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Sample records for emission spectrometry icp-oes

  1. Elemental analysis of glass by laser ablation inductively coupled plasma optical emission spectrometry (LA-ICP-OES).

    PubMed

    Schenk, Emily R; Almirall, José R

    2012-04-10

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2017-04-01

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

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

    NASA Astrophysics Data System (ADS)

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

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

  6. [Determination of heavy metals for RoHS compliance by ICP-OES spectrometry coupled with microwave extraction system].

    PubMed

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

    2008-11-01

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

  7. A matrix effect and accuracy evaluation for the determination of elements in milk powder LIBS and laser ablation/ICP-OES spectrometry.

    PubMed

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

    2011-11-01

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

  8. Elemental profiling and geographical differentiation of Ethiopian coffee samples through inductively coupled plasma-optical emission spectroscopy (ICP-OES), ICP-mass spectrometry (ICP-MS) and direct mercury analyzer (DMA).

    PubMed

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

    2016-12-01

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

  9. Selective solid phase extraction of copper using a new Cu(II)-imprinted polymer and determination by inductively coupled plasma optical emission spectroscopy (ICP-OES).

    PubMed

    Yilmaz, Vedat; Arslan, Zikri; Hazer, Orhan; Yilmaz, Hayriye

    2014-05-01

    This work reports the preparation of a novel Cu(II)-ion imprinted polymer using 2-thiozylmethacrylamide (TMA) for on-line preconcentration of Cu(II) prior to its determination by inductively coupled optical emission spectroscopy (ICP-OES). Cu(II)-TMA monomer (complex) was synthesized and copolymerized via bulk polymerization method in the presence of ethyleneglycoldimethacrylate cross-linker. The resulting polymer was washed with 5% (v/v) HNO3 to remove Cu(II) ions and then with water until a neutral pH. The ion imprinted polymer was characterized by FT-IR and scanning electron microscopy. The experimental conditions were optimized for on-line preconcentration of Cu(II) using a minicolumn of ion imprinted polymer (IIP). Quantitative retention was achieved between pH 5.0 and 6.0, whereas the recoveries for the non-imprinted polymer (NIP) were about 61%. The IIP showed about 30 times higher selectivity to Cu(II) in comparison to NIP. The IIP also exhibited excellent selectivity for Cu(II) against the competing transition and heavy metal ions, including Cd, Co, Cr, Fe, Mn, Ni, Pb and Zn. Computational calculations revealed that the selectivity of IIP was mediated by the stability of Cu(II)-TMA complex which was far more stable than those of Co(II), Ni(II) and Zn(II) that have similar charge and ionic radii to Cu(II). A volume of 10 mL sample solution was loaded onto the column at 4.0 mL min(-1) by using a sequential injection system (FIALab 3200) followed by elution with 1.0 mL of 2% (v/v) HNO3. The relative standard deviation (RSD) and limit of detection (LOD, 3s) of the method were 3.2% and 0.4 μg L(-1), respectively. The method was successfully applied to determination of Cu(II) in fish otoliths (CRM 22), bone ash (SRM 1400) and coastal seawater and estuarine water samples.

  10. Selective solid phase extraction of copper using a new Cu(II)-imprinted polymer and determination by inductively coupled plasma optical emission spectroscopy (ICP-OES)

    PubMed Central

    Yilmaz, Vedat; Arslan, Zikri; Hazer, Orhan; Yilmaz, Hayriye

    2014-01-01

    This work reports the preparation of a novel Cu(II)-ion imprinted polymer using 2-thiozylmethacrylamide (TMA) for on-line preconcentration of Cu(II) prior to its determination by inductively coupled optical emission spectroscopy (ICP-OES). Cu(II)-TMA monomer (complex) was synthesized and copolymerized via bulk polymerization method in the presence of ethyleneglycoldimethacrylate cross-linker. The resulting polymer was washed with 5% (v/v) HNO3 to remove Cu(II) ions and then with water until a neutral pH. The ion imprinted polymer was characterized by FT-IR and scanning electron microscopy. The experimental conditions were optimized for on-line preconcentration of Cu(II) using a minicolumn of ion imprinted polymer (IIP). Quantitative retention was achieved between pH 5.0 and 6.0, whereas the recoveries for the non-imprinted polymer (NIP) were about 61%. The IIP showed about 30 times higher selectivity to Cu(II) in comparison to NIP. The IIP also exhibited excellent selectivity for Cu(II) against the competing transition and heavy metal ions, including Cd, Co, Cr, Fe, Mn, Ni, Pb and Zn. Computational calculations revealed that the selectivity of IIP was mediated by the stability of Cu(II)-TMA complex which was far more stable than those of Co(II), Ni(II) and Zn(II) that have similar charge and ionic radii to Cu(II). A volume of 10 mL sample solution was loaded onto the column at 4.0 mL min−1 by using a sequential injection system (FIALab 3200) followed by elution with 1.0 mL of 2% (v/v) HNO3. The relative standard deviation (RSD) and limit of detection (LOD, 3s) of the method were 3.2% and 0.4 μg L−1, respectively. The method was successfully applied to determination of Cu(II) in fish otoliths (CRM 22), bone ash (SRM 1400) and coastal seawater and estuarine water samples. PMID:24511158

  11. Method of low tantalum amounts determination in niobium and its compounds by ICP-OES technique.

    PubMed

    Smolik, Marek; Turkowska, Magdalena

    2013-10-15

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

  12. Elemental bioimaging by means of LA-ICP-OES: investigation of the calcium, sodium and potassium distribution in tobacco plant stems and leaf petioles.

    PubMed

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

    2017-06-21

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

  13. Uncertainty estimation in the determination of metals in superficial water by ICP-OES

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

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

  14. Volatile Organic Silicon Compounds in Biogases: Development of Sampling and Analytical Methods for Total Silicon Quantification by ICP-OES

    PubMed Central

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

    2014-01-01

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

  15. Volatile organic silicon compounds in biogases: development of sampling and analytical methods for total silicon quantification by ICP-OES.

    PubMed

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

    2014-01-01

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

  16. Effect of valence state on ICP-OES value assignment of SRM 3103a arsenic spectrometric solution.

    PubMed

    Yu, Lee L; Butler, Therese A; Turk, Gregory C

    2006-03-01

    The certification of Standard Reference Material (SRM is a registered trademark of NIST) 3103a As Spectrometric Solution is based on the gravimetric preparation value that is verified by inductively coupled plasma optical emission spectrometry (ICP-OES) measurements. A disagreement between the gravimetric and the spectrometric values for a batch of As calibration solutions led to the discovery that the solutions contained a mixture of trivalent and pentavalent As species and that the pentavalent species was approximately 8% more sensitive than the trivalent species with ICP-OES determination. The kinetics of the reaction between As metal and nitric acid were studied, and the results were applied to develop a procedure that would consistently produce single-species pentavalent As standards, which eliminates As speciation as a source of measurement bias in the SRM certification process.

  17. A rapid ICP-OES strategy for determination of gold and silver in blister copper by nitric acid digestion

    NASA Astrophysics Data System (ADS)

    Zhang, Gai; Tian, Min

    2014-03-01

    A rapid strategy for the analysis of gold and silver in blister copper by inductively coupled plasma optical emission spectrometry (ICP-OES) was firstly proposed. Nitric acid was used to digest blister copper instead of commonly used sulfuric acid. This prevented forming the salt of copper sulfate in the filtration process when the volume of the mixture is very small. Thus, the time of filtration was saved. After filtrating, aqua regia was used to digest the residue and acidize the filter liquor. Two parts of gotten solution were directly determined by ICP-OES. The cycle of analysis was shortened compared with sulfuric acid-fire assay. The proposed method was successfully applied to determine gold and silver in blister copper, and the results were in good agreement with those obtained by lead fire assay.

  18. PIXE as a complement to trace metal analysis of sediments by ICP-OES

    NASA Astrophysics Data System (ADS)

    Lunderberg, J. M.; Bartlett, R. J.; Behm, A. M.; Contreras, C.; DeYoung, P. A.; Hoogeveen, N. L.; Huisman, A. J.; Peaslee, G. F.; Postma, J. K.

    2008-11-01

    The adverse effects of metal contamination in sediments require methods that can quickly and accurately assess the extent of environmental pollution. Particle induced X-ray emission spectrometry (PIXE) is demonstrated to be a viable alternative to an established method, which consists of acid digestion and Inductively coupled plasma-optical emission spectrometry (ICP-OES) to measure trace metals in sediment. The analysis of trace metal composition by both techniques on a NIST Standard Reference Material mud gives results that are consistent with the certified values for fourteen measured metals, seven of which are common to both methods. A comparison study conducted on a sediment core from a freshwater lake with a known chromium contamination in Muskegon County, MI also shows a good correlation between the methods for transition metals of environmental interest over a wide range of metal concentrations. Total sample preparation and analysis time for the PIXE measurements is roughly one third that of acid digestion and ICP-OES. Also, the acid digestion step does not elute all the metal, while the nondestructive PIXE approach is a total metals analysis method. However the PIXE method generally has higher limits of detection for many environmental metal contaminants. By combining the two techniques, the acid digestion elution factor can be quantified by running PIXE on an original sample and on the residue resulting from acid digestion.

