC with oven temperature gradient programming. Careful optimization of the pressure and temperature GC program allowed a comprehensive organotin speciation analysis including phenyltin compounds within less than 2.5 min, increasing the sample throughput 6-fold. Compatibility of MC-GC with an MIP atomic emission detector (MIP-AED) was discussed. MC-GC/MIP-AES was validated for the analysis of sediment (PACS-1 and BCR 462) and biological (NIES11) certified reference materials.

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

    Institute of Scientific and Technical Information of China (English)

    Yifei Sun; Nobuhisa Watanabe; Wei Wang; Tianle Zhu

    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 radiofrequencyhelium-plasma/atomic emission spectrometry,for the detection of semi-and low-volatile organic halogen compounds (SLVOXs),which can be collected by CarbotrapTM 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 diflicult than measuring Cl or Br,because the wavelength ofF is dose to that of air.The barrierdischarge 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 200-230℃.Under optimal analysis conditions,a chlorinecontaining plastic was destroyed using different oxygen concentrations.Lower oxygen concentrations resulted in the production of lower amounts of organic halogen compounds.

  15. Improvement of AOAC Official Method 984.27 for the determination of nine nutritional elements in food products by Inductively coupled plasma-atomic emission spectroscopy after microwave digestion: single-laboratory validation and ring trial.

    Science.gov (United States)

    Poitevin, Eric; Nicolas, Marine; Graveleau, Laetitia; Richoz, Janique; Andrey, Daniel; Monard, Florence

    2009-01-01

    A single-laboratory validation (SLV) and a ring trial (RT) were undertaken to determine nine nutritional elements in food products by inductively coupled plasma-atomic emission spectroscopy in order to improve and update AOAC Official Method 984.27. The improvements involved 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 proved through a successful internal RT using experienced 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 SLV and RT. 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 improved version of AOAC Official Method 984.27 for fortified food products, including infant formula.

  16. Combination of the ionic-to-atomic line intensity ratios from two test elements for the diagnostic of plasma temperature and electron number density in Inductively Coupled Plasma Atomic Emission Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Tognoni, E. [Istituto per i Processi Chimico-Fisici, Area della Ricerca del Consiglio Nazionale delle Ricerche Via Moruzzi 1, 56124 Pisa (Italy)], E-mail: tognoni@ipcf.cnr.it; Hidalgo, M.; Canals, A. [Departamento de Quimica Analitica, Nutricion y Bromatologia. Universidad de Alicante. Apdo. 99, 03080, Alicante (Spain); Cristoforetti, G.; Legnaioli, S.; Salvetti, A.; Palleschi, V. [Istituto per i Processi Chimico-Fisici, Area della Ricerca del Consiglio Nazionale delle Ricerche Via Moruzzi 1, 56124 Pisa (Italy)

    2007-05-15

    In Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) spectrochemical analysis, the MgII(280.270 nm)/MgI(285.213 nm) ionic to atomic line intensity ratio is commonly used as a monitor of the robustness of operating conditions. This approach is based on the univocal relationship existing between intensity ratio and plasma temperature, for a pure argon atmospheric ICP in thermodynamic equilibrium. In a multi-elemental plasma in the lower temperature range, the measurement of the intensity ratio may not be sufficient to characterize temperature and electron density. In such a range, the correct relationship between intensity ratio and plasma temperature can be calculated only when the complete plasma composition is known. We propose the combination of the line intensity ratios of two test elements (double ratio) as an effective diagnostic tool for a multi-elemental low temperature LTE plasma of unknown composition. In particular, the variation of the double ratio allows us discriminating changes in the plasma temperature from changes in the electron density. Thus, the effects on plasma excitation and ionization possibly caused by introduction of different samples and matrices in non-robust conditions can be more accurately interpreted. The method is illustrated by the measurement of plasma temperature and electron density in a specific analytic case.

  17. Determination of phosplorus, nickel, copper, titanium and vanadium in ferromanganese by microwave digestion-inductively coupled plasma atomic emission soectrometry%微波消解—电感耦合等离子体发射光谱法测定锰铁中磷镍铜钛钒

    Institute of Scientific and Technical Information of China (English)

    赵容超; 李海平; 杨大蔚; 井婷婷

    2012-01-01

    锰铁样品经微波消解后,选择327.395、231.604、177.434、334.941、309.310 nm波长的光谱线分别作为铜、镍、磷、钛、钒的分析线,用电感耦合等离子体发射光谱法测定了锰铁样品中铜、镍、磷、钛、钒含量.基体锰产生的基体效应可以通过基体匹配的方法消除,基体铁对测定没有影响.方法用于测定锰铁标样,测定值与认定值一致;用于测定锰铁试样,测定结果的相对标准偏差在0.2%0~3.6%o之间,加标回收率为97%~103%.方法可以用于中、高、低碳锰铁中铜、镍、磷、钛、钒的测定.%After pretreatment with microwave digestion and selection of spectral lines at the wavelength of 327. 395,231. 604,177. 434,334. 941 and 309. 310 nm as the analytical line of copper, nickel, phosphorus, titanium and vanadium, respectively, the content of copper, nickel, phosphorus, titanium and vanadium in ferromanganese sample was determined by inductively coupled plasma atomic e-mission spectrometry. The matrix effect produced by matrix manganese could be eliminated by matrix matching while the matrix iron did not have influence on the determination. When the method was applied to determine ferromanganese certified reference materials, the determination results were the same as the certified values. When it was applied to determine ferromanganese actual samples, relative standard deviations of the determination results were between 0. 2% and 3. 6% and recoveries were between 97% and 103%. The method could be used to determine copper, nickel, phosphorus, titanium and vanadium in the medium, high and low-carbon ferromanganese.

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

    Directory of Open Access Journals (Sweden)

    Sanda Rončević

    2012-01-01

    Full Text Available 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.

  19. Effect of HF addition on the microwave-assisted acid-digestion for the determination of metals in coal by inductively coupled plasma-atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Yan-Hua [Department of Environmental Science and Engineering, College of Urban Construction and Safety and Environmental Engineering, Nanjing University of Technology, No. 200 Zhongshan Beilu, Nanjing 210009, Jiangsu (China); Iwashita, A.; Nakajima, T.; Yamashita, H.; Takanashi, H.; Ohki, A. [Department of Bioengineering, Faculty of Engineering, Kagoshima University, 1-21-40, Korimoto, Kagoshima 890-0065 (Japan)

    2005-03-31

    The microwave-assisted acid-digestion for the determination of metals in coal by ICP-AES was investigated, especially focusing on the necessity of adding HF. By testing five certified reference materials, BCR-180, BCR-040, NIST-1632b, NIST-1632c, and SARM-20, it was found that the two-stage digestion without HF (HNO{sub 3}+H{sub 2}O{sub 2} was used) was very effective for the pretreatment of ICP-AES measurement. Both major metals (Al, Ca, Fe, and Mg) and minor or trace metals (Co, Cr, Cu, Mn, Ni, Pb, and Zn) in coal gave good recoveries for their certified or reference values. The possibility of 'HF-memory effect' was cancelled by the use of a set of vessels which had been never contacted with HF. Twenty-four Japanese standard coals (SS coals) were analyzed by the present method, and the concentrations of major metals measured by the present method provided very high accordance with those from the authentic JIS (Japanese Industrial Standard) method.

  20. Effect of HF addition on the microwave-assisted acid-digestion for the determination of metals in coal by inductively coupled plasma-atomic emission spectrometry.

    Science.gov (United States)

    Xu, Yan-Hua; Iwashita, Akira; Nakajima, Tsunenori; Yamashita, Hiroyuki; Takanashi, Hirokazu; Ohki, Akira

    2005-03-31

    The microwave-assisted acid-digestion for the determination of metals in coal by ICP-AES was investigated, especially focusing on the necessity of adding HF. By testing five certified reference materials, BCR-180, BCR-040, NIST-1632b, NIST-1632c, and SARM-20, it was found that the two-stage digestion without HF (HNO(3)+H(2)O(2) was used) was very effective for the pretreatment of ICP-AES measurement. Both major metals (Al, Ca, Fe, and Mg) and minor or trace metals (Co, Cr, Cu, Mn, Ni, Pb, and Zn) in coal gave good recoveries for their certified or reference values. The possibility of 'HF-memory effect' was cancelled by the use of a set of vessels which had been never contacted with HF. Twenty-four Japanese standard coals (SS coals) were analyzed by the present method, and the concentrations of major metals measured by the present method provided very high accordance with those from the authentic JIS (Japanese Industrial Standard) method.

  1. Direct solid analysis of powdered tungsten carbide hardmetal precursors by laser-induced argon spark ablation with inductively coupled plasma atomic emission spectrometry.

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  3. Preconcentration of Rare Earth Elements with 8-Hydroxyquinoline-5-sulfonic Acid Chelated Cellulose Filter Prior to Determination by Inductively Coupled Plasma Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    8-Hydroxyquinoline-5-sulfonic acid,covalently bound to filter cellulose,was used for preconcentrating trace rare earth element(REE) ions from complex matrices and matrix separation,respectively.Multi-REE ions were preconcentrated on the column filled with 8-hydroxyquinoline-5-sulfonic acid cellulose filter and analysed by ICP-AES after being eluted with dilute HNO3.In the given pH range,alkali and alkaline earth metal ions can be separated as matrix elements;a high concentration factor is obtained and the eluates can be measured without interference.The usefulness of the method is shown by the control analyses of standard reference materials.

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

    Science.gov (United States)

    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.

  5. Inductively coupled plasma atomic emission spectrometric determination of acid-soluble metal elements chromium,manganese, zinc and copper in talcum powder%电感耦合等离子体原子发射光谱法测定滑石粉中酸溶金属元素铬锰锌铜

    Institute of Scientific and Technical Information of China (English)

    胡晓静; 曾泽; 王长文; 仇薪越; 牟明仁; 富瑶; 沈桂玲; 刘向宽

    2011-01-01

    After digestion by aqua regia with microwave and selection of corresponding spectral lines at 267. 7, 257. 6, 213. 8 and 324. 7 nm as analytical lines, the acid-dissoluble metal elements including chromium, manganese, zinc and copper in talcum powder were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) under optimized conditions with radio frequency power of 1 250 W, auxiliary air flow rate of 0. 60 L/min and atomizer pressure of 26 psi. When the concentration of each testing element was 2. 0 μg/mL, the interferences caused by 20. 0 μg/mL of I-ron, magnesium, calcium, aluminum, zinc, nickel and copper were all less than 5 %. Since the contents of these elements in talcum powder were less than 1 %, their influence on the determination could be ignored. The detection limits of chromium, manganese, zinc and copper were 0. 004 8, 0. 003 8, 0. 001 and 0. 002 6 μg/mL, respectively. This proposed method was applied in actual samples, and the determination results were consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) with relative standard deviations (RSD, n = 8) of 1.1%-4. 2% and recoveries of 93 %-107 %.%以王水作溶剂,微波消解法消解样品,选择267.7、257.6、213.8和324.7 nm波长的光谱线分别作为铬、锰、锌和铜的分析线,在发射功率为1 250 W、辅助气流量为0.60 L/min、雾化器压力为26 psi的优化条件下以电感耦合等离子体原子发射光谱法(ICP-AES)测定了滑石粉中酸溶金属元素铬、锰、锌、铜含量.样品中的基体组分硅酸镁在王水中的溶解量很少,对测定没有影响.当测定待测元素浓度均为2.0μg/mL的溶液时,20.0 μg/mL的铁、镁、钙、铝、锌、镍、铜对待测元素的干扰均小于5%.由于滑石粉中这些元素含量小于1%,因此它们对测定的影响可以忽略.铬、锰、锌、铜的检出限分别为0.004 8、0.003 8、0.001、0.002 6μg/mL.滑石粉样品分析

  6. 40 CFR Table 7 to Subpart Uuu of... - Continuous Compliance With Operating Limits for Metal HAP Emissions From Catalytic Cracking Units

    Science.gov (United States)

    2010-07-01

    ... Method 6010B, Inductively Coupled Plasma-Atomic Emission Spectrometry, EPA Method 6020, Inductively Coupled Plasma-Mass Spectrometry, EPA Method 7520, Nickel Atomic Absorption, Direct Aspiration, or EPA Method 7521, Nickel Atomic Absorption, Direct Aspiration; or by an alternative to EPA Method 6010B,...

  7. Determinação de Cd, Ni e Zn por espectrometria de emissão atômica com plasma indutivamente acoplado, após separação e pré-concentração em coluna contendo p-dimetilaminobenzilidenorodanina adsorvida sobre sílica gel Determination of Cd, Ni and Zn by inductively coupled plasma emission atomic spectrometry after separation and preconcentration in column packed with 5-(4-dimethylaminobenzylidene rhodanine adsorbed on silica gel

    Directory of Open Access Journals (Sweden)

    Laerte da Cunha Azeredo

    1999-07-01

    Full Text Available A column packed with 5-(4-dimethylaminobenzylidenerhodanine adsorbed on silica gel was used for the preconcentration of Cd, Ni and Zn at different spiked solutions prior to their determination by inductively coupled plasma atomic emission spectrometry. This column allowed recoveries over than 98% for the above elements and accurate analyses of coastal sea-water certified reference material were also achieved.

  8. Transition probabilities for lines of Cr II, Na II and Sb I by laser produced plasma atomic emission spectroscopy; Probabilidades de transicion de algunos niveles de Cr II, Na II y Sb I medediante espectroscopia de plasma producidos por laser

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez, A. M.; Ortiz, M.; Campos, J.

    1995-07-01

    Absolute transition probabilities for lines of CR II, Na II and Sb I were determined by emission spectroscopy of laser induced plasmas. the plasma was produced focusing the emission of a pulsed Nd-Yag laser on solid samples containing the atom in study. the light arising from the plasma region was collected by and spectrometer. the detector used was a time-resolved optical multichannel analyzer (OMA III EG and G). The wavelengths of the measured transitions range from 2000 sto 4100 A. The spectral resolution of the system was 0. 2 A. The method can be used in insulators materials as Cl Na crystals and in metallic samples as Al-Cr and Sn-Sn alloys. to avoid self-absorption effects the alloys were made with low Sb or Cr content. Relative transition probabilities have been determined from measurements of emission-line intensities and were placed on an absolute scale by using, where possible, accurate experimental lifetime values form the literature or theoretical data. From these measurements, values for plasma temperature (8000-24000 K), electron densities ({approx}{approx} 10''16 cm ''-3) and self-absorption coefficients have been obtained. (Author) 56 refs.

  9. Speciation analysis of triethyl-lead and tributyl-tin compounds in human urine by liquid-liquid extraction and gas chromatography microwave-induced plasma atomic emission detection.

    Science.gov (United States)

    Zachariadis, George A; Rosenberg, Erwin

    2012-05-01

    This work describes the development of a fast method for speciation analysis of triethyl-lead and tributyl-tin species in urine samples after in situ derivatization by tetraethyl- or tetrapropyl-borate reagents. The alkylation reaction is done in the aqueous and urine medium and the less-polar derivatives are extracted in hexane by liquid-liquid extraction. The species were extracted and the extract was efficiently collected from the aqueous phase after centrifugation. Finally, the organometallic species are separated by gas chromatography and determined from the emission signals of elemental lead and tin. Atomic lead and tin are formed from the organolead and organotin compounds during atomization of the column eluate in a microwave-induced helium plasma source. The simultaneous measurement of lead (Pb) at 405.780 nm and tin (Sn) at 303.419 nm was achieved by an atomic emission detector. Finally, the analytes were determined with satisfactory precision (urine is extracted with 1 mL of hexane and 1 μL of extract is injected.

  10. Mass and emission spectrometry in the Analytical Chemistry Division of Oak Ridge National Laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Smith, D.H. (ed.)

    1978-11-01

    The capabilities of the Mass and Emission Spectrometry Section of the Analytical Chemistry Division of Oak Ridge National Laboratory are described. Many different areas of mass spectrometric expertise are represented in the section: gas analysis, high abundance sensitivity measurements, high- and low-resolution organic analyses, spark source trace constituent analysis, and ion microprobe analysis of surfaces. These capabilities are complemented by emission spectrometry. The instruments are described along with a few applications, some of which are unique.

  11. STUDY ON DETERMINATION OF SULPHATE IN WATER BY INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY%水中硫酸盐的原子发射光谱法研究

    Institute of Scientific and Technical Information of China (English)

    高玲; 杨元; 王坤明

    2009-01-01

    [目的]建立采用电感耦合等离子体发射光谱技术(ICP-AES)直接测定水中硫酸盐的方法.[方法]样品经加盐酸加热去除硫化物干扰,采用1150 W射频功率,1.85 ml/min提升量,20 psi雾化器压力,180.731 nm分析线.直接测定水中硫酸盐含量.[结果]本方法最低检出浓度为0.039 mg/L,相对标准偏差RSD在0.229%~2.4%之间,与国家标准方法比对,符合性好,测定国家标准物质在标示值范围内.[结论]ICP-AE3法简便、快速、灵敏度高、准确度高、线性范围宽,适用于大批样品的高通量分析.

  12. Determination of blood boron by inductively coupled plasma atomic emission spectrometry and investigation of boron level in children's blood%ICP-AES法测定血硼及儿童血硼质量浓度调查

    Institute of Scientific and Technical Information of China (English)

    李萌; 杨玉华; 唐吟岫

    2006-01-01

    目的 探索电感耦合等离子体原子发射光谱(ICP-AES)法测定血硼的方法,确定南京地区儿童血硼质量浓度正常值范围.方法 全血经1 mol/L HNO3处理后用ICP-AES法测定,并用该方法测定南京地区1 032名健康儿童及1 364名就诊儿童血硼.结果 方法精密度为1.60%-4.31%,回收率为93.3%-98.9%.1 032名健康儿童全血硼质量浓度为(41.8±16.7)μg/L,1 364名就诊儿童血硼质量浓度为25.1-58.5 μg/L(77%).结论 全血经硝酸处理后测定血硼,精密度及回收率均较理想,可以作为测定血硼的参考方法.并初步提出该方法的南京地区儿童血硼参考范围为25.1-58.5 μg/L(1岁以下儿童除外).

  13. Determination of impurity element aluminum in spirulina by inductively coupled plasma atomic emission spectrometry%ICP-AES法测定螺旋藻中的杂质元素铝

    Institute of Scientific and Technical Information of China (English)

    林易晨

    2015-01-01

    探讨用ICP-AES技术测定螺旋藻中杂质元素铝,并对共存元素光谱干扰及其消除进行研究,所建立的分析方法,快速、结果准确,有较好的精密度和准确度,适用于螺旋藻中铝的测定.%The determination of impurity element aluminum in spirulina by ICP-AES was studied. The spectral interference and elimination of coexisting elements was investigated. The established analytical method is fast ,precise and accurate. The method is applicable to the determination of aluminum content in spirulina.

  14. Sequential-injection on-line preconcentration using chitosan resin functionalized with 2-amino-5-hydroxy benzoic acid for the determination of trace elements in environmental water samples by inductively coupled plasma-atomic emission spectrometry

    OpenAIRE

    2007-01-01

    A new chelating resin using chitosan as a base material was synthesized. Functional moiety of 2-amino-5-hydroxy benzoic acid (AHBA) was chemically bonded to the amino group of cross-linked chitosan (CCTS) through the arm of chloromethyloxirane (CCTS-AHBA resin). Several elements, such as Ag, Be, Cd, Co, Cu, Ni, Ph, U, V, and rare earth elements (REEs), could be adsorbed on the resin. To use the resin for on-line pretreatment, the resin was packed in a mini-column and installed into a sequenti...

  15. ICP-AES法测定水中金属和非金属元素%Determination of Metals and Non-metals in Water by Inductively Coupl ed Plasma-Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    刘桂华; 谢建滨

    2002-01-01

    目的为满足生活饮用水卫生规范中多元素分析的需要,建立准确快捷测定水中23种金属和非金属元素的方法. 方法用电感耦合等离子体发射光谱ICP-AES法,同时测定Ag、Al 、B、Ba、Be、Ca、Cd、Co、Cr、Cu、Fe、K、Li、Mg、Mn、Mo、Na、Ni、Si、Sr、Ti、V、Z n.结果方法快速、灵敏,各元素的检出限分别在0.000 02mg/L~0 .06mg/L之间;线性良好,线性相关系数均≥0.998;重现性好,不同浓度的变异系数为0. 37%~2.8%;准确度高,回收率在91%~116%之间,对标样GBW08607、GSBZ50009-88、C W82、GSBE50019-90测定,数值均在允许范围内,与原子吸收分光光度法对比,P均>0.0 5,表明两种方法检测结果之间无显著性差异. 结论本法实现多元素同时测定,准确可靠,极大地提高了工作效率,适用于水质分析.

  16. Determination of Minor Elements in Manganese Ores by Inductively Coupled Plasma-atomic Emission Spectrometry%ICP-AES法测定锰矿石中的次要元素含量

    Institute of Scientific and Technical Information of China (English)

    王艳君; 蒋晓光; 赵旭东; 仲吉伟; 穆彪

    2013-01-01

    Dealing with laboratory samples of manganese ores by wet-digest and high pressure digestion method,we have analyzed the elements in test solution as iron,calcium,aluminum,magnesium,titanium,phosphorus,nickel,copper and zinc content by ICP-AES.Considering the factors of sample in a discomposed condition,matrix interference and coexisting elements interference are introduced into the working conditions of the instrument.We use the reference wavelength and precision,establishing an ICP-AES method for determination of Fe,Ca,AI,Mg,Ti,P,Ni,Cu and Zn in manganese ore.%采用敞开式湿法和高压密闭消化法2种溶样方法,用电感耦合等离子体原子发射光谱法测定了试液中铁、钙、铝、镁、钛、磷、镍、铜和锌含量.考察了溶样方法、基体干扰和共存元素干扰,给出了仪器工作条件、分析线的参考波长和方法的精密度,建立了电感耦合等离子体原子发射光谱法测定锰矿石中铁、钙、铝、镁、钛、磷、镍、铜和锌含量的方法.

  17. Determination of Nickel in Ore Samples by Inductively Coupled Plasma Atomic Emission Spectrometry%熔融辅助消解ICP-AES法测定镍矿中的镍含量

    Institute of Scientific and Technical Information of China (English)

    窦怀智; 吕翔; 侯晋

    2011-01-01

    用电感耦合等离子体原子发射光谱法测定未知镍矿样品中的镍含量,对酸度、分析谱线、检出限等仪器使用参数进行了分析,并且比较了镍矿样品的4种前处理方法.结果表明,样品溶液含酸5%,选择231.604nm谱线测定时,仪器检出限和方法检出限均能满足镍矿中镍含量的测定.4种样品前处理方法中,将难溶滤渣与硫酸氢钾共熔的方法其检测结果准确度和精密度都较高,方法的回收率可以达到95%以上.

  18. Determination of Arsenic,Antimony,Bismuth and Tin in Chinese Herb Vietnamese Sophora Root by Microwave Digestion Hydride Generation Inductively Coupled Plasma Atomic Emission Spectrometry%HG-ICP-AES法测定山豆根中的微量元素

    Institute of Scientific and Technical Information of China (English)

    孟君; 郭全海; 蒋玲; 邓必阳

    2009-01-01

    建立微波消解-氢化物发生-电感耦合等离子体发射光谱联用技术测定中药山豆根中砷、锑、铋和锡的方法,对微波消解、氢化物发生、电感耦合等离子体原子发射光谱等工作条件进行优化,对还原剂L-半胱胺酸浓度进行了选择.在最佳工作条件下,砷、锑、铋和锡的检出限分别为0.006、0.009、0.003和0.005μg·g-1,相对标准偏差分别为6%、2%、3%和3%(n=10);加标回收率分别为102%、95%、98%和110%.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Jalowy, T. E-mail: jalowy@hsb.uni-frankfurt.de; Neugebauer, R.; Hattass, M.; Fiol, J.; Afaneh, F.; Pereira, J.A.M.; Collado, V.; Silveira, E.F. da; Schmidt-Boecking, 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{sub 2}{sup +} from Al target by Ar{sup 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 deg. to normal (following the projectile radial direction). The initial energy distribution spreads out over 16 eV.

  1. Dynamics of secondary ion emission Novel energy and angular spectrometry

    CERN Document Server

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

    2002-01-01

    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 sub 2 sup + from Al target by Ar sup 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 deg. to normal (following the projectile radial direction). The initial energy distribution spreads out over 16 eV.

  2. Detection of emissions from surfaces using ion mobility spectrometry.

    Science.gov (United States)

    Vautz, Wolfgang; Baumbach, Jörg Ingo; Uhde, Erik

    2006-02-01

    Emissions from surfaces (from furniture, wall paintings or floor coverings for instance) significantly influence indoor air quality and therefore the wellbeing or even the health of the occupants. Together with metabolites from mold they are responsible for the well-known "sick building syndrome". Therefore, it is in the interest of the manufacturer as well as of the occupants to have a fast and accurate method for the detection of substances relevant to this syndrome in order to be able to monitor and control product quality and indoor air quality. The use of small and easy-to-transport ion mobility spectrometers that use UV light as the ionization source enables rapid in situ detection of such substances with high selectivity and sensitivity (detection limits in the lower ppb range). If a multicapillary column is used for preseparation as well, the selectivity is increased and the unwanted influence of humidity on the spectra can be eliminated, thus enabling the use of the instruments under normal ambient conditions. Furthermore, the use of air as carrier gas avoids the need for other sources of high-purity gas. An emission cell with a homogeneous and constant air flow over the surface to be investigated was developed in order to ensure reproducible results. Investigations of emissions from wooden surfaces with and without additional contamination as well as from complex mixtures are presented. The results demonstrate that relevant emissions can be identified and quantified with high sensitivity and selectivity in under five minutes. Therefore, the method is useful for indoor air quality monitoring, especially when miniaturized instruments are applied.

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

    Energy Technology Data Exchange (ETDEWEB)

    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)

  4. Dispersive liquid–liquid microextraction combined with laser-induced breakdown spectrometry and inductively coupled plasma optical emission spectrometry to elemental analysis

    OpenAIRE

    Gaubeur, Ivanise; Aguirre Pastor, Miguel Ángel; Kovachev, Nikolay; Hidalgo Núñez, Montserrat; Canals Hernández, Antonio

    2015-01-01

    In this paper, two analytical methodologies based on the combination of dispersive liquid–liquid microextraction with inductively coupled plasma optical emission spectrometry and laser-induced breakdown spectrometry, respectively, were evaluated for simultaneous preconcentration and detection of Cd, Co, Ni, Pb and Zn. The microextraction procedure was based on the injection of appropriate quantities of 1-undecanol and methanol into the sample solution containing the complexes formed between m...

  5. Determination of trace elements in maifanite by outer cover electrode atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    LI Jianqiang; LU Yiqiang; JIANG Wei

    2005-01-01

    Maifanite is a nature medicinal stone used in many fields for long time. The research on it showed that there are many trace elements in maifanite. In this paper, 36 trace elements in maifanite were determined by outer cover electrode atomic emission spectrometry, and the determination conditions were studied systematically. The results show that the concentrafions of elements, which are beneficial to human health, are higher, and the elements harmful to people health such as As, Cd, Hg, Cr, and Pb are tiny in maifanite. The precision and the accuracy were also discussed.

  6. Multi-elemental analysis of aqueous geological samples by inductively coupled plasma-optical emission spectrometry

    Science.gov (United States)

    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.

  7. Detailed computation of hot-plasma atomic spectra

    CERN Document Server

    Pain, Jean-Christophe; Blenski, Thomas

    2015-01-01

    We present recent evolutions of the detailed opacity code SCO-RCG which combines statistical modelings of levels and lines with fine-structure calculations. The code now includes the Partially-Resolved-Transition-Array model, which allows one to replace a complex transition array by a small-scale detailed calculation preserving energy and variance of the genuine transition array and yielding improved high-order moments. An approximate method for studying the impact of strong magnetic field on opacity and emissivity was also recently implemented. The Zeeman line profile is modeled by fourth-order Gram-Charlier expansion series, which is a Gaussian multiplied by a linear combination of Hermite polynomials. Electron collisional line broadening is often modeled by a Lorentzian function and one has to calculate the convolution of a Lorentzian with Gram-Charlier distribution for a huge number of spectral lines. Since the numerical cost of the direct convolution would be prohibitive, we propose, in order to obtain t...

  8. Synthesis of Highly Emissive CdSe Quantum Dots by Aqueous Precipitation Method

    OpenAIRE

    Bing Gao; Chao Shen; Shuanglong Yuan; Yunxia Yang; Guorong Chen

    2013-01-01

    CdSe quantum dots (QDs) with high quantum yield (QY) up to 76.57% are synthesized using the aqueous precipitation method. With the control of SeSO32- concentration in Se precursor, the nucleation speed and concentration of CdSe QDs are increased. The mass of obtained Cd2+ and Se2+ in nanocrystal is measured by inductively coupled plasma atomic emission spectrometry (ICP-AES). XRD and HRTEM are used to identify the crystal phase and morphology of the products which are pure CdSe crystals in th...

  9. Trace elemental composition of curry by inductively coupled plasma optical emission spectrometry (ICP-OES).

    Science.gov (United States)

    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.

  10. Simple procedure for nutrient analysis of coffee plant with energy dispersive X-ray fluorescence spectrometry (EDXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Tezotto, Tiago; Favarin, Jose Laercio; Neto, Ana Paula; Azevedo, Ricardo Antunes, E-mail: tiago.tezotto@usp.br [Escola Superior de Agricultura Luiz de Queiroz (ESALQ/USP), Piracicaba, SP (Brazil); Gratao, Priscila Lupino [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP/ FCAV), Jaboticabal, SP (Brazil). Dept. de Biologia Aplicada a Agropecuaria; Mazzafera, Paulo [Universidade Estadual de Campinas (UNICAMP/IB), SP (Brazil). Dept. Biologia Vegetal

    2013-07-15

    Nutrient analysis is used to estimate nutrient content of crop plants to manage fertilizer application for sustained crop production. Direct solid analysis of agricultural and environmental samples by energy dispersive X-ray fluorescence spectrometry (EDXRF) was chosen as alternative technique to evaluate the simultaneous multielemental quantification of the most important essential elements in coffee (Coffea arabica L.) plants. Inductively coupled plasma atomic emission spectrometry and certified reference materials made from leaves were used to calibrate and check the trueness of EDXRF method for the determination of the concentration of several nutrients in coffee leaves and branches. Fluorescence spectrometry proved to be advantageous and presented low cost as loose powder samples could be used. Samples collected from a field experiment where coffee plants were treated with excess of Ni and Zn were used to verify the practical application of the method. Good relationships were achieved between certified values and data obtained by EDXRF, with recoveries ranging from 82 to 117 %.(author)

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

    Science.gov (United States)

    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...

  12. [Determination of high content of tin in geochemical samples by solid emission spectrometry].

    Science.gov (United States)

    Yao, Jian-Zhen; Hao, Zhi-Hong; Tang, Rui-Ling; Li, Xiao-Jing; Li, Wen-Ge; Zhang, Qin

    2013-11-01

    A method for the determination of high content of tin in geochemical samples by solid emission spectrometry was presented. The dedicated high content tin spectrum standard series was developed. K2S2O7, NaF, Al2O3 and carbon powder were used as buffers and Ge was used as internal standard, and the ratio of sample/matrix/buffer is 1 : 1 : 2. A weak sensitive line (Sn 242. 170 0 nm) was used as the analytical line. The technologies of vertical electrodes, AC arc overlap spectrograph, interception of the exposure, quantitative computer translation spectrum and background correction were used. The determination range is 100-22 350 microg x g(-1), the detection limit is 16.64 microg x g(-1), and the precision is (RSD, n = 12) 4.11%-6.46%. The accuracy of the method has been verified by determination of high content of tin in national geochemical standard samples and the results are in agreement with certified value. The method can be used for measurement directly without dilution of high content of tin in geochemical samples, and it greatly improved the detection upper limit for the determination of tin with solid emission spectroscopy and has certain practical value.

  13. Analysis of Mussel Standard Reference Material by Inductively Coupled Plasma Atomic Emission Spectrometry and Inductively Coupled Plasma Mass Spectrometry%电感耦合等离子体光谱和质谱法分析贻贝标准物质

    Institute of Scientific and Technical Information of China (English)

    曹淑琴; 陈杭亭; 曾宪津

    1999-01-01

    采用电感耦合等离子体光谱和质谱法分析了贻贝标准物质,光谱法测定K、Na、Ca、Mg、P、Al、Fe、Zn、Mn和Sr,质谱法测定As、B、Cd、Co、Cr、Cu、Ga、Ge、Mn、Mo、Ni、Pb、De、Sr、U和V.在优化的工作条件下,测定了来自基体元素K、Na、Ca、P、Cl和C的多原子离子39K16O、39K2、40Ar23Na、43Ca16O、42Ca16O、44Ca16O、31P16O2、40Ar35Cl、40Ar37Cl、35Cl16O、37Cl16O和40Ar12C对55Mn、78Se、63Cu、59Co、58Ni、60Ni、75as、77Se、51V、53Cr和52Cr的干扰系数以及HNO3+H2O2(3+2)、HNO3+HClO4(3+0.5)和HNO3+H2SO4(3+0.5)等3种样品消解方法在一些生物重要元素的同位素处产生的表观浓度.光谱法的检出限0.001~0.75 mg/L;质谱法的检出限0.005~1.01μgL.光谱法和质谱法的相对标准偏差分别是2.7%~12.8%和3.4%~24.8%.

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

    Science.gov (United States)

    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.

  15. [Analytical figures of merit of Hildebrand grid and ultrasonic nebulizations in inductively coupled plasma atomic emission].

    Science.gov (United States)

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

    2012-05-01

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

  16. Determination of Phosphorus by Inductively Coupled Plasma Atomic Emission Spectroscopy after Hydride Generation

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    A continuous phosphine (PH3) generation was developed and applied to the sensitive detection of phosphorus by ICP-AES. Phosphate ion in aqueous solution was converted to phosphine by passing the sample solution through an incandescent copper silica-tube. Detection limit is 2 ng/mL. The relative standard deviation is 4.2% for 20 ng/mL. The method is rapid and simple with low contamination and high sensitivity.

  17. Hyphenated techniques in speciation analysis of polyoxometalates: identification of individual [PMo12-xVxO40](-3-x) (x = 1-3) in the reaction mixtures by high performance liquid chromatography and atomic emission spectrometry with inductively coupled plasma.

    Science.gov (United States)

    Shuvaeva, O V; Zhdanov, A A; Romanova, T E; Abramov, P A; Sokolov, M N

    2017-03-14

    Unambiguous identification of polyoxometalate (POM) species generated in self-assembly reactions in solution is rather problematic due to close similarity of their properties such as solubility and spectral characteristics. The situation is made more complex by protonation equilibria (which can change their analytical signals) and the lack of individual compounds to serve as standards for individual members of these mixtures. In the present work a new approach to the study of such POMs has been suggested, taking molybdovanadates [PMo12-xVxO40](-3-x) as a model. The key feature of this approach consists of generation of so-called "conditional model systems" that include most of the expected components of a mixture formed by self-assembly, tracked down by reliable detection techniques, e.g., (51)V NMR-spectroscopy in this particular case. Then the proposed composition of the mixture is verified and corrected by means of high-performance liquid chromatography coupled with inductively coupled plasma atomic emission spectrometry (HPLC-ICP-AES).

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

    Science.gov (United States)

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

  19. Rapid, high-purity chemical separation of molybdenum from iron meteorites for isotopic analysis by using thermal ionization mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Qi-Lu; Masuda, Akimasa (Tokyo Univ. (Japan). Dept. of Chemistry)

    1992-05-01

    A chemical procedure has been developed, which combines both solvent extraction and anion exchange, so that microgram amounts of Mo can be cleanly, rapidly and efficiently separated from gram amounts of iron meteorites. Particular attention was directed to the complete separation of Mo from Zr and Ru. The isotopic abundance ratios of Mo can subsequently be determined with high accuracy by using thermal ionization mass spectrometry. The experiments indicate that the behaviour of Mo during solvent extraction and anion exchange is considerably different from that reported previously. In particular, it was found that there is a very narrow range of HCl concentrations within which it is possible to separate Mo from Fe by solvent extraction. The reproducibility and recovery of the method were examined by using inductively coupled plasma atomic emission spectrometry. (Author).

  20. Spatially resolved measurements to improve analytical performance of solution-cathode glow discharge optical-emission spectrometry

    Science.gov (United States)

    Schwartz, Andrew J.; Ray, Steven J.; Chan, George C.-Y.; Hieftje, Gary M.

    2016-11-01

    Past studies of the solution-cathode glow discharge (SCGD) revealed that elemental and molecular emission are not spatially homogenous throughout the source, but rather conform to specific zones within the discharge. Exploiting this inhomogeneity can lead to improved analytical performance if emission is collected only from regions of the discharge where analyte species emit strongly and background emission (from continuum, elemental and/or molecular sources) is lower. Effects of this form of spatial discrimination on the analytical performance of SCGD optical emission spectrometry (OES) have been investigated with an imaging spectrograph for fourteen atomic lines, with emphasis on detection limits and precision. Vertical profiles of the emission intensity, signal-to-background ratio, and signal-to-noise ratio were collected and used to determine the optimal region to view the SCGD on a per-element basis. With optimized spatial filtering, detection limits ranged from 0.09-360 ppb, a 1.4-13.6 fold improvement over those obtained when emission is collected from the full vertical profile (1.1-840 ppb), with a 4.2-fold average improvement. Precision was found to be unaffected by spatial filtering, ranging from 0.5-2.6% relative standard deviation (RSD) for all elements investigated, closely comparable to the 0.4-2.4% RSD observed when no spatial filtering is used. Spatial profiles also appear useful for identifying optimal line pairs for internal standardization and for flagging the presence of matrix interferences in SCGD-OES.