  19. ICP OES and CV AAS in determination of mercury in an unusual fatal case of long-term exposure to elemental mercury in a teenager.

    PubMed

    Lech, Teresa

    2014-04-01

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

  20. Evaluation of inorganic elements in cat's claw teas using ICP OES and GF AAS.

    PubMed

    Pereira, João B; Dantas, Kelly G F

    2016-04-01

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

  1. Tandem Laser Induced Breakdown Spectroscopy (LIBS), Laser Ablation Inductively Coupled Plasma Mass Spectroscopy (LA-ICP-MS) and/or Laser Ablation Inductively Coupled Plasma Optical Emission Spectroscopy (LA-ICP-OES) for the analysis of samples of geological interest

    NASA Astrophysics Data System (ADS)

    Oropeza, D.

    2016-12-01

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

  2. Evaluation of calcium alginate beads for Ce, La and Nd preconcentration from groundwater prior to ICP OES analysis.

    PubMed

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

    2016-12-01

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

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

    PubMed

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

    2013-12-15

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

  4. [Study on the determination of 28 inorganic elements in sunflower seeds by ICP-OES/ICP-MS].

    PubMed

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

    2013-01-01

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

  5. Traceable phosphorus measurements by ICP-OES and HPLC for the quantitation of DNA.

    PubMed

    Holden, Marcia J; Rabb, Savelas A; Tewari, Yadu B; Winchester, Michael R

    2007-02-15

    Measurement of the phosphorus content of nucleotides and deoxyribonucleic acid (DNA) offers an approach to the quantitation of nucleic acids that is traceable to the SI. Such measurements can be an alternative to the commonly used spectroscopic tools that are not traceable. Phosphorus measurements of thymidine 5'-monophosphate (TMP) and acid-digested plasmid and genomic DNA preparations were made using high-performance inductively coupled plasma optical emission spectroscopy (HP-ICP-OES) and high-performance liquid chromatography (HPLC) and compared for bias and uncertainty. A prerequisite for quality measurement is the purity of the materials. Quantitation with the two platforms was comparable for the TMP. However, the HPLC values had larger uncertainties and were all statistically different from the gravimetric values at the 95% confidence level. When using ICP-OES, the digestion of the nucleotide monophosphate can be eliminated, thus simplifying the procedure. The differences between the results obtained by using the two platforms, when measuring genomic or plasmid DNA, were dependent on the mass fraction of the digest. ICP-OES measurement of phosphorus provides a highly accurate quantitation for both nucleotide monophosphates and DNA with expanded uncertainties of less than 0.1%. Currently, ICP-OES requires a significant sample size restricting its usefulness for the quantitation of DNA but represents a valuable tool for certification of reference materials. HPLC requires smaller amounts of material to perform the analysis but is less useful for certification of reference materials because of lower accuracy and 10-fold higher expanded uncertainties.

  6. In situ trapping of As, Sb and Se hydrides on nanometer-sized ceria-coated iron oxide-silica and slurry suspension introduction to ICP-OES.

    PubMed

    Dados, A; Kartsiouli, E; Chatzimitakos, Th; Papastephanou, C; Stalikas, C D

    2014-12-01

    A procedure is developed for the analysis of sub-μg L(-1) levels of arsenic, antimony and selenium after preconcentration of their hydrides. The study highlights the capability of an aqueous suspension of a nanometer-sized magnetic ceria, in the presence of iodide, to function as a sorbent for the in situ trapping and preconcentration of the hydrides of certain metalloids. After extraction, the material is magnetically separated from the trapping solution and analyzed. A slurry suspension sampling approach with inductively coupled plasma-optical emission spectrometry (ICP-OES) is employed for measurements, as the quantitative elution of the adsorbed metalloids is not feasible. The whole analytical procedure consists of five steps: (i) pre-reduction of As, Sb and Se, (ii) generation of the hydrides AsH3, SbH3 and SeH2, (iii) in situ collection in the trapping suspension of magnetic ceria, (iv) isolation of the particles by applying a magnetic field, and (v) measurement of As, Sb and Se concentrations using ICP-OES. Under the established experimental conditions, the efficiency of trapping accounted for 94 ± 2%, 89 ± 2% and 98 ± 3% for As, Sb and Se, respectively, signifying the effective implementation of the overall procedure. The applicability of the procedure has been demonstrated by analyzing tap and lake water and a reference material (soft drinking water). The obtained analytical figures of merit were satisfactory for the analysis of the above metalloids in natural waters by ICP-OES.

  7. [Analysis and Evaluation of Inorganic Elements in Euryale Semen from Different Habitats by Microwave Digestion-ICP-OES].

    PubMed

    Wang, Hong; Wu, Qi-nan; Wu, Cheng-ying; Fan, Xiu-he; Jiang, Zheng; Gu, Wei; Yue, Wei

    2015-01-01

    To establish a simple, rapid and efficient method for determination of different inorganic elements in Euryale Semen from different habitats. Inductively coupled plasma-optical emission spectrometry(ICP-OES) was applied to determine inorganic elements in Euryale Semen, and the results were analyzed by principal component analysis. Euryale Semen from different habitats contained the kind of inorganic elements ranging from 22 to 26, including micronutrient elements like Iron, Zinc, Selenium, Copper, Molybdenum, Chrome and Cobalt, as well as macronutrient elements such as Potassium, Calcium, Sodium, Magnesium and Phosphorus. Five factors were extracted and used to comprehensively evaluate Euryale Semen from 20 different habitats covered almost China. The comprehensive function was F = 0. 38828F1 + 0. 25603F2 + 0. 07617F3 + 0. 06860F4 + 0. 04868F5, which resulted in the top three samples coming from Jiangsu Gaoyou, Hunan Xiangxi and Jiangsu Suzhou respectively. The study indicates that ICP-OES is a quick, accurate and sensitive method to determine the contents of inorganic elements in Euryale Semen,which provides scientific and reliable reference for its quality control and safety assessment.

  8. Arsenic species separation by IELC-ICP/OES: Arsenocholine behavior

    SciTech Connect

    Rubio, R.; Peralta, I.; Alberti, J.; Rauret, G. )

    1993-01-01

    In the literature an increasing interest is observed in developing methods to determine arsenobetaine, arsenocholine and related compounds in sea food and in reference materials. The separation conditions and quantification of As(III), As(V), monomethylarsenate (MMA), dimethylarsinate (DMA), arsenobetaine (AsBet) and arsenocholine (AsChol) are studied by Liquid Chromatography (LC) coupled directly to an Inductively Coupled Plasma Optical Emission Spectroscopy (ICP/OES) system. The separation conditions are optimized to improve the resolution of the six arsenic species. Arsenocholine shows a particular pattern of behavior when phosphate is used as eluent: two peaks are observed in the chromatogram, thus a systematic study assaying different pH and concentration of phosphate is carried out to improve resolution and analysis time when the six arsenic compounds are analyzed in a mixture. Boric acid as mobile phase avoids the splitting of the arsenocholine peak and leads to a good separation of the six arsenic compounds. Detection limits are established for the six arsenic species.

  9. Determination of thorium by ICP-MS and ICP-OES.

    PubMed

    Holmes, L

    2001-01-01

    Natural thorium (232-Th) has traditionally been measured by radiometric techniques such as alpha and gamma spectrometry. However. with both ICP-OES and ICP-MS instruments becoming relatively common in many analytical laboratories. these techniques have become more acceptable in thorium analysis. This paper will briefly describe an overview of the instrumentation currently available and the techniques themselves applied to thorium analysis. Both techniques have low detection limits and require little sample treatment after the sample digestion. Routine sample analysis time is short and spectra easy to interpret. usually giving results with low uncertainties, Whereas ICP-OES measures total thorium only, ICP-MS also offers the potential to measure other long-lived thorium isotopes (t 1/2 > 10(4) years), such as 232Th. However, other important isotopes, such as 228Th. are still out of reach for routine analysis. The main disadvantage of the techniques is the requirement for a sample digestion stage.

  10. Trace element determination of Argentine wines using ETAAS and USN-ICP-OES.

    PubMed

    Lara, R; Cerutti, S; Salonia, J A; Olsina, R A; Martinez, L D

    2005-02-01

    The objective of this work was to develop a method to determine the metal content in wine samples from the province of Mendoza in Argentina. Ten samples of white wine and 10 samples of red wine available in the supermarket were analyzed for the metals aluminium, cadmium, calcium, chromium, copper, iron, nickel, lead and zinc by electrothermal atomic spectrometry (ETAAS) and ultrasonic nebulization was coupled to inductively coupled plasma optical emission spectrometry (USN-ICP-OES). The aluminium, cadmium, calcium, copper, iron, lead, zinc, chromium concentrations were between 17.0-18.0 microg l(-1), 1.0-4.7microg l(-1), 10.0-15.0 mg l(-1), 23.0-28.0 microg l(-1), 480-790 microg l(-1), 50-90 microg l(-1), 24-130 microg l(-1), and <0.2-6.25 microg l(-1), respectively. The levels compare well with those reported for similar wines from some other parts of the world. A significant aspect in this paper is the samples mineralization step, which allowed the direct determination of the metals. Concerning to the Cd determination, a refluxing digestion system was used for the pretreatment of the samples.

  11. Simplified multi-element analysis of ground and instant coffees by ICP-OES and FAAS.

    PubMed

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

    2015-01-01

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

  12. Determination of major and minor elements in the Malva sylvestris L. from Turkey using ICP-OES techniques.

    PubMed

    Hiçsönmez, U; Ereeş, F S; Ozdemir, C; Ozdemir, A; Cam, S

    2009-06-01

    In this work, Malva sylvestris var. mauritiana (L.) leaves were collected from different points in Muradiye region of Manisa-Turkey. The leaves were dissolved by wet digestion method using a mixture of mineral acid. Concentrations of Ag, Al, B, Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, K, La, Mg, Mn, Na, Ni, Pb, Sn, Sr, Sb, Si, Ti, U, Zn, and Zr in prepared solutions were determined by using inductively coupled plasma optical emission spectrometry (ICP-OES). High Ca (13,848 mg/kg) and Mg (1,936 mg/kg) concentrations were found at the leaves. Obtained values were compared with the internationally permitted (standard) values. The results of elements were analyzed statistically (analysis of variance test). For different leaf sizes, concentration factors were calculated.

  13. Inductively Coupled Plasma Optical Emission Spectrometry for Rare Earth Elements Analysis

    NASA Astrophysics Data System (ADS)

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

    2017-01-01

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

  14. Multielemental determinations in chocolate drink powder using multivariate optimization and ICP OES.

    PubMed

    Peixoto, Rafaella Regina Alves; Oliveira, Andrea; Cadore, Solange

    2012-08-22

    In this work multivariate experiments were conducted to optimize the operating conditions for inductively coupled plasma optical emission spectrometry (ICP OES) for multielemental determinations in chocolate drink powder. The operating conditions were investigated using a 2(3) central composite design, where the variables studied were radio frequency power, nebulization flow rate, and auxiliary argon flow rate. The effects of these parameters on plasma robustness and on signal to background ratio (SBR) were considered in parallel, allowing the evaluation of robustness and detectability using few and fast experiments to select the best conditions for the determination of the analytes. In this case, the proposed experiments were applied to the optimization of a method aimed at the determination of Al, Ba, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, P, Pb, V, and Zn in chocolate drink powder. The compromise conditions that allowed obtaining a robust and sensitive analytical method were radio frequency power of 1200 W, nebulization flow rate of 0.6 L/min, and auxiliary argon flow rate of 0.3 L/min. Using these conditions, recoveries between 95 and 105% and relative standard deviations lower than 5% were obtained for the majority of the analytes. The proposed method was successfully applied to the analysis of 15 samples of chocolate drink powder. The highest concentrations of metallic species were found in diet and light products.

  15. Focused microwave-induced combustion for digestion of botanical samples and metals determination by ICP OES and ICP-MS.

    PubMed

    Barin, J S; Pereira, J S F; Mello, P A; Knorr, C L; Moraes, D P; Mesko, M F; Nóbrega, J A; Korn, M G A; Flores, E M M

    2012-05-30

    The advantages and shortcomings of focused microwave-induced combustion (FMIC) for digestion of plant samples were studied. The effects of sample mass, absorbing solution, oxygen gas flow-rate, and time of reflux step on recoveries of major, minor and trace metals were systematically evaluated. Afterwards, Al, Ba, Ca, Co, Cr, Cu, Mg, Mn, Ni, Sr, V, and Zn were determined by inductively coupled plasma optical emission spectrometry (ICP OES) and by inductively coupled plasma mass spectrometry (ICP-MS). The main advantages of FMIC when compared to microwave-assisted wet digestion (MAWD) and focused-microwave-assisted wet digestion (FMAWD) are the possibility to digest larger masses of samples (up to 3g) using shorter heating times and diluted nitric acid solution for absorbing all analytes. Using the selected experimental conditions for FMIC, residual carbon content was lower than 0.7% for all samples and relative standard deviation (RSD) varied from 1.5 to 14.1%. Certified reference materials (NIST 1515 apple leaves and NIST 1547 peach leaves) were used for checking accuracy and determined values for all metals were in agreement with certified values at a 95% confidence level. No statistical difference (ANOVA, 95% of confidence level) was observed for results obtained by FMIC, FMAWD, and MAWD. Limits of detection were lower when using FMIC in the range of 0.02-0.15 μg g(-1) for ICP OES and 0.001-0.01 μg g(-1) for ICP-MS, which were about 3 and 6 times lower than the values obtained by FMAWD and MAWD, respectively. It is important to point out that FMIC was a suitable sample preparation method for major, minor and trace metals by both determination techniques (ICP OES and ICP-MS). Additionally, since it allows lower LODs (because up to 3g of sample can be digested) and diluted acid solutions are used (without any further dilution), the use of ICP-MS is not mandatory.

  16. Selected problems with boron determination in water treatment processes. Part I: comparison of the reference methods for ICP-MS and ICP-OES determinations.

    PubMed

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

    2016-06-01

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

  17. Application of ICP-OES for Evaluating Energy Extraction and Production Wastewater Discharge Impacts on Surface Waters in Western Pennsylvania

    EPA Science Inventory

    Oil and gas extraction and coal-fired electrical power generating stations produce wastewaters that are treated and discharged to rivers in Western Pennsylvania with public drinking water system (PDWS) intakes. Inductively coupled plasma optical emission spectroscopy (ICP-OES) w...

  18. Application of ICP-OES for Evaluating Energy Extraction and Production Wastewater Discharge Impacts on Surface Waters in Western Pennsylvania

    EPA Science Inventory

    Oil and gas extraction and coal-fired electrical power generating stations produce wastewaters that are treated and discharged to rivers in Western Pennsylvania with public drinking water system (PDWS) intakes. Inductively coupled plasma optical emission spectroscopy (ICP-OES) w...

  19. An Environmental Focus Using Inductively Coupled Plasma Optical Emission Spectrometry and Ion Chromatography

    NASA Astrophysics Data System (ADS)

    Salido, Arthur; Atterholt, Cynthia; Bacon, J. Roger; Butcher, David J.

    2003-01-01

    The Western Carolina University chemistry faculty have developed an environmental focus to their curriculum. Inductively coupled plasma-optical emission spectrometry (ICP-OES) and ion chromatography (IC) have been shown to be useful tools for the determination of elements and ions, respectively. Several novel experiments have been developed monitoring these analytes in environmental samples, including water, pressure-treated wood, and nutritional supplements. In addition, ICP-OES and IC have been used to teach seniors the principles of analytical method development. Lastly, this equipment has been employed extensively in a vigorous research program.

  20. The analysis of some evidential materials by inductively coupled plasma-optical emission spectrometry.

    PubMed

    Carpenter, R C

    1985-03-01

    Inductively coupled plasma-optical emission spectrometry (ICP-OES) is under evaluation at the Central Research Establishment for the analysis of evidential materials. The analysis of standard reference materials has demonstrated that quantitative multi-element data can be obtained from small samples of a variety of materials. The results of some determinations carried out in support of casework investigations are reported.

  1. [Determination of metal elements in PM2. 5 by ICP-OES with microwave digestion].

    PubMed

    Zhang, Liu-Yi; Fu, Chuan; Yang, Fu-Mo; Yang, Ji-Dong; Huang, Yi-Min; Zhang, Qiang; Wu, Bing-Yu

    2014-11-01

    In the present work, a method was developed for determining lead, zinc, copper, cadmium, znd chromium in PM2. 5 by inductively coupled plasma-optical emission spectrometry (ICP-OES) analysis with microwave digestion and glass fibre filter collection of samples. The microwave digestion systems were investigated and the experimental conditions were optimized. The results show that (1) HNO3-H2O02 digestion system is more stable and complete than HNO3-HCl and HNO3-H2 SO4 digestion systems; (2) The most sensitive emission wave length of lead, zinc, copper, cadmium, and chromium are 220.353, 213.857, 327.393, 228.802, and 267.716 nm, respectively; (3) The highest signal-to-noise ratios were observed under the conditions: RF power of 1 300 W, peristaltic pump flow rate of 1.5 mL x min(-1), cooling gas flow rate of 15 L x min(-1), and carrier gas flow rate of 0.8 L x min(-1). In addition, the detection limit for these elements ranged between 2.02 x 10(-3) and 8.20 x 10(-3(μg x mL(-1), the relative standard deviations (RSD, n = 6) for the samples were in the range of 1.86%-2.82%, and the recovery for the elements determined was from 91.6% to 103.7%. The proposed method was used for determination of the above five elements in atmospheric fine particulate matter at Wanzhou Monitoring Site of Chongqing Institute of Green and Intelligent Technology. The results revealed that the atmospheric fine particulate matter at this monitoring site was not polluted by cadmium and chromium, lead was at the level of potential contamination, while zinc and copper were at the level of slight pollution.