  1. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: a tutorial review. Part II. Practical considerations.

    Science.gov (United States)

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

    2015-07-23

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

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  4. Performance testing of multi-metal continuous emissions monitors

    Energy Technology Data Exchange (ETDEWEB)

    Haas, W.J. [Ames Lab., IA (United States); French, N.B. [Sky+, Inc. (United States); Brown, C.H. [Oak Ridge National Lab., TN (United States); Burns, D.B. [Westinghouse Savannah River Co., Aiken, SC (United States); Lemieux, P.M.; Ryan, J.V. [National Risk Management Research Lab., Research Triangle Park, NC (United States); Priebe, S.J. [Idaho National Engineering and Environmental Lab., Idaho Falls, ID (United States); Waterland, L.R. [Acurex Environmental Corp. (United States)

    1997-11-17

    Three prototype multi-metals continuous emissions monitors (CEMs) were tested in April 1996 at the Rotary Kiln Incinerator Simulator facility at the US Environmental Protection Agency (EPA) National Risk Management Research Laboratory, Research Triangle Park, North Carolina. The CEM instruments were: Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES); Laser Induced Breakdown Spectrometry-Atomic Emission Spectroscopy (LIBS); and Laser Spark Spectrometry, another LIBS instrument. The three CEMs were tested simultaneously during test periods in which low, medium, and high concentration levels of seven toxic metals -- antimony, arsenic, beryllium, cadmium, chromium, lead, and mercury -- were maintained under carefully controlled conditions. Two methods were used to introduce the test metals into the flue gas: (1) solution atomization, introducing metal-containing aerosol directly into the secondary combustion burner, and (2) injection of fly ash particulates. The testing addressed four measures of CEM performance: relative accuracy (RA), calibration drift, zero drift, and response time. These were accomplished by comparing the toxic metal analyte concentrations reported by the CEMs to the concentrations measured using the EPA reference method (RM) for the same analytes. Overall, the test results showed the prototype nature of the test CEMs and the clear need for further development. None of the CEMs tested consistently achieved RA values of 20% or less as required by the EPA draft performance specification. Instrument size reduction and automation will also likely need additional attention before multi-metal CEMs systems become commercially available for service as envisioned by regulators and citizens.

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

    Energy Technology Data Exchange (ETDEWEB)

    Flores, O.; Castillo, F.; Martinez, H. [Laboratorio de Espectroscopia, Instituto de Ciencias Físicas, Universidad Nacional Autónoma de México, Apartado Postal 48-3, 62251, Cuernavaca, Morelos (Mexico); Villa, M.; Reyes, P. G. [Facultad de Ciencias, Universidad Autónoma del Estado de México, Estado de México (Mexico); Villalobos, S. [Laboratorio de Espectroscopia, Instituto de Ciencias Físicas, Universidad Nacional Autónoma de México, Apartado Postal 48-3, 62251, Cuernavaca, Morelos (Mexico); Facultad de Ingeniería, Universidad Nacional Autónoma de México, México D.F. (Mexico)

    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.

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

    Science.gov (United States)

    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.

  7. Glow Discharge Emission Spectrometry (GDOES): Theoretical Introduction, General Aspects, and its Applications within the Framework of the Technofusion Programs; Glow Discharge Emission Spectrometry (GDOES): Introduccion Teorica, Aspectos Generales y Aplicabilidad en el Marco del Programa Technofusion

    Energy Technology Data Exchange (ETDEWEB)

    Martin-Rojo, A. B.; Gonzalez, M.; Tabares, F. L.

    2013-02-01

    The demand by material research groups for the direct composition analysis of solids is increasing as a solution to the time-consuming problems and errors inherent to classical chemical analysis, where the attack and solubilisation of the starting material is mandatory, often producing the introduction of impurities and component loss of the initial matrix. From the existing solid analysis techniques the present work is focused on the Glow Discharge Emission Spectrometry (GDOES), a fast, simply-executed technique, for which quantitative, high resolution depth profile determination of any element in the periodic table can be performed with a high sensibility and detection limit. The theoretical concepts, the required instrumentation and the basic analytic applications are revised, giving especial attention to the issues related to the analysis of materials for fusion applications. Finally, a comparative study with a more advanced spectroscopic technique (Secondary Ion Mass Spectrometry (SIMS)) is performed and the concomitance of both techniques to correct limitations such as the spatial resolution and the quantification of the analysis, important factors that are required in the chemical analysis of the complex materials used in Fusion, is addressed. (Author) 41 refs.

  8. INVESTIGATION OF IRON SPECIATION USING CAPILLARY ELECTROPHORESIS INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY%用毛细管电泳电感耦合等离子体原子发射光谱法分析铁的形态

    Institute of Scientific and Technical Information of China (English)

    邓必阳

    2003-01-01

    @@ During the last 20 years,metal speciation has attained great interest. The main reason for this is that the toxicity of an element and its biological role are critically dependent on the chemical form[1]. Especial ly,in recent years,various methods for the speciation of metal with different oxidation states have been introduced. Previous methods using different separation techniques such as gas chromatography (GC) and high performance liquid chromatography (HPLC) have been commonly used for element speciation.Consequently,capillary electrophoresis (CE) has shown considerable developments owing to its high separation efficiency,low sample and electrolyte consumption.

  9. 微波消解-等离子体发射光谱法测定果汁及其饮料中的钾和磷%Determination of potassium and phosphate in fruit juice and fruit juice drinks by inductively coupled plasma atomic emission spectrometry (ICP-OES)

    Institute of Scientific and Technical Information of China (English)

    孙丽萍

    2011-01-01

    采用微波消解——等离子体发射光谱法测定果汁及其饮料中的钾和磷,两种元素标准曲线线性关系良好,相关系数均在0.999以上,加标回收率在96%-108%之间,RSD值均低于5%。该方法适用于果汁及其饮料中钾和磷的测定。%Potassium and phosphate are simultaneously determined in fruit juice and fruit juice drinks by Microwave Digestion Method and ICP-OES. Standard curve linear relationship of two elements was very good. Correlation coefficients were above 0.999,and the recovery rate was from 96% to 108%. RSD values were less than 5% ,So the method is suitable to determine potassium and phosphorus in fruit juices and fruit juice drinks.

  10. Simultaneous Determination of Au, Cu, Ni and Fe in waste cyanide solution for Gold Plating by Inductively Coupled Plasma-Atomic Emission Spectrometry(ICP-AES)%ICP-AES同时测定废氰化镀金溶液中Au,Cu,Ni,Fe含量

    Institute of Scientific and Technical Information of China (English)

    彭义华

    2008-01-01

    为了快速测定废氰化镀金溶液中Au,Cu,Ni,Fe四种元素含量,采用一步消解直接进行ICP-AES测定.并对分析谱线、元素干扰和等离子体参数进行了讨论.结果表明,方法检出限为0.014~0.019μg/ml,加标回收率在97.3~101.0%之间,相对标准偏差(RSD)小于2.54%.该方法准确、快速、简便.应用于废氰化镀金溶液的回收生产,结果令人满意.

  11. Determination of Gold in Geological Samples by Inductively Coupled Plasma Atomic Emission Spectrometry with Flow-injection On-line Preconcentration%金的流动注射在线富集-电感耦合等离子体光谱法测定

    Institute of Scientific and Technical Information of China (English)

    曹淑琴; 陈杭亭; 刘杰; 曾宪津

    1999-01-01

    采用流动注射在线PVC尼龙6树脂微柱分离富集电感耦合等离子体光谱法测定地质样品中的痕量金2mL样品以流速1.85 mL/min上柱,2 g/L硫脲0.2 mL以相同速度反向洗脱,分析速度为每小时、10个样品.方法检出限(3σ)是0 002 mg/L.对Au含量是0.15 × 10-6的样品测定10次的相对标准偏差为10.6%.通过对地质标样和实际样品对照分析征明该法准确可靠.

  12. 电感耦合等离子体原子发射光谱法测定铋及氧化铋中5种杂质元素%Determination of five impurity elements in bismuth and bismuth oxide by inductively coupled plasma-atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    胡汉祥; 李立波

    2006-01-01

    研究了微波消解样品,电感耦合等离子体原子发射光谱(ICP-AES)法同时测定铋及氧化铋中Cu,Fe,Pb,Ni,Cr的新方法;详细地讨论仪器工作参数的优化和样品基体、共存离子以及待测元素间的干扰,确定实验的最佳测定条件.结果表明,方法的检出限为0.003~0.013μg/mL,回收率为95.1%~106.4%,RSD小于2.8%.该法已应用于铋和氧化铋中上述5种杂质元素的测定.

  13. Determination of seven elements in nickel-iron alloy by microwave digestion-inductively coupled plasma atomic emission spectrometry%微波消解-电感耦合等离子体原子发射光谱法测定镍铁合金中7种元素

    Institute of Scientific and Technical Information of China (English)

    荚江霞; 陆军; 陆尹

    2016-01-01

    使用王水并利用微波消解的方式处理样品,微波消解采用分步升温的方法,第1步升温5 min到120℃,维持6 min;第2步再升温5 min到180℃,并保持6 min.选择Si 251.612nm、Mn 293.930 nm、P 213.618 nm、Cr 206.149 nm、Cu 324.754 nm、Co 238.892 nm、Ni221.647 nm为分析线并设置合适的背景扣除位置,采用基体匹配法绘制校准曲线可消除基体效应的影响,利用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定硅、锰、磷、铬、铜、钴、镍,建立了镍铁合金中硅、锰、磷、铬、铜、钴、镍的测定方法.各待测元素校准曲线的线性相关系数均大于0.999 5;镍铁中各元素的检出限为0.000 9%~0.003%(质量分数).方法应用于镍铁合金标准样品JSS 760-3中硅、锰、磷、铬、铜、钴、镍的测定,结果与认定值相符,结果的相对标准偏差(RSD,n=10)为0.36%~5.2%.

  14. ICP-AES法测定红土镍矿中镍、钙、钛、锰、铜、钴、铬、锌与磷的含量%Determination of Ni, Ca, Ti, Mn, Cu, Co, Cr, Zn and P in laterite-nickel ores by inductively coupled plasma-atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    王艳君; 蒋晓光; 李卫刚; 王艳; 褚宁; 仲吉伟

    2012-01-01

    建立了ICP-AES法测定红土镍矿中Ni;Ca;Ti;Mn;Cu;Co;Cr;Zn 和P含量的方法.样品用HCl、HNO3溶解,加入HF和HCIO4,加热至HCIO4烟冒尽,用HCl溶解盐类,过滤,采用ICP-AES法同时测定滤液中Ni、Ca、Mn、Cu、Co、Zn、P;残渣经灼烧、挥硅、K2S2O7熔融、HCl浸取,所得溶液与滤液合并,测定溶液中Cr和Ti含量.方法检出限:P为0.022 μg/mL,其它元素在0.0032~0.0085 μg/mL之间,方法的精密度(n=7)在1.4%~2.9%之间.分析结果与分光光度法、XRF法和AAS法分析结果的相对误差:Ni、Cu、Co、Cr小于5%,Ti和Mn小于10%,Zn小于15%,Ca和P小于19%.%An ICP-AES method was established for the determination of nickel in nickel laterite ore, calcium, titanium, manganese, copper, cobalt, chromium, zinc and phosphorus contents. Samples were dissolved with hydrochloric acid and nitric acid, and then hydrofluoric acid and perchloric acid were added and heated till the smoke disappeared. The salt was dissolved in hydrochloric acid, followed by filtering, calcium, manganese, nickel, copper, cobalt, zinc, phosphorus in filter were simultaneously determined using ICP-AES method ; the residue was processed by burning, volatile silicon, potassium pyrosulfate fusion, hydrochloric acid leaching to obtain the solution, and chromium and titanium contents in the solution were determined. The detection limits of the method were 0. 022 g/mL for P and in range of 0. 0032 ~ 0. 0085 g/mL for other elements. The precisions of the method ( RSD, n=7) were in range of 1. 4% ~ 2. 9%. Compared with the results of spectrophotometric method, XRF method and A AS method, the relative errors of the results were less than 5% for nickel, copper, cobalt, chromium, less than 10% for manganese and titanium, less than 15% for Zinc and less than 19% for calcium and phosphorus.

  15. Determination of Copper, Nickel, Lead, Zinc and Cobalt in Copper-Nickel Ore and Lead- Zinc Ore by Inductively Coupled Plasma Atomic Emission Spectrometry%ICP-AES法测定铜镍矿、铅锌矿中铜、镍、铅、锌、钴

    Institute of Scientific and Technical Information of China (English)

    袁秀茹; 谈建安; 王建波; 毛振才

    2009-01-01

    用电感耦合等离子体发射光谱法测定铜镍矿、铅锌矿石中铜、镍、铅、锌、钴,样品用盐酸-硝酸溶解,在选定的测量条件下以ICP-AES测定溶液中的Cu、Pb、Zn、Co、Ni的含量.对国家一级标准物质进行测定,方法精密度(RSD,n=12)为Cu 2.92%~6.62%,Pb 1.88%~2.61%,Zn 1.30%~2.05%,Co 6.90%,Ni 2.23%.本方法具有线性范围宽、干扰少、快速、简便、检出限低等优点.用于实际使用,结果满意.

  16. Determination of Pt,Pd,Ir and Au in Ores by Inductively Coupled Plasma Atomic Emission Spectrometry after Preconcentration by Minified Nickel Sulfide Fire Assay%硫化镍试金预富集-ICP-AES测定矿石中的Pt、Pd、Ir、Au

    Institute of Scientific and Technical Information of China (English)

    刘小荣; 董守安; 冯忠; 陈丁文

    2003-01-01

    The effect of various factors on the determination o f Pt,Pd,Ir and Au by ICP-AES was investigated in detail using minified nickel su lfide fire assay preconcentration.The results indicated that after the nickel su lfide bead was dissolved in HCl,filtering the solution by fritted glass crucible and dissolving the residue with HCl+H2O2 were a comparatively ideal analyti cal scheme.During the bead dissolving the losses of Pt and Pd were negligible,th e loss of Au was quite high,and the determination of Au was only semiqantitative .The average recoveries for Pt,Pd and Ir ranged from 96% to 99% for the determin ation of μg/g level,the relative standard derivation(RSD) was 1.7 %~6.8%(n=5).The proposed procedure has been applied to analyse o f ores and concentrates.%详细研究了硫化镍试金预富集-ICP-AES测定矿石中的P t、Pd、Ir、Au的多种影响因素.结果表明硫化镍扣用盐酸溶解,多孔玻砂坩埚过滤溶液, 盐酸和双氧水溶解残渣是比较理想的分析方案.硫化镍扣溶解过程中,Pt、Pd的损失可忽略 .Au的损失相当高,仅能半定量.对于μg/g级的样品,Pt、Pd、Ir、Au的平均回收率在96% ~99%之间,相对标准偏差为1.7%~6.8%(n=5).拟定的方法已用于矿石、精矿的分析.

  17. ICP-AES法同时测定镍矿中8种杂质元素的含量%DETERMINATION OF Cd、Cr、Cu、Pb、Sn、Bi、Co AND Zn IN NICKEL ORES BY INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY

    Institute of Scientific and Technical Information of China (English)

    黄健; 曲强; 陈广文; 洪武兴; 朱燕

    2008-01-01

    用电感耦合等离子体原子发射光谱仪测定镍矿中的镉、铬、铜、铅、锡、铋、钴和锌.样品用盐酸溶解,氢氟酸助溶,高氯酸冒烟除去氢氟酸,用盐酸溶解盐类后,在选定的测量条件下以ICP-AES测定溶液中的镉、铬、铜、铅、锡、铋、钴和锌的浓度.本法测定范围为0.002%~0.3%,回收率在96.90%~101.35%之间,相对标准偏差0.34%~1.78%(n=8).

  18. Determination of Ni, Co, Mg, Al and Fe in Laterite Nickel Ore by Inductively Coupled Plasma-Atomic Emission Spectrometry%电感耦合等离子体发射光谱法测定红土镍矿中镍钴镁铝铁

    Institute of Scientific and Technical Information of China (English)

    刘久苗

    2013-01-01

    红土镍矿分析没有统一的国家标准,行业标准于2013年初刚制定,其应用处于起步阶段,且行业标准中红土镍矿各元素主要采用化学分析法测定,操作程序繁琐耗时,工作量大,分析效率低.本文建立了电感耦合等离子体发射光谱测定红土镍矿中镍、钴、镁、铝和铁含量的方法.红土镍矿样采用王水溶解,加入氢氟酸和高氯酸,加热至高氯酸烟冒尽,再用盐酸溶解盐类,对消解后溶液中镍、钴、镁、铝和铁等目标元素选择了合适的分析谱线消除干扰.方法检出限镍为2.98 μg/g,钴为1.60μg/g,镁为1.68 μg/g,铝为3.79 μg/g,铁为9.52 μg/g;方法精密度(RSD,n=l1)为1.5%~2.2%;加标回收率为96.0% ~ 102.5%.国家标准物质分析的测定值与标准值和外检值吻合较好.该方法简便快速,单元素不需分别处理,提高了分析效率,能够满足红土镍矿冶炼生产和地质探矿样品测定及时性的要求.

  19. Determination of Trace Impurities in High Purity Metal Tin by Ultrasonic Nebulization Inductively Coupled Plasma-Atomic Emission Spectrometry%超声雾化电感耦合等离子体原子发射光谱法测定高纯锡锭中痕量杂质元素

    Institute of Scientific and Technical Information of China (English)

    周世萍; 朱光辉; 尹家元; 胡秋芬; 王光灿

    2002-01-01

    建立了高纯锡锭中砷、锑、镉等12种痕量杂质元素的超声雾化-ICP-AES测定方法.考察了基体对杂质元素的干扰影响.采用HCl+H2O2 沸水浴蒸干排Sn处理,使样品中90%的Sn基体挥发与待测元素分离消除基体干扰.方法快速、准确,具有比气动雾化更低的检出限,回收率为88%~103%,RSD均小于5%.

  20. ICP-AES法测定氧化铝粉中硅、钙、铁、钛、钒和锌%Determination of Silica, Iron, Calcium, Titanium, Vanadium and Zinc Content in Aluminium Oxide by Inductively Coupled Plasma Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    王艳君; 蒋晓光

    2002-01-01

    采用高压盐酸消化,电感耦合等离子发射光谱法测定氧化铝中硅、铁、钙、钛、钒和锌等6元素,研究了铝基体对被测元素的影响,并选择了最佳工作条件.被测元素的检出限为0.34~52 ng/mL,样品加标回收率为95.7%~108.6%.

  1. 电感耦合等离子体发射光谱法(ICP-AES)测定食品添加剂磷酸二氢铵中砷和铅%Determination of Arsenic and Lead in Food Additives Ammonium Dihydrogen Phosphate by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

    Institute of Scientific and Technical Information of China (English)

    王娜; 张敏; 刘鹏; 神兴明

    2013-01-01

    采用电感耦合等离子体原子发射光谱法(ICP-AES)对食品添加剂磷酸二氢铵中砷和重金属铅进行分析.实验过程确定了最佳测量条件,采用标准曲线法为定量依据,样品的加标回收率为98.12%~99.54%,相对标准偏差(RSD)为0.33%~1.2%,检出限为0.010 76~0.035 05 mg/L,实验结果表明方法具有简单、快速、重现性好等优点.

  2. ICP-AES法测定钴基合金及钴基钎料中La,Ce,Pr,Nd,Gd元素含量%Determination of La,Ce,Pr,Nd,Gd in Co-Based Filler Metals and Co-Based Alloy by Inductively Coupled Plasma Atomic Emission Spectrometry

    Institute of Scientific and Technical Information of China (English)

    高颂; 庞晓辉; 房丽娜; 张艳

    2011-01-01

    研究了钴基合金及钴基钎料样品溶解方法,采用盐酸、硝酸、氢氟酸溶解样品;选择待测元素灵敏度高、光谱干扰少的谱线为分析线,校准曲线溶液采用基体匹配消除了基体效应影响,实现了用电感耦合等离子体原子发射光谱法测定钴基合金及钴基钎料中La,Ce,Pr,Nd,Cd元素含量.并行了加入回收实验,回收率95%~110%,相对标准偏差小于4.86%.%A method for determination of La,Ce,Pr,Nd,Gd elements in Co-Based Filler Metals and Co-Based alloy by ICP-AES was proposed. The experiment of instrument parameters, sample dissolution, selection of analysis lines, the effect of matrix and coexist elements on the determination and the analysis results were carried out. The recovery rate is from 95% to 110% , the RSD are less than 4.86%.

  3. Study of mineral and essential trace elements in milk and dairy products by inductively coupled plasma atomic emission spectrometry and neutron activation analysis; Estudo da composicao mineral e dos elementos-traco essenciais em amostras de leite e produtos lacteos por espectrometria de emissao atomica com plasma induzido e analise por ativacao com neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Kira, Carmen Silvia

    2002-07-01

    The importance of food composition related to nutritional and toxicological contents has been emphasized in recent years. Some chemical elements are needed for cell metabolism, while excess or deficiency may be responsible for disorders. Milk is considered the most important food during the first months of life, nutritional needs of children being satisfied by milk and dairy products. These foods provide the main trace elements for the good growth of different tissues as well as the functioning of several enzymatic systems. Important deficiencies in mineral during this period can interfere with children's development. Determination of mineral and trace elements by using spectroscopic techniques generally involves a pretreatment of sample. Sample preparation is the most critical part of the analysis because of the long preparation time and the possibilities for contamination and losses of the analyte associated with this step. Different procedures of sample preparation (dry ashing digestion, wet digestion using an open focused microwave and a hot plate) were evaluated for determining Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P and Zn in milk and dairy products by the ICP OES technique. In this work the concentrations obtained for the elements determined by the ICP OES technique after using the different treatments of sample were compared to the results obtained by the INAA technique, that does not require dissolution of sample. The partial digestion with diluted hydrochloric acid was found to be suitable for determining Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P and Zn in milk samples and dairy products. (author)

  4. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part I. Theoretical considerations

    Energy Technology Data Exchange (ETDEWEB)

    Leclercq, Amélie, E-mail: amelie.leclercq@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Nonell, Anthony, E-mail: anthony.nonell@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Todolí Torró, José Luis, E-mail: jose.todoli@ua.es [Universidad de Alicante, Departamento de Quimica Analitica, Nutricion y Bromatología, Ap. de Correos, 99, 03080 Alicante (Spain); Bresson, Carole, E-mail: carole.bresson@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vio, Laurent, E-mail: laurent.vio@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vercouter, Thomas, E-mail: thomas.vercouter@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Chartier, Frédéric, E-mail: frederic.chartier@cea.fr [CEA Saclay, DEN, DANS, DPC, 91191 Gif-sur-Yvette (France)

    2015-07-23

    Highlights: • Tutorial review addressed to beginners or more experienced analysts. • Theoretical background of effects caused by organic matrices on ICP techniques. • Spatial distribution of carbon species and analytes in plasma. • Carbon spectroscopic and non-spectroscopic interferences in ICP. - Abstract: Due to their outstanding analytical performances, inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are widely used for multi-elemental measurements and also for isotopic characterization in the case of ICP-MS. While most studies are carried out in aqueous matrices, applications involving organic/hydro-organic matrices become increasingly widespread. This kind of matrices is introduced in ICP based instruments when classical “matrix removal” approaches such as acid digestion or extraction procedures cannot be implemented. Due to the physico-chemical properties of organic/hydro-organic matrices and their associated effects on instrumentation and analytical performances, their introduction into ICP sources is particularly challenging and has become a full topic. In this framework, numerous theoretical and phenomenological studies of these effects have been performed in the past, mainly by ICP-OES, while recent literature is more focused on applications and associated instrumental developments. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP-OES and ICP-MS. The present Part I, provides theoretical considerations in connection with the physico-chemical properties of organic/hydro-organic matrices, in order to better understand the induced phenomena. This focal point is divided in four chapters highlighting: (i) the impact of organic/hydro-organic matrices from aerosol generation to atomization/excitation/ionization processes; (ii) the production of carbon molecular constituents and their spatial distribution in the

  5. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part II. Practical considerations

    Energy Technology Data Exchange (ETDEWEB)

    Leclercq, Amélie, E-mail: amelie.leclercq@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Nonell, Anthony, E-mail: anthony.nonell@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Todolí Torró, José Luis, E-mail: jose.todoli@ua.es [Universidad de Alicante, Departamento de Quimica Analitica, Nutricion y Bromatología, Ap. de Correos, 99, 03080 Alicante (Spain); Bresson, Carole, E-mail: carole.bresson@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vio, Laurent, E-mail: laurent.vio@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vercouter, Thomas, E-mail: thomas.vercouter@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Chartier, Frédéric, E-mail: frederic.chartier@cea.fr [CEA Saclay, DEN, DANS, DPC, 91191 Gif-sur-Yvette (France)

    2015-07-23

    Graphical abstract: This tutorial review is dedicated to the analysis of organic/hydro-organic matrices by ICP techniques. A state-of-the-art focusing on sample introduction, relevant operating parameters optimization and analytical strategies for elemental quantification is provided. - Highlights: • Practical considerations to perform analyses in organic/hydro-organic matrices. • Description, benefits and drawbacks of recent introduction devices. • Optimization to improve plasma tolerance towards organic/hydro-organic matrices. • Analytical strategies for elemental quantification in organic/hydro-organic matrices. - Abstract: Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review

  6. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: a tutorial review. Part I. Theoretical considerations.

    Science.gov (United States)

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

    2015-07-23

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

  7. Online Determination of Sm, Eu and Yb in Environmental Samples by Inductively Coupled Plasma – Optical Emission Spectrometry

    Directory of Open Access Journals (Sweden)

    J. Dilip Kumar

    2007-01-01

    Full Text Available A procedure was developed for the determination of Sm, Eu and Yb in water samples by inductively coupled plasma-optical emission spectrometry (ICP-OES after preconcentration on synthesized 5-(4-pyridyl azo-8-quinolinol supported by Borassus flabellifer inflorescence (BFI. The sorbed element was subsequently eluted with 0.4 M HNO3 and the acid eluates were analyzed by ICP-OES. Under the optimal conditions, Sm, Eu and Yb in aqueous samples were concentrated 100-fold. Recoveries were obtained by the proposed method in the range of 98.6 -99.8%. This method was also applied for the analysis of spiked and natural water samples. The results provide strong evidence to support the hypothesis of an adsorption mechanism.

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

    Energy Technology Data Exchange (ETDEWEB)

    Menezes, E.A.; Carapelli, R.; Bianchi, S.R. [Grupo de Analise Instrumental Aplicada, Departamento de Quimica, Universidade Federal de Sao Carlos, Sao Carlos, SP (Brazil); Embrapa Pecuaria Sudeste, C.P. 339, Sao Carlos, SP 13560-970 (Brazil); Souza, S.N.P. [Grupo de Analise Instrumental Aplicada, Departamento de Quimica, Universidade Federal de Sao Carlos, Sao Carlos, SP (Brazil); Matos, W.O. [Departamento de Quimica Analitica e Fisico-Quimica, Universidade Federal do Ceara, Fortaleza, CE (Brazil); Pereira-Filho, E.R. [Grupo de Analise Instrumental Aplicada, Departamento de Quimica, Universidade Federal de Sao Carlos, Sao Carlos, SP (Brazil); Nogueira, A.R.A., E-mail: anarita@cppse.embrapa.br [Embrapa Pecuaria Sudeste, C.P. 339, Sao Carlos, SP 13560-970 (Brazil)

    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{sup -1} for Ca and from 0.3 to 7.0 mg kg{sup -1} for all other analytes through the microwave-assisted decomposition procedure.

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

    Science.gov (United States)

    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.

  10. Liquid electrode plasma-optical emission spectrometry combined with solid-phase preconcentration for on-site analysis of lead.

    Science.gov (United States)

    Barua, Suman; Rahman, Ismail M M; Alam, Iftakharul; Miyaguchi, Maho; Sawai, Hikaru; Maki, Teruya; Hasegawa, Hiroshi

    2017-08-15

    A relatively rapid and precise method is presented for the determination of lead in aqueous matrix. The method consists of analyte quantitation using the liquid electrode plasma-optical emission spectrometry (LEP-OES) coupled with selective separation/preconcentration by solid-phase extraction (SPE). The impact of operating variables on the retention of lead in SPEs such as pH, flow rate of the sample solution; type, volume, flow rate of the eluent; and matrix effects were investigated. Selective SPE-separation/preconcentration minimized the interfering effect due to manganese in solution and limitations in lead-detection in low-concentration samples by LEP-OES. The LEP-OES operating parameters such as the electrical conductivity of sample solution; applied voltage; on-time, off-time, pulse count for applied voltage; number of measurements; and matrix effects have also been optimized to obtain a distinct peak for the lead at λmax=405.8nm. The limit of detection (3σ) and the limit of quantification (10σ) for lead determination using the technique were found as 1.9 and 6.5ng mL(-1), respectively. The precision, as relative standard deviation, was lower than 5% at 0.1μg mL(-1) Pb, and the preconcentration factor was found to be 187. The proposed method was applied to the analysis of lead contents in the natural aqueous matrix (recovery rate:>95%). The method accuracy was verified using certified reference material of wastewaters: SPS-WW1 and ERM-CA713. The results from LEP-OES were in good agreement with inductively coupled plasma optical emission spectrometry measurements of the same samples. The application of the method is rapid (≤5min, without preconcentration) with a reliable detection limit at trace levels. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Montaser, A.

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Dancsak, Stacia E. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Silva, Sidnei G.; Nóbrega, Joaquim A. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, São Carlos, SP (Brazil); Jones, Bradley T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Donati, George L., E-mail: georgedonati@yahoo.com.br [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States)

    2014-01-02

    Graphical abstract: -- Highlights: •Direct analysis of biodiesel on a tungsten coil atomizer. •Determination of Na, K, Cr and V by tungsten coil atomic emission spectrometry. •Sample dilution with methanol or ethanol. •Ten-microliter sample aliquots and limits of detection between 20 and 90 μg kg{sup −1}. •Low consumption of reagents, samples and gases in a 140 s per run procedure. -- Abstract: 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{sup −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{sup −1} for Na and K, and between 0.22 and 0.43 mg kg{sup −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

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

    Science.gov (United States)

    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.

  17. Potential of Solid Sampling Electrothermal Vaporization for solving spectral interference in Inductively Coupled Plasma Optical Emission Spectrometry

    Science.gov (United States)

    Asfaw, Alemayehu; Wibetoe, Grethe

    2009-05-01

    Spectral interference is one of the main causes of erroneous results in Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). This paper describes some cases of spectral interferences with conventional nebulization ICP-OES and the potential of solving them utilizing electrothermal vaporization for volatility-based separation. The cases studied were, the well-known spectral overlap between the As and Cd lines at 228.8 nm that are only 10 pm apart, and the interference of Fe on the main emission lines of As, Cd and Pb. The spectral interferences were studied by monitoring the typical signals of solutions that contain the analytes and the potential interferent, by studying the spectra and calculating Background Equivalent Concentration (BEC)-values. A three step temperature program was developed to be used for direct analysis of solid soil samples by Electrothermal Vaporization (ETV)-ICP-OES: step 1 (760 °C, 40 s), step 2 (1620 °C, 20 s) and a cleaning step (2250 °C, 10 s) where Cd vaporizes in step 1, As, Pb and part of Fe in step 2 and the major part of Fe in the cleaning step. Because As and Cd were time-separated using this program, their prominent lines at 228.8 nm, could be used for determination of each element by ETV-ICP-OES, in spite of the serious wavelength overlap. Selective vaporization was also shown to reduce or eliminate the Fe background emission on As, Cd and Pb lines. To confirm the applicability of the method, a solid soil certified reference materials was analyzed directly without any sample treatment. Good or reasonable accuracy was obtained for the three elements.

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

    Energy Technology Data Exchange (ETDEWEB)

    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)

  19. Chemical Characterisation of Bulk and Melt-spun Ribbons of NiMnIn Alloy using Inductively Coupled Plasma Optical Emission Spectrometry

    Directory of Open Access Journals (Sweden)

    S.S. Kalyan Kamal

    2011-05-01

    Full Text Available Method development for the analysis of NiMnIn, a new magnetocaloric effect (MCE material using inductively-coupled plasma optical emission spectrometry (ICPOES is discussed. Spectral interference of Ni and Mn on the analysis of In were studied. The process of method validation was carried out using various analytical techniques like conventional wet chemical techniques and instrumental techniques such as atomic absorption spectrometry. All the techniques show a close agreement in values, thus this method could be applied for regular analysis of NiMnIn alloys. A comparative chemical analysis of bulk and melt-spun ribbons of this alloy is also discussed.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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).

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

    Science.gov (United States)

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

    2014-01-02

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Frentiu, Tiberiu, E-mail: ftibi@chem.ubbcluj.ro [Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca (Romania); Mihaltan, Alin I., E-mail: alinblaj2005@yahoo.com [National Institute for Research and Development of Optoelectronics Bucharest - Research Institute for Analytical Instrumentation, Donath 67, 400293 Cluj-Napoca (Romania); Ponta, Michaela, E-mail: mponta@chem.ubbcluj.ro [Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca (Romania); Darvasi, Eugen, E-mail: edarvasi@chem.ubbcluj.ro [Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca (Romania); Frentiu, Maria, E-mail: frentiu.maria@yahoo.com [National Institute for Research and Development of Optoelectronics Bucharest - Research Institute for Analytical Instrumentation, Donath 67, 400293 Cluj-Napoca (Romania); Cordos, Emil, E-mail: emilcordos@gmail.com [National Institute for Research and Development of Optoelectronics Bucharest - Research Institute for Analytical Instrumentation, Donath 67, 400293 Cluj-Napoca (Romania)

    2011-10-15

    Highlights: {yields} Use of a miniaturized analytical system with microtorch plasma for Hg determination. {yields} Determination of Hg in non- and biodegradable materials using cold vapor generation. {yields} Figures of merit and advantages of the miniaturized system for Hg determination. - Abstract: A new analytical system consisting of a low power capacitively coupled plasma microtorch (20 W, 13.56 MHz, 150 ml min{sup -1} Ar) and a microspectrometer was investigated for the Hg determination in non- and biodegradable materials by cold-vapor generation, using SnCl{sub 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{sub 3}-H{sub 2}SO{sub 4} mixture in a high-pressure microwave system. The detection limits of 0.05 ng ml{sup -1} or 0.08 {mu}g g{sup -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{sup -1}, while recovery in two polyethylene certified reference materials in the range 98.7 {+-} 4.5% (95% confidence level).

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

    Science.gov (United States)

    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).

  5. Rf glow discharge optical emission spectrometry for the analysis of arrays of Ni nanowires in nanoporous alumina and titania membranes

    Energy Technology Data Exchange (ETDEWEB)

    Prida, V.M.; Bordel, N.; Hernando, B. [Depto. Fisica, Universidad Oviedo, Calvo Sotelo s/n, 33007 Oviedo (Spain); Navas, D.; Pirota, K.R.; Vazquez, M. [Instituto de Ciencia de Materiales de Madrid (CSIC), Cantoblanco, 28049 Madrid (Spain); Hernandez-Velez, M. [Instituto de Ciencia de Materiales de Madrid (CSIC), Cantoblanco, 28049 Madrid (Spain); Depto. Fisica Aplicada, C-XII, Universidad Autonoma Madrid, Cantoblanco, 28049 Madrid (Spain); Menendez, A.; Pereiro, R.; Sanz-Medel, A. [Depto. Quimica Fisica y Analitica, Facultad de Quimica, Julian Claveria 8, 33006 Oviedo (Spain)

    2006-05-15

    Anodic alumina (Al{sub 2}O{sub 3}) and titania (TiO{sub 2}) nanoporous oxide membranes are among the most widely studied self-organized nanopore templates, formed by uniform and well aligned arrays of synthetized nanometric pores or tubes. Here, we perform a comparative study of the depth profiling analysis in self-ordered alumina and titania nanoporous membrane templates by means of the radiofrequency glow discharge coupled to optical emission spectrometry (rf-GD-OES) technique. The densely packed columnar arrays of hexagonally self-ordered nanoporous alumina membranes investigated, with an average inner pore diameter of 35 nm and 105 nm interspacing, give an uniform thickness pore length about more than 5 {mu}m, depending on the anodization time. Meanwhile, the analysis of the anodized titania nanotubes, with an average inner pore diameter of 100 nm and 40 nm wall thickness, shown to be about 300 nm in length. Each type of membranes were also studied in both cases, when the nanopores were empty and after filling with electrodeposited Ni. The direct analysis by rf-GD-OES reveals the ability of this technique to control the quality of these so synthesized nanocomposites formed by electrodeposited Ni nanowires into the alumina and titania nanoporous templates. (copyright 2006 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  6. Rf glow discharge optical emission spectrometry for the analysis of arrays of Ni nanowires in nanoporous alumina and titania membranes

    Science.gov (United States)

    Prida, V. M.; Navas, D.; Pirota, K. R.; Hernandez-Velez, M.; Menéndez, A.; Bordel, N.; Pereiro, R.; Sanz-Medel, A.; Hernando, B.; Vazquez, M.

    2006-05-01

    Anodic alumina (Al2O3) and titania (TiO2) nanoporous oxide membranes are among the most widely studied self-organized nanopore templates, formed by uniform and well aligned arrays of synthetized nanometric pores or tubes. Here, we perform a comparative study of the depth profiling analysis in self-ordered alumina and titania nanoporous membrane templates by means of the radiofrequency glow discharge coupled to optical emission spectrometry (rf-GD-OES) technique. The densely packed columnar arrays of hexagonally self-ordered nanoporous alumina membranes investigated, with an average inner pore diameter of 35 nm and 105 nm interspacing, give an uniform thickness pore length about more than 5 μm, depending on the anodization time. Meanwhile, the analysis of the anodized titania nanotubes, with an average inner pore diameter of 100 nm and 40 nm wall thickness, shown to be about 300 nm in length. Each type of membranes were also studied in both cases, when the nanopores were empty and after filling with electrodeposited Ni. The direct analysis by rf-GD-OES reveals the ability of this technique to control the quality of these so synthesized nanocomposites formed by electrodeposited Ni nanowires into the alumina and titania nanoporous templates.

  7. On-line system for preconcentration and determination of metals in vegetables by Inductively Coupled Plasma Optical Emission Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bezerra, Marcos A. [Universidade Federal da Bahia, Instituto de Quimica, Grupo de Pesquisa em Quimica Analitica, Campus Universitario de Ondina, Salvador, Bahia 40170-290 (Brazil); Universidade Estadual do Sudoeste da Bahia, Laboratorio de Quimica Analitica, Campus de Jequie, Jequie, Bahia 45206-190 (Brazil); Santos, Walter N.L. dos [Departamento de Ciencias Exatas e da Terra, Universidade do Estado da Bahia, R. Silveira Martins, 2555, Salvador, Bahia 41195-001 (Brazil); Lemos, Valfredo A. [Universidade Estadual do Sudoeste da Bahia, Laboratorio de Quimica Analitica, Campus de Jequie, Jequie, Bahia 45206-190 (Brazil)], E-mail: vlemos@uesb.br; Korn, Maria das Gracas A.; Ferreira, Sergio L.C. [Universidade Federal da Bahia, Instituto de Quimica, Grupo de Pesquisa em Quimica Analitica, Campus Universitario de Ondina, Salvador, Bahia 40170-290 (Brazil)

    2007-09-05

    A procedure has been developed for the simultaneous determination of trace amounts of cadmium, copper, chromium, nickel and lead in digested vegetable samples. The method involves solid-phase extraction of the metals using a minicolumn of Amberlite XAD-4 modified with dihydroxybenzoic acid (DHB) and detection by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The elution of the metals from minicolumn was performed with 1.0 mol L{sup -1} hydrochloric acid. Variables associated with flow preconcentration system performance, such as pH, buffer concentration, eluent concentration and sampling flow rate, were optimized. The developed procedure provides enrichment factors of 100, 72, 16, 91 and 53, for cadmium, copper, chromium, nickel and lead, respectively. Detection limits (3{sigma}{sub B}) were 0.02 (Cd), 0.23 (Cu), 0.58 (Cr), 0.060 (Ni) and 0.54 (Pb) {mu}g L{sup -1}. The procedure was applied for determination of metals in samples of guarana and cabbage. The accuracy of the method was checked by the analysis of a certified reference material (NIST 1571, Orchard leaves). Results found were in agreement with certified values.

  8. Possibilities of High Resolution Inductively Coupled Plasma Optical Emission Spectrometry in the Determination of Trace Elements in Environmental Materials

    Directory of Open Access Journals (Sweden)

    Nikolaya Velitchkova

    2013-01-01

    Full Text Available This paper presents new quantitative data for the spectral interferences obtained by high resolution 40.68 MHz radial viewing inductively coupled plasma optical emission spectrometry (HR-ICP-OES in the determination of Zn, Cd, Sb, Cu, Mn, Pb, Sn, Cr, U, and Ba in environmental materials in the presence of a complex matrix, containing Al, Ca, Fe, Mg, and Ti. The -concept for quantification of spectral interferences was used. The optimum line selection for trace analysis of a variety of multicomponent matrices requires the choice of prominent lines, which are free or negligibly influenced by line interference problems. The versatility of -concept as basic methodology was experimentally demonstrated in the determination of trace of elements in soil and drinking water. The detection limits are lower in comparison with corresponding threshold concentration levels for soil and drinking water in accordance with environmental regulations. This paper shows the possibilities of present day ICP-OES equipment in the direct determination of trace elements (without preconcentration of impurities in environmental samples.

  9. Solid-Sampling Electrothermal Vaporization Inductively Coupled Plasma Optical Emission Spectrometry for Direct Determination of Total Oxygen in Coal.

    Science.gov (United States)

    Vogt, Thomas; Bauer, Daniela; Nennstiel, David; Otto, Matthias

    2015-10-20

    A new analytical method for direct determination of total oxygen contents in eight coal samples of the Argonne Premium Coal (APC) series and in the NIST SRM 1632d is presented. The development of a suitable calibration procedure, optimization of measurement conditions, and the application of a tailored data processing for handling of plasma effects and high blanks enable the quantification of oxygen simultaneously with other trace, minor, or major elements in whole coal samples by means of electrothermal vaporization inductively coupled plasma optical emission spectrometry (ETV-ICP OES). For comparison, the oxygen contents were determined by a direct oxygen analyzer. The obtained oxygen values of the APC and the reference material NIST SRM 1632d were compared to data in the literature. The precision of the ETV-ICP OES was within ±3.5%, and the recovery better than 92%. With this good accuracy, the developed direct solid sampling method ETV-ICP OES is well suited for the fast determination of oxygen in coals, varying in rank from lignite to semianthracite, in a content range of about 100 ppm up to 27% using 1.5 mg sample weight. This direct analysis method represents an accurate, advantageous alternative to currently used methods for estimation of total oxygen contents in coals.

  10. Direct determination of impurities in high purity silicon carbide by inductively coupled plasma optical emission spectrometry using slurry nebulization technique.

    Science.gov (United States)

    Wang, Zheng; Qiu, Deren; Ni, Zheming; Tao, Guangyi; Yang, Pengyuan

    2006-09-08

    A novel method for the determination of Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni and Ti in high purity silicon carbide (SiC) using slurry introduction axial viewed inductively coupled plasma optical emission spectrometry (ICP-OES) was described. The various sizes of SiC slurry were dispersed by adding dispersant polyethylene imine (PEI). The stability of slurry was characterized by zeta potential measurement, SEM observation and signal stability testing. The optimal concentration of PEI was found to be 0.5 wt% for the SiC slurry. Analytical results of sub-mum size SiC by the slurry introduction were in good accordance with those by the alkaline fusion method which verified that determination could be calibrated by aqueous standards. For mum size SiC, results of most elements have a negative deviation and should be calibrated by the Certified Reference Material slurry. Owing to a rather low contamination in the sample preparation and stability of the slurry, the limits of detection (LODs), which are in the range of 40-2000 ng g(-1), superior to those of the conventional nebulization technique by ICP-OES or ICP-MS.

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

    Energy Technology Data Exchange (ETDEWEB)

    Tyburska, Anna; Jankowski, Krzysztof, E-mail: kj@ch.pw.edu.pl; Rodzik, Agnieszka

    2011-07-15

    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{sup -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.

  12. Aerosol generation of As and Se hydrides using a new Flow Blurring® multiple nebulizer for sample introduction in inductively coupled plasma optical emission spectrometry

    OpenAIRE

    Pereira, Catarinie D.; Aguirre Pastor, Miguel Ángel; NÓBREGA, Joaquim A.; Hidalgo Núñez, Montserrat; Canals Hernández, Antonio

    2014-01-01

    A new Flow Blurring® multiple nebulizer (FBMN) has been used for the efficient generation of As and Se hydrides directly into the aerosol formed inside the spray chamber before detection by inductively coupled plasma optical emission spectrometry (ICP OES). The FBMN allowed the hydride generation directly into the spray chamber without using any additional device either for solution and gas control or for gas phase separation. Synthetic solutions containing As and Se plus Ca, Mg and K were us...

  13. The determination of trace element concentrations in fly ash samples using ultrasound-assisted digestion followed with inductively coupled plasma optical emission spectrometry

    OpenAIRE

    Ilander, Aki; Väisänen, Ari

    2009-01-01

    A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of trace element (chromium, copper, lead, nickel, vanadium and zinc) concentrations in fly ash samples was developed. All the measurements were performed in robust plasma conditions. Ultrasound-assisted digestion procedures using digestion solutions of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 80% for all the analyte...

  14. An ultrasound-assisted digestion method for the determination of toxic element concentrations in ash samples by inductively coupled plasma optical emission spectrometry

    OpenAIRE

    Ilander, Aki; Väisänen, Ari

    2007-01-01

    method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of toxic element concentrations (arsenic, barium, cobalt, copper, lead, nickel, strontium, vanadium and zinc) in ash samples was developed. All the measurements were performed in robust plasma conditions which were tested by measuring the Mg(II) 280.270 nm/Mg(I) 285.213 nm line intensity ratios. The highest line intensity ratios were observed when a...

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

    Energy Technology Data Exchange (ETDEWEB)

    Gomes, Marcos S. [Departamento de Química, Universidade Federal de São Carlos, Rod. Washington Luís, km 235, 13565-905 São Carlos, SP (Brazil); Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Av. Centenário 303, 13416-000 Piracicaba, SP (Brazil); Schenk, Emily R. [Department of Chemistry and Biochemistry, Florida International University, Miami, FL (United States); International Forensic Research Institute, Florida International University, Miami, FL (United States); Santos, Dário [Departamento de Ciências Exatas e da Terra, Universidade Federal de São Paulo, Rua Professor Arthur Riedel 275, Diadema, SP (Brazil); Krug, Francisco José [Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Av. Centenário 303, 13416-000 Piracicaba, SP (Brazil); Almirall, José R., E-mail: almirall@fiu.edu [Department of Chemistry and Biochemistry, Florida International University, Miami, FL (United States); International Forensic Research Institute, Florida International University, Miami, FL (United States)

    2014-04-01

    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{sup −1} for Zn to as high as 94 mg kg{sup −1} for K but were generally below 6 mg kg{sup −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. - Highlights: • An evaluation of LA-ICP-OES for the direct analysis of pelleted plant material is reported. • Orange citrus, soy and sugarcane plants were pressed into pellets and sampled directly. • The element menu consisted of Ca, Mg, P, K, Fe, Mn, Zn and B. • LODs for the method ranged from 0.1 mg kg{sup −1} for Zn to 94 mg kg{sup −1} for K. • The precision ranged from 4% RSD for Mn to 17% RSD for Zn (∼ 6.5% RSD average)

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

    Science.gov (United States)

    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 (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 (incense by approximately 50%.

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

    Energy Technology Data Exchange (ETDEWEB)

    Matos, Wladiana O. [Grupo de Analise Instrumental Aplicada, Universidade Federal de Sao Carlos, Sao Carlos SP (Brazil); Grupo de Analise Instrumental Aplicada, Embrapa Pecuaria Sudeste, Sao Carlos, SP (Brazil)], E-mail: wladianamatos@yahoo.com.br; Menezes, Eveline A. [Grupo de Analise Instrumental Aplicada, Universidade Federal de Sao Carlos, Sao Carlos SP (Brazil); Grupo de Analise Instrumental Aplicada, Embrapa Pecuaria Sudeste, Sao Carlos, SP (Brazil); Gonzalez, Mario H. [Grupo de Analise Instrumental Aplicada, Universidade Federal de Sao Carlos, Sao Carlos SP (Brazil); Costa, Leticia M. [Departamento de Quimica-ICEx, Universidade Federal de Minas Gerais, Belo Horizonte MG (Brazil); Trevizan, Lilian C. [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Piracicaba SP (Brazil); Nogueira, Ana Rita A. [Grupo de Analise Instrumental Aplicada, Embrapa Pecuaria Sudeste, Sao Carlos, SP (Brazil)

    2009-06-15

    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 {mu}L. 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{sup 4-1} fractional factorial design: 650 W microwave power, 7 min digestion time, 50 {mu}L 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.

  18. Inductively Coupled Plasma(ICP) Mass Spectrometry(MS) Hyphenated with Atomic Emission Spectrometry(AES) for Simultaneous Determination of Major, Minor and Micro Amounts of Elements in Geochemical Samples

    Institute of Scientific and Technical Information of China (English)

    HUANG Zhen-yu; ZHANG Qin; HU Ke; WU Jian-ling; YANG Peng-yuan

    2005-01-01

    @@ Introduction Geological resource survey demands for determining various constituents including major, minor, micro, trace and ultra-trace levels of elements for preparing the map of resource distribution of our country. As a powerful and popularly used technique for multi-element analysis, inductively coupled plasma(ICP) atomic emission spectrometry (AES) has been applied to this field for a period of time[1-3]. However, ICP spectrometric determination of those micro, trace and ultratrace elements needs enrichment procedures for improving the detection limit, which is unacceptable in case a great mass of samples should be analyzed as that in the task of geological resource survey. On the other hand, although ICP mass spectrometry(MS) is considered the most powerful method for trace elements determination[4,5], it is difficult for ICP-MS to be used to determine the trace and major analytes simultaneously in a spectrum.

  19. Cobalt as chemical modifier to improve chromium sensitivity and minimize matrix effects in tungsten coil atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Sidnei G. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, P.O. Box 676, São Carlos, SP 13560-970 (Brazil); Donati, George L., E-mail: georgedonati@yahoo.com.br [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Santos, Luana N. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, P.O. Box 676, São Carlos, SP 13560-970 (Brazil); Jones, Bradley T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Nóbrega, Joaquim A. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, P.O. Box 676, São Carlos, SP 13560-970 (Brazil)

    2013-05-30

    Graphical abstract: -- Highlights: •Charge transfer reactions increase the population of Cr{sup +}. •Chromium ions and electrons recombine to form excited-state Cr atoms. •A 10-fold improvement in LOD is observed for Cr emission measurements. •The two-step ionization/excitation mechanism improves sensitivity and accuracy. •High concentrations of Co also minimize matrix effects. -- Abstract: 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{sup −1} Co, WCAES limit of detection for Cr (λ = 425.4 nm) is calculated as 0.070 mg L{sup −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{sup +} by charge transfer reactions. In a second step, Cr{sup +}/e{sup −} 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{sup −1} and repeatability of 3.8% (RSD, n = 10) for a 2.0 mg L{sup −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

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

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira Souza, Sidnei de [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Silvério Lopes da Costa, Silvânio [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Coordenação de Química, Universidade Federal de Alagoas (UFAL), Campus Arapiraca, 57309-005, Arapiraca, AL (Brazil); Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); and others

    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{sup −1} for Mn to 77.3 mg kg{sup −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). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO{sub 3} and H{sub 2}O{sub 2}) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The

  1. Direct multielement trace analyses of silicon carbide powders by spark ablation simultaneous inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kiera, Arne F.; Schmidt-Lehr, Sebastian; Song, Ming [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Bings, Nicolas H. [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)], E-mail: bings@chemie.uni-hamburg.de; Broekaert, Jose A.C. [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)

    2008-02-15

    A procedure for the direct analysis of silicon carbide powders (SiC) by simultaneous detection inductively coupled plasma optical emission spectrometry using a Spectro-CIROS{sup TM} spectrometer (CCD-ICP-OES) and a novel spark ablation system Spectro-SASSy (SA) as sample introduction technique is described. The sample preparation procedure for SA of non-conducting material is based on mixing the sample powders with a conducting matrix, in this case copper and briquetting pellets. Pressing time, pressure and mixing ratio are shown to be important parameters of the pelleting technique with respect to their mechanical stability for the reliability of the analysis results. A mixing ratio of 0.2 g +0.6 g for SiC and Cu, a pressure of 10 t cm{sup -2} and a pressing time of 8 min have been found optimum. It has also been shown that the spark parameters selected are crucial for uniform volatilization. Electron probe micrographs of the burning spots and the analytical signal magnitude showed that a rather hard spark at 100 Hz was optimum. The determination of trace elements in silicon carbide powders is demonstrated using a calibration based on the addition of standard solutions. For Al, Ti, V, Mn and Fe detection limits in the lower {mu}g g{sup -1} range can be achieved. Internal standardization with Y in combination with the addition of standard solutions allows relative standard deviations in the range of 4 to 24% for concentration levels of the order of 3 to 350 {mu}g g{sup -1}.

  2. Macro- and micro-element analysis in milk samples by inductively coupled plasma-optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    Petrović Sanja M.

    2016-01-01

    Full Text Available The paper describes the determination of Ag, Al, B, Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Na, Ni, Pb, Sr, Tl and Zn, as well as total fat content of milk samples, originated from different sources. The analyzed milk samples were: human milk, fresh cow milk, pasteurized cow milk from a local market, and reconstituted powder milk. The milk samples were obtained from Jablanica District (Serbia territory. Preparation of samples for macro- and micro-analyses was done by wet digestion. Concentrations of the elements after digestion were determined by inductively coupled plasma optical emission spectrometry (ICP-OES. Total fat content of milk samples was determinate by the Weibull and Stoldt method. The results showed that potassium and calcium concentrations were the highest in all samples: 1840.64 - 2993.26 mg/L and 456.05 - 1318.08 mg/L, respectively. Of all heavy metals from the examined milk samples (copper, zinc, manganese, nickel, cadmium, and lead, the most common were zinc and copper, with approximately similar content in the range of 5 - 12 mg/l, while cadmium nickel and manganese were not detected at all. Samples of fresh cow milk and human milk showed the highest fat content of 3.6 and 4.2 %, respectively. Results for total fat and macro- and micro-analyses showed that fresh cow milk has the highest contents of fat and calcium, making it the most nutritious. [Projekat Ministarstva nauke Republike Srbije, br. TR 34012

  3. Low gas flow inductively coupled plasma optical emission spectrometry for the analysis of food samples after microwave digestion.

    Science.gov (United States)

    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. Slurry micro-sampling technique for use in argon-helium microwave induced plasma optical emission spectrometry.

    Science.gov (United States)

    Ślachciński, Mariusz

    2016-12-01

    The Flow Focusing Pneumatic Nebulizer (FFPN) working at low liquid flow rates was evaluated for the elemental analysis in slurried samples by argon-helium microwave induced plasma optical emission spectrometry (MIP-OES). The obtained results achieved were compared with commercially available V-groove Babington type nebulizer (VBPN). A univariate approach and the simplex optimization procedure were used to achieve optimized conditions and derive analytical figures of merit. Analytical performance of the micro nebulization system was characterized by a determination of the limits of detection (LODs), the precision (RSDs) and the wash-out times for Ba, Ca, Cd, Cu, Fe, Mg, Mn, Pb and Sr. The experimental concentration detection limits for simultaneous determination, calculated as the concentration giving a signal equal to three times of the standard deviation of the blank (LOD, 3σblank criterion, peak height) were 0.9, 0.2, 0.3, 0.2, 0.3, 0.1, 0.2, 0.4, 0.4 and 0.3ngmL(-1) for Ba, Ca, Cd, Cu, Fe, Mg, Mn, Pb and Sr, respectively. The method offers relatively good precision (RSD ranged from 5% to 8%) for micro-slurry sampling analysis. Analyses of the certified reference materials (NRCC DOLT-2, GBW 07302 and SRM 2710) were performed in order to determine the accuracy available with the presented nebulization systems. The measured contents of elements in the reference materials were in satisfactory agreement with the certified values. In addition, these elements were determined in two real samples. Slurry concentration up to 3% m/v (particles technique. An ultrasonic probe was used to homogenize the slurry in the polypropylene bottle just before its introduction into the nebulizer. The nebulizers exhibited no clogging problems. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Determination of metals in coal fly ashes using ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Pontes, Fernanda V M; Mendes, Bruna A de O; de Souza, Evelyn M F; Ferreira, Fernanda N; da Silva, Lílian I D; Carneiro, Manuel C; Monteiro, Maria I C; de Almeida, Marcelo D; Neto, Arnaldo A; Vaitsman, Delmo S

    2010-02-05

    A method for determination of Co, Cr, Cu, Fe, Mn, Ni, Ti, V and Zn in coal fly ash samples using ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) is proposed. The digestion procedure consisted in the sonication of the previously dried sample with hydrofluoric acid and aqua regia at 80 degrees C for 30 min, elimination of fluorides by heating until dryness for about 1h and dissolution of the residue with nitric acid solution. A classical digestion method, used as comparative method, consisted in the addition of HCl, HNO(3) and HF to 1 g of sample, and heating on a hot plate until dryness for about 6h. The proposed method presents several advantages: it requires lower amounts of sample and reagents, and it is faster. It is also advantageous when compared to the published methods, which also use ultrasound-assisted digestion procedure: lower detection limits for Co, Cu, Ni, V and Zn, and it does not require shaking during the digestion. The detection limits (microg g(-1)) for Co, Cr, Cu, Fe, Mn, Ni, Ti, V and Zn were 0.06, 0.37, 1.0, 25, 0.93, 0.45, 4.0, 1.7 and 4.3, respectively. The results were in good agreement with those obtained by the classical method and reference values. The exception was Cr, which presented low recoveries in classical and proposed methods (83 and 87%, respectively). Also, the concentration for Cu obtained by the proposed method was significantly different from the reference value, in spite of the good recovery (91+/-1%).

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  7. 40 CFR Appendix C to Part 136 - Inductively Coupled Plasma-Atomic Emission Spectrometric Method for Trace Element Analysis of...

    Science.gov (United States)

    2010-07-01

    ... extremely toxic and may be fatal if swallowed. Wash hands thoroughly after handling.) Typical stock solution....1000 g of manganese metal in the acid mixture 10 mL conc. HCl and 1 mL conc. HNO3, and dilute to 1,000... standard solution I—Manganese, beryllium, cadmium, lead, and zinc. 7.4.2Mixed standard solution...

  8. Water analysis via portable X-ray fluorescence spectrometry

    Science.gov (United States)

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

    2017-01-01

    Rapid, in-situ elemental water analysis would be an invaluable tool in studying polluted and/or salt-impacted waters. Analysis of water salinity has commonly used electrical conductance (EC); however, the identity of the elements responsible for the salinity are not revealed using EC. Several studies have established the viability of using portable X-ray fluorescence (PXRF) spectrometry for elemental data analysis of soil, sediment, and other matrices. However, the accuracy of PXRF is known to be affected while scanning moisture-laden soil samples. This study used PXRF elemental data in water samples to predict water EC. A total of 256 water samples, from 10 different countries were collected and analyzed via PXRF, inductively coupled plasma atomic emission spectroscopy (ICP-AES), and a digital salinity bridge. The PXRF detected some elements more effectively than others, but overall results indicated that PXRF can successfully predict water EC via quantifying Cl in water samples (validation R2 and RMSE of 0.77 and 0.95 log μS cm-1, respectively). The findings of this study elucidated the potential of PXRF for future analysis of pollutant and/or metal contaminated waters.

  9. Chemical Characterisation of Bulk and Melt-spun Ribbons of NiMnIn alloy using Inductively Coupled Plasma Optical Emission Spectrometry

    Directory of Open Access Journals (Sweden)

    S.S. Kalyan Kamal

    2011-04-01

    Full Text Available Method development for the analysis of NiMnIn, a new magnetocaloric effect (MCE material using inductively coupled plasma optical emission spectrometry (ICPOES is discussed. Spectral interference of Ni and Mn on the analysis of In were studied. The process of method validation was carried out using various analytical techniques like conventional wet chemical techniques and instrumental techniques such as atomic absorption spectrometry. All the techniques show a close agreement in values, thus this method could be applied for regular analysis of NiMnIn alloys. A comparative chemical analysis of bulk and melt-spun ribbons of this alloy is also discussed.Defence Science Journal, 2011, 61(3, pp.270-274, DOI:http://dx.doi.org/10.14429/dsj.61.397

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

    Energy Technology Data Exchange (ETDEWEB)

    Li Yingjie [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)], E-mail: binhu@whu.edu.cn

    2007-10-15

    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{sup 2+} was complexed with I{sup -} to form HgI{sub 4}{sup 2-}, and the HgI{sub 4}{sup 2-} 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{sup +}) in the initial solution by centrifugation. The surfactant-rich phase containing Hg(II) was diluted with 0.5 mol L{sup -1} HNO{sub 3} for ICP-OES determination. The supernatant is also subjected to the similar CPE procedure for the preconcentration of MeHg{sup +} by the addition of a chelating agent, ammonium pyrrolidine dithiocarbamate (APDC), in order to form water-insolvable complex with MeHg{sup +}. The MeHg{sup +} 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{sup +} with the enrichment factor of 18.7 for Hg(II) and 10.3 for MeHg{sup +}, respectively. The limits of detection (LODs) were 56.3 ng L{sup -1} for Hg(II) and 94.6 ng L{sup -1} for MeHg{sup +} (as Hg) with the relative standard deviations (RSDs) of 3.6% for Hg(II) and 4.5% for MeHg{sup +} (C = 10 {mu}g L{sup -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.

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

    Science.gov (United States)

    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.

  12. 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.

    Science.gov (United States)

    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.

  13. Efficient high-resolution X-ray emission spectrometry using synchrotron radiation; Effiziente hochaufloesende Roentgenemissionssprektrometrie mit Synchrotronstrahlung

    Energy Technology Data Exchange (ETDEWEB)

    Unterumsberger, Rainer

    2015-07-01

    The aim of the present work is to get access to high-resolution X-Ray Emission Spectrometry (XES) at nanoscaled materials, consisting of light elements and transition metals, by the increase of the sensitivity of a Wavelength-Dispersive Spectrometer (WDS) in the soft X-Ray range. The increase of the sensitivity was achieved by a refocusing of the incident radiation. With the increased sensitivity of the WDS, it was possible to determine the chemical species of different, nominal 100 nm thin titanium oxides. The combination of the refocusing optic and calibrated spectrometer enabled the detection and deconvolution of the L-fluorescence radiation of these nanoscaled titanium oxides. Due to the calibration of the spectrometer, a reliable determination of the transition probabilities of the titanium La- and Ll-fluorescence lines as a function of the chemical state is possible. To the best of my knowledge, the determination of the transition probabilities as a function of the chemical state in the soft X-Ray range has not been investigated yet. The quality of the refocusing was characterized using different diagnostic tools. Vertical full width at half maximum (FWHM) values of the focused beam between 10 μm to 20 μm and horizontal FWHM values between 12 μm and 25 μm could be achieved over an energy range of 180 eV to 1310 eV. Using calibrated photodiodes, it was possible to determine the absolute transmission of the used single bounce monocapillary as well as to monitor the absolute photon flux. By means of the refocusing, it was possible to increase the photon flux by a factor of 4.9 experimentally. The increase of the photon flux enables the analysis of nanoscaled materials with the used spectrometer. This could be shown based on the determination of the lower limit of detection of boron Ka and titanium La. In both cases, the lower limit of detection of 0.4 nm equivalent layer thickness was achieved (about 1.10{sup -7} g/cm{sup 2} to 2.10{sup -7} g/cm{sup 2} or 3

  14. Speciation of mercury compounds by gas chromatography with atomic emission detection. Simultaneous optimization of a headspace solid-phase microextraction and derivatization procedure by use of chemometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Carro, A.M.; Neira, I.; Rodil, R.; Lorenzo, R. A. [Univ. Santiago de Compostela (Spain). Dpto. Quimica Analitica, Nutricion y Bromatologia

    2003-06-01

    A method is proposed for the extraction and determination of organomercury compounds and Hg(II) in seawater samples by headspace solid-phase microextraction (HS-SPME) combined with capillary gas chromatography-microwave-induced plasma atomic emission spectrometry. The mercury species were derivatized with sodium tetraphenylborate, sorbed on a polydimethylsiloxane-coated fused-silica fibre, and desorbed in the injection port of the GC, in splitless mode. Experimental design methodology was used to evaluate the effect of six HS-SPME-derivatization variables: sample volume, NaBPh{sub 4} volume, pH, sorption time, extraction-derivatization temperature, and rate of stirring. Use of a multicriterion decision-making approach, with the desirability function, enabled determination of the optimum working conditions of the procedure for simultaneous analysis of three mercury species. (orig.)

  15. Direct determination of sulfur species in coals from the Argonne premium sample program by solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Bauer, Daniela; Vogt, Thomas; Klinger, Mathias; Masset, Patrick Joseph; Otto, Matthias

    2014-10-21

    A new direct solid sampling method for speciation of sulfur in coals by electrothermal vaporization inductively coupled plasma optical emission spectrometry (ETV-ICP OES) is presented. On the basis of the controlled thermal decomposition of coal in an argon atmosphere, it is possible to determine the different sulfur species in addition to elemental sulfur in coals. For the assignment of the obtained peaks from the sulfur transient emission signal, several analytical techniques (reflected light microscopy, scanning electron microscopy with energy dispersive X-ray spectroscopy and X-ray diffraction) were used. The developed direct solid sampling method enables a good accuracy (relative standard deviation ≤ 6%), precision and was applied to determine the sulfur forms in the Argonne premium coals, varying in rank. The generated method is time- and cost-effective and well suited for the fast characterization of sulfur species in coal. It can be automated to a large extent and is applicable for process-accompanying analyses.

  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.

    Science.gov (United States)

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

    2016-09-06

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

  17. Optimization of the operating conditions of solid sampling electrothermal vaporization coupled to inductively coupled plasma optical emission spectrometry for the sensitive direct analysis of powdered rice.

    Science.gov (United States)

    Sadiq, Nausheen; Beauchemin, Diane

    2014-12-03

    Two different approaches were used to improve the capabilities of solid sampling (SS) electrothermal vaporization (ETV) coupled to inductively coupled plasma optical emission spectrometry (ICP-OES) for the direct analysis of powdered rice. Firstly, a cooling step immediately before and after the vaporization step in the ETV temperature program resulted in a much sharper analyte signal peak. Secondly, point-by-point internal standardization with an Ar emission line significantly improved the linearity of calibration curves obtained with an increasing amount of rice flour certified reference material (CRM). Under the optimized conditions, detection limits ranged from 0.01 to 6ngg(-1) in the solid, depending on the element and wavelength selected. The method was validated through the quantitative analysis of corn bran and wheat flour CRMs. Application of the method to the multi-elemental analysis of 4-mg aliquots of real organic long grain rice (white and brown) also gave results for Al, As, Co, Cu, Fe, Mg, Se, Pb and Zn in agreement with those obtained by inductively coupled plasma mass spectrometry following acid digestion of 0.2-g aliquots. As the analysis takes roughly 5min per sample (2.5min for grinding, 0.5-1min for weighing a 4-mg aliquot and 87s for the ETV program), this approach shows great promise for fast screening of food samples.

  18. Forensic analysis of tempered sheet glass by particle induced X-ray emission (PIXE)

    Energy Technology Data Exchange (ETDEWEB)

    Jisonna, L.J. [Department of Chemistry and Department of Physics, Hope College, Holland, MI 49422-9000 (United States); DeYoung, P.A., E-mail: deyoung@hope.ed [Department of Chemistry and Department of Physics, Hope College, Holland, MI 49422-9000 (United States); Ferens, J.; Hall, C.; Lunderberg, J.M.; Mears, P. [Department of Chemistry and Department of Physics, Hope College, Holland, MI 49422-9000 (United States); Padilla, D. [Department of Physics, San Diego State University, San Diego, CA 92182-1233 (United States); Peaslee, G.F. [Department of Chemistry and Department of Physics, Hope College, Holland, MI 49422-9000 (United States); Sampson, R. [Department of Physics, Columbia University, New York, NY 10027 (United States)

    2011-05-15

    Highlights: {yields} PIXE was found to give the same results for trace elements in glass as ICP. {yields} PIXE can non-destructively determine trace element concentrations in auto glass. {yields} Measured Ca, Fe, Ti, Mn, and Sr in auto glass with PIXE. -- Abstract: The elemental concentrations of five trace elements in tempered sheet glass fragments were determined using particle-induced X-ray emission (PIXE) spectrometry. The trace element concentrations for calcium, iron, manganese, strontium, and titanium are compared to those obtained by inductively-coupled plasma-atomic emission spectrometry (ICP-AES) following complete digestion by hydrofluoric acid. For these five elements, the absolute concentrations obtained by both methods are shown to agree well over a wide range of concentrations. The limits of detection for trace elements are typically lower for the ICP-AES method. However, we show that the concentrations of these five elements can be accurately measured by the PIXE method. Since PIXE is an entirely non-destructive method, there exists a niche for this technique to be used as a complement to the more sensitive ICP-AES technique in the forensic analysis of sheet glass.

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

    Science.gov (United States)

    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

    2016-02-02

    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.

  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.

    Science.gov (United States)

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

    2016-04-01

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

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

    Science.gov (United States)

    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.

  2. Characterization of gas-phase organics using proton transfer reaction time-of-flight mass spectrometry: fresh and aged residential wood combustion emissions

    Science.gov (United States)

    Bruns, Emily A.; Slowik, Jay G.; El Haddad, Imad; Kilic, Dogushan; Klein, Felix; Dommen, Josef; Temime-Roussel, Brice; Marchand, Nicolas; Baltensperger, Urs; Prévôt, André S. H.

    2017-01-01

    Organic gases emitted during the flaming phase of residential wood combustion are characterized individually and by functionality using proton transfer reaction time-of-flight mass spectrometry. The evolution of the organic gases is monitored during photochemical aging. Primary gaseous emissions are dominated by oxygenated species (e.g., acetic acid, acetaldehyde, phenol and methanol), many of which have deleterious health effects and play an important role in atmospheric processes such as secondary organic aerosol formation and ozone production. Residential wood combustion emissions differ considerably from open biomass burning in both absolute magnitude and relative composition. Ratios of acetonitrile, a potential biomass burning marker, to CO are considerably lower ( ˜ 0.09 pptv ppbv-1) than those observed in air masses influenced by open burning ( ˜ 1-2 pptv ppbv-1), which may make differentiation from background levels difficult, even in regions heavily impacted by residential wood burning. A considerable amount of formic acid forms during aging ( ˜ 200-600 mg kg-1 at an OH exposure of (4.5-5.5) × 107 molec cm-3 h), indicating residential wood combustion can be an important local source for this acid, the quantities of which are currently underestimated in models. Phthalic anhydride, a naphthalene oxidation product, is also formed in considerable quantities with aging ( ˜ 55-75 mg kg-1 at an OH exposure of (4.5-5.5) × 107 molec cm-3 h). Although total NMOG emissions vary by up to a factor of ˜ 9 between burns, SOA formation potential does not scale with total NMOG emissions and is similar in all experiments. This study is the first thorough characterization of both primary and aged organic gases from residential wood combustion and provides a benchmark for comparison of emissions generated under different burn parameters.

  3. Analysis of cobalt, tantalum, titanium, vanadium and chromium in tungsten carbide by inductively coupled plasma-optical emission spectrometry

    CSIR Research Space (South Africa)

    Archer, M

    2003-12-01

    Full Text Available Inductively coupled plasma optical emission spectroscopy (ICP-OES) was used to measure the concentrations of cobalt, tantalum, titanium, vanadium and chromium in solutions of tungsten carbide. The main advantage of the method described here lies...

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

    Science.gov (United States)

    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

  5. Current opportunities and challenges of magnetic resonance spectroscopy, positron emission tomography, and mass spectrometry imaging for mapping cancer metabolism in vivo.

    Science.gov (United States)

    Lin, Gigin; 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.

  6. Energy-dispersive x-ray fluorescence spectroscopy and inductively coupled plasma emission spectrometry evaluated for multielement analysis in complex biological matrices.

    Science.gov (United States)

    Irons, R D; Schenk, E A; Giauque, R D

    1976-12-01

    Energy-dispersive x-ray spectroscopy and inductively coupled plasma emission spectrometry were evaluated as methods for routine multielement analysis of biological material. Standard samples included Standard Reference Materials (National Bureau of Standards), compounded mixtures, and supplements that provided a wide range of elemental concentrations for analysis. Elements included in this study were Zn, Pb, Ni, Mn, Fe, Mg, Cu, Ca, As, Se, Br, Rb, and Sr. Standards were analyzed as unknowns by participating laboratories. The two methods were evaluated for sensitivity, precision, and accuracy, and the results compared to those obtained for atomic absorption spectrometric analysis of identical standard unknowns. Both methods compared favorably and both were determined to be highly reliable for such an application. Advantages and disadvantages of each method are compared and discussed.