  2. Challenges in the quality assurance of elemental and isotopic analyses in the nuclear domain benefitting from high resolution ICP-OES and sector field ICP-MS.

    PubMed

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

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

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

    PubMed

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

    2014-11-01

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

  4. Using ICP-OES and SEM-EDX in biosorption studies

    PubMed Central

    Chojnacka, Katarzyna; Marycz, Krzysztof

    2010-01-01

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

  5. Using ICP-OES and SEM-EDX in biosorption studies.

    PubMed

    Michalak, Izabela; Chojnacka, Katarzyna; Marycz, Krzysztof

    2011-02-01

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

  6. [Determination of high concentrations of rubidium chloride by ICP-OES].

    PubMed

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

    2015-01-01

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

  7. [Determination of 22 inorganic elements in different parts of Lantana camara by ICP-OES].

    PubMed

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

    2014-10-01

    To determine the contents of 22 inorganic elements in different parts of Lantana camara by inductively coupled plasma optical emission spectroscopy (ICP-OES). HNO3-H2O2 digested system was used to completely decompose the organic compounds effectually by microwave digestion. The 22 inorganic elements such as K, Ca, Mg, Fe, Al, Na, Zn, Mn and Cr were determined by ICP-OES under set up working conditions. The contents of K, Ca and Mg were the most in different parts of Lantana camara; The contents of K, Ca, Mg, Mn, Sr and Cu in the leaf were more those that in the root and branch; The contents of Fe, Na, Cr and Ni in the root were more than those in the leaf and branch; The contents of Mn, Zn, Sr and Cu in the branch were more than those in the root and the leaf; The contents of Pb and Cd were higher than the national standard and Cr had high content in different parts of Lantana camara. The determination method is quick, easy and accurate with high sensitivity, which can determine the contents of 22 inorganic elements accurately in different parts of Lantana camara.

  8. [Simultaneous Determination of Sn and S in Methyltin Mercaptide by Microwave-Assisted Acid Digestion and ICP-OES].

    PubMed

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

    2015-09-01

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

  9. [Determination and principal component analysis of mineral elements based on ICP-OES in Nitraria roborowskii fruits from different regions].

    PubMed

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

    2017-06-01

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

  10. ICP-OES and Micronucleus Test to Evaluate Heavy Metal Contamination in Commercially Available Brazilian Herbal Teas.

    PubMed

    Schunk, Priscila Francisca Tschaen; Kalil, Ieda Carneiro; Pimentel-Schmitt, Elisangela Flavia; Lenz, Dominik; de Andrade, Tadeu Uggere; Ribeiro, Juliano Souza; Endringer, Denise Coutinho

    2016-07-01

    Increased tea consumption in combination with intensive pesticide use is generating heavy metal contaminations amongst Brazilian tea consumers, causing health concerns. Inductively coupled plasma optical emission spectrometry (ICP-OES) was applied to quantify minerals and heavy metals such as aluminum, barium, cadmium, lead, cobalt, copper, chromium, tin, manganese, molybdenum, nickel, selenium, silver, thallium, vanadium and zinc in Brazilian chamomile, lemongrass, fennel and yerba mate teas. Teas, purchased in local supermarkets, were prepared using infusion and acid digestion. Higher concentrations of Al were present in all samples. In the digested samples, the Al mean concentration was 2.41 μg g(-1) (sd = 0.72) for fennel and 33.42 μg g(-1) (sd = 17.18) for chamomile, whilst the sample C for chamomile tea presented the highest concentration with 51.62 μg g(-1) (sd = 9.17). The safety relation in decreasing order is fennel, lemongrass, chamomile and yerba mate. Chemometric analyses demonstrated a strong correlation between the elements Cd and Pb in the samples. Yerba mate had the highest amount of metal (100 mg kg(-1)), being the subject of a micronucleus test assay for cytotoxicity. The metals found in Yerba mate did not present cytotoxicity/mutagenicity using the micronucleus test. The inorganic contaminants in teas should have their impact carefully monitored.

  11. Development and validation of an ICP-OES method for quantitation of elemental impurities in tablets according to coming US pharmacopeia chapters.

    PubMed

    Støving, Celina; Jensen, Henrik; Gammelgaard, Bente; Stürup, Stefan

    2013-10-01

    May 1, 2014 the United States Pharmacopeia (USP) will implement two new chapters stating limit concentrations of elemental impurities in pharmaceuticals applying inductively coupled plasma methods. In the present work an inductively coupled plasma optical emission spectrometry (ICP-OES) method for quantitation of As, Cd, Cu, Cr, Fe, Hg, Ir, Mn, Mo, Ni, Os, Pb, Pd, Pt, Rh, Ru, V and Zn in tablets according to the new USP chapters was developed. Sample preparation was performed by microwave-assisted acid digestion using a mixture of 65% HNO3 and 37% HCl (3:1, v/v). Limits of detection and quantitation were at least a factor of ten below the USP limit concentrations showing that the ICP-OES technique is well suited for quantitation of elemental impurities. Excluding Os, spike recoveries in the range of 85.3-103.8% were obtained with relative standard deviations (%RSD) ranging from 1.3 to 3.2%. Due to memory effects the spike recovery and %RSD of Os were 161.5% and 13.7%, respectively, thus the method will need further development with respect to elimination of the memory effect of Os. The method was proven to be specific but with potential spectral interference for Ir, Os, Pb, Pt and Rh necessitating visual examination of the spectra. Hg memory effect was handled by using lower spike levels combined with rinsing with 0.1M HCl. The tablets had a content of Fe and Pt of 182.8 ± 18.1 and 2.8 ± 0.2 μg/g, respectively and did therefore not exceed the limit concentration defined by USP. It is suggested that the developed method is applicable to pharmaceutical products with a composition and maximal amount of daily intake (g drug product/day) similar to the tablets used in this work. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Microwave-assisted ultraviolet digestion of petroleum coke for the simultaneous determination of nickel, vanadium and sulfur by ICP-OES.

    PubMed

    Oliveira, Jussiane S S; Picoloto, Rochele S; Bizzi, Cezar A; Mello, Paola A; Barin, Juliano S; Flores, Erico M M

    2015-11-01

    A method for the simultaneous determination of Ni, V and S in petroleum coke by inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave-assisted ultraviolet digestion (MW-UV) in closed vessels was proposed. Digestion was performed using electrodeless discharge lamps positioned inside quartz vessels and turned on by microwave radiation. The following parameters were evaluated: HNO3 concentration (15 mL of 1, 4, 7, 10 or 14.4 mol L(-1)), volume of H2O2 (30%, 1 or 3 mL), sample mass (100, 250 or 500 mg) and heating time (40 or 60 min) with or without the use of UV lamps. Digestion efficiency was evaluated by the determination of the residual carbon content (RCC) in digests. Using UV lamps lower RCC was obtained and the combination of 4 mol L(-1) HNO3 with 3 mL of H2O2 and 60 min of heating allowed a suitable digestion of up to 500 mg of petroleum coke (RCC< 21%). The agreement with the reference values for Ni, V and S (obtained by digestion of petroleum coke by microwave-induced combustion) and with a certified reference material of petroleum coke was between 96 and 101%. The proposed method was considered as advantageous when compared to American Society for Testing and Materials method because it allowed the simultaneous determination of Ni, V and S with lower limit of detection (0.22, 0.12 and 8.7 µg g(-1) for Ni, V and S, respectively) avoiding the use of concentrated nitric acid and providing digests suitable for routine analysis by ICP-OES.

  13. ICP/OES application for assessing cadmium uptake (or toxicity) in glomerular cells: influence of extracellular calcium.