  7. Simultaneous Determination of Cd, Co, Cu, Mg,Mn, Ni, Pb, Zn and Ca in Laterite Nickel Ore by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)%电感耦合等离子体原子发射光谱法(ICP-AES)测定红土镍矿中的Cd、Co、Cu、Mg、Mn、Ni、Pb、Zn、Ca9种元素

    Institute of Scientific and Technical Information of China (English)

    何飞顶; 李华昌; 冯先进

    2011-01-01

    提出了使用电感耦合等离子体-原子发射光谱法同时测定红土镍矿中Cd、Co、Cu、Mg、Mn、Ni、Pb、Zn、Ca的分析方法.采用盐酸、硝酸和氢氟酸处理样品,以盐酸作为测定介质,在选定的仪器工作条件下直接测定.各元素的测定检出限为0.0001~0.0033μg/mL,相对标准偏差(RSD,n=6)为0.15%~1.89%.对样品进行加标回收试验,回收率在91.4%~107.2%之间.经比对试验证明,本法测定值与火焰原子吸收光谱法测定值一致.

  8. 电感耦合等离子体原子发射光谱法测定锂离子电池三元正极材料LiNi1-x-yCox MnyO2中钠%Determination of sodium in ternary cathode material (LiNi1-x-yCoxMnyO2) for lithium ion battery by inductively coupled plasma atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    欧阳曦; 陈珍华; 郑雪琴

    2014-01-01

    在锂离子三元正极材料LiNi1-x-y CoxMnyO2中,钠离子会占据锂离子的位置,钠离子的存在会降低材料的克容量,因此需要严格控制材料中钠含量.在研究采用电感耦合等离子体原子发射光谱法(ICP-AES)测定锂离子三元正极材料LiNi1-xyCoxMnyO2中的杂质元素钠含量的条件包括样品的溶解方法、测定介质盐酸的浓度、称样量、仪器参数基础上、建立了锂离子三元正极材料LiNi1-x-yCoxMnyO2中钠的测定方法.方法无需进行基体匹配、添加消电离剂等烦琐操作步骤就能得到准确、稳定的测量结果.方法的回收率在97.8%~103.6%之间,样品分析结果相对标准偏差小于2.5%,完全能够满足三元正极材料分析的要求.

  9. Improvement of the thermal stability of nickel silicide using a ruthenium interlayer deposited via remote plasma atomic layer deposition

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Inhye [Department of Materials Science and Engineering, Hanyang University, Seoul 04763, South Korea and System LSI Manufacturing Operation Center, Samsung Electronics Co., Ltd, Gyeonggi-do 17113 (Korea, Republic of); Park, Jingyu; Jeon, Heeyoung; Kim, Hyunjung; Shin, Changhee [Department of Nano-scale Semiconductor Engineering, Hanyang University, Seoul 04763 (Korea, Republic of); Shin, Seokyoon; Lee, Kunyoung [Department of Materials Science and Engineering, Hanyang University, Seoul 04763 (Korea, Republic of); Jeon, Hyeongtag, E-mail: hjeon@hanyang.ac.kr [Department of Materials Science and Engineering, Hanyang University, Seoul 04763, South Korea and Department of Nano-scale Semiconductor Engineering, Hanyang University, Seoul 04763 (Korea, Republic of)

    2016-05-15

    In this study, the effects of a thin Ru interlayer on the thermal and morphological stability of NiSi have been investigated. Ru and Ni thin films were deposited sequentially to form a Ni/Ru/Si bilayered structure, without breaking the vacuum, by remote plasma atomic layer deposition (RPALD) on a p-type Si wafer. After annealing at various temperatures, the thermal stabilities of the Ni/Ru/Si and Ni/Si structures were investigated by various analysis techniques. The results showed that the sheet resistance of the Ni/Ru/Si sample was consistently lower compared to the Ni/Si sample over the entire temperature range. Although both samples exhibited the formation of NiSi{sub 2} phases at an annealing temperature of 800 °C, as seen with glancing angle x-ray diffraction, the peaks of the Ni/Ru/Si sample were observed to have much weaker intensities than those obtained for the Ni/Si sample. Moreover, the NiSi film with a Ru interlayer exhibited a better interface and improved surface morphologies compared to the NiSi film without a Ru interlayer. These results show that the phase transformation of NiSi to NiSi{sub 2} was retarded and that the smooth NiSi/Si interface was retained due to the activation energy increment for NiSi{sub 2} nucleation that is caused by adding a Ru interlayer. Hence, it can be said that the Ru interlayer deposited by RPALD can be used to control the phase transformation and physical properties of nickel silicide phases.

  10. Use of mass spectrometry techniques for the characterization of metal bound to proteins (metallomics) in biological systems

    Energy Technology Data Exchange (ETDEWEB)

    Gomez-Ariza, J.L.; Garcia-Barrera, T.; Lorenzo, F.; Bernal, V.; Villegas, M.J.; Oliveira, V

    2004-10-25

    The need to determine the individual chemical species (speciation), especially when they are known to have a differential action and behavior in relation to toxicity, mobility, or bioavailability, is discussed. The analytical approaches for small mass metal species characterization, as well as sample treatment and storage, is now well established on the basis of chromatographic-atomic detector combinations. The description of a new scenario centered on endogenous and exogenous metallic species in biological systems, bioactive macromolecules, such as proteins, DNA restriction fragments, phytochelatins, metallothioneins and others is fulfilled. Many of these systems are not well known at present and require a new generation of analytical tools that substitute the traditional atomic detectors based in the use of photons (atomic absorption spectrometry (AAS), flame photoionization detector (FPD), inductively coupled plasma-atomic emission spectroscopy (ICP-AES), atomic fluorescence spectroscopy (AFS)) by mass detectors (mass spectrometry (MS) and inductively coupled plasma-mass spectrometry (ICP-MS)) that characterize ions. The photonic analytical tool is now being substituted by the ionic paradigm. Many cases related to biological molecules involving proteins and multiprotein systems, in which metals frequently participate (metallomics) are described, and a generic metallomics analytical approach is proposed for the identification and quantification of metalloproteins, and other metallomacromolecules present in life systems, on the basis of three experimental focuses: (i) a separation technique - selectivity component; (ii) an element-high sensitivity detector--sensitivity component; and (iii) a molecule-specific detector, generally based on mass spectrometry-structural component. This multiplexed analytical approach brings together both elemental and molecular detectors for easy metalloproteins identification. Finally, the possibilities of the metallomics approach in

  11. MeV-range velocity-space tomography from gamma-ray and neutron emission spectrometry measurements at JET

    DEFF Research Database (Denmark)

    Salewski, Mirko; Nocente, M.; Jacobsen, Asger Schou

    2017-01-01

    We demonstrate the measurement of a 2D MeV-range ion velocity distribution function by velocity-space tomography at JET. Deuterium ions were accelerated into the MeV-range by third harmonic ion cyclotron resonance heating. We made measurements with three neutron emission spectrometers and a high-...

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

    Science.gov (United States)

    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

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

    Science.gov (United States)

    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

  14. 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.

    Science.gov (United States)

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

    2016-09-06

    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%.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Luan, Shen [Iowa State Univ., Ames, IA (United States)

    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. Straightforward way to enhance robustness in ultrasonic nebulization-axial view inductively coupled plasma optical emission spectrometry via an additional N2 gas stream

    Science.gov (United States)

    Scheffler, Guilherme Luiz; Pozebon, Dirce

    2015-11-01

    In the present study a low flow of N2 is mixed with the aerosol produced by ultrasonic nebulization (USN) prior analysis using inductively coupled plasma optical emission spectrometry (ICP OES). The foreign gas is added for improving plasma characteristics in axially-viewed ICP. By computing the Mg ionic to atomic ratio (plasma robustness) it was concluded that N2 dissociates closer to the load coil when USN is used as sample introduction system. The maximum emission intensity of Mg(II) for pneumatic nebulization (PN) was observed at 11 mm from the load coil while it was 8 mm for USN, indicating earlier aerosol desolvation, atomization and excitation processes in the ICP. Emission profiles of Ar(I) 415.861 nm, Ba(II) 486.601 nm and Ba(II) 233.527 nm indicated that metastable Ar species are overpopulated in the ICP under the N2 flow. Copper and manganese ionic lines with energy close to 16 eV (Ar ionization) were monitored to evaluate spatially dependent charge-transfer reaction along the ICP axis in the presence and absence of the N2 flow. The Cu(II) signal profiles indicated abundance of Ar+ species at low distances from the load coil when N2 was added. On the other hand, differences were not observed at longer distances from the load coil for both plasmas (mixed-gas and pure Ar-ICP). The calculated limits of detection (LODs) for both plasmas had the same order of magnitude. Analysis of certified reference samples demonstrated that the accuracy was preserved by adding the low flow of N2. It was concluded that adding a low flow of N2 to the aerosol produced by USN is a simple way to increase plasma robustness, which is usually lower than that achieved using conventional PN.

  18. Determination of total fluorine in five coal reference materials by proton-induced gamma-ray emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Roelandts, I.; Robaye, G.; Delbrouck-Habaru, J.M.; Weber, G. [University of Liege, Sart (Belgium). Dept. of Geology, Petrology and Geochemistry

    1996-03-01

    The direct non-destructive proton-induced gamma-ray emission (PIGE) technique with a germanium detector was applied to the determination of total fluorine concentration in five coal reference materials (BCR 30, NIST 1632b, NIST 1635, SARM 20 and USGS CLB-1). Duplicate analyses were made from five randomly selected bottles of each coal. Individual data are presented and some problems (calibration, proton stopping power, effects of sample heating by the proton beam, background estimation) which were encountered during this study are discussed. Sensitivity and reproducibility of the determinations, and homogeneity of the coal samples with respect to fluorine contents by analysis of variance were investigated. The present data are also compared with the few published values for these reference samples, including other PIGE data. The use of synthetic standards and spiked samples in the present study suggested that the PIGE method was more accurate than other techniques.

  19. Synthesis of Highly Emissive CdSe Quantum Dots by Aqueous Precipitation Method

    Directory of Open Access Journals (Sweden)

    Bing Gao

    2013-01-01

    Full Text Available CdSe quantum dots (QDs with high quantum yield (QY up to 76.57% are synthesized using the aqueous precipitation method. With the control of SeSO32- concentration in Se precursor, the nucleation speed and concentration of CdSe QDs are increased. The mass of obtained Cd2+ and Se2+ in nanocrystal is measured by inductively coupled plasma atomic emission spectrometry (ICP-AES. XRD and HRTEM are used to identify the crystal phase and morphology of the products which are pure CdSe crystals in the cubic zinc blende phase and uniformly dispersed in the solution with the size between 2 nm and 2.3 nm. Results demonstrate that the emission wavelength of CdSe QDs is 500 nm~560 nm along with the increased temperature 50°C~90°C and prolonged time 5 min~25 min.

  20. Investigation of the direct hydride generation nebulizer for the determination of arsenic, antimony and selenium in inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Rojas, Illiana; Murillo, Miguel; Carrion, Nereida; Chirinos, Jose [Centro de Quimica Analitica, Escuela de Quimica, Facultad de Ciencias, Universidad Central de Venezuela, P.O. Box 47102, 1041a, Caracas (Venezuela)

    2003-05-01

    A direct hydride generation nebulizer (DHGN) was explored for introduction of the sample in inductively coupled plasma-optical emission spectrometry (ICP-OES) using radially viewed mode. This simple hydride generation system was constructed in our laboratory and requires similar plasma operating conditions to conventional nebulizer-spray-chamber arrangements. This work was focused on the optimization of the operating conditions for hydride generation and evaluation of the main analytical figures of merit for the determination of As, Sb and Se. The excitation conditions of the ICP-OES instrument operated with the DHGN were also explored. Results showed that the analytical performance of the new system for the determination of As, Sb and Se was superior to that of conventional nebulization systems. The DHGN also enabled the determination of elements that do not form volatile hydrides, but with less sensitivity than conventional nebulization systems. Evaluation of the plasma robustness showed that gases generated in hydride generation do not significantly affects the plasma discharge. Similar to conventional hydride generation techniques, analysis with DHGN was susceptible to non-spectroscopic interferences produced by transition metals. Finally, the utility of the DHGN in practical ICP-OES studies was demonstrated in the determination of trace elements in an oyster tissue standard reference material. (orig.)

  1. 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.

    Science.gov (United States)

    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.

  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

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Eder Jose dos [Instituto de Tecnologia do Parana (TECPAR), 81350-010 Curitiba, PR (Brazil)], E-mail: eder@tecpar.br; Herrmann, Amanda Beatriz; Kulik de Caires, Suzete [Instituto de Tecnologia do Parana (TECPAR), 81350-010 Curitiba, PR (Brazil); Azzolin Frescura, Vera Lucia; Curtius, Adilson Jose [Departamento de Quimica, Universidade Federal de Santa Catarina (UFSC), 880400-900 Florianopolis, SC (Brazil)

    2009-06-15

    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{sub 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 {mu}g L{sup -} {sup 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{sup -} {sup 1} was 0.10 {mu}g g{sup -} {sup 1}. The obtained concentration values were in agreement with the total certified concentrations, according to the t-test for a 95% confidence level.

  3. Determination of Hg(2+) by on-line separation and pre-concentration with atmospheric-pressure solution-cathode glow discharge atomic emission spectrometry.

    Science.gov (United States)

    Li, Qing; Zhang, Zhen; Wang, Zheng

    2014-10-03

    A simple and sensitive method to determine Hg(2+) was developed by combining solution-cathode glow discharge atomic emission spectrometry (SCGD-AES) with flow injection (FI) based on on-line solid-phase extraction (SPE). We synthesized l-cysteine-modified mesoporous silica and packed it in an SPE microcolumn, which was experimentally determined to possess a good mercury adsorption capacity. An enrichment factor of 42 was achieved under optimized Hg(2+) elution conditions, namely, an FI flow rate of 2.0 mL min(-1) and an eluent comprised of 10% thiourea in 0.2 mol L(-1) HNO3. The detection limit of FI-SCGD-AES was determined to be 0.75 μg L(-1), and the precision of the 11 replicate Hg(2+) measurements was 0.86% at a concentration of 100 μg L(-1). The proposed method was validated by determining Hg(2+) in certified reference materials such as human hair (GBW09101b) and stream sediment (GBW07310).

  4. 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.

    Science.gov (United States)

    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.

  5. Optimization of an open-focused microwave oven digestion procedure for determination of metals in diesel oil by inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Sant'Ana, Flavio W; Santelli, Ricardo E; Cassella, Alessandra R; Cassella, Ricardo J

    2007-10-01

    This work reports the optimization of a focused microwave assisted procedure for the wet acid dissolution of diesel oil in order to allow the determination of metals in the samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The dissolution process was monitored by measuring residual carbon content (RCC), also by ICP-OES, in the final solutions obtained after application of digestion program. All experimental work was performed using a commercial sample of diesel oil containing 85.74+/-0.13% of carbon. The initial dissolution program comprised three steps: (i) carbonization with H(2)SO(4); (ii) oxidation with HNO(3) and (iii) final oxidation with H(2)O(2). During work it was verified that the first step played an important role on the dissolution process of this kind of sample. It is therefore, necessary to give a detailed optimization of such step. Employing the optimized conditions it was possible to digest 2.5 g of diesel oil with a 40 min-heating program. At these conditions, residual carbon content was always lower than 5%. Optimized methodology was applied in the determination of metals in three diesel oil samples by ICP-OES. Recovery tests were also performed by adding 10 microg of metals, as organic standards, to the samples before digestion. Recovery percentages always higher than 90% were obtained for the metals of interest (Al, Cu, Fe and Ni), except for Zn, which presented recoveries between 70 and 78%.

  6. Determination of arsenic, cadmium, cobalt, chromium, lead, molybdenum, nickel, and selenium in fertilizers by microwave digestion and inductively coupled plasma-optical emission spectrometry detection: collaborative study.

    Science.gov (United States)

    Kane, Peter F; Hall, William L

    2006-01-01

    There is increasing regulatory interest in the non-nutritive metals content of fertilizer materials, but at present there is no consensus analytical method for acid digestion and instrument detection of those elements in fertilizer matrixes. This lack of method standardization has resulted in unacceptable variability of results between fertilizer laboratories performing metals analysis. A method has been developed using microwave digestion with nitric acid at 200 degrees C, followed by inductively coupled plasma-optical emission spectrometry instrument detection, for the elements arsenic, cadmium, cobalt, chromium, molybdenum, nickel, lead, and selenium. The method has been collaboratively studied, and statistical results are here reported. Fourteen collaborators were sent 62 sample materials in a blind duplicate design. Materials represented a broad cross section of fertilizer types, including phosphate ore, manufactured phosphate products, N-P-K blends, organic fertilizers, and micro-nutrient materials. As much as possible within the limit of the number of samples, materials were selected from different regions of the United States and the world. Limit of detection (LOD) was determined using synthetic fertilizers consisting of reagent grade chemicals with near zero levels of the non-nutritive elements, analyzed blindly. Samples with high iron content caused the most variability between laboratories. Most samples reasonably above LOD gave HorRat values within the range 0.5 to 2.0, indicating acceptable method performance according to AOAC guidelines for analyses in the mg/kg range. The method is recommended for AOAC Official First Action status.

  7. The determination of trace element concentrations in fly ash samples using ultrasound-assisted digestion followed with inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Ilander, Aki; Väisänen, Ari

    2009-08-01

    A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of trace element (chromium, copper, lead, nickel, vanadium and zinc) concentrations in fly ash samples was developed. All the measurements were performed in robust plasma conditions. Ultrasound-assisted digestion procedures using digestion solutions of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 80% for all the analyte elements. Ultrasound-assisted two-step digestion with digestion solutions of 6mL of HNO(3) (Step 1) and 3mL of HNO(3)+3mL of HF (Step 2) resulted in recovery rates of over 92% for all the analyte elements with one exception, chromium, which had a recovery of about 85%. The analysis of SRM 1633b showed that the two-step ultrasound-assisted digestion method developed resulted in chromium, copper, nickel and zinc concentrations higher than the microwave digestion method standardized by the United States Environmental Protection Agency (USEPA method 3052). This is the very first time when a digestion method using ultrasound resulted in higher efficiency than microwave (USEPA method 3052) for chromium and nickel in very hard to dissolve samples. The major advantages of the ultrasound-assisted digestion over microwave digestion is the high treatment rate (about 30 samples simultaneously with a sonication time of 18min) and the possibility to use new sample vessels without a significant increase in costs.

  8. An ultrasound-assisted digestion method for the determination of toxic element concentrations in ash samples by inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Ilander, Aki; Väisänen, Ari

    2007-10-29

    A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of toxic element concentrations (arsenic, barium, cobalt, copper, lead, nickel, strontium, vanadium and zinc) in ash samples was developed. All the measurements were performed in robust plasma conditions which were tested by measuring the Mg(II) 280.270 nm/Mg(I) 285.213 nm line intensity ratios. The highest line intensity ratios were observed when a nebulizer gas flow of 0.6 L min(-1), auxiliary gas flow of 0.2 L min(-1) and plasma power of 1400 W were used for radially viewed plasma. The analysis of SRM 1633b showed that the ultrasound-assisted method developed is highly comparable with the microwave digestion method standardized by the United States Environmental Protection Agency (EPA-3052). The ultrasound-assisted digestion with a digestion solution of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 81%. One exception is arsenic which resulted in recoveries of about 60% only; however, it could be digested with good recovery (>90%) using a digestion solution of 5 mL of water and 5 mL of aqua regia. The major advantage of the ultrasound-assisted digestion over microwave digestion is the high treatment rate (30 samples simultaneously with a sonication time of 18 min).

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

    Energy Technology Data Exchange (ETDEWEB)

    Masson, Pierre, E-mail: masson@bordeaux.inra.fr

    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.

  10. Determination of heavy metals and their speciation in street dusts by inductively coupled plasma-optical emission spectrometry after a Community Bureau of Reference sequential extraction procedure.

    Science.gov (United States)

    Altundag, Huseyin; Imamoglu, Mustafa; Doganci, Secil; Baysal, Erkan; Albayrak, Sinem; Tuzen, Mustafa

    2013-01-01

    Sequential selective extraction techniques are commonly used to fractionate the solid-phase forms of metals in soils. This procedure provides measurements of extractable metals from media, such as acetic acid (0.11 M), hydroxyl ammonium chloride (0.1 M), hydrogen peroxide (8.8 M) plus ammonium acetate (1 M), and aqua regia stages of the sequential extraction procedure. In this work, the extractable Pb, Cu, Mn, Sr, Ni, V, Fe, Zn, and Cr were evaluated in street dust samples from Sakarya, Turkey, between May and October 2009 using the three-step sequential extraction procedure described by the Community Bureau of Reference (BCR, now the Standards, Measurements, and Testing Programme) of the European Union. The sampling sites were divided into 10 categories; a total of 50 street dusts were analyzed. The determination of multielements in the samples was performed by inductively coupled plasma-optical emission spectrometry. Validation of the proposed method was performed using BCR 701 certified reference material. The results showed good agreement between the obtained and the certified values for the metals analyzed.

  11. Spectral interferences in the determination of rhenium in molybdenum and copper concentrates by inductively coupled plasma optical emission spectrometry (ICP-OES)

    Science.gov (United States)

    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.

  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.

    Science.gov (United States)

    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.

  13. Determination of rare earth elements in waters by inductively coupled plasma optical emission spectrometry after preconcentration with 6-(2-thienyl)-2-pyridinecarboxaldehyde functionalized Amberlite XAD-4 resin.

    Science.gov (United States)

    Karadaş, Cennet; Kara, Derya

    2014-01-01

    A new method has been developed for the determination of rare earth elements (REEs) (Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu) in water samples based on preconcentration with a mini-column packed with 6-(2-thienyl)-2-pyridinecarboxaldehyde functionalized Amberlite XAD-4 resin prior to their determination using inductively coupled plasma optical emission spectrometry (ICP-OES). The optimum experimental parameters for preconcentration of REEs, such as pH of the sample, sample and eluent flow rates and sample volume, were investigated. The optimum pH values for quantitative (90-110%) sorption of the REE ions were between 6.0 and 8.0. The elution process was carried out using 2 mL of 1.0 mol L(-1) HNO3 solution. Under the optimum conditions, detection limits between 0.032 and 0.963 μg L(-1) for a 10 mL sample volume and 0.006 and 0.193 μg L(-1) for a 50 mL sample volume were determined. The proposed method was successfully applied to the determination of REEs in water samples with recoveries in the range of 90.1-110.5%.

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

    Science.gov (United States)

    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 (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.

  15. Preliminary study of trace element emissions and control during coal combustion

    Institute of Scientific and Technical Information of China (English)

    ZHANG Junying; ZHAO Yongchun; DING Feng; ZENG Hancai; ZHENG Chuguang

    2007-01-01

    Hazardous trace element emissions have caused serious harm to human health in China.Several typical high-toxic trace element coals were collected from different districts and were used to investigate the emission characteristics of toxic trace elements (As,Se,Cr,Hg) and to explore preliminary control methods.Coal combustion tests were conducted in several bench-scale furnaces including drop tube furnace (DTF),circulating fluidized bed (CFB) combustion furnace,and fixed-bed combustion furnace.Calcium oxide was used to control the emission of arsenic and selenium.The granular activated carbons (AC) and activatedcarbon fibers (ACF) were used to remove mercury in the flue gas from coal combustion.The chemical composition and trace element contents of ash and particulate matter (PM)were determined by X-ray fluorescence (XRF) spectrometry and inductively coupled plasma-atomic emission spectrometry (ICP-AES),respectively.The speciation and concentration of mercury were investigated using the Ontario-Hydro method.X-ray diffraction spectrometry (XRD) was used to determine the mineral composition of production during combustion experiments.With the addition of a calciumbased sorbent,arsenic concentration in PM1 sharply decreased from 0.25-0.11 mg/m3.In fixed-bed combustion of coal,the retention rates of selenium volatiles were between 11.6% and 50.7% using lime.In the circulating fluidized-bed combustion of coal,the content of selenium in ash from the chimney was reduced to one-fourth of its original value and that in leaching water from the chimney decreased by two orders of magnitude using lime.Calcium-based sorbent is an effective additive to control the emission of As and Se during coal combustion.The emission of chromium is influenced by the occurrence mode of Cr in coal.Chromium emission in PM2.5 during coal combustion is 55.5 and 34.7 μg/m3 for Shenbei coal and mixed Pingdingshan coal,respectively.The adsorptive capacity of granular activated carbon for Hg0 is

  16. Development of a direct hydride generation nebulizer for the determination of selenium by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Carrion, Nereida E-mail: ncarrion@strix.ciens.ucv.ve; Murillo, Miguel; Montiel, Edie; Diaz, Dorfe

    2003-08-15

    A study was conducted to evaluate the performance of a new direct hydride generation nebulizer system for determination of hydride forming elements by inductively coupled plasma optical emission spectroscopy. This system was designed and optimized to obtain the highest sensitivity. Several experimental designs were used for these purposes. To optimize the individual parameters of the system, and to study the interaction between these parameters for both direct hydride generation nebulizers, a central composite orthogonal design with eight factors was set up. Significant behavioral differences were observed in the two direct hydride generation nebulizers studied. Finally, a 70 {mu}m gas orifice nebulizer exhibits a better detection limit than the 120 {mu}m nebulizer. Generally, for determination of selenium, this new direct hydride generation nebulizer system exhibits a linear dynamic range and detection limit (3{sigma}b) of 3 orders of magnitude and 0.2 {mu}g l{sup -1} for selenium, respectively. This new hydride generator is much simpler system that conventional hydride generation systems, which does not need to be changed to work in normal mode with the inductively coupled plasma, since this system may be used for hydride forming elements and those that do not form them. It produces a rapid response with low memory effect. It reduces the interference level of Ni, Co and Cu to 600, 500 and 5 mg l{sup -1}, respectively. The accuracy of the system was verified by the determination of selenium in several standard reference materials of ambient, food and clinical sample matrices. No statistically significant differences (95 confidence level) were obtained between our method and the reference values.

  17. Environmental Indicators of Metal Pollution and Emission: An Experiment for the Instrumental Analysis Laboratory

    Science.gov (United States)

    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…

  18. Resonant laser ablation of metals detected by atomic emission in a microwave plasma and by inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Cleveland, Danielle; Stchur, Peter; Hou, Xiandeng; Yang, Karl X; Zhou, Jack; Michel, Robert G

    2005-12-01

    It has been shown that an increase in sensitivity and selectivity of detection of an analyte can be achieved by tuning the ablation laser wavelength to match that of a resonant gas-phase transition of that analyte. This has been termed resonant laser ablation (RLA). For a pulsed tunable nanosecond laser, the data presented here illustrate the resonant enhancement effect in pure copper and aluminum samples, chromium oxide thin films, and for trace molybdenum in stainless steel samples, and indicate two main characteristics of the RLA phenomenon. The first is that there is an increase in the number of atoms ablated from the surface. The second is that the bandwidth of the wavelength dependence of the ablation is on the order of 1 nm. The effect was found to be virtually identical whether the atoms were detected by use of a microwave-induced plasma with atomic emission detection, by an inductively coupled plasma with mass spectrometric detection, or by observation of the number of laser pulses required to penetrate through thin films. The data indicate that a distinct ablation laser wavelength dependence exists, probably initiated via resonant radiation trapping, and accompanied by collisional broadening. Desorption contributions through radiation trapping are substantiated by changes in crater morphology as a function of wavelength and by the relatively broad linewidth of the ablation laser wavelength scans, compared to gas-phase excitation spectra. Also, other experiments with thin films demonstrate the existence of a distinct laser-material interaction and suggest that a combination of desorption induced by electronic transition (DIET) with resonant radiation trapping could assist in the enhancement of desorption yields. These results were obtained by a detailed inspection of the effect of the wavelength of the ablation laser over a narrow range of energy densities that lie between the threshold of laser-induced desorption of species and the usual analytical

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

    Directory of Open Access Journals (Sweden)

    Rahman Mohammed M

    2012-12-01

    Full Text Available Abstract 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.

  20. Comparative analysis of urban atmospheric aerosol by particle-induced X-ray emission (PIXE), proton elastic scattering analysis (PESA), and aerosol mass spectrometry (AMS).

    Science.gov (United States)

    Johnson, K S; Laskin, A; Jimenez, J L; Shutthanandan, V; Molina, L T; Salcedo, D; Dzepina, K; Molina, M 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 of fline under a 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 SO4(2-)) and AMS-measured sulfate during 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 a vacuum. However approximately 25% of the organics does remain under a vacuum, which is only possible with low-vapor-pressure compounds, and which supports the presence of high-molecular-weight 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.

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

    Science.gov (United States)

    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.

  2. Monitoring the emission of volatile organic compounds from flowers of Jasminum sambac using solid-phase micro-extraction fibers and gas chromatography with mass spectrometry detection.

    Science.gov (United States)

    Pragadheesh, Vppalayam Shanmugam; Yadav, Anju; Chanotiya, Chandan Singh; Rout, Prasanta Kumar; Uniyal, Girish Chandra

    2011-09-01

    Solid-phase micro-extraction (SPME) was studied as a solvent free alternative method for the extraction and characterization of volatile compounds in intact and plucked flowers of Jasminum sambac at different day time intervals using gas chromatography (GC-FID) and gas chromatography-quadrupole mass spectrometry. The analytes identified included alcohols, esters, phenolic compounds, and terpenoids. The main constituents identified in the flower aroma using different fibers were cis-3-hexenyl acetate, (E)-beta-ocimene, linalool, benzyl acetate, and (E,E)-alpha-farnesene. The benzyl acetate proportion decreased from morning to afternoon and then increased in evening collections. PDMS fiber showed a high proportion of (E,E)-alpha-farnesene in jasmine floral aroma. Among other constituents identified, cis-3-hexenyl acetate, linalool, and benzyl acetate were major aroma contributors in plucked and living flowers extracts using PDMS/DVB, Carboxen/PDMS, and DVB/Carboxen/PDMS fibers. PDMS/DVB recorded the highest emission for benzyl acetate while the (E)-beta-ocimene proportion was highest in DVB/Carboxen/PDMS when compared with the rest. The highest linalool content, with increasing proportion from morning to noon, was found using mixed coating fibers. Almost negligible volatile adsorption was recorded for the polyacrylate fiber for intact flower aroma, whereas it was most effective for benzyl acetate, followed by indole under plucked conditions. Moreover, the highest amounts extracted, evaluated from the sum of peak areas, were achieved using Carboxen/PDMS, and DVB/Carboxen/PDMS. Introduction of a rapid, and solvent free SPME method for the analysis of multicomponent volatiles can be successfully employed to monitor the extraction and characterization of flower aroma constituents.

  3. Multivariate optimization by exploratory analysis applied to the determination of microelements in fruit juice by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Santos Froes, Roberta Eliane; Borges Neto, Waldomiro [Departamento de Quimica, Universidade Federal de Minas Gerais, Campus Pampulha, Cx Postal 702, Belo Horizonte, MG, 31270-901 (Brazil); Oliveira Couto e Silva, Nilton; Lopes Pereira Naveira, Rita [Fundacao Ezequiel Diaz, FUNED, Belo Horizonte, MG (Brazil); Nascentes, Clesia Cristina [Departamento de Quimica, Universidade Federal de Minas Gerais, Campus Pampulha, Cx Postal 702, Belo Horizonte, MG, 31270-901 (Brazil)], E-mail: clesia@qui.ufmg.br; Bento Borba da Silva, Jose [Departamento de Quimica, Universidade Federal de Minas Gerais, Campus Pampulha, Cx Postal 702, Belo Horizonte, MG, 31270-901 (Brazil)

    2009-06-15

    A method for the direct determination (without sample pre-digestion) of microelements in fruit juice by inductively coupled plasma optical emission spectrometry has been developed. The method has been optimized by a 2{sup 3} factorial design, which evaluated the plasma conditions (nebulization gas flow rate, applied power, and sample flow rate). A 1:1 diluted juice sample with 2% HNO{sub 3} (Tetra Packed, peach flavor) and spiked with 0.5 mg L{sup - 1} of Al, Ba, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Sb, Sn, and Zn was employed in the optimization. The results of the factorial design were evaluated by exploratory analysis (Hierarchical Cluster Analysis, HCA, and Principal Component Analysis, PCA) to determine the optimum analytical conditions for all elements. Central point condition differentiation (0.75 L min{sup - 1}, 1.3 kW, and 1.25 mL min{sup - 1}) was observed for both methods, Principal Component Analysis and Hierarchical Cluster Analysis, with higher analytical signal values, suggesting that these are the optimal analytical conditions. F and t-student tests were used to compare the slopes of the calibration curves for aqueous and matrix-matched standards. No significant differences were observed at 95% confidence level. The correlation coefficient was higher than 0.99 for all the elements evaluated. The limits of quantification were: Al 253, Cu 3.6, Fe 84, Mn 0.4, Zn 71, Ni 67, Cd 69, Pb 129, Sn 206, Cr 79, Co 24, and Ba 2.1 {mu}g L{sup - 1}. The spiking experiments with fruit juice samples resulted in recoveries between 80 and 120%, except for Co and Sn. Al, Cd, Pb, Sn and Cr could not be quantified in any of the samples investigated. The method was applied to the determination of several elements in fruit juice samples commercialized in Brazil.

  4. Multivariate optimization by exploratory analysis applied to the determination of microelements in fruit juice by inductively coupled plasma optical emission spectrometry

    Science.gov (United States)

    Froes, Roberta Eliane Santos; Neto, Waldomiro Borges; Silva, Nilton Oliveira Couto e.; Naveira, Rita Lopes Pereira; Nascentes, Clésia Cristina; da Silva, José Bento Borba

    2009-06-01

    A method for the direct determination (without sample pre-digestion) of microelements in fruit juice by inductively coupled plasma optical emission spectrometry has been developed. The method has been optimized by a 2 3 factorial design, which evaluated the plasma conditions (nebulization gas flow rate, applied power, and sample flow rate). A 1:1 diluted juice sample with 2% HNO 3 (Tetra Packed, peach flavor) and spiked with 0.5 mg L - 1 of Al, Ba, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Sb, Sn, and Zn was employed in the optimization. The results of the factorial design were evaluated by exploratory analysis (Hierarchical Cluster Analysis, HCA, and Principal Component Analysis, PCA) to determine the optimum analytical conditions for all elements. Central point condition differentiation (0.75 L min - 1 , 1.3 kW, and 1.25 mL min - 1 ) was observed for both methods, Principal Component Analysis and Hierarchical Cluster Analysis, with higher analytical signal values, suggesting that these are the optimal analytical conditions. F and t-student tests were used to compare the slopes of the calibration curves for aqueous and matrix-matched standards. No significant differences were observed at 95% confidence level. The correlation coefficient was higher than 0.99 for all the elements evaluated. The limits of quantification were: Al 253, Cu 3.6, Fe 84, Mn 0.4, Zn 71, Ni 67, Cd 69, Pb 129, Sn 206, Cr 79, Co 24, and Ba 2.1 µg L - 1 . The spiking experiments with fruit juice samples resulted in recoveries between 80 and 120%, except for Co and Sn. Al, Cd, Pb, Sn and Cr could not be quantified in any of the samples investigated. The method was applied to the determination of several elements in fruit juice samples commercialized in Brazil.

  5. An evaluation of microwave-assisted fusion and microwave-assisted acid digestion methods for determining elemental impurities in carbon nanostructures using inductively coupled plasma optical emission spectrometry

    KAUST Repository

    Patole, Shashikant P.

    2015-10-21

    It is common for as-prepared carbon nanotube (CNT) and graphene samples to contain remnants of the transition metals used to catalyze their growth; contamination may also leave other trace elemental impurities in the samples. Although a full quantification of impurities in as-prepared samples of carbon nanostructures is difficult, particularly when trace elements are intercalated or encapsulated within a protective layer of graphitic carbon, reliable information is essential for reasons such as quantifying the adulteration of physico-chemical properties of the materials and for evaluating environmental issues. Here, we introduce a microwave-based fusion method to degrade single- and double-walled CNTs and graphene nanoplatelets into a fusion flux thereby thoroughly leaching all metallic impurities. Subsequent dissolution of the fusion product in diluted hydrochloric and nitric acid allowed us to identify their trace elemental impurities using inductively coupled plasma optical emission spectrometry. Comparisons of the results from the proposed microwave-assisted fusion method against those of a more classical microwave-assisted acid digestion approach suggest complementarity between the two that ultimately could lead to a more reliable and less costly determination of trace elemental impurities in carbon nanostructured materials. Graphical abstract A method for the complete digestion of carbon nanostructures has been demonstrated. Photographs (on the left side) show zirconium crucibles containing SWCNTs with flux of Na2CO3 and K2CO3, before and after microwave fusion; (on the right side) the appearance of the final solutions containing dissolved samples, from microwave-assisted fusion and microwave-assisted acid digestion. These solutions were used for determining the trace elemental impurities by ICP‒OES.

  6. Assessment of heavy metal contamination in core sediment samples in Gulf of Izmir, Aegean Sea, Turkey (by inductively coupled plasma-optical emission spectrometry (ICP-OES))

    Science.gov (United States)

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

    2017-04-01

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

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

    Science.gov (United States)

    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.

  8. Determination of Hg{sup 2+} by on-line separation and pre-concentration with atmospheric-pressure solution-cathode glow discharge atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, Qing [Shanghai Institute of Ceramics, Chinese Academy of Science, Shanghai 200050 (China); Zhang, Zhen [Shanghai Institute of Ceramics, Chinese Academy of Science, Shanghai 200050 (China); School of Materials Science and Engineering, Shanghai University, Shanghai 200072 (China); Wang, Zheng, E-mail: wangzheng@mail.sic.ac.cn [Shanghai Institute of Ceramics, Chinese Academy of Science, Shanghai 200050 (China)

    2014-10-03

    Highlights: • A modified SBA-15 mesoporous silica (SH-SBA-15) was synthesized as a sorbent. • On-line SPE combined with SCGD-AES based on FIA was used to detect Hg{sup 2+} firstly. • A simple, low-cost Hg{sup 2+} analysis in a complex matrix was established. • The sensitive detection of Hg{sup 2+} was achieved with a detection limit of 0.75 μg L{sup −1}. - Abstract: A simple and sensitive method to determine Hg{sup 2+} was developed by combining solution-cathode glow discharge atomic emission spectrometry (SCGD-AES) with flow injection (FI) based on on-line solid-phase extraction (SPE). We synthesized L-cysteine-modified mesoporous silica and packed it in an SPE microcolumn, which was experimentally determined to possess a good mercury adsorption capacity. An enrichment factor of 42 was achieved under optimized Hg{sup 2+} elution conditions, namely, an FI flow rate of 2.0 mL min{sup −1} and an eluent comprised of 10% thiourea in 0.2 mol L{sup −1} HNO{sub 3}. The detection limit of FI–SCGD-AES was determined to be 0.75 μg L{sup −1}, and the precision of the 11 replicate Hg{sup 2+} measurements was 0.86% at a concentration of 100 μg L{sup −1}. The proposed method was validated by determining Hg{sup 2+} in certified reference materials such as human hair (GBW09101b) and stream sediment (GBW07310)

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

    Science.gov (United States)

    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.

  10. Freon (CHF3)-assisted atomization for the determination of titanium using ultrasonic slurry sampling-graphite furnace atomic absorption spectrometry (USS-GFAAS): a simple and advantageous method for solid samples.

    Science.gov (United States)

    Asfaw, Alemayehu; Wibetoe, Grethe

    2004-06-01

    A simple and advantageous method for the determination of titanium using graphite furnace atomic absorption spectrometry with slurry sampling has been developed. Titanium is one of the refractory elements that form thermally stable carbides in the graphite tube, which leads to severe memory effects. Trifluoromethane (Freon-23) was applied in the purge gas during the atomization step or alternatively just prior to the atomization to successfully eliminate the problems of carbide formation and increase the lifetime of the furnace tube which could be used for more than 600 heating cycles. A flow rate of 40 mL min(-1) (5% of Freon in argon) was used to obtain symmetrical peaks with no tailing. However, when the gas flow rate was too high (250 mL min(-1)) the peak-tailing and memory effects reappeared. Ti was determined in various materials covering a wide range of concentrations, from 2.8 microg g(-1) to 12% (m/m) Ti. The accuracy of the method was confirmed by analyzing certified reference materials (CRMs) or by comparing the results with those obtained using inductively coupled plasma-atomic emission spectrometry (ICP-AES) after decomposition of the samples. The materials analyzed were soil, plant, human hair, coal, urban particulate matters, toothpaste, and powdered paint.

  11. Total sulfur determination in gasoline, kerosene and diesel fuel using inductively coupled plasma optical emission spectrometry after direct sample introduction as detergent emulsions

    Energy Technology Data Exchange (ETDEWEB)

    Santelli, Ricardo Erthal [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil)], E-mail: santelli@geoq.uff.br; Padua Oliveira, Eliane [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Departamento de Engenharia Quimica e de Petroleo, Universidade Federal Fluminense, Rua Passos da Patria 156, Sao Domingos, Niteroi/RJ, 24210-230 (Brazil); Batista de Carvalho, Maria de Fatima [Centro de Pesquisas e Desenvolvimento da PETROBRAS, Avaliacao e Monitoramento Ambiental, Av. Horacio Macedo, 950, Cidade Universitaria, Rio de Janeiro/RJ, 21941-598 (Brazil); Almeida Bezerra, Marcos [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Universidade Estadual do Sudoeste da Bahia, Laboratorio de Quimica Analitica, Rua Jose Moreira Sobrinho s/n, Jequiezinho, Jequie/BA, 45206-190 (Brazil); Soares Freire, Aline [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil)

    2008-07-15

    Herein, we present the development of a procedure for the determination of total sulfur in petroleum-derived products (gasoline, kerosene and diesel fuel) employing inductively coupled plasma optical emission spectrometry (ICP OES). For this procedure, samples were prepared as emulsions that were made using concentrated nitric acid, Triton X-100, sample, and ultra pure water in proportions of 5/10/7/78% (v/v), respectively. Sample volumes were weighed because of the density differences, and oxygen was added to the sheat gas entrance of the ICP OES in order to decrease carbon deposition in the torch and to minimize background effects. A Doehlert design was applied as an experimental matrix to investigate the flow ratios of argon (sheat and plasma gas) and oxygen in relation to the signal-to-background ratio. A comparative study among the slopes of the analytical curves built in aqueous media, surfactant/HNO{sub 3}, and by spike addition for several sample emulsions indicates that a unique solution of surfactant in acidic media can be employed to perform the external calibration for analysis of the emulsions. The developed procedure allows for the determination of the total sulfur content in petroleum derivatives with a limit of detection (LOD) and limit of quantification (LOQ) of 0.72 and 2.4 {mu}g g{sup -1}, respectively. Precision values, expressed as the relative standard deviations (% RSD, n = 10) for 12 and 400 {mu}g g{sup -1}, were 2.2% and 1.3%, respectively. The proposed procedure was applied toward the determination of total sulfur in samples of gasoline, kerosene, and diesel fuel commercialized in the city of Niteroi/RJ, Brazil. The accuracy of the proposed method was evaluated by the determination of the total sulfur in three different standard reference materials (SRM): NIST 2723a (sulfur in diesel fuel oil), NIST 1616b (sulfur in kerosene), and NIST 2298 (sulfur in gasoline). The data indicate that the methodology can be successfully applied to these

  12. A methodology for quantifying trace elements in the exoskeletons of Florida stone crab (Menippe mercenaria) larvae using inductively coupled plasma optical emission spectrometry (ICP–OES)

    Science.gov (United States)

    Gravinese, Philip M.; Flannery, Jennifer A.; Toth, Lauren T.

    2016-11-23

    The larvae of the Florida stone crab, Menippe mercenaria, migrate through a variety of habitats as they develop and, therefore, experience a broad range of environmental conditions through ontogeny. Environmental variability experienced by the larvae may result in distinct elemental signatures within the exoskeletons, which could provide a tool for tracking the environmental history of larval stone crab populations. A method was developed to examine trace-element ratios, specifically magnesium-to-calcium (Mg/Ca) and strontium-to-calcium (Sr/Ca) ratios, in the exoskeletons of M. mercenaria larvae. Two developmental stages of stone crab larvae were analyzed—stage III and stage V. Specimens were reared in a laboratory environment under stable conditions to quantify the average ratios of Mg/Ca and Sr/Ca of larval stone crab exoskeletons and to determine if the ratios differed through ontogeny. The elemental compositions (Ca, Mg, and Sr) in samples of stage III larvae (n = 50 per sample) from 11 different broods (mean Sr/Ca = 5.916 ± 0.161 millimole per mole [mmol mol−1]; mean Mg/Ca = 218.275 ± 59.957 mmol mol−1) and stage V larvae (n = 10 per sample) from 12 different broods (mean Sr/Ca = 6.110 ± 0.300 mmol mol−1; mean Mg/Ca = 267.081 ± 67.211 mmol mol–1) were measured using inductively coupled plasma optical emission spectrometry (ICP–OES). The ratio of Sr/Ca significantly increased from stage III to stage V larvae, suggesting an ontogenic shift in Sr/Ca ratios between larval stages. The ratio of Mg/Ca did not change significantly between larval stages, but variability among broods was high. The method used to examine the trace-element ratios provided robust, highly reproducible estimates of Sr/Ca and Mg/Ca ratios in the larvae of M. mercenaria, demonstrating that ICP–OES can be used to determine the trace-element composition of chitinous organisms like the Florida stone crab.

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

    Science.gov (United States)

    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.

  14. Standard test method for determination of impurities in plutonium: acid dissolution, ion exchange matrix separation, and inductively coupled plasma-atomic emission spectroscopic (ICP/AES) analysis

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2003-01-01

    1.1 This specification covers blended uranium trioxide (UO3), U3O8, or mixtures of the two, powders that are intended for conversion into a sinterable uranium dioxide (UO2) powder by means of a direct reduction process. The UO2 powder product of the reduction process must meet the requirements of Specification C 753 and be suitable for subsequent UO2 pellet fabrication by pressing and sintering methods. This specification applies to uranium oxides with a 235U enrichment less than 5 %. 1.2 This specification includes chemical, physical, and test method requirements for uranium oxide powders as they relate to the suitability of the powder for storage, transportation, and direct reduction to UO2 powder. This specification is applicable to uranium oxide powders for such use from any source. 1.3 The scope of this specification does not comprehensively cover all provisions for preventing criticality accidents, for health and safety, or for shipping. Observance of this specification does not relieve the user of th...

  15. [Determination of ru, rh and Pd in 30% trialkyl phosphine oxide (TRPO)-kerosene by inductively coupled plasma-atomic emission spectrum (ICP-AES)].

    Science.gov (United States)

    Wang, Jian-Chen; Zhang, Lin

    2013-07-01

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

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

    Science.gov (United States)

    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 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.

  17. Determination of metallic elements in natural and waste water by inductively coupled plasma-optical emission spectrometry (Icp-OES); Determinazione di specie metalliche in acque naturali e reflue mediante spettroscopia di emissione in sorgente al plasma (ICP-OES)

    Energy Technology Data Exchange (ETDEWEB)

    Petruzzelli, D. [Consiglio Nazionale delle Ricerche, Bari (Italy). Ist. di Ricerca sulle Acque; Bettinelli, M.; Spezia, S. [ENEL UML, Piacenza (Italy); Mastroianni, D.; Capri, S.; Pettine, M. [Consiglio Nazionale delle Ricerche, Rome (Italy). Ist. di Ricerca sulle Acque

    1998-12-31

    A method is described for multielement determination of 33 elements in liquids samples by inductively coupled plasma-optical emission spectrometry (Icp-OES). In this method the intensity of the light emitted at specific wavelengths from excited atoms and ions of a sample is measured and used to determine the concentrations of the element of interest. [Italiano] Viene descritto un metodo per la determinazione multielementare di 33 elementi in campioni liquidi basato sull`uso del plasma ottico. In questo metodo si misura l`intensita` della radiazione elettromagnetica emessa dagli atomi e ioni eccitati delle specie presenti nel campione.

  18. Analysis of trace rare earth elements in misch metal by means of ITP-PIXE (isotachophoresis - Particle Induced X-ray Emission) method

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jian-Ying; Hirokawa, Takeshi; Nishiyama, Fumitaka; Kimura, Goji; Kiso, Yoshiyuki; Ito, Kazuaki; Shoto, Eiji [Hiroshima Univ., Higashi-Hiroshima (Japan). Faculty of Engineering

    1993-12-31

    A misch metal, an alloy of light rare earth elements, was analyzed by a new coupled analytical method, ITP-PIXE (isotachophoresis - Particle Induced X-ray Emission): The sample solution containing ca.1 mg misch metal was separated and fractionated by the use of a preparative isotachophoretic analyzer. The dropwise fractions containing nanomole rare earth elements were analyzed off-line by PIXE. The matrix effect in X-ray measurement was reduced by the isotachophoretic removing of the dominant lanthanoids and preconcentration of the trace elements of interest. Consequently the minor elements, Sm, Gd, Tb, Dy, Ho, Er, Yb and Y could be determined accurately. The most trace element found was Yb (4ppm, 4ng in 1mg sample). The good accuracy of ITP-PIXE method was also demonstrated for several model samples of lanthanoids, where La was the dominant element and the thirteen lanthanoids were the minor elements. The ratio was varied from 500:1 to 50000:1. Even in the case of 50000:1, ca.10% accuracy was achieved for each minor element except for Sm(23%), Gd(17%) and Yb(18%). The analytical results by ITP-PIXE were compared with those by means of ICP-AES (Inductively Coupled Plasma - Atomic Emission Spectrometry). (author).

  19. Evaluation of analyte additions method for sodium determination in fuel ethanol by flame atomic emission spectrometry; Avaliacao do metodo das adicoes de analito para a determinacao de sodio em alcool combustivel por espectrometria de emissao atomica em chama

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Adriana Paiva de; Okumura, Leonardo Luiz; Gomes Neto, Jose Anchieta [UNESP, Araraquara, SP (Brazil). Inst. de Quimica. Dept. de Quimica Analitica

    2002-07-01

    The analyte additions method was applied for sodium determination in fuel ethanol by atomic emission spectrometry. Graphics involving emission intensity versus analyte concentration in the 0 - 0.300 mg Na L{sup -1} interval concentration range containing 2.1 g K L{sup -1} as an ionisation buffer. Twenty samples of commercial fuel ethanol were collected in different gas stations located in Araraquara city, analyzed and results obtained varied from 0.0072 to 1.55 mg Na L{sup -1}. The limits of detection (L.O.D.) varied from 0.0026 to 0.0239 mg Na L{sup -1}. Recoveries varied in the 95 - 104 % interval. The relative standard deviations (n=12) for three analyte additions in all samples were {<=}4,1 %. (author)

  20. Proton Transfer Reaction Mass Spectrometry detects rapid changes in volatile metabolite emission by Mycobacterium smegmatis after the addition of specific antimicrobial agents

    NARCIS (Netherlands)

    Crespo, E.; Cristescu, S. M.; de Ronde, H.; Kuijper, S.; Kolk, A.H.J.; Anthony, R.M.; Harren, F. J. M.

    2011-01-01

    The metabolic activity of plants, animals or microbes can be monitored by gas headspace analysis. This can be achieved using Proton Transfer Reaction Mass Spectrometry (PTR-MS), a highly sensitive detection method for trace gas analysis. PTR-MS is rapid and can detect metabolic responses on-line as

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

    Science.gov (United States)

    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...

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

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Salgado, S. [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain); Quijano, M.A., E-mail: marian.quijano@upm.es [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain); Bonilla, M.M. [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain)

    2012-02-10

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

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

    Directory of Open Access Journals (Sweden)

    F. Reyes

    2006-01-01

    Full Text Available 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 extit{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.

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

    Science.gov (United States)

    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.

  5. Characteristics of a nickel thin film and formation of nickel silicide by using remote plasma atomic layer deposition with Ni( i Pr-DAD)2

    Science.gov (United States)

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

    2015-03-01

    In this study, the characteristics of nickel thin film deposited by remote plasma atomic layer deposition (RPALD) on p-type Si substrate and formation of nickel silicide using rapid thermal annealing were determined. Bis(1,4-di-isopropyl-1,3-diazabutadienyl)nickel, Ni(iPr-DAD)2, was used as a Ni precursor and ammonia plasma was used as a reactant. This was the first attempt to deposit Ni thin film using Ni(iPr-DAD)2 as a precursor for the ALD process. The RPALD Ni film was deposited with a growth rate of around 2.2{\\AA}/cycle at 250 {\\deg}C and showed significant low resistivity of 33 {\\mu}{\\Omega}cm with a total impurity concentration of around 10 at. %.The impurities of the thin film, carbon and nitrogen, were existent by the forms of C-C and C-N in a bonding state. The impurities removal tendency was investigated by comparing of experimental conditions, namely process temperature and pressure. Nitrogen impurity was removed by thermal desorption during each ALD cycle and carbon impurity was reduced by the optimizing of the process pressure which is directly related with a mean free path of NH3 plasma. After Ni deposition, nickel silicide was formed by RTA in a vacuum ambient for 1 minute. A nickel silicide layer from ALD Ni and PVD Ni was compared at the annealing temperature from 500 to 900 {\\deg}C. NiSi from ALD Ni showed better thermal stability due to the contribution of small amounts of carbon and nitrogen in the asdeposited Ni thin film. Degradation of the silicide layer was effectively suppressed with a use of ALD Ni.

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

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    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.

  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

    Science.gov (United States)

    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. Volatile Profiles of Emissions from Different Activities Analyzed Using Canister Samplers and Gas Chromatography-Mass Spectrometry (GC/MS) Analysis: A Case Study

    Science.gov (United States)

    Orecchio, Santino; Fiore, Michele; Barreca, Salvatore; Vara, Gabriele

    2017-01-01

    The objective of present study was to identify volatile organic compounds (VOCs) emitted from several sources (fuels, traffic, landfills, coffee roasting, a street-food laboratory, building work, indoor use of incense and candles, a dental laboratory, etc.) located in Palermo (Italy) by using canister autosamplers and gas chromatography-mass spectrometry (GC-MS) technique. In this study, 181 VOCs were monitored. In the atmosphere of Palermo city, propane, butane, isopentane, methyl pentane, hexane, benzene, toluene, meta- and para-xylene, 1,2,4 trimethyl benzene, 1,3,5 trimethyl benzene, ethylbenzene, 4 ethyl toluene and heptane were identified and quantified in all sampling sites. PMID:28212294

  9. 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

    Science.gov (United States)

    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.

  10. Direct current plasma emission spectrometric determination of major, minor and trace elements in microwave oven acid leachates of powdered whole coal samples

    Energy Technology Data Exchange (ETDEWEB)

    Fadda, S. [CNR, Cagliari (Italy)

    2005-07-01

    Major concentrations of Al{sub 2}O{sub 3}, Fe{sub 2}O{sub 3}, MgO, CaO, Na{sub 2}O and K{sub 2}O, minor levels of TiO{sub 2}, P{sub 2}O{sub 5} and thirty petrologically, geochemically and environmentally significant trace elements have been determined in microwave oven acid leachates of whole powdered coal samples by direct current plasma-atomic emission spectrometry (DCP-AES). A single sample preparation procedure was suitable for all the determinations with no additional dilution step for major elements solution. Dried samples (0.5 g) were treated in low-pressure PFA digestion vessels with HF/HCl/HNO{sub 3}/HClO{sub 4} acids to quantitatively extract the analytes from the bulk material, while leaving the major part of organic matrix as a residue. To evaluate the accuracy of the microwave oven-DCP method a suite of eight certified coal reference materials of differing rank, were analysed with good agreement with the certified and/or available published data. Results are presented for the uncertified major oxides in the AR series reference materials.

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

    Science.gov (United States)

    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.

  12. 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

    Science.gov (United States)

    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...

  13. 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

    Science.gov (United States)

    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.

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

    Directory of Open Access Journals (Sweden)

    A. Setyan

    2012-09-01

    Full Text Available An Aerodyne high resolution time-of-flight aerosol mass spectrometer (HR-ToF-AMS was deployed during the Carbonaceous Aerosols and Radiative Effects Study (CARES that took place in northern California in June 2010. We present results obtained at Cool (denoted as the T1 site of the project in the foothills 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. During this study, the average mass loading of submicrometer particles (PM1 was 3.0 μg m−3, dominated by organics (80% and sulfate (9.9%. The organic aerosol (OA had a nominal formula of C1H1.38N0.004OM0.44, thus an average organic mass-to-carbon (OM/OC ratio of 1.70. Two distinct oxygenated OA factors were identified via Positive matrix factorization (PMF of the high-resolution mass spectra of organics. The more oxidized MO-OOA (O/C = 0.54 was interpreted as a surrogate for secondary OA (SOA influenced by biogenic emissions whereas the less oxidized LO-OOA (O/C = 0.42 was found to represent SOA formed in photochemically processed urban emissions. LO-OOA correlated strongly with ozone and MO-OOA correlated well with two 1st generation isoprene oxidation products (methacrolein and methyl vinyl ketone, indicating that both SOAs were relatively fresh. A hydrocarbon like OA (HOA factor was also identified, representing primary emissions mainly due to local traffic. On average, SOA (= MO-OOA + LO-OOA accounted for 91% of the total OA mass and 72% of the PM1 mass observed at Cool. Twenty three periods of urban plumes from T0 (Sacramento to T1 (Cool were identified using the Weather Research and Forecasting model coupled with Chemistry (WRF-Chem. The average PM1 mass loading was considerably higher in urban plumes than in air masses dominated by biogenic SOA. The change in OA

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

    Science.gov (United States)

    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)

  16. Understanding the effects of potassium ferricyanide on lead hydride formation in tetrahydroborate system and its application for determination of lead in milk using hydride generation inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Deng, Biyang; Xu, Xiangshu; Xiao, Yan; Zhu, Pingchuan; Wang, Yingzi

    2015-01-01

    To understand the formation of plumbane in the Pb(II)-NaBH4-K3Fe(CN)6 system, the intermediate products produced in the reaction of lead(II) and NaBH4 in the presence of K3Fe(CN)6 were studied. The produced plumbane and elemental lead were measured through continuous flow hydride generation (HG)-inductively coupled plasma optical emission spectrometry (ICP OES) and X-ray diffraction spectrometry techniques, respectively. Based on the experimental results, the explanations can be depicted in the following steps: (1) plumbane and black lead sediment (black Pb) are formed in the reaction of lead(II) and NaBH4; (2) the black Pb is oxidized by K3Fe(CN)6 to form Pb2[Fe(CN)6], which further reacts with NaBH4 to form more plumbane and black Pb; and (3) another round starts in which the produced black Pb from the step 2 is then oxidized continuously by K3Fe(CN)6 to form more Pb2[Fe(CN)6] complex, which would produce more plumbane. In short, the black Pb and Pb2[Fe(CN)6] complex are the key intermediate products for the formation of plumbane in the Pb(II)-NaBH4-K3Fe(CN)6 system. Based on the enhancement effect of potassium ferricyanide and potassium ferrocyanide, a method was developed to analyze lead in milk with HG-ICP OES technique. The detection limit of the method was observed as 0.081 μg L(-1). The linearity range of lead was found between 0.3 and 50,000 μg L(-1) with correlation coefficient of 0.9993. The recovery of lead was determined as 97.6% (n=5) for adding 10 μg L(-1) lead into the milk sample.

  17. Mass spectrometry

    DEFF Research Database (Denmark)

    Nyvang Hartmeyer, Gitte; Jensen, Anne Kvistholm; Böcher, Sidsel

    2010-01-01

    Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) is currently being introduced for the rapid and accurate identification of bacteria. We describe 2 MALDI-TOF MS identification cases - 1 directly on spinal fluid and 1 on grown bacteria. Rapidly obtained r...

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

    CERN Document Server

    Henley, D B; 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 Carinae, 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, suggestin...

  19. Development of open-air type electrolyte-as-cathode glow discharge-atomic emission spectrometry for determination of trace metals in water

    Science.gov (United States)

    Kim, Hyo J.; Lee, Jeong H.; Kim, Myung Y.; Cserfalvi, T.; Mezei, P.

    2000-07-01

    The open-air type electrolyte cathode atomic glow discharge (ELCAD) has been developed and studied for fundamental and analytical applications for determination of trace heavy metals in water. The normal closed-type discharge cell shows some problems such as unstable plasma due to changes in the pressure inside the cell during the discharge, and water vapor condensing onto the window. Applying approximately 1500 V to the several-millimeter gap between the electrolyte solution cathode and a Pt rod anode in atmospheric air pressure produced a stable plasma and significantly improved sensitivity. The emission spectrum of de-ionized water containing 100 mg/l Cu was measured and some emission lines were found from Cu I (324.7 nm, 327.4 nm and 510.5 nm) and Cu II (224.7 nm and 229.4 nm). The LODs of Cr, Cu, Fe, Mn, Ni, Pb, and Zn are in the ranges from 0.01 mg/l to 0.6 mg/l. The LODs of Cu, Mn, Pb and Zn improve by approximately one order of magnitude compared to the previous closed-type ELCAD.

  20. Trace determination of Hg together with As, Sb, Se by miniaturized optical emission spectrometry integrated with chemical vapor generation and capacitively coupled argon microwave miniplasma discharge

    Science.gov (United States)

    Matusiewicz, Henryk; Ślachciński, Mariusz

    2017-07-01

    A miniaturized optical emission spectrometer (OES) with capacitively coupled argon microwave microplasma (μCMP) as and excitation source and chemical vapor generation (CVG) for sample introduction was constructed for the determination of trace Hg, As, Sb and Se. The applied method enabled simultaneous determination of hydride-forming elements (As, Sb, Se) and volatile Hg. Mercury cold vapor and the hydride volatile species of As, Sb and Se were generated when standard or sample solutions were separated from the liquid phase for transport to the capacitively coupled microwave microplasma and detection of their atomic emission. A univariate approach and the simplex optimization procedure were used to achieve optimized conditions and derive analytical figures of merit. The experimental concentration detection limits (LODs) for simultaneous determination, calculated as the concentration giving a signal equal to three times of the standard deviation of the blank (LOD, 3σblank criterion, peak height) were 3.0, 1.4, 1.5 and 3.8 ng mL- 1 for Hg, As, Sb and Se, respectively. The method was validated by the analysis of three Certified Reference Materials (NIST 2711, NRCC DOLT-2, NIST 1643e) of different matrix composition and by the standard addition technique. The method offers relatively good precision (RSD ranged from 5% to 8%) for microsampling (200 μL) analysis. The measured of contents of elements in certified reference materials were in good agreement with the certified values (Hg 1.99-6.25 μg g- 1, As 16.6-105 μg g- 1, Sb 19.4-56.88 μg g- 1, Se 1.52-11.68 μg g- 1), according to the Student t-test, for a confidence level of 95%.

  1. Decomposição de argilas em forno de microondas e determinação simultânea dos seus constituintes principais por espectrometria de emissão óptica em plasma indutivamente acoplado Analysis of clays by inductively coupled plasma optical emission spectrometry after closed-vessel microwave-assisted acid decomposition

    Directory of Open Access Journals (Sweden)

    Claudineia R. Silva

    2005-02-01

    Full Text Available In this work a closed-vessel microwave-assisted acid decomposition procedure for clays was developed. Aluminum, Ca, Fe, K, Mg, Na, Si, and Ti were determined in clay digestates by inductively coupled plasma optical emission spectrometry. The most critical parameter for total decomposition of clays was the composition of the reagent mixture. The applied power and the heating time exerted a less critical influence. Best decomposition conditions were attained using a reagent mixture containing 4 mL aqua regia plus 3 mL HF and the heating program was implemented in 12 min. The accuracy of the results was demonstrated using two standard reference materials and a paired t-test showed a good agreement between determined and certified values at a 95% confidence level.

  2. Deviation from Boltzmann distribution in excited energy levels of singly-ionized iron in an argon glow discharge plasma for atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Lei; Kashiwakura, Shunsuke; Wagatsuma, Kazuaki, E-mail: wagatuma@imr.tohoku.ac.jp

    2012-01-15

    A Boltzmann plot for many iron ionic lines having excitation energies of 4.7-9.1 eV was investigated in an argon glow discharge plasma when the discharge parameters, such as the voltage/current and the gas pressure, were varied. A Grimm-style radiation source was employed in a DC voltage range of 400-800 V at argon pressures of 400-930 Pa. The plot did not follow a linear relationship over a wide range of the excitation energy, but it yielded a normal Boltzmann distribution in the range of 4.7-5.8 eV and a large overpopulation in higher-lying excitation levels of iron ion. A probable reason for this phenomenon is that excitations for higher excited energy levels of iron ion would be predominantly caused by non-thermal collisions with argon species, the internal energy of which is received by iron atoms for the ionization. Particular intense ionic lines, which gave a maximum peak of the Boltzmann plot, were observed at an excitation energy of ca. 7.7 eV. They were the Fe II 257.297-nm and the Fe II 258.111-nm lines, derived from the 3d{sup 5}4s4p {sup 6}P excited levels. The 3d{sup 5}4s4p {sup 6}P excited levels can be highly populated through a resonance charge transfer from the ground state of argon ion, because of good matching in the excitation energy as well as the conservation of the total spin before and after the collision. An enhancement factor of the emission intensity for various Fe II lines could be obtained from a deviation from the normal Boltzmann plot, which comprised the emission lines of 4.7-5.8 eV. It would roughly correspond to a contribution of the charge transfer excitation to the excited levels of iron ion, suggesting that the charge-transfer collision could elevate the number density of the corresponding excited levels by a factor of ca.10{sup 4}. The Boltzmann plots give important information on the reason why a variety of iron ionic lines can be emitted from glow discharge plasmas.

  3. 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

    Science.gov (United States)

    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.

  4. 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

    Energy Technology Data Exchange (ETDEWEB)

    Almeida Bezerra, Marcos [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Universidade Estadual do Sudoeste da Bahia, Departamento de Quimica e Exatas, Rua Jose Moreira Sobrinho s/n, Jequiezinho, Jequie/BA, 45206-190 (Brazil)], E-mail: mbezerra@uesb.br; Mitihiro do Nascimento Maeda, Sergio; Padua Oliveira, Eliane [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Fatima Batista de Carvalho, Maria de [Centro de Pesquisas e Desenvolvimento da PETROBRAS, Avaliacao e Monitoramento Ambiental, Av. Jequitiba, 950, Cidade Universitaria, Rio de Janeiro/RJ, 21941-598 (Brazil); Erthal Santelli, Ricardo [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil)

    2007-09-15

    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 per mille and 70 per mille. 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 {mu}g L{sup -1}, and precision expressed as relative standard deviation (n = 8, 20.0 {mu}g L{sup -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 per mille.

  5. 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

    Science.gov (United States)

    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‰.

  6. Simultaneous preconcentration of copper, zinc, cadmium, and nickel in water samples by cloud point extraction using 4-(2-pyridylazo)-resorcinol and their determination by inductively coupled plasma optic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Edson Luiz, E-mail: edsonqmc@hotmail.com [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Av. Centenario, 303, CP 96, 13416-000 Piracicaba, SP (Brazil); Santos Roldan, Paulo dos [Universidade Federal de Alagoas, Campus A.C. Simoes, Av. Lourival Melo Mota, Tabuleiro do Martins, CEP: 57072-970 AL (Brazil); Gine, Maria Fernanda [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Av. Centenario, 303, CP 96, 13416-000 Piracicaba, SP (Brazil)

    2009-11-15

    A procedure for simultaneous separation/preconcentration of copper, zinc, cadmium, and nickel in water samples, based on cloud point extraction (CPE) as a prior step to their determination by inductively coupled plasma optic emission spectrometry (ICP-OES), has been developed. The analytes reacted with 4-(2-pyridylazo)-resorcinol (PAR) at pH 5 to form hydrophobic chelates, which were separated and preconcentrated in a surfactant-rich phase of octylphenoxypolyethoxyethanol (Triton X-114). The parameters affecting the extraction efficiency of the proposed method, such as sample pH, complexing agent concentration, buffer amount, surfactant concentration, temperature, kinetics of complexation reaction, and incubation time were optimized and their respective values were 5, 0.6 mmol L{sup -1}, 0.3 mL, 0.15% (w/v), 50 deg. C, 40 min, and 10 min for 15 mL of preconcentrated solution. The method presented precision (R.S.D.) between 1.3% and 2.6% (n = 9). The concentration factors with and without dilution of the surfactant-rich phase for the analytes ranged from 9.4 to 10.1 and from 94.0 to 100.1, respectively. The limits of detection (L.O.D.) obtained for copper, zinc, cadmium, and nickel were 1.2, 1.1, 1.0, and 6.3 {mu}g L{sup -1}, respectively. The accuracy of the procedure was evaluated through recovery experiments on aqueous samples.

  7. Cloud point extraction with/without chelating agent on-line coupled with inductively coupled plasma optical emission spectrometry for the determination of trace rare earth elements in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Li Yingjie [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin, E-mail: binhu@whu.edu.cn [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2010-02-15

    The on-line incorporation of cloud point extraction (CPE) with/without 8-hydroxyquinoline (8-Ox) as chelating agent into flow injection analysis associated with inductively coupled plasma optical emission spectrometry (ICP-OES) for determining trace rare earth elements (REEs) is presented and evaluated. The significant parameters affecting on-line cloud point extraction of REEs such as sample pH, flow rate, 8-Ox concentration, Triton X-114 concentration were systematically studied. Under the optimized conditions, with the consumption of 3.0 mL sample solution, the limits of detection (3{sigma}) were ranged from 41.4 pg mL{sup -1} (Yb) to 448 pg mL{sup -1} (Gd) with relative standard deviations (RSDs) of 1.0% (Eu)-5.9% (Sm) for on-line CPE-ICP-OES with 8-Ox as chelating agent, and 69.0 pg mL{sup -1} (Sc) to 509.5 pg mL{sup -1} (Sm) with RSDs of 2.9% (Yb)-7.5% (Ho) for on-line CPE-ICP-OES without 8-Ox as chelating agent, respectively. The sample throughput of 17 samples h{sup -1} was obtained for both systems. The developed methods of on-line CPE-ICP-OES were validated by the analysis of certified reference material (GBW07605, tea leaves) and real biological samples of pig liver, Auricularia auricula and mushroom.

  8. 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.

    Science.gov (United States)

    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.

  9. Simultaneous preconcentration of copper, zinc, cadmium, and nickel in water samples by cloud point extraction using 4-(2-pyridylazo)-resorcinol and their determination by inductively coupled plasma optic emission spectrometry.

    Science.gov (United States)

    Silva, Edson Luiz; Roldan, Paulo dos Santos; Giné, Maria Fernanda

    2009-11-15

    A procedure for simultaneous separation/preconcentration of copper, zinc, cadmium, and nickel in water samples, based on cloud point extraction (CPE) as a prior step to their determination by inductively coupled plasma optic emission spectrometry (ICP-OES), has been developed. The analytes reacted with 4-(2-pyridylazo)-resorcinol (PAR) at pH 5 to form hydrophobic chelates, which were separated and preconcentrated in a surfactant-rich phase of octylphenoxypolyethoxyethanol (Triton X-114). The parameters affecting the extraction efficiency of the proposed method, such as sample pH, complexing agent concentration, buffer amount, surfactant concentration, temperature, kinetics of complexation reaction, and incubation time were optimized and their respective values were 5, 0.6 mmol L(-1), 0.3 mL, 0.15% (w/v), 50 degrees C, 40 min, and 10 min for 15 mL of preconcentrated solution. The method presented precision (R.S.D.) between 1.3% and 2.6% (n=9). The concentration factors with and without dilution of the surfactant-rich phase for the analytes ranged from 9.4 to 10.1 and from 94.0 to 100.1, respectively. The limits of detection (L.O.D.) obtained for copper, zinc, cadmium, and nickel were 1.2, 1.1, 1.0, and 6.3 microg L(-1), respectively. The accuracy of the procedure was evaluated through recovery experiments on aqueous samples.

  10. 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.

    Science.gov (United States)

    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. © 2013 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  12. Characterization of rapidly-prototyped, battery-operated, argon-hydrogen microplasma on a hybrid chip for elemental analysis of microsamples by portable optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Weagant, Scott; Dulai, Gurjit; Li, Lu; Karanassios, Vassili, E-mail: vkaranassios@uwaterloo.ca

    2015-04-01

    A rapidly-prototyped, battery-operated, atmospheric-pressure, self-igniting Ar-H{sub 2} microplasma was interfaced to a portable fiber-optic spectrometer. The microplasma-spectrometer combination was used to document the spectral lines emitted when μL of dilute solutions of single element standards of Ag, Ba, Ca, Eu, Pd, Rb and Sr were first dried and then vaporized into the microplasma. A small-size, electrothermal vaporization system was used for microsample introduction. Identification of the prominent spectral lines for these elements is reported. It was found that the most prominent spectral line for Ba, Ca and Sr was different than that emitted from an inductively coupled plasma (ICP). In general, prominent spectral lines with low excitation energy were dominating, thus resulting in spectra simpler than those emitted from an ICP. Detection limits were between 45 and 180 pg (expressed in absolute amounts). When expressed in relative concentration units, they ranged between 15 and 60 μg/L (obtained using 3 μL diluted standards). Calibration curves were linear (on the average) for 1.5 orders-of-magnitude. Average precision was 15%. Analytical capability and utility was demonstrated using the determination of Ca and Mg in (medicinal) thermal spring water. - Highlights: • Microplasma emission spectra for Ag, Ba, Ca, Eu, Pd, Rb and Sr are reported. • Absolute amount detection limits ranged between 45 pg and 180 pg. • Relative unit detection limits ranged between 15 and 60 μg/L (using 3 μL). • The effect of vaporization temperature on analyte signals is reported. • Ca and Mg concentrations in (medicinal) thermal spring water were determined.

  13. Determinação de elementos essenciais maiores e traço em queijos por espectrometria de emissão atômica com plasma de argônio induzido após digestão parcial Determination of minerals and trace elements in cheese by inductively-coupled plasma optical emission spectrometry after partial digestion

    Directory of Open Access Journals (Sweden)

    Carmen Silvia Kira

    2007-09-01

    Full Text Available Concentrações de Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P e Zn foram determinadas em amostras de quatro tipos de queijo (mussarela, minas, prato e parmesão por espectrometria de emissão atômica com plasma de argônio acoplado indutivamente após dissolução parcial (hidrólise com HCl e total da matéria orgânica (digestão por via seca. As concentrações da maioria dos elementos essenciais maiores e traço, usando o método de dissolução parcial, foram consideradas estatisticamente iguais às obtidas com o método de dissolução total da matéria orgânica, demonstrando a potencialidade da digestão parcial em análises de rotina.Concentrations of Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P and Zn in four different types of cheese (mozzarella, white cheese, prato and parmesan were analyzed by inductively-coupled plasma optical emission spectrometry (ICP-OES after partial digestion (HCl hydrolysis and total digestion of organic matter (dry ashing. The results obtained for most of the elements analyzed here by the partial digestion (HCl hydrolysis and dry ashing methods were found to be statistically congruent, demonstrating the promising potential of the partial digestion method in routine analyses.