    PubMed

    Ohayon-Courtès, Céline; Passagne, Isabelle; De Portal, Caroline; Pouvreau, Carole; Cambar, Jean; L'Azou, Béatrice

    2007-05-01

    The risks of metals for health are highlighted by their chemical stability and their persistence in the environment. Chronic exposure to low cadmium (Cd) concentrations results in renal dysfunction mainly. Cd has been regarded primarily as a renal tubular toxicant, but glomerular structures may also be affected. Since the cellular environment may influence metal toxicity, differences concerning Cd uptake and toxicity were evaluated according to calcium (Ca) medium concentrations. An optimized inductively coupled plasma emission spectrometry method (ICP/OES) was developed under defined conditions, as a selective analytical tool to determine cadmium uptake in glomerular mesangial cells. The performance characteristics of the analytical system were evaluated for both Cd and Ca by calibration (50 to 250 microg/L and 1 to 5 mg/L), linearity (r2 .9968 and .9943), limits of detection (1 microg/L and 0.1 mg/L) and quantitation (3 microg/L and 0.3 mg/L), accuracy with spiking, and repeatability (1.2 and 2.9%) with matrix matched standards. Total intracellular Cd content was significantly threefold lower in 0.175 mM Ca medium (Ca-free Eagle's minimum essential medium [EMEM] medium with 5% fetal bovine serum [FBS]) than in EMEM medium (1.8 mM Ca) with respectively 0.16 and 0.37 microg/mg proteins after 24 h of Cd (1 microM) exposure. Similar differences were obtained in cytotoxicity studies with a fourfold reduction in the mortality index (IC50). Complementary assays using Ca-spiked medium reinforced that Cd cytotoxicity and uptake were significantly dependent on the concentration of extracellular Ca. These findings suggest direct link between Cd uptake and toxicity, underlining the relevance of the analytical method.

  14. Application of ICP-OES to the determination of barium in blood and urine in clinical and forensic analysis.

    PubMed

    Lech, Teresa

    2013-05-01

    Exposure to barium (Ba) mostly occurs in the workplace or from drinking water, but it may sometimes be due to accidental or intentional intoxication. This paper presents a reliable, sensitive method for the determination of Ba in blood and urine: inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave digestion of samples. The overall procedure was checked using Seronorm Whole Blood L-2, Trace Elements Urine and spiked blood and urine samples (0.5-10 µg/mL of Ba). The accuracy of the whole procedure (relative error) was 4% (blood) and 7% (urine); the recovery was 76-104% (blood) and 85-101% (urine). The limits of detection and quantification (Ba λ = 455.403 nm) were 0.11 and 0.4 µg/L of Ba, respectively; precision (relative standard deviation) was below 6% at the level of 15 µg/L of Ba for blood. This method was applied to a case of the poisoning of a man who had been exposed at the workplace for over two years to powdered BaCO3, and who suffered from paralysis and heart disorders. The concentrations of Ba, in μg/L, were 160 (blood), 460 (serum) and 1,458 (urine) upon his admission to the hospital, and 6.1 (blood) and 4.9 (urine) after 11 months (reference values: 3.34 ± 2.20 µg/L of Ba for blood and 4.43 ± 4.60 µg/L of Ba for urine).

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

    USGS Publications Warehouse

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

    2014-01-01

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

  16. Online elemental analysis of process gases with ICP-OES: A case study on waste wood combustion

    SciTech Connect

    Wellinger, Marco; Wochele, Joerg; Biollaz, Serge M.A.; Ludwig, Christian

    2012-10-15

    Highlights: Black-Right-Pointing-Pointer Simultaneous measurements of 23 elements in process gases of a waste wood combustor. Black-Right-Pointing-Pointer Mobile ICP spectrometer allows measurements of high quality at industrial plants. Black-Right-Pointing-Pointer Continuous online measurements with high temporal resolution. Black-Right-Pointing-Pointer Linear correlations among element concentrations in the raw flue gas were detected. Black-Right-Pointing-Pointer Novel sampling and calibration methods for ICP-OES analysis of process gases. - Abstract: A mobile sampling and measurement system for the analysis of gaseous and liquid samples in the field was developed. An inductively coupled plasma optical emission spectrometer (ICP-OES), which is built into a van, was used as detector. The analytical system was calibrated with liquid and/or gaseous standards. It was shown that identical mass flows of either gaseous or liquid standards resulted in identical ICP-OES signal intensities. In a field measurement campaign trace and minor elements in the raw flue gas of a waste wood combustor were monitored. Sampling was performed with a highly transport efficient liquid quench system, which allowed to observe temporal variations in the elemental process gas composition. After a change in feedstock an immediate change of the element concentrations in the flue gas was detected. A comparison of the average element concentrations during the combustion of the two feedstocks showed a high reproducibility for matrix elements that are expected to be present in similar concentrations. On the other hand elements that showed strong differences in their concentration in the feedstock were also represented by a higher concentration in the flue gas. Following the temporal variations of different elements revealed strong correlations between a number of elements, such as chlorine with sodium, potassium and zinc, as well as arsenic with lead, and calcium with strontium.

  17. Application of ICP-OES for evaluating energy extraction and production wastewater discharge impacts on surface waters in Western Pennsylvania.

    PubMed

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

    2015-10-01

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

  18. [Development of ICP-OES, ICP-MS and GF-AAS Methods for Simultaneous Quantification of Lead, Total Arsenic and Cadmium in Soft Drinks].

    PubMed

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

    2015-01-01

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

  19. [Study on microwave digestion of coal for the determination of multi-element by ICP-OES and ICP-MS].

    PubMed

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

    2012-06-01

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

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

    PubMed

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

    2014-04-01

    We prepared genomic DNA from human placenta, Escherichia coli, and Bacillus subtilis using various DNA extraction methods and quantified the genomic DNA using ultraviolet (UV) spectrophotometry, capillary electrophoresis (CE), and inductively coupled plasma optical emission spectrometry (ICP-OES). Application of ICP-OES unexpectedly led to a serious overestimation of phosphorus in B. subtilis genomic DNA prepared using cetyltrimethyl ammonium bromide (CTAB). Further investigations using reversed-phase high-performance liquid chromatography (RP-HPLC), ultra-performance liquid chromatography electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS), and (31)P nuclear magnetic resonance (NMR) identified the phosphorus impurity as lipoteichoic acid (LTA). Copyright © 2014 Elsevier Inc. All rights reserved.

  1. Comparison of extraction induced by emulsion breaking, ultrasonic extraction and wet digestion procedures for determination of metals in edible oil samples in Turkey using ICP-OES.

    PubMed

    Bakircioglu, Dilek; Kurtulus, Yasemin Bakircioglu; Yurtsever, Selcuk

    2013-06-01

    The content of elements (Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn) in edible oils (sunflower, hazelnut, canola, corn and olive oils) from Turkey was determined using inductively coupled plasma optical emission spectrometry (ICP-OES) after ultrasonic extraction, wet digestion, and extraction induced by emulsion breaking procedures (EIEB). In order to evaluate the best sample preparation procedure, EIEB procedure was compared by ultrasonic extraction and wet digestion procedures. The results in the samples (minimum-maximum in mgkg(-1)) were : 0.022-0.058, Cr 0.126-7.106, Cu 0.570-4.504, Fe 8.004-12.588, Mn 0.035-0.054, Ni 0.908-2.182, Pb 0.099-0.134 and Zn 2.206-8.982. The EIEB procedure was found to be fast, reliable, simple, and excellent in comparison with the other studied procedures. The recovery test was performed by spiking the samples with known amounts of the metals in the form of organometallic standards and applying the EIEB procedure. The recoveries were in the range of 96-109%. Copyright © 2012 Elsevier Ltd. All rights reserved.

  2. Assessment of status of three water bodies in Serbia based on tissue metal and metalloid concentration (ICP-OES) and genotoxicity (comet assay).

    PubMed

    Sunjog, Karolina; Kolarević, Stoimir; Kračun-Kolarević, Margareta; Višnjić-Jeftić, Željka; Skorić, Stefan; Gačić, Zoran; Lenhardt, Mirjana; Vasić, Nebojša; Vuković-Gačić, Branka

    2016-06-01

    Metals and metalloids are natural components of the biosphere, which are not produced per se by human beings, but whose form and distribution can be affected by human activities. Like all substances, they are a contaminant if present in excess compared to background levels and/or in a form that would not normally occur in the environment. Samples of liver, gills, gonads and muscle from European chub, Squalius cephalus, were analyzed for Al, As, B, Ba, Cr, Cu, Fe, Hg, Mn, Mo, Sr and Zn using inductively coupled plasma optical emission spectrometry (ICP-OES) to highlight the importance of tissue selection in monitoring research. The comet assay or single cell gel electrophoresis (SCGE) was selected as an in vivo genotoxicity assay, a rapid and sensitive method for measuring genotoxic effects in blood, liver and gills of the European chub. Microscopic images of comets were scored using Comet IV Computer Software (Perceptive Instruments, UK). The objective of our study was to investigate two reservoirs, Zlatar and Garasi, and one river, Pestan by: (i) determining and comparing metal and metalloid concentrations in sediment, water and tissues of European chub: liver, gills, muscle and gonads (ii) comparing these findings with genotoxicity of water expressed through DNA damage of fish tissues. A clear link between the level of metals in water, sediment and tissues and between metal and genotoxicity levels at examined sites was not found. This suggests that other xenobiotics (possibly the organic compounds), contribute to DNA damage.