  14. Investigations on the use of pneumatic cross-flow nebulizers with dual solution loading including the correction of matrix effects in elemental determinations by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bauer, Mathieu [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Broekaert, Jose A.C. [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)], E-mail: jose.broekaert@chemie.uni-hamburg.de

    2007-02-15

    The use of a so-called trihedral and a T-shaped cross-flow pneumatic nebulizer with dual solution loading for inductively coupled plasma optical emission spectrometry has been studied. By these devices analyte clouds from two solutions can be mixed during the aerosol generation step. For both nebulizers the correction of matrix effects using internal standardization and standard addition calibration in an on-line way was investigated and compared to elemental determinations using a conventional cross-flow nebulizer and calibration with synthetic standard solutions without matrix matching. A significant improvement of accuracy, both for calibration with internal standardization and standard addition, was obtained in the case of four synthetic solutions containing each 40 mmol L{sup -1} Na, K, Rb and Ba as matrix elements and 300 {mu}g L{sup -1} Cd, Co, Cr, Cu, Fe, Mn, Ni and Pb as analytes. Calibration by standard addition in the case of dual solution loading has been shown to be very useful in the determination of elements at minor and trace levels in steel and alumina reference materials. The results of analysis for minor concentrations of Cr, Cu and Ni in steel as well as for Ca, Fe, Ga, Li, Mg, Mn, Na, Si and Zn in alumina powder certified reference materials subsequent to sample dissolution were found to be in good agreement with the certificates. Limits of detection were found to be only slightly above those for a conventional cross-flow nebulizer and a precision better than 3% was realized with both novel nebulizers.

  15. Analysis of metals and phosphorus in biodiesel B100 from different feedstock using a Flow Blurring® multinebulizer in inductively coupled plasma-optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Avila Orozco, Francisco D. [Lab. FIA, Sección Química Analítica, INQUISUR (UNS-CONICET), Universidad Nacional del Sur, Avenida Alem 1253, B8000CPB, Bahía Blanca (Argentina); Kovachev, Nikolay; Aguirre Pastor, Miguel Ángel [Dpto. Química Analítica, Nutrición y Bromatología e Instituto Universitario de Materiales, Facultad de Ciencias, Universidad de Alicante, Apdo. 99, Alicante (Spain); Domini, Claudia E.; Fernández Band, Beatriz S. [Lab. FIA, Sección Química Analítica, INQUISUR (UNS-CONICET), Universidad Nacional del Sur, Avenida Alem 1253, B8000CPB, Bahía Blanca (Argentina); Canals Hernández, Antonio, E-mail: a.canals@ua.es [Dpto. Química Analítica, Nutrición y Bromatología e Instituto Universitario de Materiales, Facultad de Ciencias, Universidad de Alicante, Apdo. 99, Alicante (Spain)

    2014-05-01

    Highlights: • The elemental analysis of biodiesel by the proposed method is simple and fast. • Two-nozzles Flow Blurring® nebulizer allow to reduce the spectral interferences. • Two-nozzles Flow Blurring® nebulizer avoid the formation of carbon deposits. • The analysis may be carried out without any sample pretreatment. Abstract: A simple and fast method for determining the content of Na, K, Ca, Mg, P, and 20 heavy metals in biodiesel samples with inductively coupled plasma optical emission spectrometry (ICP OES) using a two-nozzle Flow Blurring® multinebulizer prototype and on-line internal standard calibration, are proposed. The biodiesel samples were produced from different feedstock such as sunflower, corn, soybean and grape seed oils, via a base catalyst transesterification. The analysis was carried out without any sample pretreatment. The standards and samples were introduced through one of the multinebulizer nozzles, while the aqueous solution containing yttrium as an internal standard was introduced through the second nozzle. Thus, the spectral interferences were compensated and the formation of carbon deposits on the ICP torch was prevented. The determination coefficients (R²) were greater than 0.99 for the studied analytes, in the range 0.21–14.75 mg kg⁻¹. Short-term and long-term precisions were estimated as relative standard deviation. These were acceptable, their values being lower than 10%. The LOQ for major components such as Ca, K, Mg, Na, and P, were within a range between 4.9 ng g⁻¹ for Mg (279.553 nm) and 531.1 ng g⁻¹ for Na (588.995 nm), and for the other 20 minor components they were within a range between 1.1 ng g⁻¹ for Ba (455.403 nm) and 2913.9 ng g⁻¹ for Pb (220.353 nm). Recovery values ranged between 95% and 106%.

  16. ROCKS & MINERALS DETERMINATION AND ANALYSIS

    Institute of Scientific and Technical Information of China (English)

    2012-01-01

    <正>20122362 Cai Shuwei ( Nanjing Institute of Geology and Mineral Resources,Nanjing 210016,China );Zhu Jiaping Evaluating on Uncertainty of Determination of Manganese Contents in Groundwater by Inductively Coupled Plasma Atomic Emission Spectrometry ( Resources Survey & Environment,ISSN1671-4814,CN32-1640 / N,32 ( 4 ), 2011,p.307-310,2tables,8refs. ) Key words:inductively coupled plasma atomic emission spectroscopy,manganese

  17. Understanding the effects of potassium ferricyanide on lead hydride formation in tetrahydroborate system and its application for determination of lead in milk using hydride generation inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Biyang, E-mail: dengby16@163.com; Xu, Xiangshu; Xiao, Yan; Zhu, Pingchuan; Wang, Yingzi

    2015-01-01

    Highlights: • Proposed a novel explanation for plumbane generation. • Expounded the role of K{sub 3}Fe(CN){sub 6} in plumbane generation. • Clarified the controversial aspects in the mechanism of K{sub 3}Fe(CN){sub 6} enhancement. • Used X-ray diffractometry to analyze the intermediates. • Developed a method to analyze lead in milk using K{sub 3}Fe(CN){sub 6} and K{sub 4}Fe(CN){sub 6} as new additives. - Absract: To understand the formation of plumbane in the Pb{sup II}-NaBH{sub 4}-K{sub 3}Fe(CN){sub 6} system, the intermediate products produced in the reaction of lead(II) and NaBH{sub 4} in the presence of K{sub 3}Fe(CN){sub 6} were studied. The produced plumbane and elemental lead were measured through continuous flow hydride generation (HG)-inductively coupled plasma optical emission spectrometry (ICP OES) and X-ray diffraction spectrometry techniques, respectively. Based on the experimental results, the explanations can be depicted in the following steps: (1) plumbane and black lead sediment (black Pb) are formed in the reaction of lead(II) and NaBH{sub 4}; (2) the black Pb is oxidized by K{sub 3}Fe(CN){sub 6} to form Pb{sub 2}[Fe(CN){sub 6}], which further reacts with NaBH{sub 4} to form more plumbane and black Pb; and (3) another round starts in which the produced black Pb from the step 2 is then oxidized continuously by K{sub 3}Fe(CN){sub 6} to form more Pb{sub 2}[Fe(CN){sub 6}] complex, which would produce more plumbane. In short, the black Pb and Pb{sub 2}[Fe(CN){sub 6}] complex are the key intermediate products for the formation of plumbane in the Pb{sup II}-NaBH{sub 4}-K{sub 3}Fe(CN){sub 6} system. Based on the enhancement effect of potassium ferricyanide and potassium ferrocyanide, a method was developed to analyze lead in milk with HG-ICP OES technique. The detection limit of the method was observed as 0.081 μg L{sup −1}. The linearity range of lead was found between 0.3 and 50,000 μg L{sup −1} with correlation coefficient of 0

  18. Simultaneous determination of 11 trace elements in coal by inductively coupled plasma-optical emission spectrometry%ICP-OES法同时测定煤中11种微量元素

    Institute of Scientific and Technical Information of China (English)

    吕鑫磊

    2015-01-01

    To quickly determine microelements of coal in batch,the coal sample was ashed first at high temperature,then the product was dissolved by the mixture of HCl,HF and HClO4 ,the third step was to extract the microelements with HCl. The microelements which were Ga,Th,V,P,Cu,Co,Ni,Zn,Pb,Cr,Cd were determined with ICP-OES (Inductively Coupled Plasma-Optical Emission Spectrometry). With reasonable sample dissolution methods,radio-frequency power,analytical spectral line and experimental data,the influence of spec-tral interference on determination was eliminated by off-peak background deduction method, meanwhile, the 11 kinds of microelements could be determined by ICP-OES at the same time. The detection limits for the elements was 0. 03~1. 17 μg/g. The method was applied to the determination of 11 microelements in Soil National Standard Reference Materials and the results were in agreement with certified val-ues with precision of 0. 32% ~3. 19% RSD (n=11).%为实现煤中多种微量元素的批量快速测定,煤样经高温灰化、盐酸-氢氟酸-高氯酸三元体系溶解、盐酸提取后,使用电感耦合等离子体发射光谱( ICP-OES )同时测定煤中镓钍钒磷铜钴镍锌铅铬镉11种微量元素. 在对样品分解方法、射频功率、分析谱线和积分点数合理选择的基础上,通过离峰扣背景法消除了各种光谱干扰对测定的影响,建立了采用ICP-OES同时测定煤中镓钍钒磷铜钴镍锌铅铬镉 11 种微量元素的实验方法. 方法检出限为 0. 03 ~1. 17 μg/g,方法精密度( n=11 ) 0. 32% ~3. 19%,土壤国家标准物质的分析测定值与标准值吻合较好. 与传统化学方法相比,该方法快速准确,提高了分析效率,满足煤质分析的一般要求.

  19. 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

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Lingling; Zhong, Shuxian; Fang, Keming; Qian, Zhaosheng [College of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua 321004 (China); Chen, Jianrong, E-mail: cjr@zjnu.cn [College of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua 321004 (China); College of Geography and Environmental Sciences, Zhejiang Normal University, Jinhua 321004 (China)

    2012-11-15

    Highlights: Black-Right-Pointing-Pointer A dual-cloud point extraction (d-CPE) procedure was firstly developed for simultaneous pre-concentration and separation of trace metal ions combining with ICP-OES. Black-Right-Pointing-Pointer The developed d-CPE can significantly eliminate the surfactant of Triton X-114 and successfully extend to the determination of water samples with good performance. Black-Right-Pointing-Pointer The designed method is simple, high efficient, low cost, and in accordance with the green chemistry concept. - Abstract: A dual-cloud point extraction (d-CPE) procedure has been developed for simultaneous pre-concentration and separation of heavy metal ions (Cd{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Pb{sup 2+}, Zn{sup 2+}, and Cu{sup 2+} 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 Multiplication-Sign 10{sup -4} mol L{sup -1}, HNO{sub 3} = 0.8 mol L{sup -1}), the detection limits for Cd{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Pb{sup 2+}, Zn{sup 2+}, and Cu{sup 2+} ions were 0.01, 0.04, 0.01, 0.34, 0.05, and 0.04 {mu}g L{sup -1}, respectively. Relative standard deviation (RSD) values for 10 replicates at 100 {mu}g L{sup -1} were lower than 6.0%. The proposed method could be successfully applied to the determination of Cd{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Pb{sup 2+}, Zn{sup 2+}, and Cu{sup 2+} ion in water samples.

  20. Analysis of accumulation, extractability, and metabolization of five different phenylarsenic compounds in plants by ion chromatography with mass spectrometric detection and by atomic emission spectroscopy.

    Science.gov (United States)

    Schmidt, Anne-Christine; Kutschera, Kristin; Mattusch, Jürgen; Otto, Matthias

    2008-12-01

    Phenylated arsenic compounds occur as highly toxic contaminants in former military areas where they were formed as degradation products of chemical warfare agents. Some phenylarsenic compounds such as roxarsone and aminophenylarsonic acids were applied as food additive and veterinary drugs in stock-breeding and therefore pose an environmental risk in agricultural used sites. Very few data exist in the literature concerning uptake and effects of phenylarsenic compounds in plants growing on contaminated soils. In this study, the accumulation, extractability, and metabolization of five different phenylarsenic compounds, phenylarsonic acid, p- and o-aminophenylarsonic acid, phenylarsine oxide, and 3-nitro-4-hydroxyphenylarsonic acid called roxarsone, by the terrestrial plant Tropaeolum majus were investigated. Ion chromatography coupled to inductively coupled plasma mass spectrometry was used to differentiate these arsenic compounds, and inductively coupled plasma atomic emission spectroscopy was used for total arsenic quantification. All compounds considered were taken up by the roots and transferred to stalks, leaves, and flowers. The strongest accumulation was observed for unsubstituted phenylarsonic acid followed by its trivalent analogue phenylarsine oxide that was mostly oxidized in soil whereas the amino- or nitro- and hydroxy-substituted phenylarsonic acids were accumulated to a smaller degree. The highest extraction yield of 90% for ground leaf material was achieved by 0.1M phosphate buffer, pH 7.7, in a two-step extraction with a total extraction time of 24h. The extraction of higher amounts of arsenic (50-70% of total arsenic present in leaves depending on arsenic species application) from non-ground intact leaves with deionized water in comparison with the buffer (20-40% of total arsenic) is ascribed to osmotic effects. The arsenic species analysis revealed a cleavage of the amino groups from the phenyl ring for plants treated with aminophenylarsonic acids

  1. The use of electro spray mass spectrometry for the determination of dissolved species application for determination of zirconium complexes in reprocessing spent fuel matrice; Electrospray/spectrometrie de masse, technique d'avenir pour l'etude des complexes. Applications aux systemes U(6)/Zr(4) dans les conditions simulees du procede Purex

    Energy Technology Data Exchange (ETDEWEB)

    Lamouroux, Ch.; Moulin, Ch. [CEA Saclay, Dept. des Procedes d' Enrichissement (DCC/DPE/SPCP), 91 - Gif-sur-Yvette (France); Blanc, P. [CEA Valrho, (DCC/DRRV/SEMP), 30 - Marcoule (France)

    2000-07-01

    Liquid-liquid extraction of Zirconium one of the most important fission products, was investigated by Electro-spray Mass Spectrometry (ESI/MS) in simulated nuclear reprocessing spent fuel process conditions. Zr{sup IV} can precipitate at the organic / water interface after its extraction by dibutyl-phosphoric acid (HDBP), the most common degradation product of tributylphosphate (TBP) under radiolysis. However, precipitation of ZrI{sup IV} is restricted and particularly dependent on the ratio 'r': (HDBP){sub tot}/(Zr{sup IV}]{sub tot}. The type and characterization of the precipitate is reported in different papers as Zr(NO{sub 3}){sub 2}(DBP){sub 2}. complex. However, some uncertainties exist about the composition and structures of the dissolved Zr species extracted. Techniques already used for such purposes are NMR (Nuclear Magnetic Resonance) and vibrational spectroscopy, but identification of the extracted metal complex structures is debatable. To obtain more definitive information, the use of ESI/MS could be a complementary tool for characterizing the extracted metal complexes. ESI allows ionization/desorption of non-volatile analytes into gas phase detected by mass spectrometry with high sensitivity, making it a complementary tool for examining the speciation of dissolved metal species. Extractions were carried out for the system (ZrI{sup IV} in HNO{sub 3} 3M)/(TBP/C{sub 12}H{sub 26} 30/70 spiked with HDBP) by varying the ratio r. ZrI{sup IV} extraction was confirmed by ICP-AES (Inductively Coupled plasma-Atomic Emission Spectroscopy) measurements on the aqueous phase, and dissolved metal complexes were identified by ESI/MS experiments on the organic phase. Different complexes could be detected with ESI used in positive and negative ion mode as a function of the extraction conditions such as the ratio r. Good agreement is observed between the variation in mass spectra and Zr behavior described for solutions. For a ratio 0

  2. Experimental benchmark of non-local-thermodynamic-equilibrium plasma atomic physics codes; Validation experimentale des codes de physique atomique des plasmas hors equilibre thermodynamique local

    Energy Technology Data Exchange (ETDEWEB)

    Nagels-Silvert, V

    2004-09-15

    The main purpose of this thesis is to get experimental data for the testing and validation of atomic physics codes dealing with non-local-thermodynamical-equilibrium plasmas. The first part is dedicated to the spectroscopic study of xenon and krypton plasmas that have been produced by a nanosecond laser pulse interacting with a gas jet. A Thomson scattering diagnostic has allowed us to measure independently plasma parameters such as electron temperature, electron density and the average ionisation state. We have obtained time integrated spectra in the range between 5 and 10 angstroms. We have identified about one hundred xenon rays between 8.6 and 9.6 angstroms via the use of the Relac code. We have discovered unknown rays for the krypton between 5.2 and 7.5 angstroms. In a second experiment we have extended the wavelength range to the X UV domain. The Averroes/Transpec code has been tested in the ranges from 9 to 15 angstroms and from 10 to 130 angstroms, the first range has been well reproduced while the second range requires a more complex data analysis. The second part is dedicated to the spectroscopic study of aluminium, selenium and samarium plasmas in femtosecond operating rate. We have designed an interferometry diagnostic in the frequency domain that has allowed us to measure the expanding speed of the target's backside. Via the use of an adequate isothermal model this parameter has led us to know the plasma electron temperature. Spectra and emission times of various rays from the aluminium and selenium plasmas have been computed satisfactorily with the Averroes/Transpec code coupled with Film and Multif hydrodynamical codes. (A.C.)

  3. Determinação dos teores de minerais em sucos de frutas por espectrometria de emissão óptica em plasma indutivamente acoplado (ICP-OES Minerals determination in juices by inductively coupled plasma optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    Marcelo Antônio MORGANO

    1999-12-01

    Full Text Available Dois métodos de preparação de amostra para determinação de minerais em suco de uva foram comparados: extração com ácido clorídrico a frio com agitação e digestão em sistema fechado, sob pressão, empregando-se energia de microondas. As concentrações dos minerais foram obtidas empregando-se a técnica de Espectrometria de Emissão Óptica em Plasma Indutivamente Acoplado (ICP-OES. Os teores dos minerais Ca, P, Na, K, Mg, Zn, Fe, Mn e Cu não diferiram significativamente ao nível de 5% (Teste F para as duas metodologias empregadas. A precisão e exatidão dos métodos foi avaliada usando o suco de uva. A metodologia de extração com ácido clorídrico foi empregada para a determinação dos teores de minerais em sucos processados de abacaxi, acerola, caju, goiaba, manga, maracujá e uva. Para facilitar a interpretação dos teores dos minerais encontrados, foram utilizadas as técnicas de Análise por Componentes Principais (PCA e Análise Hierárquica por Agrupamento (HCA.Two sample preparation methods for the determination of minerals from grape juice were investigated for the purpose of methodological evaluation: using hydrochloric acid by shaking, and digestion in closed system, under pressure, using microwave power. The concentrations of minerals were evaluated by the technique of Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES. The minerals contents of Ca, P, Na, K, Mg, Zn, Fe, Mn, and Cu did not differ significantly at the level of 5% (it Tests F for both methodologies used. The precision and accuracy of both methodologies were evaluated using grape juice. The extraction methodology with hydrochloric acid was used for the determination of mineral amounts in processed juices from pineapple, acerola, cashew, guava, mango, passion fruit and grape. To enhance the interpretation of the amounts of minerals, from a nutritional point of view, techniques of Principal Components Analysis (PCA and Hierarchic Cluster

  4. Analytical Figures of Merit of Hildebrand Grid and Ultrasonic Nebulizations in Inductively Coupled Plasma Atomic Emission%双铂网雾化和超声雾化进样系统对ICP-AES分析性能的影响

    Institute of Scientific and Technical Information of China (English)

    田梅; 韩小元; 卓尚军; 张瑞荣

    2012-01-01

    Hildebrand grid nebulizer is a kind of improved Babington nebulizer, which can nebulize solutions with high total dissolved solids. And the ultrasonic nebulizer(USN) possesses advantage of high nebulization efficiency and fine droplets. In the present paper, the detection limits, matrix effects, ICP robustness and memory effects of Hildebrand grid and ultrasonic nebulizers for ICF-AES were studied The results show that the detection limits using USN are improved by a factor of 6~23 in comparison to Hildebrand grid nebulizer for Cu, Pb, Zn, Cr, Cd and Ni. With the USN the matrix effects were heavier, and the degree of intensity enhancement and lowering depends on the element line, the composition and concentrations of matrices. Moreover, matrix effects induced by Ca and Mg are more significant than those caused by Na and Mg, and intensities of ionic lines are affected more easily than those of atomic lines. At the same time, with the USN ICP has less robustness. In addition, memory effect of the USN is also heavier than that of Hildebrand grid nebulizer.%从元素检出限、基体效应、ICP稳健性及记忆效应方面实验研究了双铂网雾化与超声雾化两种进样方式对ICP-AES分析性能的影响.结果表明,在超声雾化进样条件下,Cu,Pb,Zn,Cr,Cd,Ni的检出限较双铂网雾化的检出限降低了6~23倍;在基体效应方面,超声雾化进样时基体对元素原子及离子谱线强度的影响均较双铂网雾化系统明显,元素谱线增强/减弱的幅度受元素谱线、基体组成和浓度的影响;Ca和Mg基体对谱线强度的影响强于K和Na基体;离子谱线受基体的影响明显强于原子谱线.超声雾化系统进样时ICP的稳健性要劣于双铂网雾化系统,而且超声雾化系统的记忆效应较双铂网雾化器严重.

  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.

    Science.gov (United States)

    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. 等离子发射光谱法测定催化剂中的钯%Determination of Palladium Content in Catalyst by Inductively Coupled Plasma Atomic Emission Spectrometry(ICP-AES)

    Institute of Scientific and Technical Information of China (English)

    刘东艳; 张园力

    2001-01-01

    提出了以ICP-AES测定催化剂中钯含量的方法。考查了试样的分解方法,载体及所用试剂对钯测定的影响,发现氧化铝载体、硫酸等对钯的测定均有负干扰,2%王水、2%高氯酸对钯的测定无影响。提出采用载体匹配法测定Pd/Al2O3中钯的质量分数,该方法简单、准确、快速,回收率在95%以上。%A method for determining palladium content in catalysts supported on active carbon and aluminum oxide by ICP-AES was reported.The dissolution conditions of catalyst samples as well as interference conditions of inorganic acid and carrier were inspected.The recoveries are more than 96%,and the relative standard deviation of palladium determination on six samples are lower than 3%.

  7. Solid phase extraction of Cd, Cu, and Ni from leafy vegetables and plant leaves using amberlite XAD-2 functionalized with 2-hydroxy-acetophenone-thiosemicarbazone (HAPTSC) and determination by inductively coupled plasma atomic emission spectroscopy.

    Science.gov (United States)

    Rao, G Purna Chandra; Seshaiah, Kalluru; Rao, Yerra Koteswara; Wang, M C

    2006-04-19

    A method for solid phase extraction of trace metals, namely, Cd, Cu, and Ni, using Amberlite XAD-2 functionalized with a new chelating ligand, 2-hydroxy-acetophenone-3-thiosemicarbazone (Amberlite XAD-2-HAPTSC), has been developed. The optimum experimental conditions for the quantitative sorption of three metals, pH, effect of flow rate, concentration of eluent, sorption capacity, kinetics of sorption, and the effect of diverse ions on the sorption of analytes have been investigated. The chelating resin could be reused for more than 20 cycles of sorption-desorption without any significant change (<1.5%). The accuracy of the proposed procedure was evaluated by standard reference materials. The proposed method was applied for the determination of trace metal ions in leafy vegetable samples collected from different sources and medicinal plant leaves.

  8. A geração química de vapor em espectrometria atômica Chemical vapor generation in atomic spectrometry

    Directory of Open Access Journals (Sweden)

    Iracema Takase

    2002-12-01

    Full Text Available The historical development of atomic spectrometry techniques based on chemical vapor generation by both batch and flow injection sampling formats is presented. Detection via atomic absorption spectrometry (AAS, microwave induced plasma optical emission spectrometry (MIP-OES, inductively coupled plasma optical emission spectrometry (ICP-OES , inductively coupled plasma mass spectrometry (ICP-MS and furnace atomic nonthermal excitation spectrometry (FANES are considered. Hydride generation is separately considered in contrast to other methods of generation of volatile derivatives. Hg ¾ CVAAS (cold vapor atomic absorption spectrometry is not considered here. The current state-of-the-art, including extension, advantages and limitations of this approach is discussed.

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

    Science.gov (United States)

    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…

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

    Science.gov (United States)

    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…

  11. 微波马弗炉处理—火焰原子吸收光谱法测定废旧电路板中金银铂钯%Determination of gold, silver, platinum, palladium in waste circuit boards samples by flame atomic absorption spectrometry with microwave muffle furnace pretreatment

    Institute of Scientific and Technical Information of China (English)

    叶艳青; 羊波; 杨新周; 李银科; 胡秋芬

    2012-01-01

    A novel method for the determination of gold, silver, platinum and palladium in waste circuit board samples was investigated in this paper by flame atomic absorption spectrometry with microwave muffle furnace pretreatment. 5. 0 g of crashed waste circuit board samples was weighed and burned in microwave muffle furnace at 550 ℃ for 30 min to decompose organic matter. After the burning things were dissolved with aqua regia, gold, silver, platinum and palladium in the sample solution were determined by flame atomic absorption spectrometry. The detection limit of gold, silver, platinum and palladium was 0. 078, 0. 12, 0. 15 and 0. 15 mg/mL, respectively. The recoveries were between 90% and 108%. The method was applied to the same waste circuit board sample for 7 times. The relative standard deviations on the same day were between 2. 2% and 2. 9%, and the relative standard deviations on different day between 3,3% and 3. 5%. The method was applied to the analysis of waste circuit board and the results were consistent with those obtained by microwave digestion inductively coupled plasma atomic emission spectrometry.%研究了微波马弗炉加热处理样品,火焰原子吸收光谱法测定废旧电路板中金、银、铂、钯的方法.称取5.0g粉碎后废旧电路板样品,用微波马弗炉在550℃灼烧30 min分解有机物,用王水溶解样品,样品溶液中的金、银、铂、钯用火焰原子吸收光谱法进行测定.金、银、铂、钯的方法检出限分别为0.078、0.12、0.15和0.15 mg/mL;方法回收率在90%~108%之间;用本方法平行测定同一废旧电路板样品7次,日内相对标准偏差为2.2%~2.9%;日间相对标准偏差为3.3%~3.5%.将本方法用于废旧电路板分析,测得结果与微波消解—电感耦合等离子体发射光谱法一致.

  12. Detection of metal ions in potassium hydroxide with inductively coupled plasma optical emission spectrometry method%电感耦合等离子光谱法测定氢氧化钾中金属离子

    Institute of Scientific and Technical Information of China (English)

    丁灵; 张天兰; 弓创周; 夏俊玲

    2012-01-01

    Silicate,iron,sodium,aluminum,calcium,and nickel in high-quality flaky potassium hydroxide were respectively detected with visual colorimetry, spectrophotorrietry, and atomic absorption spectrometry .These methods are too complex and need too much time.Now the six elements (silicate, iron, sodium, aluminum, calcium, and nickel) can be detected at the same time with inductively coupled plasma spectrometry .The method is simple and rapid, and has a high precision and accuracy.%高品质片状氢氧化钾中硅酸盐、铁、钠、铝、钙、镍6项指标通常分别采用目视比色法、分光光度法、原子吸收法测定,其操作繁琐并且耗费时间较长.采用电感耦合等离子发射光谱仪可同时测定硅酸盐、铁、钠、铝、钙、镍6项指标.该法简便、快速,并有较高的精密度和准确度.

  13. X-ray spectrometry with synchrotron radiation; Roentgenspektrometrie mit Synchrotronstrahlung

    Energy Technology Data Exchange (ETDEWEB)

    Mueller, Matthias [Physikalisch-Technische Bundesanstalt (PTB), Berlin (Germany). Arbeitsgruppe ' Roentgen- und IR-Spektrometrie' ; Gerlach, Martin; Holfelder, Ina; Hoenicke, Philipp; Lubeck, Janin; Nutsch, Andreas; Pollakowski, Beatrix; Streeck, Cornelia; Unterumsberger, Rainer; Weser, Jan; Beckhoff, Burkhard

    2014-12-15

    The X-ray spectrometry of the PTB at the BESSY II storage ring with radiation in the range from 78 eV to 10.5 keV is described. After a description of the instrumentation development reference-sample free X-ray fluorescence analysis, the determination of fundamental atomic parameters, X-ray fluorescence analysis under glance-angle incidence, highly-resolving absorption spectrometry, and emission spectrometry are considered. Finally liquid cells and in-situ measurement techniques are described. (HSI)

  14. Method of trivalent chromium concentration determination by atomic spectrometry

    Science.gov (United States)

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

    2006-12-12

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

  15. Improvement of determination for the content of potassium and sodium in food by Flame Atomic ;Emission Spectrometry%火焰原子发射光谱法测定食品中钾和钠含量的方法改进

    Institute of Scientific and Technical Information of China (English)

    林凯; 刘桂华; 张慧敏; 张红宇; 许欣欣; 姜杰

    2015-01-01

    目的对火焰原子发射光谱法测定食品中钾和钠含量的方法进行改进和探讨。方法采用高压密闭消解样品后,用火焰原子发射光谱法测定其中钾和钠的含量,并与原子吸收光谱法进行对比。结果在优化实验条件下,钾和钠的发射光谱法线性范围为0.1~4.0 mg/L,标准曲线线性关系良好,钾、钠的检出限分别为0.2 mg/100g和0.8mg/100g;各种食品基质标准物质的测定值均在证书参考值范围内,RSD<4%,原子发射光谱法与原子吸收光谱法的测定结果无差异。结论该方法准确、简便快速,精密度高,适用于食品中钾和钠含量的测定。%Objective To improve and discuss the flame atomic emission spectrometry method to determine the content of Potassium(K) and Sodium(Na) in food.Method The samples were digested in airtight pressure closed vessel,then were analyzed by flame atomic emission spectrometry.The results obtained by this method were compared with flame atomic absorption spectrometry meanwhile. Results Under the optimized condition, the determine range of K and Na was 0.1~4.0 mg/L,the calibration curve showed good,and the detection limit were 0.2mg/100g and 0.8mg/100g respectively.The determination value of various food matrix material were within the range of certificate value,RSD<4% ,no difference between two methods’ results were found.Conclusion This method is accurate ,simple and rapid, and has high precision,suitable for determinating the content of K and Na in food.

  16. Volatile Organic Compound emissions from soil: using Proton-Transfer-Reaction Time-of-Flight Mass Spectrometry (PTR-TOF-MS) for the real time observation of microbial processes

    Science.gov (United States)

    Veres, P. R.; Behrendt, T.; Klapthor, A.; Meixner, F. X.; Williams, J.

    2014-08-01

    In this study we report on the emissions of volatile organic compounds (VOC) and nitric oxide (NO) from two contrasting soils (equatorial rainforest and arid cotton field) analyzed in a laboratory based dynamic chamber system. The effect of soil moisture and soil temperature on VOC and NO emission was examined in laboratory incubation experiments by measuring as a pre-saturated soil dried out. Our results suggest that real time monitoring of VOC emissions from soil using a proton-transfer-reaction time-of-flight mass spectrometer (PTR-TOF-MS) instrument can be used to improve our understanding of the release mechanisms of trace gases (e.g. NO, N2O) that are involved in the nitrogen cycle. Moreover, we report on the release rate of various VOC species, many of which exhibit a temperature dependent response indicative of biological production, namely a temperature amplification factor (Q10) ∼ 2-3. Contrary to the conventional modeling of NO emissions from soils, that the release of NO from the overall community across the range of soil water content can be modeled as an optimum function, we suggest that VOC measurements indicate there exist multiple distinct contributing microbial guilds releasing NO. These microbial guilds could likely be individually identified with the observed VOC profiles. Using a cotton field soil sample from a Sache oasis (Taklimakan desert, Xinijang, P. R. China), we identify five VOC emission groups with varying degrees of NO co-emission. An equatorial rainforest soil (Suriname) was shown to emit a variety of VOC including acetaldehyde, acetone, DMS, formaldehyde, and isoprene that vary strongly and individually as a function of temperature and soil moisture content. PTR-TOF-MS with high time resolution, sensitivity, and molecular specificity is an ideal tool for the real time analysis of VOC and NO emitting processes in soil systems. These experiments can be used as a template for future experiments to more completely and specifically

  17. Emission Trading

    OpenAIRE

    2009-01-01

    The work concerns Emission Trading Scheme from perspektive of taxes and accounting. I should show problems with emission trading. The work concerns practical example of trading with emission allowance.

  18. A novel method for fast enrichment and monitoring of hexavalent and trivalent chromium at the ppt level with modified silica MCM-41 and its determination by inductively coupled plasma optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    Ganjali Mohammad Reza

    2006-01-01

    Full Text Available Chromium(III at the ng L-1 level was extracted using partially silylated MCM-41 modified by a tetraazamacrocyclic compound (TAMC and determined by inductively coupled plasma optical emision spectrometry (ICP OES. The extraction time and efficiency, pH and flow rate, type and minimum amount of stripping acid, and break- through volume were investigated. The method's enrichment factor and detection limit are 300 and 45.5 pg mL-1, respectively. The maximum capacity of the 10 mg of modified silylated MCM-41 was found to be 400.5?4.7 µg for Cr(III. The method was applied to the determination of Cr(III and Cr(VI in the wastewater of the chromium electroplating industry and in environmental and biological samples (black tea, hot and black pepper.

  19. Ion mobility spectrometry

    CERN Document Server

    Eiceman, GA

    2005-01-01

    Key Developments for Faster, More Precise Detection Capabilities Driven by the demand for the rapid and advanced detection of explosives, chemical and biological warfare agents, and narcotics, ion mobility spectrometry (IMS) undergone significant refinements in technology, computational capabilities, and understanding of the principles of gas phase ion chemistry and mobility. Beginning with a thorough discussion of the fundamental theories and physics of ion mobility, Ion Mobility Spectrometry, Second Edition describes the recent advances in instrumentation and newly

  20. 甲基异丁基甲酮萃取—氢化物发生原子荧光光谱法测定锑锭和氧化锑中汞%Determination of mercury in antimony ingot and antimony oxide by methyl isobutyl ketone extraction-hydride generation atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    陆建平; 谭芳维; 石建荣

    2012-01-01

    After the samples were dissolved in aqua regia/HBr and tartaric acid was added to mask antimony, then mercury in antimony ingot and antimony oxide was extracted into the organic phase with methyl isobutyl ketone (MIBK) and determined by organic phase injection-intermittent flow injection atomic fluorescence spectrometry. Sample dissolution methods and interferences caused by coexisting ions were investigated, and instrument working conditions, extraction conditions, acidity and other factors were optimized. The results showed that under optimal conditions, the mercury content within the range of 0. 02 to 50 μg/L was in good linear relationship, and the detection limit was 0. 013 jxg/L. This method was applied to the actual antimony ingot and antimony oxide sample analysis. It was found that the results were consistent with those obtained by inductive coupled plasma atomic emission spectrometry with relative standard deviations (RSDs, n = 6) of 0. 65%-2. 4% and recoveries of 94 %-99%.%采用王水/HBr溶解样品,酒石酸掩蔽锑,用甲基异丁基甲酮(MIBK)将汞萃取到有机相中,建立了有机相进样—断续流动注射原子荧光光谱法测定锑锭和氧化锑中汞含量的方法.研究了溶样方法和共存离子可能引起的干扰,优化了仪器工作条件、萃取条件、酸度及其他影响因素.结果表明,在最佳条件下,汞含量在0.02~50 μg/L范围内线性关系良好,方法检出限为0.013 μg/L.将方法应用于锑锭和氧化锑实际样品分析,测得结果与电感耦合等离子体原子发射光谱法一致,相对标准偏差(RSD,n=6)在0.65%~2.4%之间,加标回收率为94%~99%.

  1. Fluorescence preselection of bioaerosol for single-particle mass spectrometry

    Science.gov (United States)

    Stowers, M. A.; van Wuijckhuijse, A. L.; Marijnissen, J. C. M.; Kientz, Ch. E.; Ciach, T.

    2006-11-01

    We have designed, constructed, and tested a system that preselects the biological fraction of airborne particles from the overall aerosol. The preselection is based on fluorescence emission excited by a continuous 266 nm laser beam. This beam is one of two cw beams used to measure the aerodynamic particle size of sampled particles. The intention in our system is that single particles, based on size and fluorescence emission, can be selected and further examined for chemical composition by mass spectrometry.

  2. 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.

    Science.gov (United States)

    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 (RSDfilter (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.

  3. Forensic Mass Spectrometry

    Science.gov (United States)

    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.

  4. Velocity-space sensitivity of neutron spectrometry measurements

    DEFF Research Database (Denmark)

    Jacobsen, Asger Schou; Salewski, Mirko; Eriksson, J.;

    2015-01-01

    Neutron emission spectrometry (NES) measures the energies of neutrons produced in fusion reactions. Here we present velocity-space weight functions for NES and neutron yield measurements. Weight functions show the sensitivity as well as the accessible regions in velocity space for a given range...

  5. Fourier transform mass spectrometry.

    Science.gov (United States)

    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.

  6. Emissions Trading

    NARCIS (Netherlands)

    Woerdman, Edwin; Backhaus, Juergen

    2014-01-01

    Emissions trading is a market-based instrument to achieve environmental targets in a cost-effective way by allowing legal entities to buy and sell emission rights. The current international dissemination and intended linking of emissions trading schemes underlines the growing relevance of this

  7. Emissions Trading

    NARCIS (Netherlands)

    Woerdman, Edwin; Backhaus, Juergen

    2014-01-01

    Emissions trading is a market-based instrument to achieve environmental targets in a cost-effective way by allowing legal entities to buy and sell emission rights. The current international dissemination and intended linking of emissions trading schemes underlines the growing relevance of this instr

  8. Determination of Trace Platinum, Palladium and Gold in Geochemical Samples by Emission Spectrometry With Lead Fire Assaying Concentration%铅火试金富集-发射光谱法测定化探样品痕量金、铂和钯

    Institute of Scientific and Technical Information of China (English)

    陈春军; 钟宁

    2014-01-01

    试样用铅火试金富集铂组元素及金,加入1 mg银,在950℃熔融得到含贵金属的铅扣。铅扣与熔渣分离后在900℃灰吹得含铂、钯和金的银合金粒。把合金粒装入电极,以发射光谱法同时测定铂、钯和金的含量。%Platinum group elements and gold in sample were enriched by lead fire assaying, after adding 1 mg silver and melting at 950 ℃, lead button containing precious metals was obtained. Then lead button was separated from slag, silver grains containing platinum, palladium and gold were obtained by soot blowing at 900 ℃. Putting the alloy grain into the electrode, contents of platinum, palladium and gold were simultaneously determined by the emission spectrometry.

  9. Spectrometry and emission tomographic image reconstruction stimulated by neutrons via EM algorithm and Monte Carlo Method; Espectrometria e reconstrucao de imagens tomograficas de emissao estimulada por neutrons via algoritmo EM e metodo de Monte Carlo

    Energy Technology Data Exchange (ETDEWEB)

    Viana, Rodrigo Sartorelo Salemi

    2014-07-01

    The NSECT (Neutron Stimulated Emission Computed Tomography) figures as a new spectrographic technique able to evaluate in vivo the concentration of elements using the inelastic scattering reaction (n,n'). Since its introduction, several improvements have been proposed with the aim of investigating applications for clinical diagnosis and reduction of absorbed dose associated with CT acquisition. In this context, two new diagnostic applications are presented using spectroscopic and tomographic approaches from NSECT. A new methodology has also been proposed to optimize the sinogram sampling that is directly related to the quality of the reconstruction by the irradiation protocol. The studies were developed based on simulations with MCNP5 code. Diagnosis of Renal Cell Carcinoma (RCC) and the detection of breast microcalcifications were evaluated in studies conducted using a human phantom. The obtained results demonstrate the ability of the NSECT technique to detect changes in the composition of the modeled tissues as a function of the development of evaluated pathologies. The proposed method for optimizing sinograms was able to analytically simulate the composition of the irradiated medium allowing the assessment of quality of reconstruction and effective dose in terms of the sampling rate. However, future research must be conducted to quantify the sensitivity of detection according to the selected elements. (author)

  10. Miniaturization and Mass Spectrometry

    NARCIS (Netherlands)

    le Gac, S.; le Gac, Severine; van den Berg, Albert; van den Berg, A.; Unknown, [Unknown

    2009-01-01

    With this book we want to illustrate how two quickly growing fields of instrumentation and technology, both applied to life sciences, mass spectrometry and microfluidics (or microfabrication) naturally came to meet at the end of the last century and how this marriage impacts on several types of appl

  11. Analytical mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    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)

  12. Analytical mass spectrometry. Abstracts

    Energy Technology Data Exchange (ETDEWEB)

    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)

  13. Emission Facilities - Air Emission Plants

    Data.gov (United States)

    NSGIC Education | GIS Inventory — Represents the Primary Facility type Air Emission Plant (AEP) point features. Air Emissions Plant is a DEP primary facility type related to the Air Quality Program....

  14. Emission Facilities - Air Emission Plants

    Data.gov (United States)

    NSGIC GIS Inventory (aka Ramona) — Represents the Primary Facility type Air Emission Plant (AEP) point features. Air Emissions Plant is a DEP primary facility type related to the Air Quality Program....

  15. Emission inventory; Inventaire des emissions

    Energy Technology Data Exchange (ETDEWEB)

    Fontelle, J.P. [CITEPA, Centre Interprofessionnel Technique d`Etudes de la Pollution Atmospherique, 75 - Paris (France)

    1997-12-31

    Statistics on air pollutant (sulfur dioxide, nitrogen oxides and ammonium) emissions, acid equivalent emissions and their evolution since 1990 in the various countries of Europe and the USA, are presented. Emission data from the industrial, agricultural, transportation and power sectors are given, and comparisons are carried out between countries based on Gnp and population, pollution import/export fluxes and compliance to the previous emission reduction objectives

  16. Rapid Determination of Micro Beryllium in Silicate Samples by Emission Spectrometry%发射光谱法快速测定硅酸盐样品中的微量铍

    Institute of Scientific and Technical Information of China (English)

    张鑫; 李源; 柳金良; 刘朝

    2015-01-01

    Determination of micro beryllium in silicate was determinated by a meter grating spectrograph,which improved the working standard,spectrum perturbation and interpretation of emission spectra in the semi-quantitative analysis.The detection limit was 0.25 μg/g,and the precision of the method(RSD)is less than 10%.The results were agreement with the values after determinate of national standard material.External inspection by random sampling 10% of a batch and results basically consistent with chemical analysis,which in accordance with the quality assessment requirements.This method is without chemical pretreatment,the measurement result is reliable,low cost, and meets requirements of quantitative analysis of micro beryllium in silicate.%通过在发射光谱半定量分析的基础上改进工作标准配制和摄、译谱方法,利用一米平面光栅摄谱仪测定硅酸盐样品中的微量铍。方法检出限为0.25μg/g,方法精密度(RSD)小于10%;测定国家标准物质,结果与标准值吻合;抽取某批次10%的未知样品外检进行验证,测定结果与化学分析基本一致,符合质量评估要求。该方法无须化学前处理、测量结果可靠,成本低廉,完全符合定量分析硅酸盐样品中微量铍的要求。

  17. Daily and hourly sourcing of metallic and mineral dust in urban air contaminated by traffic and coal-burning emissions

    NARCIS (Netherlands)

    Moreno, T.; Karanasiou, A.; Amato, F.; Lucarelli, F.; Nava, S.; Calzolai, G.; Chiari, M.; Coz, E.; Artíñano, B.; Lumbreras, J.; Borge, R.; Boldo, E.; Linares, C.; Alastuey, A.; Querol, X.; Gibbons, W.

    2013-01-01

    A multi-analytical approach to chemical analysis of inhalable urban atmospheric particulate matter (PM), integrating particle induced X-ray emission, inductively coupled plasma mass spectrometry/atomic emission spectroscopy, chromatography and thermal-optical transmission methods, allows comparison

  18. Hydrogen Exchange Mass Spectrometry.

    Science.gov (United States)

    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.

  19. Mass spectrometry with accelerators.

    Science.gov (United States)

    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

  20. Análise de suspensões de argilas por espectrometria de emissão óptica com plasma induzido com configuração axial Clay slurries analysis using inductively coupled plasma optical emission spectrometry with axial view configuration

    Directory of Open Access Journals (Sweden)

    Cíntia S. Silva

    2002-12-01

    Full Text Available The goal of this study was to evaluate the feasibility of direct introduction of clay slurries in an inductively coupled plasma optical emission spectrometer with axial view configuration. Calibration was performed using a certified reference material with a mean particle size of 13 µm (IPT-42 and the analytical curve was applied for quantification of two others reference materials (IPT-28 and IPT-32 and four samples. It was demonstrated that the analytical curve thus obtained was not completely suitable for IPT-28 and samples due to different mineralogical phases determined by X-ray diffraction. After considering this effect, it was possible for most elements to obtain results in agreement with certified values or with values obtained by a conventional technique at a 95% confidence level. It was demonstrated that the ICP-OES with axial view configuration did not present any incompatibility with the direct introduction of a complex inorganic suspension.

  1. "Magic" Ionization Mass Spectrometry

    Science.gov (United States)

    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.

  2. International Mass Spectrometry Society (IMSS).

    Science.gov (United States)

    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.

  3. 火焰原子吸收光谱法测定红土镍矿中的铅%Determination of Lead in Laterice Nickel Ore by Flame Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    王慧; 刘烽; 许玉宇; 俞璐; 吴骋; 王国新

    2012-01-01

    Laterice nickel ore was digested with mixed acids of HC1 and HNO3 mixed acids. HF was used to remove silicon, and residual HF was volatilized by using HClO4. Lead content in the HNO3 solution was determined by Flame Atomic Absorption Spectrometry. The different acid digestion systems and interferences of coexistent elements are presented in this paper. The results showed that the samples were completely dissolved by HC1-HNO3-HF-HClO4 mixed acids. The Pb level content was not influenced by HNO3 when its acidity was below 5% ( V/V). The coexistent elements of Fe (1000μg/mL), Ni (60 μg/mL), Cu (10μg/mL), Ca (50 μg/mL), Mn (20 μg/mL), Cr (10 μg/mL) , Co (10 μg/mL) and Zn (10 μg/mL) did not interfere with the Pb result (1μg/mL). The detection limit was 0.044 μg/mL at selected working conditions. The accuracy of the Pb content was verified by adding a standard solution to the laterice nickel ore. The recoveries ranged from 97% to 106% , and the results of this method were in agreement with inductively coupled plasma atomic emission spectrometry. The proposed method is a useful technique with good repeatability and accuracy.%样品用盐酸-硝酸溶解,氢氟酸挥发硅,高氯酸冒烟除去氢氟酸,然后以稀硝酸溶解可溶性盐类,火焰原子吸收光谱法测定红土镍矿中铅的含量.考察了不同的酸对样品的溶解效果,对介质酸度和共存元素干扰情况进行了实验.结果表明:盐酸-硝酸-氢氟酸-高氯酸可以将样品消解完全;5%以内的硝酸不影响铅的测定;100mL体积内,100mg铁、6mg镍、1mg铜、5mg钙、2mg锰、1mg铬、1mg钴、1mg锌等共存元素对0.1mg铅的测定不产生干扰.在选定的仪器工作参数下,Pb的检出限为0.044μg/mL,加标回收率为97%~106%,测定值与电感耦合等离子体发射光谱法结果一致.方法重复性好、准确度高,可满足准确测定红土镍矿中铅含量的分析要求.

  4. Analysis of trace elements in food fortificants with inductively coupled plasma optical emission spectrometry%电感耦合等离子体原子发射光谱分析食品营养强化剂中的痕量元素

    Institute of Scientific and Technical Information of China (English)

    段建坤; 曾爱民; 杨永; 朱有涛; 唐立平; 沈丽

    2011-01-01

    A simple and fast method was developed for the determination of Ca, K, Na, Fe, Zn, Mn, Pb and As in food fortificants by inductively coupled plasma optical emission spectrometry (ICP-OES). The effect of the sample matrix was studied and the results showed that there was little matrix effect existing if the concentration of the organic food fortificants and inorganic metal ion in the sample solution were no more than 20 and 2 g/L, respectively. Three methods for sample pretreatment were investigated and compared. External standard and matrix matching methods were used for quantification of the analytes in the samples. It is found than the former showed better analytical performances. The proposed method was applied for the analysis of six food fortificants with satisfied recoveries.%以电感耦合等离子体发射光谱(ICP—OES)作为检测手段分析了营养强化剂中的钙、钾、钠、铁、锌、锰、铅和砷等元素。研究了样品基体对于分析过程的影响,实验结果表明,有机强化剂浓度不超过20g/L,无机强化剂中的无机金属元素含量不超过2g/L时,可以认为基体没有影响。考察了不同的样品处理方式的优缺点。比较了校正曲线法(外标法)和基体匹配法两种定量分析方法,发现前者的分析性能更为优越。分析了6种强化剂中的钙、钾、钠、铁、锌、锰、铅和砷,加标回收结果满意。

  5. Simultaneous Determination of Five Alcohols in E-cigarette Emissions by Gas Chromatography-Mass Spectrometry%GC/MS法同时测定电子烟烟气释放物中的5种醇类化合物

    Institute of Scientific and Technical Information of China (English)

    段沅杏; 吴亿勤; 杨威; 杨继; 韩敬美; 田永峰; 赵伟; 杨柳; 陈永宽

    2015-01-01

    In order to accurately determine the contents of alcohols in e-cigarette emissions, a gas chromatography-mass spectrometry (GC/MS) method was developed for simultaneously determining 1, 2-propylene glycol, 1,3-butanediol, glycerol, diethylene glycol and triethylene glycol, wherein 1, 4-butanediol was used as an internal standard. Sixteen samples of e-cigarette were tested by the developed method. The results showed that: 1) The limit of detection and limit of quantitation were 0.08-0.32 and 0.27-1.07 μg/puff, respectively; the recoveries were 90.0%-99.5% with the relative standard deviations (RSD) ranged from 1.20% to 4.93%. 2) 1,2-Propylene glycol and glycerin were detectable, while diethylene glycol and triethylene glycol were undetectable in all samples; and 1,3-butanediol was detectable in four samples. 3) This method was suitable for the qualitative and quantitative determination of 1,2-propylene glycol, 1,3-butanediol, glycerol, diethylene glycol, triethylene glycol in e-cigarette emissions.%为了准确测定电子烟烟气释放物中醇类化合物的量,以1,4-丁二醇为内标建立了同时检测电子烟烟气释放物中1,2-丙二醇、1,3-丁二醇、丙三醇、二甘醇和三甘醇的气相色谱/质谱(GC/MS)方法,采用该法测定了16种电子烟样品.结果表明:①该法的检出限和定量限范围在0.08~0.32 μg/口和0.27~1.07 μg/口之间;回收率在90.0%~99.5%之间,相对标准偏差(RSD)为1.20%~4.93%.②所测样品中均检出1,2-丙二醇、丙三醇,均未检出二甘醇和三甘醇;4个样品中检测出1,3-丁二醇.该法灵敏度高、定性准确,适合电子烟样品烟气释放物中1,2-丙二醇、1,3-丁二醇、丙三醇、二甘醇和三甘醇的定性定量分析.

  6. Determination of Beryllium in Soils by Graphite Furnace Atomic Absorption Spectrometry with Palladium Chloride as a Matrix Modifier%氯化钯作基体改进剂石墨炉原子吸收光谱法测定土壤中的铍

    Institute of Scientific and Technical Information of China (English)

    姚朝英; 任兰

    2012-01-01

    Beryllium is a harmful metal element and there is no national standard method for its determination in soils. A method system was established for the determination of Beryllium in soils by Graphite Furnace Atomic Absorption Spectrometry ( GFAAS) with hydrochloric acid-nitric acid-hydrofluoric as microwave digestion. The sensitizing effects of palladium, aluminum nitrate, magnesium nitrate and calcium salt were investigated. The results showed that atomic shape was sharp, background absorption was small and sensitivity was improved with palladium chloride as the matrix modifier when the ashing temperature and atomization temperature were increased to llOOt and 2650^ , respectively. The other 3 modifiers improved sensitivity but background absorptions were larger. The conditions of experiment were optimized and the coexisting elements Fe, Mg, K, Na, Ca, Ti, Cu, Ba, Mn, Zn, Pb and Sr had no interference. The results showed that good linearity ranged from 0 (xg/L to 4. 00 H-g/L, detection limit was 0.01 |JLg/g ( sampling quality was 0. 2000 g and constant volume was 50 mL) , RSD of standard samples were from 3.5% to 6. 7% , and spiked recoveries of the actual soil sample were from 84.0% to 113.0%. The result of national standard material was in the range of certified values. Compared with extraction spectrophotometric method, Inductively Coupled Plasma-Atomic Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry, this method is simple and inexpensive.%铍是一种对人体有害的金属元素,土壤中铍的测定目前尚无国家标准方法.本文采用盐酸-硝酸-氢氟酸体系微波消解、石墨炉原子吸收光谱法测定土壤样品中的铍,实验了钯、硝酸铝、硝酸镁、钙盐的增敏效果.结果表明,以氯化钯为基体改进剂,灰化温度和原子化温度分别提高到1100℃和2650℃,原子化峰形尖锐,背景吸收很小,提高了测定灵敏度;其他三种基体改进剂虽然也能提高测定灵敏度,但

  7. Mass Spectrometry of Halopyrazolium Salts

    DEFF Research Database (Denmark)

    Larsen, Elfinn; Egsgaard, Helge; Pande, U. C.;

    1983-01-01

    Eleven halogen substituted 1-methyl-2-phenylpyrazolium bromides or chlorides were investigated by field desorption, field ionization, and electron impact mass spectrometry. Dealkylation was found to be the predominant thermal decomposition. An exchange between covalent and ionic halogen prior...

  8. Accelerator mass spectrometry.

    Science.gov (United States)

    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.

  9. Methods for Neutron Spectrometry

    Science.gov (United States)

    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)

  10. Biomedical accelerator mass spectrometry

    Science.gov (United States)

    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.

  11. Effect of a Chinese herbal prescription on femur calcium deposition in rats under simulated weightlessness: by using 41 Ca tracing-accelerator mass spectrometry analysis%中药干预模拟失重大鼠股骨外源钙沉积研究

    Institute of Scientific and Technical Information of China (English)

    胡素敏; 周鹏; 姜山; 何明; 傅骞; 杨佳佳; 高学敏

    2009-01-01

    To study the effect of a Chinese herbal prescription on external calcium deposition to weight-bearing bone in simula-ted weightlessness rats. Method:Twenty-one male Wistar rats were divided into 3 groups: control group, tail suspension group, tail suspension with Chinese medicine group which takes a Chinese herbal prescription extract ( containing Radix Rehmanniae Preparata,Radix Acanthopanacis Bidentatae, Radix Astragali, Radix Angelicae Sinensis, Concha Ostreae prepared by acetic acid) by intragastric administration. After 1 week adaption, there start off 3 weeks simulated weightlessness by tail suspension. At the eleventh day of simu-lated weightlessness , every rat was given one equal dose of ~(41)Ca tracer by intragnstric administration. Right femurs were separated as experiment over, and the ratio of ~(41)Ca to ~(40) Ca ( ~(41) Ca / ~(40) Ca) was measured by accelerator mass spectrometry ( AMS ) , while total femur calcium was measured by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Femur ~(41) Ca deposition amount (DA) and femur ~(41) Ca deposition ratio (DR) were calculated. Result:The results showed that compared with control group, ~(41) Ca / ~(40) Ca de-creased significantly (P <0.001 ) in tail suspension group, while in tail suspension with Chinese medicine group, it significantly in-creased ( P < 0.05 ). DA and DR were both decreased significantly ( P < 0.001 ) in tail suspension group, but no significant change in tail suspension with Chinese medicine group as compared with control group. Compared with tail suspension group, DA and DR in-creased significantly (P < 0. 001 ) in tail suspension with Chinese medicine group. Conclusion:Simulated weightlessness by tail sus-pension can cause decreased deposition of external calcium to weight-bearing bone, and the Chinese herbal prescription in this trial is effective to prevent the decrease. Moreover, multiple mechanisms may contribute to weightlessness induced osteoporosis, besides

  12. Determination of Nb and Ta in Nb-Ta Ore by Inductively Coupled Plasma-Optical Emission Spectrometry with a Combined Microwave Digestion Hydrofluoric Acid-resistant System%微波消解-耐氢氟酸系统电感耦合等离子体发射光谱法测定铌钽矿中的铌和钽

    Institute of Scientific and Technical Information of China (English)

    马生凤; 温宏利; 李冰; 王蕾; 朱云

    2016-01-01

    Niobium and tantalum in hydrofluoric acid can form a stable solution,and thus the Nb and Ta content of Nb-Ta ore can be determined accurately by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) with a hydrofluoric acid resistant system.The determination method described in this paper for Nb and Ta in Nb-Ta ore,uses the microwave digestion mode of modular small tank and multiple digestion tank assembly (70 tank /group),and hydrofluoric acid resistant system of ICP-OES.This method shortens the dissolution time from 48 h to 1 h.By using a hydrofluoric acid medium the hydrolysis of high-level Nb and Ta in low acid concentration media is avoided.The detection limits of this method are 5.58 μg/g for Nb and 5.87 μg/g for Ta.The result of Nb-Ta concentrate with 19% Nb2 O5 and 27% Ta2 O5 is consistent with that acquired by the alkali fusion method and can be used to determine both high-grade and low-grade Nb-Ta ore with 42 μg/g -19% of Nb2 O5 and 86 μg/g -27%of Ta2 O5 .The main advantage of this method is to accurately determine Nb and Ta in high-grade Nb-Ta ore.%铌、钽在氢氟酸介质中能够形成稳定的溶液,使用耐氢氟酸进样系统的电感耦合等离子体发射光谱(ICP -OES)有利于提高分析的准确性。本文采用模块化的小罐型、多罐体组合(70罐/组)酸溶罐体的微波消解溶样模式,结合 ICP -OES 仪器的耐氢氟酸进样系统,建立了测定铌钽矿中铌、钽的分析方法。本方法加快了酸溶的溶样速度,溶样时间从原来的48 h 减少至1 h,且在氢氟酸介质中测定避免了高含量铌、钽在低酸度介质中容易水解的影响。方法检出限为铌5.58μg/g,钽5.87μg/g。本方法应用于测定铌钽精矿(19%Nb2 O5,27%Ta2 O5)的分析结果与碱熔方法一致,能够测定 Nb2 O5含量在42μg/g ~19%和 Ta2 O5含量在86μg/g ~27%高低品位的铌钽矿,尤其对于铌、钽在百分含量以上的铌钽矿具有优势。

  13. Determination of Metal Ions in Environmental Samples by Matrix-Assisted Microwave Induced Plasma Surface Sampling Atomic Emission Spectrometry%基体辅助微波诱导等离子体表面进样原子发射光谱检测环境样品

    Institute of Scientific and Technical Information of China (English)

    袁欣; 段忆翔

    2015-01-01

    采用基体辅助等离子体表面进样原子发射光谱技术对环境样品中的13种金属元素( Ag, Au, Ba, Cd, Cr, Cu, Eu, La, Mn, Ni, Pb, Sr, Y)进行检测。实验采用滤纸作为样品基体,样品直接滴加在滤纸上。将等离子体射流尾焰烧蚀滤纸表面,滤纸受热燃烧并释放出燃烧热,样品在等离子体辐射热和滤纸燃烧热的共同作用下原子化并激发,即可得到样品的特征光谱。液/固态样品均采用表面进样的方式实现样品引入,无需复杂的流动进样系统,并简化了繁琐的样品处理过程。本方法具有分析速度快(≤15 s)、用样量少(微升/微克级)、装置简洁、操作简单等优点,可实现对大量环境样品的现场高通量分析。在实验优化条件下,样品体积为1μL 时,本方法对以上13种元素的检出限为1.0~88 ng/mL,相对标准偏差为2.3%~6.8%(n=10)。该技术成功用于水样、土壤、海底沉积物等环境样品中金属元素的分析,结果均与理论值吻合。%A novel method for the determination of metallic elements in environmental samples was developed based on the matrix-assisted plasma surface sampling atomic emission spectrometry ( AES system) . A piece of filter paper was used as sample substrate. By direct interaction of the plasma tail plume with the filter paper surface, the filter paper absorbed energy from the plasma source and released combustion heating to the analytes originally present on its surface, thus to promote the atomization and excitation process. Surface sampling was performed in both cases of liquid and solid state analytes. Therefore, no flow injection system was required and sample pretreatment process was simplified. The proposed method provides several advantages, including fast analysis speed ( about 240 samples/h ) , little sample consumption (μL or μg level) , simplicity in instrument design, and also ease of system operation. These advantages made it attractive as a

  14. Monoterpene emissions from boreal tree species: Determination of de novo and pool emissions

    Science.gov (United States)

    Ghirardo, Andrea; Koch, Kristine; Taipale, Risto; Zimmer, Ina; Schnitzler, Joerg-Peter; Rinne, Janne

    2010-05-01

    Boreal forests emit a large amount of monoterpenes into the atmosphere. Traditionally these emissions are assumed to originate as evaporation from large storage pools. Thus their diurnal cycle would depend mostly on temperature. However, there is indication that a significant part of the monoterpene emission would originate directly from de novo synthesis. By applying 13CO2 fumigation and analyzing the isotope fractions with proton transfer reaction mass spectrometry (PTR-MS) and classical GC-MS we studied the origin of monoterpene emissions from some major Eurasian boreal and alpine tree species. We determined the fractions originating from de novo biosynthesis and from large internal monoterpene storages for three coniferous tree species with specialized monoterpene storage structures and one dicotyledon species without such structures. The emission from dicotyledon species Betula pendula originated solely from the de novo synthesis. The origin of the emissions from coniferous species was mixed with varying fraction originating from de novo synthesis (Pinus sylvestris 58 %, Picea abies 33.5 %, Larix decidua 9.8 %) and the rest from large internal monoterpene storage pools. We have also measured the ecosystem scale monoterpene emission fluxes from a boreal Pinus sylvestris forest by disjunct eddy covariance technique. Application of the observed fraction of emission originating from de novo synthesis and large storage pools in a hybrid emission algorithm resulted in a better description of ecosystem scale monoterpene emissions, as compared to the measured fluxes.

  15. Symposium on accelerator mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    None

    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.

  16. Mass spectrometry. [in organic chemistry

    Science.gov (United States)

    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.

  17. Functional genomics by mass spectrometry

    DEFF Research Database (Denmark)

    Andersen, Jens S.; Mann, M

    2000-01-01

    Systematic analysis of the function of genes can take place at the oligonucleotide or protein level. The latter has the advantage of being closest to function, since it is proteins that perform most of the reactions necessary for the cell. For most protein based ('proteomic') approaches to gene...... function, mass spectrometry is the method of choice. Mass spectrometry can now identify proteins with very high sensitivity and medium to high throughput. New instrumentation for the analysis of the proteome has been developed including a MALDI hybrid quadrupole time of flight instrument which combines...... numbers of intact proteins by mass spectrometry directly. Examples from this laboratory illustrate biological problem solving by modern mass spectrometric techniques. These include the analysis of the structure and function of the nucleolus and the analysis of signaling complexes....

  18. Speciation of organotin in sediments by multicapillary gas chromatography with atomic emission detection after microwave-assisted leaching and solvent extraction-derivatization

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez Pereiro, I.; Wasik, A.; Lobinski, R. [CNRS, Pau (France)

    1999-03-01

    Microwave-assisted leaching of organotin compounds from sediment samples followed by the simultaneous extraction-derivatization of the extracted species was revisited with the goal to compare the existing procedures, improve their recoveries and extend them to phenyltin compounds. The stability of butyl- and phenyltin compounds under microwave field, real recoveries of the whole analytical procedure, effect of the extraction solvent, and the necessity for an internal standard were evaluated using two candidate reference sediments. The combination of the optimized sample preparation procedure with multicapillary chromatography resulted in a rapid (2 min leaching + 5 min extraction-derivatization + 3 min chromatographic separation) and efficient analytical procedure for speciation analysis of organotin compounds in sediment samples. The detection limit achieved with a microwave-induced plasma atomic emission detector was 2 ng g{sup -1}. (orig.) With 4 figs., 3 tabs., 24 refs.

  19. Speciation of mercury in human whole blood by capillary gas chromatography with a microwave-induced plasma emission detector system following complexometric extraction and butylation.

    Science.gov (United States)

    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.

  20. Mass spectrometry for biomarker development

    Energy Technology Data Exchange (ETDEWEB)

    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.

  1. Cluster secondary ion mass spectrometry microscope mode mass spectrometry imaging

    NARCIS (Netherlands)

    Kiss, A.; Smith, D.F.; Jungmann, JH; Heeren, R.M.A.

    2013-01-01

    RATIONALE: Microscope mode imaging for secondary ion mass spectrometry is a technique with the promise of simultaneous high spatial resolution and high-speed imaging of biomolecules from complex surfaces. Technological developments such as new position-sensitive detectors, in combination with

  2. Mass Spectrometry Instrumentation in Proteomics

    DEFF Research Database (Denmark)

    Sprenger, Richard Remko; Roepstorff, Peter

    2012-01-01

    Mass spectrometry has evolved into a crucial technology for the field of proteomics, enabling the comprehensive study of proteins in biological systems. Innovative developments have yielded flexible and versatile mass spectrometric tools, including quadrupole time-of-flight, linear ion trap...

  3. 火焰原子吸收光谱法测定尾气净化金属载体催化剂中铂钯铑%Determination of platinum, palladium, rhodium in metal carrier catalyst for exhaust gas purification by flame atomic absorption spectrometry

    Institute of Scientific and Technical Information of China (English)

    施意华; 王晟; 杨仲平; 靳晓珠; 胡圣虹; 邓水平

    2012-01-01

    the determination of actual samples, and the results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry. The relative standard deviations(RSD, n = 11) for palladium, platinum and rhodium were 3. 0% , 1.9% and 4.2%, respectively.

  4. Determination of As in tree-rings of poplar (Populus alba L.) by U-shaped DC arc.

    Science.gov (United States)

    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.

  5. Gamma-emissions of some meteorites and terrestrial rocks. Evaluation of lunar soil radioactivity; Emissions gamma de quelques meteorites et roches terrestres. Evaluation de la radioactivite du sol lunaire

    Energy Technology Data Exchange (ETDEWEB)

    Nordemann, D. [Commissariat a l' Energie Atomique, Centre d' Etudes Nucleaires de Saclay, 91 - Gif-sur-Yvette (France)

    1966-07-01

    The gamma-emissions of some terrestrial rocks and of the following meteorites: Bogou, Eagle-Station, Granes, and Dosso were studied by quantitative low background gamma spectrometry. These measurements and their interpretation lead to the evaluation of the possible gamma-emissions of several models of lunar soils. (author) [French] Les emissions gamma des meteorites Bogou, Eagle-Station, Granes et Dosso et de quelques roches terrestres ont ete etudiees par spectrometrie gamma quantitative a faible mouvement propre. Ces mesures et leur interpretation permettent d'evaluer les principales contributions des emissions gamma du sol lunaire pour des modeles de compositions possibles variees. (auteur)

  6. Plutonium ion emission from carburized rhenium mass spectrometer filaments

    Energy Technology Data Exchange (ETDEWEB)

    Kelley, J.M.; Robertson, D.M.

    1985-01-01

    Physicochemical processes important to the application of thermal emission mass spectrometry were identified and clarified. Effects of filament carbon concentration and temperature on plutonium ion emissions from a carburized rhenium filament were determined. Filament carbon concentration profoundly affected the appearance and duration of an ion signal. A useful ion signal was produced only when the carbon saturation temperature of the filament was exceeded, at which point first-order kinetics were either achieved or closely approached. This paper explains observed ion emission behavior in terms of pausible carbothermic reduction reactions and carbon diffusion processes that direct the course of those reactions. 31 references, 5 figures.

  7. A mass spectrometry primer for mass spectrometry imaging.

    Science.gov (United States)

    Rubakhin, Stanislav S; Sweedler, Jonathan V

    2010-01-01

    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.

  8. 活性炭富集电感耦合等离子体原子发射光谱测定铋系超导粉中痕量铁%Enrichment of Trace Iron with Activated Carbon in Bi-Based Superconductor Powder and Determination by Inductively Coupled Plasma Atomic Emission Spectroscopy

    Institute of Scientific and Technical Information of China (English)

    黄文杰; 李建强; 范慧俐; 范丽新; 包蕊; 张霞; 王杰; 陆青

    2012-01-01

    建立了电感耦合等离子体原子发射光谱(ICP-AES)测定超导粉中痕量铁的新方法.优化了仪器工作参数,对痕量铁测定时的基体干扰及消除干扰的方法进行了系统研究,结果表明:大量存在的基体元素产生一定基体效应,并使重现性变差,且由于铁含量甚微,仪器灵敏度不能满足测定的要求,需采用分离富集方法以提高测定结果的准确度和精密度.以三乙醇胺掩蔽基体元素铋和铜,在适宜的酸度条件下,铁与邻二氮菲生成配合物,以活性炭定量吸附,用1∶1硝酸解吸,并对分离富集条件进行了优化.对模拟标准样品进行测定,分析结果与理论值一致,相对标准偏差为2.4%,方法检出限为0.033μg·g-1.该方法已用于超导前驱粉样品中痕量铁的分析,结果令人满意,并进行了回收实验,回收率为95.6%~98.0%.%A new method for determination of trace iron in superconductor powder by ICP-AES was proposed. The instrument parameters were optimized, and the matrix effects as well as the method of eliminating interferences were also studied systemical-ly. The results showed that matrix interference was serious when the amount of matrix increased, and the repeatability was poor, so it was necessary that separation and preconcentration were used to improve the accuracy and precision. In the experiment , complex was formed with Fe and phenanthroline after the matrix elements Bi and Cu were masked by triethanolamine in an appropriate acidity condition. Then the complex was quantitatively adsorbed by activated carbon, and desorbed by 1 : 1 HNO3.The enrichment conditions were investigated in detail. Under the optimal condition, an artificial sample was analysed, and the result was identical with reference values, with the RSD and detection limit being 2. 42% and 0. 033μg ? G-1, respectively. The method was applied for the determination of trace iron in Bi-based superconductor powder samples with satisfactory results, in which the recoveries experiment was performed with the recovery coefficient falling in the range of 95. 6% to 98. 0%.

  9. Determination of Trace Nickel in Bi-Based Superconductor Powder by Inductively Coupled Plasma Atomic Emission Spectroscopy after Separation with Anion Exchange Resin and Extraction with Methylbenzene%阴离子交换树脂分离甲苯萃取ICP-AES测定铋系超导粉中的痕量镍

    Institute of Scientific and Technical Information of China (English)

    范丽新; 李建强; 范慧俐; 孙建伶; 张霞; 包蕊; 陆青; 王杰

    2011-01-01

    A new method for the determination of trace nickel in superconductor powder by ICP-AES was proposed. The instrument parameters were optimized) and the matrix effects as well as the method of eliminating interferences were also studied sys-temically. The results showed that matrix interference in the superconductor powder was serious when the amount of matrix increased, and the repeatability as well as the accuracy was poor, so it was necessary to used separation and preconcentration to improve the accuracy and precision. In this experiment, Ni-diacetyl dioxime complexes were enriched by toluene extraction in alkaline condition after eliminating the interference of major element Bi and partial Pb, Sr, Ca and Cu by eluting with anion exchange resin, then the Ni-complexes were back extracted by diluted hydrochloric acid. The enrichment conditions were investigated in detail and the recovery rate of Ni was higher than 95%. Under the optimal condition, an artificial sample was analysed, the result showed that the found values were identical with reference values, and the RSD and detection limit were 1. 9% and 0.19 μg ? g-1, respectively. The method has been applied to the determination of trace nickel in Bi-based superconductor powder samples with satisfactory results.%建立了ICP-AES测定超导粉中痕量镍的新方法.优化了仪器工作参数,对超导前驱粉中痕量镍测定时的基体干扰及干扰消除方法进行了系统研究,结果表明:大量存在的基体元素产生严重基体效应,导致测定重现性及准确度变差,实验采用分离富集方法以提高测定结果的准确度和精密度.实验中首先用阴离子交换树脂,除去Bi3+及部分pb2+,Sr2+,Ca2+,Cu2十等基体元素;在碱性条件下再通过甲苯萃取镍与丁二酮肟的络合物、稀盐酸反萃取富集镍;对分离富集条件进行了优化.对模拟标准样品进行测定,分析结果与理论值一致,相对标准偏差为1.9%,方法检出限为0.19 μg·g-1.该方法已用于超导前驱粉样品中痕量镍的分析,结果令人满意.

  10. Determination of As, Mo, V, W in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Ferri, T.; Sangiorgio, P.; Valentini, M. [Rome Univ. La Sapienza, Rome (Italy). Dipt. di Chmica; Morabito, R. [ENEA Centro Ricerche Casaccia, Rome (Italy). Dipt. Ambiente

    1999-10-01

    The paper describes the combined use of a preconcentration method using resin and ICP-AES (inductively coupled plasma atomic emission spectrometry) for determining As, Mo, V and W simultaneously in polluted waters and has been applied to five geological reference samples kindly supplied by USGS (united States Geological Survey). The method, whose reliability has been checked on standard reference materials by NIST (National Institute of Standards and Technology), is easy to apply and also characterized by good precision. [Italian] Il lavoro descrive l'uso combinato di una resina chelante come mezzo di preconcentrazione e l'ICP-AES (inductively coupled plasma atomic emission spectrometry) come mezzo di quantizzazione per determinare simultaneamente As, Mo, V, W nelle acque. Il metodo, che e' stato provato su materiale certificato dal NIST (National Institute of Standards and Technology), si e' dimostrato di facile impiego e caratterizzato da buona precisione.

  11. Detection of negative ions in glow discharge mass spectrometry for analysis of solid specimens

    DEFF Research Database (Denmark)

    Canulescu, Stela; Molchan, Igor S.; Tauziede, C.