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

    PubMed

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

    2013-07-01

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

  4. Microwave-assisted wet digestion with H2O2 at high temperature and pressure using single reaction chamber for elemental determination in milk powder by ICP-OES and ICP-MS.

    PubMed

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

    2016-08-15

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

  5. Determination of trace impurities in boron nitride by graphite furnace atomic absorption spectrometry and electrothermal vaporization inductively coupled plasma optical emission spectrometry using solid sampling

    NASA Astrophysics Data System (ADS)

    Barth, P.; Hassler, J.; Kudrik, I.; Krivan, V.

    2007-09-01

    Two digestion-free methods for trace analysis of boron nitride based on graphite furnace atomic absorption spectrometry (GFAAS) and electrothermal vaporization inductively coupled plasma spectrometry optical emission (ETV-ICP-OES) using direct solid sampling have been developed and applied to the determination of Al, Ca, Cr, Cu, Fe, Mg, Mn, Si, Ti and Zr in four boron nitride materials in concentration intervals of 1-23, 54-735, 0.05-21, 0.005-1.3, 1.6-112, 4.5-20, 0.03-1.8, 6-46, 38-170 and 0.4-2.3 μg g - 1 , respectively. At optimized experimental conditions, with both methods, effective in-situ analyte/matrix separation was achieved and calibration could be performed using calibration curves measured with aqueous standard solutions. In solid sampling GFAAS, before sampling, the platform was covered with graphite powder and, for determination of Si, also the Pd/Mg(NO 3) 2 modifier was used. In the determination of all analyte elements by solid sampling ETV-ICP-OES, Freon R12 was added to argon carrier gas. For solid sampling GFAAS and ETV-ICP-OES, the achievable limits of detection were within 5 (Cu)-130 (Si) ng g - 1 and 8 (Cu)-200 (Si) ng g - 1 , respectively. The results obtained by these two methods for four boron nitride materials of different purity grades are compared each with the other and with those obtained in analysis of digests by ICP-OES. The performance of the two solid sampling methods is compared and discussed.

  6. Method development for the determination of manganese, cobalt and copper in green coffee comparing direct solid sampling electrothermal atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry.

    PubMed

    Oleszczuk, Nédio; Castro, Jacira T; da Silva, Márcia M; Korn, Maria das Graças A; Welz, Bernhard; Vale, Maria Goreti R

    2007-10-31

    A method has been developed for the determination of cobalt, copper and manganese in green coffee using direct solid sampling electrothermal atomic absorption spectrometry (SS-ET AAS). The motivation for the study was that only a few elements might be suitable to determine the origin of green coffee so that the multi-element techniques usually applied for this purpose might not be necessary. The three elements have been chosen as test elements as they were found to be significant in previous investigations. A number of botanical certified reference materials (CRM) and pre-analyzed samples of green coffee have been used for method validation, and inductively coupled plasma optical emission spectrometry (ICP OES) after microwave-assisted acid digestion of the samples as reference method. Calibration against aqueous standards could be used for the determination of Mn and Co by SS-ET AAS, but calibration against solid CRM was necessary for the determination of Cu. No significant difference was found between the results obtained with the proposed method and certified or independently determined values. The limits of detection for Mn, Cu and Co were 0.012, 0.006 and 0.004mugg(-1) using SS-ET AAS and 0.015, 0.13 and 0.10mugg(-1) using ICP OES. Seven samples of Brazilian green coffee have been analyzed, and there was no significant difference between the values obtained with SS-ET AAS and ICP OES for Mn and Cu. ICP OES could not be used as a reference method for Co, as essentially all values were below the limit of quantification of this technique.

  7. Certification of beryllium mass fraction in SRM 1877 Beryllium Oxide Powder using high-performance inductively coupled plasma optical emission spectrometry with exact matching.

    PubMed

    Winchester, Michael R; Turk, Gregory C; Butler, Therese A; Oatts, Thomas J; Coleman, Charles; Nadratowski, Donald; Sud, Ritu; Hoover, Mark D; Stefaniak, Aleksandr B

    2009-03-15

    High-performance inductively coupled plasma optical emission spectrometry (HP-ICP-OES) was used to certify the Be mass fraction in National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) 1877 Beryllium Oxide Powder. The certified value and expanded uncertainty expressed at a 95% confidence level is (0.3576 +/- 0.0024) g/g. To obtain best results, the Be mass fractions, Mn (internal standard) mass fractions, and matrix compositions of the calibration solutions were carefully matched to those of the sample solutions for each individual HP-ICP-OES analysis. This "exact matching" approach was used because experience at NIST has shown that it often affords improved accuracy and precision in HP-ICP-OES analysis. NIST has never published these observations. Due to the toxicity of BeO and the difficulty of containing the very fine powder material, sets of solutions for HP-ICP-OES analysis were prepared by laboratories collaborating with NIST who have the experience and equipment needed to work with the material safely. Each laboratory utilized a unique digestion protocol(s). After preparing the sets of solutions, the collaborating laboratories shipped them to NIST for HP-ICP-OES analysis. NIST provided the collaborating laboratories with solution preparation kits and spreadsheets to help establish traceability of the HP-ICP-OES results to the International System of Units (SI) and to allow exact matching to be accomplished. The agreement observed among the four individual Be mass fraction values determined from the sets of solutions prepared by the collaborating laboratories was 0.074% relative (1s of mean). The excellent agreement provides a measure of confidence in the robustness of each of the digestion procedures, as well as in the certified Be mass fraction value. The analytical benefits of using exact matching for this particular certification were investigated. Results show that exactly matching the matrix compositions of the

  8. Multielement trace determination in SiC powders: assessment of interlaboratory comparisons aimed at the validation and standardization of analytical procedures with direct solid sampling based on ETV ICP OES and DC arc OES.

    PubMed

    Matschat, Ralf; Hassler, Jürgen; Traub, Heike; Dette, Angelika

    2005-12-01

    The members of the committee NMP 264 "Chemical analysis of non-oxidic raw and basic materials" of the German Standards Institute (DIN) have organized two interlaboratory comparisons for multielement determination of trace elements in silicon carbide (SiC) powders via direct solid sampling methods. One of the interlaboratory comparisons was based on the application of inductively coupled plasma optical emission spectrometry with electrothermal vaporization (ETV ICP OES), and the other on the application of optical emission spectrometry with direct current arc (DC arc OES). The interlaboratory comparisons were organized and performed in the framework of the development of two standards related to "the determination of mass fractions of metallic impurities in powders and grain sizes of ceramic raw and basic materials" by both methods. SiC powders were used as typical examples of this category of material. The aim of the interlaboratory comparisons was to determine the repeatability and reproducibility of both analytical methods to be standardized. This was an important contribution to the practical applicability of both draft standards. Eight laboratories participated in the interlaboratory comparison with ETV ICP OES and nine in the interlaboratory comparison with DC arc OES. Ten analytes were investigated by ETV ICP OES and eleven by DC arc OES. Six different SiC powders were used for the calibration. The mass fractions of their relevant trace elements were determined after wet chemical digestion. All participants followed the analytical requirements described in the draft standards. In the calculation process, three of the calibration materials were used successively as analytical samples. This was managed in the following manner: the material that had just been used as the analytical sample was excluded from the calibration, so the five other materials were used to establish the calibration plot. The results from the interlaboratory comparisons were summarized and

  9. Application of ICP-OES to the determination of CuIn(1-x)Ga(x)Se2 thin films used as absorber materials in solar cell devices.

    PubMed

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

    2005-05-01

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

  10. Nanometer-sized ceria-coated silica-iron oxide for the reagentless microextraction/preconcentration of heavy metals in environmental and biological samples followed by slurry introduction to ICP-OES.

    PubMed

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

    2014-04-01

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

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

    NASA Astrophysics Data System (ADS)

    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.

  12. Selective determination of gold(III) ion using CuO microsheets as a solid phase adsorbent prior by ICP-OES measurement.

    PubMed

    Rahman, Mohammed M; Khan, Sher Bahadar; Marwani, Hadi M; Asiri, Abdullah M; Alamry, Khalid A; Al-Youbi, Abdulrahman O

    2013-01-30

    We have prepared calcined CuO microsheets (MSs) by a wet-chemical process using reducing agents in alkaline medium and characterized by UV/vis., fourier transform infrared (FT-IR) spectroscopy, powder X-ray diffraction (XRD), and field-emission scanning electron microscopy (FESEM) etc. The detailed structural, compositional, and optical characterizations of the MSs were evaluated by XRD pattern, FT-IR, X-ray photoelectron spectroscopy (XPS), and UV-vis spectroscopy, respectively which confirmed that the obtained MSs are well-crystalline CuO and possessed good optical properties. The CuO MSs morphology was investigated by FESEM, which confirmed that the calcined nanomaterials were sheet-shaped and grown in large-quantity. Here, the efficiency of the CuO MS was applied for a selective adsorption of gold(III) ion prior to its detection by inductively coupled plasma-optical emission spectrometry (ICP-OES). The selectivity of CuO MSs towards various metal ions, including Au(III), Cd(II), Co(II), Cr(III), Fe(III), Pd(II), and Zn(II) was analyzed. Based on the adsorption isotherm study, it was confirmed that the selectivity of MSs phase was mostly towards Au(III) ion. The static adsorption capacity for Au(III) was calculated to be 57.0 mg g(-1). From Langmuir adsorption isotherm, it was confirmed that the adsorption process was mainly monolayer-adsorption onto a surface containing a finite number of adsorption sites.