    2010-01-01

    A new method is presented for elemental and molecular analysis of halogen-containing samples by glow discharge time-of-flight mass spectrometry, consisting of detection of negative ions from a pulsed RF glow discharge in argon. Analyte signals are mainly extracted from the afterglow regime...... be used to study the distribution of a tantalum fluoride layer within the anodized tantala layer. Further, comparison is made with data obtained using glow-discharge optical emission spectroscopy, where elemental fluorine can only be detected using a neon plasma. The ionization mechanisms responsible...... for the formation of negative ions in glow discharge time-of-flight mass spectrometry are briefly discussed....

  12. Emission Inventory for Fugitive Emissions in Denmark

    DEFF Research Database (Denmark)

    Plejdrup, Marlene Schmidt; Nielsen, Ole-Kenneth; Nielsen, Malene

    This report presents the methodology and data used in the Danish inventory of fugitive emissions from fuels for the years until 2007. The inventory of fugitive emissions includes CO2, CH4, N2O, NOx, CO, NMVOC, SO2, dioxin, PAH and particulate matter. In 2007 the total Danish emission of greenhouse...

  13. Instrumentation for mass spectrometry: 1997

    Energy Technology Data Exchange (ETDEWEB)

    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.

  14. ROCKS & MINERALS DETERMINATION AND ANALYSIS

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    <正>20101621 Chen Heping (Nanyang Geology Testing & Research Center of Henan Province, Nanyang 473000, China); Sha Yanmei Simultaneous Determination of Major and Minor Elements in Carbonates by Inductively Coupled Plasma-Atomic Emission Spectrometry with Multi-direction Viewing Mode (Rock and Mineral Analysis, ISSN0254-5357, CN11-2131/TD, 28(4), 2009, p.367-369, 5 tables, 10 refs.)

  15. Urban gamma spectrometry. Report 2

    Energy Technology Data Exchange (ETDEWEB)

    Aage, H.K. (Technical Univ. of Denmark, Kgs. Lyngby (Denmark)); Kuukankorpi, S.; Moring, M.; Smolander, P.; Toivonen, H. (Radiation and Nuclear Safety Authority, Helsinki (Finland))

    2009-06-15

    Urban gamma spectrometry has been given only minor attention with the focus being on rural gamma spectrometry. However, in recent years the Nordic emergency management authorities have turned focus towards border control and lost or stolen sources. Gamma spectra measured in urban areas are characterized by a wide variety of spectrum shapes and very fast changes in environmental background. In 2004 a Danish CGS (Carborne Gamma Spectrometry) survey took place in Copenhagen. It was found that gamma spectrometry in urban areas is far more complicated to interpret than had previously been thought and a new method 'Fitting with Spectral Components', FSC, based on NASVD, was tested with some success. In Finland, a database 'LINSSI' has been developed for spectral data management. In CGS search mode a 'peak hypothesis test' is applied to the measured spectra. This system was tested during the Helsinki 2005 Athletics World Championship and it provides fast and reliable automated alarms for intermediate and high level signals. In Sweden mobile detector systems are used for border controls and problems are encountered when making measurement in harbour, container areas. The methods for handling data and for interpretation of urban gamma spectrometry measurements were compared and tested on the same data sets from Copenhagen and Helsinki. Software tools were developed for converting data between the Finnish LINSSI database and the binary file formats used in Denmark and Sweden. The Processing methods used at DTU and STUK have different goals. The ASSS and FSC methods are designed to optimize the overall detection capability of the system, while sacrificing speed, usability and to a certain level robustness. These methods cannot always be used for real time analysis. The Peak Significance method is designed to give robust alarms in real time, while sacrificing some of the detection capability. Thus these methods are not interchangeable, but rather

  16. X-Ray fluorescence analysis of trace elements in fruit juice

    Science.gov (United States)

    Bao, Sheng-Xiang; Wang, Zhi-Hong; Liu, Jing-Song

    1999-12-01

    X-Ray fluorescence spectrometry is applied to the determination of trace elements in fruit juice characterized by a high content of sugar and other soluble solid substances. Samples are prepared by evaporation, carbonization and pressing into discs. The synthesis of standards is described in detail. All element concentrations are directly estimated from linear calibration curves obtained without any matrix correction. The results of the analysis are in good agreement with those given by inductively coupled plasma-atomic emission spectrometry and atomic absorption spectrometry techniques.

  17. Recent progress in the determination of gallium, indium, and thallium

    Institute of Scientific and Technical Information of China (English)

    GAO Jinzhang

    2005-01-01

    This mini-review covers the literatures of the determination of gallium, indium, and thallium by instrumental analysis with computer-assisted searching over the period of 1994 to 2003. Some papers appearing in the early of 2004 are also included. Because the rapid progress in the instrument has been made, these new papers are prioritized in selection in the similar papers. The contents are considered to be separation and preconcentration, spectrophotometry, spectrofluorimetry, electroanalyses, atomic absorption spectrometry, inductively coupled plasma-atomic emission spectrometry, inductively coupled plasma-mass spectrometry and so forth.

  18. Mass Spectrometry in Polymer Chemistry

    CERN Document Server

    Barner-Kowollik, Christopher; Falkenhagen, Jana; Weidner, Steffen

    2011-01-01

    Combining an up-to-date insight into mass-spectrometric polymer analysis beyond MALDI with application details of the instrumentation, this is a balanced and thorough presentation of the most important and widely used mass-spectrometric methods.Written by the world's most proficient experts in the field, the book focuses on the latest developments, covering such technologies and applications as ionization protocols, tandem and liquid chromatography mass spectrometry, gas-phase ion-separation techniques and automated data processing. Chapters on sample preparation, polymer degradation and the u

  19. Applied gamma-ray spectrometry

    CERN Document Server

    Dams, R; Crouthamel, Carl E

    1970-01-01

    Applied Gamma-Ray Spectrometry covers real life application of the gamma-ray and the devices used in their experimental studies. This book is organized into 9 chapters, and starts with discussions of the various decay processes, the possible interaction mechanisms of gamma radiation with matter, and the intrinsic and extrinsic variables, which affect the observed gamma-ray and X-ray spectra. The subsequent chapters deal with the properties and fabrication of scintillation detectors, semiconductor detectors, and proportional gas counters. These chapters present some of the most widely utilized

  20. Ion cyclotron emission by spontaneous emission

    Energy Technology Data Exchange (ETDEWEB)

    Da Costa, O. [Commission of the European Communities, Abingdon (United Kingdom). JET Joint Undertaking; Gresillon, D. [Ecole Polytechnique, 91 - Palaiseau (France). Lab. de Physique des Milieux Ionises

    1994-07-01

    The goal of the study is to examine whether the spontaneous emission can account for ICE (ion cyclotron emission) experimental results, or part of them. A straightforward approach to plasma emission is chosen, investigating the near equilibrium wave radiation by gyrating ions, and thus building from the majority and fast fusion ions the plasma fluctuations and emission on the fast magnetoacoustic or compressional Alfven wave mode in the IC frequency range. Similarities with the ICE experiments are shown: the emission temperature in the presence of fast ions (even in a very small amount), the strong fast ion emission increase with the harmonic, the fine double-line splitting of each peak, the linear but not proportional increase of the peak width with the harmonic. 3 refs., 2 figs.

  1. A simple method for the absolute determination of uranium enrichment by high-resolution {gamma} spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Korob, R.O. [Unidad de Actividad Radioquimica y Quimica de las Radiaciones, Comision Nacional de Energia Atomica, Centro Atomico Ezeiza, Presbitero Juan Gonzalez y Aragon No. 15 Partido de Ezeiza, Provincia de Buenos Aires (Argentina)]. E-mail: korob@cae.cnea.gov.ar; Blasiyh Nuno, G.A. [Unidad de Actividad Gestion de Residuos Radiactivos, Comision Nacional de Energia Atomica, Centro Atomico Ezeiza, Presbitero Juan Gonzalez y Aragon No. 15 Partido de Ezeiza, Provincia de Buenos Aires (Argentina)

    2006-05-15

    A simple method for the determination of uranium enrichment using high-resolution {gamma} spectrometry is presented in this paper. The method relies solely on the {gamma}-ray emission probabilities of {sup 235}U and {sup 234m}Pa, and an iterative procedure for the least squares fit of a polynomial to a set of experimentally determined data. To ensure the reliability of the {sup 234m}Pa {gamma}-ray emission probabilities employed, a new determination of these probabilities was carried out using a combination of {gamma} spectrometry and Cerenkov counting of a purified {sup 234}Th solution. Using these new data, a maximum difference of {approx}5% has been found between the experimental and declared uranium enrichment in a set of solid and liquid samples containing uranium compounds.

  2. Gas chromatography of organic microcontaminants using atomic emission and mass spectrometric detection combined in one instrument (GC-AED/MS)

    NARCIS (Netherlands)

    Mol, H.G.J.; Hankemeier, T.; Brinkman, U.A.T.

    1999-01-01

    This study describes the coupling of an atomic-emission detector and mass-spectrometric detector to a single gas chromatograph. Splitting of the column effluent enables simultaneous detection by atomic-emission detection (AED) and mass spectrometry (MS) and yields a powerful system for the target an

  3. Oxygenated VOC and monoterpene emissions from a boreal coniferous forest

    Science.gov (United States)

    Taipale, R.; Rantala, P.; Kajos, M. K.; Patokoski, J.; Ruuskanen, T. M.; Aalto, J.; Kolari, P.; Bäck, J.; Hari, P.; Kulmala, M.; Rinne, J.

    2012-04-01

    Compared with terpenoids, emissions of oxygenated volatile organic compounds (VOCs) from boreal ecosystems have been poorly characterized. We measured ecosystem scale emissions of three oxygenated compounds (methanol, acetaldehyde, and acetone) and monoterpenes from a Scots pine dominated forest in southern Finland during the summers 2006-2008. The measurements were conducted using the disjunct eddy covariance method combined with proton transfer reaction mass spectrometry. The contribution of the three oxygenated compounds to the measured total emissions was 40-60 %. The highest oxygenated VOC emissions were those of methanol, comprising 20-30 % of the total, followed by acetone with a share of 10-20 %. The acetaldehyde emissions were 5-10 % of the total. This emission composition will be compared with that obtained from shoot enclosure measurements. Methanol showed deposition during some periods although its overall flux was towards the atmosphere. The monoterpene emissions had a light dependent component, suggesting that part of the emissions originated directly from monoterpene biosynthesis. Diurnal, seasonal, and inter-annual variations in the emissions, along with temperature and light dependencies, will be discussed.

  4. Mass Spectrometry Applications for Toxicology

    Science.gov (United States)

    Mbughuni, Michael M.; Jannetto, Paul J.

    2016-01-01

    Toxicology is a multidisciplinary study of poisons, aimed to correlate the quantitative and qualitative relationships between poisons and their physiological and behavioural effects in living systems. Other key aspects of toxicology focus on elucidation of the mechanisms of action of poisons and development of remedies and treatment plans for associated toxic effects. In these endeavours, Mass spectrometry (MS) has become a powerful analytical technique with a wide range of application used in the Toxicological analysis of drugs, poisons, and metabolites of both. To date, MS applications have permeated all fields of toxicology which include; environmental, clinical, and forensic toxicology. While many different analytical applications are used in these fields, MS and its hyphenated applications such as; gas chromatography MS (GC-MS), liquid chromatography MS (LC-MS), inductively coupled plasma ionization MS (ICP-MS), tandem mass spectrometry (MS/MS and MSn) have emerged as powerful tools used in toxicology laboratories. This review will focus on these hyphenated MS technologies and their applications for toxicology.

  5. Quantitative mass spectrometry: an overview

    Science.gov (United States)

    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'.

  6. Mass Spectrometry Applications for Toxicology.

    Science.gov (United States)

    Mbughuni, Michael M; Jannetto, Paul J; Langman, Loralie J

    2016-12-01

    Toxicology is a multidisciplinary study of poisons, aimed to correlate the quantitative and qualitative relationships between poisons and their physiological and behavioural effects in living systems. Other key aspects of toxicology focus on elucidation of the mechanisms of action of poisons and development of remedies and treatment plans for associated toxic effects. In these endeavours, Mass spectrometry (MS) has become a powerful analytical technique with a wide range of application used in the Toxicological analysis of drugs, poisons, and metabolites of both. To date, MS applications have permeated all fields of toxicology which include; environmental, clinical, and forensic toxicology. While many different analytical applications are used in these fields, MS and its hyphenated applications such as; gas chromatography MS (GC-MS), liquid chromatography MS (LC-MS), inductively coupled plasma ionization MS (ICP-MS), tandem mass spectrometry (MS/MS and MS(n)) have emerged as powerful tools used in toxicology laboratories. This review will focus on these hyphenated MS technologies and their applications for toxicology.

  7. Triazolobithiophene Light Absorbing Self-Assembled Monolayers: Synthesis and Mass Spectrometry Applications

    Directory of Open Access Journals (Sweden)

    Denis Séraphin

    2011-10-01

    Full Text Available The synthesis of five light absorbing triazolobithiophenic thiols, which were utilized for producing self-assembled monolayers (SAMs on gold surfaces, is presented. The monolayer formation was monitored by cyclic voltammetry, indicating excellent surface coverage. The new triazolobithiophenic compounds exhibited an absorption maximum around 340 nm, which is close to the emission wavelength of a standard nitrogen laser. Consequently these compounds could be used to aid ionization in laser desorption mass spectrometry (MS.

  8. Ammonia emissions in Europe

    DEFF Research Database (Denmark)

    Jacobsen, Brian H.

    2012-01-01

    The NEC (National Emission Ceiling) directive has set targets for the 2010 ammonia emissions from a number of European countries. The target will be reached by most EU-countries and the total emission for EU-27 has been reduced by 22% from 1990 to 2007. Denmark is one of the countries with the la......The NEC (National Emission Ceiling) directive has set targets for the 2010 ammonia emissions from a number of European countries. The target will be reached by most EU-countries and the total emission for EU-27 has been reduced by 22% from 1990 to 2007. Denmark is one of the countries...

  9. Handbook on Mobile Gamma-ray Spectrometry

    DEFF Research Database (Denmark)

    Aage, Helle Karina; Korsbech, Uffe C C

    2003-01-01

    Basic physics and mathematics for Airborne and Car-borne Gamma-ray Spectrometry supplemented with practical examples and methods for advanced data processing......Basic physics and mathematics for Airborne and Car-borne Gamma-ray Spectrometry supplemented with practical examples and methods for advanced data processing...

  10. Handbook on Mobile Gamma-ray Spectrometry

    DEFF Research Database (Denmark)

    Aage, Helle Karina; Korsbech, Uffe C C

    2003-01-01

    Basic physics and mathematics for Airborne and Car-borne Gamma-ray Spectrometry supplemented with practical examples and methods for advanced data processing......Basic physics and mathematics for Airborne and Car-borne Gamma-ray Spectrometry supplemented with practical examples and methods for advanced data processing...

  11. Interface for time-resolved introduction of gaseous analytes for atomic spectrometry by purge-and-trap multicapillary gas chromatography (PTMGC)

    Science.gov (United States)

    Wasik, Andrzej; Rodriguez Pereiro, Isaac; Łobiński, Ryszard

    1998-08-01

    A semi-automated compact interface that enables time-resolved introduction of gaseous analytes from aqueous solutions into an atomic spectrometer without the need for a full-size GC-oven is described. The interface is based on purging the gaseous analytes with an inert gas, drying the gas stream using a 30-cm tubular Nafion membrane and trapping the compounds in a thick film-coated capillary tube followed by their isothermal separation on a 1-m multicapillary GC column. Developments regarding each of the steps of the analytical procedure and effects of operational variables (sample volume, purge flow, trap temperature, speed of injection, GC separation conditions) are discussed using the speciation analysis of a mixture of tetraalkyllead compounds as an example. Recoveries are quantitative up to a sample volume of 50 ml. Figures of merit for the interface coupled to a microwave-induced plasma atomic emission detector are given. The interface allows the full speciation analysis (including sample preparation) to be carried out within less than 5 min with detection limits down to 5 pg l -1.

  12. Emissions Modeling Clearinghouse

    Data.gov (United States)

    U.S. Environmental Protection Agency — The Emissions Modeling Clearinghouse (EMCH) supports and promotes emissions modeling activities both internal and external to the EPA. Through this site, the EPA...

  13. Walkable dual emissions

    National Research Council Canada - National Science Library

    Xu, Hai-Bing; Jiao, Peng-Chong; Kang, Bin; Deng, Jian-Guo; Zhang, Yan

    2013-01-01

    Walkable dual emissions, in which the emission bands of the walker reversibly cross or leave those of the stationary ones depending on temperature and concentration, have been demonstrated in cyclic...

  14. National Emission Inventory

    Data.gov (United States)

    U.S. Environmental Protection Agency — The National Emission Inventory contains measured, modeled, and estimated data for emissions of all known source categories in the US (stationary sources, fires,...

  15. World Emission RETRO ANTHRO

    Data.gov (United States)

    Washington University St Louis — Anthropogenic and vegetation fire emissions data were generated monthly covering a period of 1960 to 2000. Anthropogenic emissions in the RETRO inventory are derived...

  16. Emissions & Measurements - Black Carbon

    Science.gov (United States)

    Emissions and Measurement (EM) research activities performed within the National Risk Management Research Lab NRMRL) of EPA's Office of Research and Development (ORD) support measurement and laboratory analysis approaches to accurately characterize source emissions, and near sour...

  17. What Is Emissions Trading?

    Science.gov (United States)

    Learn the basics about how emissions trading uses a market-based policy tool used to control large amounts of pollution emissions from a group of sources in order to protect human health and the environment.

  18. National Emission Inventory

    Data.gov (United States)

    U.S. Environmental Protection Agency — The National Emission Inventory contains measured, modeled, and estimated data for emissions of all known source categories in the US (stationary sources, fires,...

  19. Neuroscience and Accelerator Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    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.

  20. Laser sputter neutral mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    King, B.V.; Clarke, M.; Hu, H.; Betz [Newcastle Univ., NSW (Australia). Dept. of Physics

    1993-12-31

    Laser sputter neutral mass spectrometry (LSNMS) is an emerging technique for highly sensitive surface analysis. In this technique a target is bombarded with a pulsed beam of keV ions. The sputtered particles are intercepted by a high intensity pulsed laser beam above the surface and ionised with almost 100% efficiency. The photions may then be mass analysed using a quadrupole or, more commonly, using time of flight (TOF) techniques. In this method photoions are extracted from the ionisation region, accelerated to a known energy E{sub o} and strike a channelplate detector a distance `d` away. The flight time `t` of the photoions is then related to their mass by `d` {radical}m / {radical} 2E{sub o} so measurement of `t` allows mass spectra to be obtained. It is found that LSNMS is an emerging technique of great sensitivity and flexibility, useful for both applied analysis and to investigate basic sputtering processes. 4 refs., 3 figs.

  1. Electrophoresis-mass spectrometry probe

    Science.gov (United States)

    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.

  2. Volatile organic compound emissions from elephant grass and bamboo cultivars used as potential bioethanol crop

    Science.gov (United States)

    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.

  3. Determination of seven elements in laterite nickel ore by portable energy dispersive X-ray fluorescence spectrometry%便携式能量色散X射线荧光光谱仪测定红土镍矿中7种元素

    Institute of Scientific and Technical Information of China (English)

    屈太原; 李华昌; 冯先进

    2012-01-01

    选取具有代表性的红土镍矿样品为校准样品,建立了便携式能量色散X射线荧光光谱仪直接测定粉末红土镍矿样品中Fe、Ni、Cr、Mn、Ti、Zn、Ca含量的分析方法.实验采用滴定法对校准样品中主量元素铁,电感耦合等离子体原子发射光谱法(ICP-AES)对其它元素进行定值,解决了红土镍矿标准样品短缺的问题.对校准样品的前处理方法及测定条件等进行了探讨,并通过研磨使校准样品与测试样品达到相同颗粒度以降低颗粒效应的干扰,同时利用仪器自带的NDTr软件,以基本参数法(FP法)自动校正元素间相互干扰效应.精密度试验结果表明,各组分相对标准偏差(n=7)在0.16%~8.3%之间.方法用于红土镍矿实际样品分析,测定结果与湿法分析结果吻合,能够满足现场大批量样品主次元素同时快速分析的需要.%A direct determination method of Fe, Ni, Cr, Mn, Ti, Zn and Ca in powdered laterite nickel ore by portable energy dispersion X-ray fluorescence spectrometer was established using representative laterite nickel ore samples as calibration sample. The main element iron in calibration sample was certified by titration, while other elements were certified by inductively coupled plasma atomic emission spectrometry (ICP-AES). This solved the shortage problem of laterite nickel ore certified reference materials. The pretreatment methods of calibration sample and determination conditions were discussed. The particle size of calibration sample and testing sample was ground to the same level to reduce the interference of grain effect. Meanwhile, the mutual interference effect among elements was automatically corrected by fundamental parameter method (FP) with the NDTr software in instrument. The results of precision test indicated that, the relative standard deviations (RSD, n = 7) of testing elements were 0.16 %-8. 3 %. The proposed method was applied to the determination of actual laterite

  4. Quinone emissions from gasoline and diesel motor vehicles.

    Science.gov (United States)

    Jakober, Chris A; Riddle, Sarah G; Robert, Michael A; Destaillats, Hugo; Charles, M Judith; Green, Peter G; Kleeman, Michael J

    2007-07-01

    Gas- and particle-phase emissions from gasoline and diesel vehicles operated on chassis dynamometers were collected using annular denuders, quartz filters, and PUF substrates. Quinone species were measured using O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine derivatization in conjunction with gas chromatography-mass spectrometry and high-performance liquid chromatography-mass spectrometry. Nine quinones were observed, ranging from C6 to C16. New species identified in motor vehicle exhaust include methyl-1,4-benzoquinone, 2-methyl-1,4-naphthoquinone (MNQN), and aceanthrenequinone. Gas-phase motor vehicle emissions of quinones are also reported for the first time. Six gas-phase quinones were quantified with emission rates of 2-28 000 microg L(-1) fuel consumed. The most abundant gas-phase quinones were 1,4-benzoquinone (BON) and MNQN. The gas-phase fraction was > or = 69% of quinone mass for light-duty gasoline emissions, and > or = 84% for heavy-duty diesel emissions. Eight particle-phase quinones were observed between 2 and 1600 microg L(-1), with BQN the most abundant species followed by 9,10-phenanthrenequinone and 1,2-naphthoquinone. Current particle-phase quinone measurements agree well with the few available previous results. Further research is needed concerning the gas-particle partitioning behavior of quinones in ambient and combustion source conditions.

  5. Attomole quantitation of protein separations with accelerator mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    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.

  6. Off-season biogenic volatile organic compound emissions from heath mesocosms

    DEFF Research Database (Denmark)

    Rinnan, Riikka; Gierth, Diana; Bilde, Merete;

    2013-01-01

    measured in growth chambers by an enclosure method using gas chromatography-mass spectrometry. CO2 exchange, soil microbial biomass and soil carbon and nitrogen concentrations were also analyzed. Vegetation cutting increased BVOC emissions by more than 20-fold, and the induced compounds were mainly eight-carbon......Biogenic volatile organic compounds (BVOCs) affect both atmospheric processes and ecological interactions. Our primary aim was to differentiate between BVOC emissions from above- and belowground plant parts and heath soil outside the growing season. The second aim was to assess emissions from...... compounds and sesquiterpenes. In the Deschampsia heath, the overall low BVOC emissions originated mainly from soil. In the mixed heath, root and soil emissions were negligible. Net BVOC emissions from roots and soil of these well-drained heaths do not significantly contribute to ecosystem emissions...

  7. Wireless Data Acquisition of Transient Signals for Mobile Spectrometry Applications.

    Science.gov (United States)

    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.

  8. Shipping emissions in ports

    OpenAIRE

    2014-01-01

    Shipping emissions in ports are substantial, accounting for 18 million tonnes of CO2 emissions, 0.4 million tonnes of NOx, 0.2 million of SOx and 0.03 million tonnes of PM10 in 2011. Around 85% of emissions come from containerships and tankers. Containerships have short port stays, but high emissions during these stays. Most of CO2 emissions in ports from shipping are in Asia and Europe (58%), but this share is low compared to their share of port calls (70%). European ports have much less emi...

  9. International emissions trading

    DEFF Research Database (Denmark)

    Boom, Jan Tjeerd

    This thesis discusses the design and political acceptability of international emissions trading. It is shown that there are several designs options for emissions trading at the national level that have a different impact on output and thereby related factors such as employment and consumer prices....... The differences in impact of the design make that governments may prefer different designs of emissions trading in different situations. The thesis furthermore establishes that international emissions trading may lead to higher overall emissions, which may make it a less attractive instrument....

  10. Origin of monoterpene emissions from boreal tree species: Determination of de novo and pool emissions by 13CO2 labeling

    Science.gov (United States)

    Rinne, J.; Ghirardo, A.; Koch, K.; Taipale, R.; Zimmer, I.; Schnitzler, J.

    2009-12-01

    Boreal forests emit a large amount of monoterpenes into the atmosphere. Traditionally these emissions are assumed to originate as evaporation from large storage pools. Thus their diurnal cycle would depend mostly on temperature. However, there is indication that a significant part of the monoterpene emission would originate directly from de novo synthesis. By applying 13CO2 fumigation and analyzing the isotope fractions with proton transfer reaction mass spectrometry (PTR-MS) and classical GC-MS we studied the origin of monoterpene emissions from some major Eurasian boreal and alpine tree species. We determined the fractions originating from de novo biosynthesis and from large internal monoterpene storages for three coniferous tree species with specialized monoterpene storage structures and one dicotyledon species without such structures. The emission from dicotyledon species Betula pendula originated solely from the de novo synthesis. The origin of the emissions from coniferous species was mixed with varying fraction originating from de novo synthesis (Pinus sylvestris 58%, Picea abies 33.5%, Larix decidua 9.8%) and the rest from large internal monoterpene storage pools. Application of the observed fractions of emission originating from de novo synthesis and large storage pools in a hybrid emission algorithm resulted in a better description of ecosystem scale monoterpene emissions from a boreal Scots pine forest stand.

  11. Peculiarities of the modern neutron spectrometry

    Indian Academy of Sciences (India)

    Yu P Popov

    2001-08-01

    Neutron spectrometry provides many branches of science and technology with the necessary data. Usually the main part of the data is supplied by powerful neutron time-of-flight spectrometers. Nevertheless there are many other very effective but simpler and cheaper neutron spectroscopy methods on accelerators, suitable for solution of plenty of scientific and applied problems (for example, in astrophysics and radioactive waste transmutation). The methods of slowing-down spectrometry in lead and graphite, generating of neutron spectra, characteristic for nucleosynthesis in the stars, and neutron spectrometry by means of primary -transition shift are discussed in the report.

  12. Protein Analysis by Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Cindic, M.

    2008-04-01

    Full Text Available Soft ionization techniques, electrospray (ESI and matrix-assisted laser desorption/ionization (MALDI make the analysis of biomolecules by mass spectrometry (MS possible. MS is used for determination of the molecular weight of peptides and protein, sequence analysis, characterization of protein-ligand interactions etc. The detection limit, resolution and mass accuracy depend on instrument used (Table 1. Impurities (buffers, salts, detergents can reduce the ion intensities or even totally suppress them, so a separation method (chromatography, 2D-gel electrophoresis must be used for purification of the sample.Molecular mass of intact protein can be determined by ESI or MALDI MS. Multiply charged ions are produced by ESI MS, while singly charged ions are predominant in MALDI spectra (Fig. 2.Sequence analysis of proteins by MS can be performed using peptide mass fingerprint. In this method, proteins are separated by 2-D gel electrophoresis and digested with specific protease (Table 2 or digested and then separated by two-dimensional chromatography (Fig. 1. The obtained peptide mixtures are analyzed by MS or MALDI-TOF technique. The masses determined by MS are compared with calculated masses from database entries. Different algorithms have been developed for protein identification. Example of posttranslational modifications (N- and O-glycosylation and protein sequence complex analysis after dual digestion (endoproteinase digestion followed by endoglycosidase digestion is shown in Fig. 3.It is known that detection of peptides by MS is influenced by intrinsic properties like amino acid composition, the basicity of the C-terminal amino acid, hydrophobicity, etc. Arginine-containing peptides dominate in MS spectra of tryptic digest, so the chemical derivatization of lysine terminal residue by O-methilisourea or 2-methoxy-4,5-1H-imidazole was suggested (Fig. 4.The peptide mass fingerprint method can be improved further by peptide fragmentation using tandem

  13. Role of de novo biosynthesis in ecosystem scale monoterpene emissions from a boreal Scots pine forest

    Directory of Open Access Journals (Sweden)

    R. Taipale

    2011-08-01

    Full Text Available Monoterpene emissions from Scots pine have traditionally been assumed to originate as evaporation from specialized storage pools. More recently, the significance of de novo emissions, originating directly from monoterpene biosynthesis, has been recognized. To study the role of biosynthesis at the ecosystem scale, we measured monoterpene emissions from a Scots pine dominated forest in southern Finland using the disjunct eddy covariance method combined with proton transfer reaction mass spectrometry. The interpretation of the measurements was based on a correlation analysis and a hybrid emission algorithm describing both de novo and pool emissions. During the measurement period May–August 2007, the monthly medians of daytime emissions were 200, 290, 180, and 200 μg m−2 h−1. The emissions were partly light dependent, probably due to de novo biosynthesis. The emission potential for both de novo and pool emissions exhibited a decreasing summertime trend. The ratio of the de novo emission potential to the total emission potential varied between 30 % and 46 %. Although the monthly changes were not significant, the ratio always differed statistically from zero, suggesting that the role of de novo biosynthesis was observable. Given the uncertainties in this study, we conclude that more accurate estimates of the contribution of de novo emissions are required for improving monoterpene emission algorithms for Scots pine dominated forests.

  14. Warming increases isoprene emissions from an arctic fen.

    Science.gov (United States)

    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.

  15. Introduction to mass spectrometry-based proteomics

    DEFF Research Database (Denmark)

    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...

  16. Pyrolysis - gas chromatography - mass spectrometry of lignins

    Energy Technology Data Exchange (ETDEWEB)

    Martin, F.; Saiz-Jimenez, C.; Gonzalez-Vila, F.J.

    1979-01-01

    Milled wood lignins from spruce, beech and bamboo were pyrolysed. The high-boiling products of pyrolysis were studied by GLC and mass spectrometry. The forty-three products identified provide information on the structural units of lignin.

  17. NICHD Biomedical Mass Spectrometry Core Facility

    Data.gov (United States)

    Federal Laboratory Consortium — The NICHD Biomedical Mass Spectrometry Core Facility was created under the auspices of the Office of the Scientific Director to provide high-end mass-spectrometric...

  18. Mass spectrometry of fluorocarbon-labeled glycosphingolipids

    DEFF Research Database (Denmark)

    Li, Yunsen; Arigi, Emma; Eichert, Heather;

    2010-01-01

    A method for generation of novel fluorocarbon derivatives of glycosphingolipids (GSLs) with high affinity for fluorocarbon phases has been developed, and their potential applications to mass spectrometry (MS)-based methodologies for glycosphingolipidomics have been investigated. Sphingolipid...

  19. Difraction spectrometry by laser beams

    Directory of Open Access Journals (Sweden)

    Frías, M.

    1988-12-01

    Full Text Available The advances in laser technology have permitted the development of numerous applications, in particular diffraction spectrometry by laser beams for the determination of the distribution curve of the particle sizes of different materials; this permits one to obtain the distribution of particle size in both wet and dry materials. In the present paper a brief description of the technique and its principles is offered. The results obtained with different materials-limestone clay, gypsum, Portland cement and siliceous materials are given.

    Los avances en la tecnología laser han permitido el desarrollo de múltiples aplicaciones, en concreto la espectrometría de difracción de rayos laser para la determinación de la curva de distribución del tamaño de partícula de diferentes materiales, y que permite la obtención de la misma tanto en seco como en húmedo. En este trabajo se hace una descripción breve de la técnica y de sus fundamentos. Se presentan resultados con diferentes materiales: caliza, arcilla, yeso, cemento Portland y materiales silíceos.

  20. Quantitative mass spectrometry: an overview

    Science.gov (United States)

    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

  1. Anomalous Microwave Emission

    CERN Document Server

    Kogut, A J

    1999-01-01

    Improved knowledge of diffuse Galactic emission is important to maximize the scientific return from scheduled CMB anisotropy missions. Cross-correlation of microwave maps with maps of the far-IR dust continuum show a ubiquitous microwave emission component whose spatial distribution is traced by far-IR dust emission. The spectral index of this emission, beta_{radio} = -2.2 (+0.5 -0.7) is suggestive of free-free emission but does not preclude other candidates. Comparison of H-alpha and microwave results show that both data sets have positive correlations with the far-IR dust emission. Microwave data, however, are consistently brighter than can be explained solely from free-free emission traced by H-alpha. This ``anomalous'' microwave emission can be explained as electric dipole radiation from small spinning dust grains. The anomalous component at 53 GHz is 2.5 times as bright as the free-free emission traced by H-alpha, providing an approximate normalization for models with significant spinning dust emission.

  2. Global Seabird Ammonia Emissions

    Science.gov (United States)

    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

  3. Carbon emissions Inventory Games

    OpenAIRE

    Al-Emadi, Eiman Ali

    2016-01-01

    Carbon emissions reduction has been the center of attention in many organizations during the past few decades. Many international entities developed rules and regulations to monitor and control carbon emissions especially under supply chain context. Furthermore, researchers investigated techniques and methods on how reduce carbon emissions under operational adjustment which can be done by cooperation or coordination. The main contribution of this thesis is to measure to what extend cooperatio...

  4. [Multivariate analysis of heavy metal element concentrations in atmospheric deposition in Harbin City, northeast China].

    Science.gov (United States)

    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.

  5. Properties, performance and emissions of biofuels in blends with gasoline

    Science.gov (United States)

    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.

  6. Volatilization behavior of Cd and Zn based on continuous emission measurement of flue gas from laboratory-scale coal combustion.

    Science.gov (United States)

    Liu, J; Falcoz, Q; Gauthier, D; Flamant, G; Zheng, C Z

    2010-06-01

    The accumulation of toxic metals generated by coal-fired power stations presents a serious threat to the environment. The volatilization behavior of two representative metals (Cd and Zn), and the influence of temperature were investigated during coal combustion. An inductively coupled plasma atomic emission spectrometric (ICP-AES) method was developed to continuously measure the heavy metal concentrations quantitatively in flue gas under combustion conditions in order to track the metal release process. This continuous heavy metal analysis system was implemented by coupling it to two types of high temperature reactors: a bubbling fluidized bed reactor and a fixed bed reactor with diameter of 0.1 m and 0.08 m respectively. For the two metals considered in this study (Cd and Zn), the experimental setup was successfully used to continuously monitor the metal vaporization process during coal combustion independent of reactor design, and at different temperatures. Cd is more easily vaporized than Zn during coal combustion. Temperature significantly influences the metal vaporization process. In general, the higher the temperature, the higher the metal vaporization, although the vaporization is not proportional to temperature. In addition to the experimental study, a thermodynamic calculation was carried out to simulate the heavy metal speciation during coal combustion process. The theoretical volatilization tendency is consistent with the experiment. The thermodynamic calculation identified the formation of binary oxides retarding heavy metal vaporization.

  7. Managing Refrigerant Emissions

    Science.gov (United States)

    Access information on EPA's efforts to address ozone layer depletion by reducing emissions of refrigerants from stationary refrigeration and air conditioning systems and motor vehicle air conditioning systems.

  8. VOC emissions chambers

    Data.gov (United States)

    Federal Laboratory Consortium — In order to support the development of test methods and reference materials for volatile organic compounds (VOC) emissions from building materials and furnishings,...

  9. Microgravity Emissions Laboratory (MEL)

    Data.gov (United States)

    Federal Laboratory Consortium — The Microgravity Emissions Laboratory (MEL) utilizes a low-frequency acceleration measurement system for the characterization of rigid body inertial forces generated...

  10. Toluene emissions from plants

    Science.gov (United States)

    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.

  11. 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.

    Science.gov (United States)

    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.

  12. REAL-TIME EMISSION CHARACTERIZATION OF ORGANIC AIR TOXIC POLLUTANTS DURING STEADY STATE AND TRANSIENT OPERATION OF A MEDIUM DUTY DIESEL ENGINE

    Science.gov (United States)

    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...

  13. Outsourcing CO2 Emissions

    Science.gov (United States)

    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.

  14. Air Emission Inventory for the INEEL -- 1999 Emission Report

    Energy Technology Data Exchange (ETDEWEB)

    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. Time-resolved analysis of particle emissions from residential biomass combustion - Emissions of refractory black carbon, PAHs and organic tracers

    Science.gov (United States)

    Nielsen, Ingeborg E.; Eriksson, Axel C.; Lindgren, Robert; Martinsson, Johan; Nyström, Robin; Nordin, Erik Z.; Sadiktsis, Ioannis; Boman, Christoffer; Nøjgaard, Jacob K.; Pagels, Joakim

    2017-09-01

    Time-resolved particle emissions from a conventional wood stove were investigated with aerosol mass spectrometry to provide links between combustion conditions, emission factors, mixing state of refractory black carbon and implications for organic tracer methods. The addition of a new batch of fuel results in low temperature pyrolysis as the fuel heats up, resulting in strong,