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

    PubMed

    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.

  14. Selective Divalent Cobalt Ions Detection Using Ag2O3-ZnO Nanocones by ICP-OES Method for Environmental Remediation

    PubMed Central

    Rahman, Mohammed M.; Khan, Sher Bahadar; Marwani, Hadi M.; Asiri, Abdullah M.

    2014-01-01

    Here, we have synthesized Ag2O3-ZnO nanocones (NCs) by a wet-chemical route using reducing agents at low temperature. The structural, optical and morphological properties of Ag2O3-ZnO NCs were investigated by several conventional techniques such as powder XRD, XPS, FESEM, XEDS, FTIR and UV/vis. spectroscopy. The analytical parameters of prepared NCs were also calculated for a selective detection of divalent cobalt [Co(II)] prior to its determination by inductively coupled plasma-optical emission spectrometry (ICP-OES). The selectivity of NCs toward various metal ions, including Cd(II), Co(II), Cr(III), Cu(II), Fe(III), Ni(II), and Zn(II) was studied. Results of the selectivity study demonstrated that Ag2O3-ZnO NC phase was the most selective towards Co(II) ion. The uptake capacity for Co(II) ion was experimentally calculated to be ∼76.69 mgg−1. Moreover, adsorption isotherm data provided that the adsorption process was mainly monolayer on homogeneous adsorbent surfaces of Ag2O3-ZnO NCs. Kinetic study revealed that the adsorption of Co(II) on Ag2O3-ZnO NCs phase followed the pseudo-second-order kinetic model. In addition, thermodynamic results provided that the adsorption mechanism of Co(II) ions on Ag2O3-ZnO NCs was a spontaneous process and thermodynamically favorable. Finally, the proposed method was validated by applying it to real environmental water samples with reasonable results. PMID:25464507

  15. Simultaneous determination of trace rare-earth elements in simulated water samples using ICP-OES with TODGA extraction/back-extraction.

    PubMed

    Li, FuKai; Gong, AiJun; Qiu, LiNa; Zhang, WeiWei; Li, JingRui; Liu, Yu; Liu, YuNing; Yuan, HuiTing

    2017-01-01

    The determination of trace rare-earth elements (REEs) can be used for the assessment of environmental pollution, and is of great significance to the study of toxicity and toxicology in animals and plants. N, N, N', N'-tetraoctyl diglycolamide (TODGA) is an environmental friendly extractant that is highly selective to REEs. In this study, an analytical method was developed for the simultaneous determination of 16 trace REEs in simulated water samples by inductively coupled plasma optical emission spectroscopy (ICP-OES). With this method, TODGA was used as the extractant to perform the liquid-liquid extraction (LLE) sample pretreatment procedure. All 16 REEs were extracted from a 3 M nitric acid medium into an organic phase by a 0.025 M TODGA petroleum ether solution. A 0.03 M ethylenediaminetetraacetic acid disodium salt (EDTA) solution was used for back-extraction to strip the REEs from the organic phase into the aqueous phase. The aqueous phase was concentrated using a vacuum rotary evaporator and the concentration of the 16 REEs was detected by ICP-OES. Under the optimum experimental conditions, the limits of detection (3σ, n = 7) for the REEs ranged from 0.0405 ng mL-1 (Nd) to 0.5038 ng mL-1 (Ho). The relative standard deviations (c = 100 ng mL-1, n = 7) were from 0.5% (Eu) to 4.0% (Tm) with a linear range of 4-1000 ng mL-1 (R2 > 0.999). The recoveries of 16 REEs ranged from 95% to 106%. The LLE-ICP-OES method established in this study has the advantages of simple operation, low detection limits, fast analysis speed and the ability to simultaneously determine 16 REEs, thereby acting as a viable alternative for the simultaneous detection of trace amounts of REEs in water samples.

  16. Comparision of ICP-OES and MP-AES in determing soil nutrients by Mechlich3 method

    NASA Astrophysics Data System (ADS)

    Tonutare, Tonu; Penu, Priit; Krebstein, Kadri; Rodima, Ako; Kolli, Raimo; Shanskiy, Merrit

    2014-05-01

    Accurate, routine testing of nutrients in soil samples is critical to understanding soil potential fertility. There are different factors which must be taken into account selecting the best analytical technique for soil laboratory analysis. Several techniques can provide adequate detection range for same analytical subject. In similar cases the choise of technique will depend on factors such as sample throughput, required infrastructure, ease of use, used chemicals and need for gas supply and operating costs. Mehlich 3 extraction method is widely used for the determination of the plant available nutrient elements contents in agricultural soils. For determination of Ca, K, and Mg from soil extract depending of laboratory ICP and AAS techniques are used, also flame photometry for K in some laboratories. For the determination of extracted P is used ICP or Vis spectrometry. The excellent sensitivity and wide working range for all extracted elements make ICP a nearly ideal method, so long as the sample throughput is big enough to justify the initial capital outlay. Other advantage of ICP techniques is the multiplex character (simultaneous acquisition of all wavelengths). Depending on element the detection limits are in range 0.1 - 1000 μg/L. For smaller laboratories with low sample throughput requirements the use of AAS is more common. Flame AAS is a fast, relatively cheap and easy technique for analysis of elements. The disadvantages of the method is single element analysis and use of flammable gas, like C2H2 and oxidation gas N2O for some elements. Detection limits of elements for AAS lays from 1 to 1000 μg/L. MP-AES offers a unique alternative to both, AAS and ICP-OES techniques with its detection power, speed of analysis. MP-AES is quite new, simple and relatively inexpensive multielemental technique, which is use self-sustained atmospheric pressure microwave plasma (MP) using nitrogen gas generated by nitrogen generator. Therefore not needs for argon and

  17. Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Elements in Whole-Water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry

    USGS Publications Warehouse

    Garbarino, John R.; Struzeski, Tedmund M.

    1998-01-01

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

  18. High precision measurement of silicon in naphthas by ICP-OES using isooctane as diluent.

    PubMed

    Gazulla, M F; Rodrigo, M; Orduña, M; Ventura, M J; Andreu, C

    2017-03-01

    An analytical protocol for the accurate and precise determination of Si in naphthas is presented by using ICP-OES, optimizing from the sample preparation to the measurement conditions, in order to be able to analyze for the first time silicon contents below 100µgkg(-1) in a relatively short time thus being used as a control method. In the petrochemical industry, silicon can be present as a contaminant in different petroleum products such as gasoline, ethanol, or naphthas, forming different silicon compounds during the treatment of these products that are irreversibly adsorbed onto catalyst surfaces decreasing its time life. The complex nature of the organic naphtha sample together with the low detection limits needed make the analysis of silicon quite difficult. The aim of this work is to optimize the measurement of silicon in naphthas by ICP-OES introducing as an improvement the use of isooctane as diluent. The set up was carried out by optimizing the measurement conditions (power, nebulizer flow, pump rate, read time, and viewing mode) and the sample preparation (type of diluent, cleaning process, blanks, and studying various dilution ratios depending on the sample characteristics). Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Studying the evaporation behavior of heavy metals by thermo-desorption spectrometry.

    PubMed

    Ludwig, C; Lutz, H; Wochele, J; Stucki, S

    2001-12-01

    "Thermal desorption experiments" were carried out during which heavy metal evaporation was studied by on-line monitoring. This could be achieved by the use of a tubular furnace connected to a heavy metal detector, i.e. an ICP-OES (inductively coupled plasma optical emission spectrometer), by a specially designed and patented interface. The spectrograms typically had a time resolution of four different elements per minute using a conventional (sequentially operating) ICP-OES. This study shows how thermo-desorption spectrometry (TDS) can be applied to study the evaporation of high boiling substances, such as heavy metal and alkali metal compounds. The future scope of the method is discussed.

  20. High-Resolution Inductively Coupled Plasma Optical Emission Spectrometry for (234)U/(238)Pu Age Dating of Plutonium Materials and Comparison to Sector Field Inductively Coupled Plasma Mass Spectrometry.

    PubMed

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

    2016-09-06

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

  1. Effect of zinc cations on the kinetics of supramolecular assembly and the chirality of porphyrin J-aggregates† †Electronic supplementary information (ESI) available: UV/Vis spectral changes during metallation (SI1) and demetallation (SI2) of TPPS, RLS profiles (SI3), fluorescence emission decay and time resolved and fluorescence anisotropy (SI4), m and n kinetic parameters as a function of Zn(ii) (SI5), ICP-OES analysis experimental conditions (Table SI1), and acquisition parameters for ICP-OES analysis (Table SI2). See DOI: 10.1039/c6sc02686a Click here for additional data file.

    PubMed Central

    Romeo, A.; Zagami, R.; Pollicino, G.; Pasternack, R. F.

    2017-01-01

    Dilute aqueous solutions of anionic meso-4-sulfonatophenyl-porphyrin (TPPS) extract zinc(ii) ions from glass or quartz surfaces at room temperature and efficiently form the corresponding metal complex (ZnTPPS). The partial or complete formation of ZnTPPS has been probed by UV/Vis spectroscopy and both static and time-resolved fluorescence. The source of zinc(ii) ions has been clearly identified through inductively coupled plasma optical emission spectrometry. The presence of increasing amounts of ZnTPPS slows down the rate of TPPS J-aggregate formation in acid solution. This influences the nucleation step and has a profound impact on the onset of chirality in these species. This evidence indicates the important role of this adventitious metal ion in the interpretation of various spectroscopic and kinetic data for the self-assembly of the TPPS porphyrin and provides some insights into controversial findings on their chirality. The use of this metal derivative as the starting compound for in situ formation of monomeric TPPS is suggested. PMID:28451233

  2. Using SEM-EDX and ICP-OES to investigate the elemental composition of green macroalga Vaucheria sessilis.

    PubMed

    Michalak, Izabela; Marycz, Krzysztof; Basińska, Katarzyna; Chojnacka, Katarzyna

    2014-01-01

    The biomass of Vaucheria sessilis forms algal mats in many freshwaters. There is a need to find the method of algal biomass utilization. Vaucheria sessilis is a rich source of micro- and macronutrients and can be used as a soil amendment. In the paper, the elemental composition of enriched, via bioaccumulation process, macroalga was investigated. For this purpose, two independent techniques were used: scanning electron microscopy with an energy dispersive X-ray analytical system (SEMEDX) and inductively coupled plasma optical emission spectroscopy (ICP-OES). The biomass was exposed to two microelemental solutions, with Cu(II) and Zn(II) ions. After two weeks of the experiment, macroalga accumulated 98.5 mg of Zn(II) ions in 1 g of dry biomass and 68.9 mg g(-1) of Cu(II) ions. Micrographs performed by SEM proved that bioaccumulation occurred. Metal ions were bound on the surface and in the interior of cells. Mappings of all cations showed that in the case of the surface of biomass (biosorption), the elements constituted aggregations and in the case of the cross section (bioaccumulation) they were evenly distributed. The algal biomass with permanently bound microelements can find an application in many branches of the industry (feed, natural fertilizers, etc.).

  3. Elemental fingerprinting of Hypericum perforatum (St John's Wort) herb and preparations using ICP-OES and chemometrics.

    PubMed

    Owen, Jade D; Kirton, Stewart B; Evans, Sara J; Stair, Jacqueline L

    2016-06-05

    St. John's wort (SJW) (Hypericum perforatum) is a herbal remedy commonly used to treat mild depression. The elemental profiles of 54 samples (i.e., dry herbs, tablets and capsules) were evaluated by monitoring 25 elements using Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). The major elemental constituents in the SJW samples were Ca (300-199,000μg/g), Mg (410-3,530μg/g), Al (4.4-900μg/g), Fe (1.154-760μg/g), Mn (2.4-261μg/g), Sr (0.88-83.6μg/g), and Zn (7-64μg/g). For the sixteen elements that could be reliably quantified, principal component analysis (PCA) was used to investigate underlying patterns in the data. PCA models identified 7 key elements (i.e., Ba, Ca, Cd, Mg, Mo, Ni and Y), which described 85% of the variance in the dataset in the first three principal components. The PCA approach resulted in a general delineation between the three different formulations and provides a basis for monitoring product quality in this manner.

  4. Emission Spectrometry.

    ERIC Educational Resources Information Center

    Keliher, Peter N.; And Others

    1984-01-01

    Presented is a review of selected literature on emission spectrometry published during 1982 and 1983. The review is organized under these headings: books and reviews; spectral descriptions and classifications; instrumentation; standards, samples, nomenclature, calibration, calculations; excitation sources; selected applications; and meetings. (JN)

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

    PubMed

    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. A rapid and practical strategy for the determination of platinum, palladium, ruthenium, rhodium, iridium and gold in large amounts of ultrabasic rock by inductively coupled plasma optical emission spectrometry combined with ultrasound extraction

    NASA Astrophysics Data System (ADS)

    Zhang, Gai; Tian, Min

    2015-04-01

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

  7. Multivariate Optimization of Conditions for Digestion of Wet Feeds for Dogs and Cats Using a Closed Digester Block and Multielement Determination by ICP-OES.

    PubMed

    Ávila, Dayara Virgínia Lino; Souza, Sidnei Oliveira; Costa, Silvânio Silvério Lopes; Garcia, Carlos Alexandre Borges; Alves, José do Patrocínio Hora; Araujo, Rennan Geovanny Oliveira; Passos, Elisangela Andrade

    2017-09-01

    A full 24 factorial design was applied to find the best combination of diluted reagents (HNO3 and H2O2), time, and temperature for the digestion of samples of wet feed for dogs and cats using a closed digestion block. The residual carbon concentration (RCC) was used as the response in the factorial design. All variables and their interactions significantly influenced the digestion of the feed samples, as indicated by the RCC. The conditions established for the digestion of 0.05 g (dry mass) wet feed samples were the addition of 3.0 mol/L HNO3 and 5.0% m/m H2O2 in a final volume of 10 mL, followed by heating in a closed digestion block at a temperature of 170°C for 120 min. Analyses were performed by inductively coupled plasma (ICP) optical emission spectrometry (OES). LOQs ranged from 0.2 μg/g (Mg and Sr) to 51 μg/g (P). Accuracy of the analytical method was confirmed through the analysis of the Standard Reference Materials Tomato Leaves (NIST 1573), Apple Leaves (NIST 1515), and Peach Leaves (NIST 1547). The agreement values achieved ranged from 80.2 ± 0.3% for Ba to 113.8 ± 7.1% for Zn (n = 3). Addition and recovery tests were carried out by adding the analytes to a feed sample at two concentration levels, and the recoveries were between 84 ± 6 and 114 ± 10% for macroelements (Ca, K, Mg, and P; n = 3) and between 88 ± 3 and 113 ± 7% for microelements and trace elements (B, Cu, Fe, Sr, and Zn; n = 3). The precision values achieved for the different elements, expressed as RSDs, were better than 7.3% (Zn; n = 3) except for Cu determination, that was 14.6% (n=3). The optimized analytical method was applied to 10 commercial samples of wet feed for cats and dogs, with the concentrations of Al, B, Ba, Ca, Cu, Fe, K, Mg, Mn, P, Sr, and Zn determined by ICP-OES.

  8. Pleurotus eryngii immobilized Amberlite XAD-16 as a solid-phase biosorbent for preconcentrations of Cd2+ and Co2+ and their determination by ICP-OES.

    PubMed

    Özdemir, Sadin; Okumuş, Veysi; Kılınç, Ersin; Bilgetekin, Havin; Dündar, Abdurrahman; Ziyadanogˇulları, Berrin

    2012-09-15

    This article reports a method that is used for the preconcentration and determination of Cd(2+) and Co(2+) in vegetables, using Pleurotus eryngii immobilized Amberlite XAD-16 as a solid-phase biosorbent. The concentrations of metals were determined by inductively coupled plasma-optical spectrometry (ICP-OES). Critical parameters, such as the pH of the solution, flow rate, the amount of biosorbent, type and volume of eluent, and the sample volume, that affect the solid-phase extraction (SPE) procedure were optimized. The optimum extraction conditions were determined as being a pH of 6.0 for Cd(2+) and of 5.0 for Co(2+); a sample flow rate of 2.0 mL min(-1); 200.0mg of biosorbent; and 5.0 mL of 1.0 mol L(-1) HCl as eluent. The capacities of the biosorbent for metal uptake were found to be 11.3 and 9.8 mg g(-1) for Cd(2+) and Co(2+) ions, respectively. Limit of quantitations (LOQs) were found to be 0.67 and 0.82 ng mL(-1), respectively, for Cd(2+) and Co(2+). The linear working curves were observed to be in the linear range from 1.0 to 50.0 ng mL(-1), and possessed high correlation coefficients. The use of the SPE method showed 50.7- and 35.7-fold improvements in the sensitivities of ICP-OES. The developed method was successfully applied to NCS ZC-73014 (a certified reference tea sample). Relative standard deviations (RSD) were lower than 5.0%. The Cd(2+) and Co(2+) concentrations in the different parts (leave, root, stem, and fruit) of purslane, onion, rocket, okra, and aubergine were determined after microwave digestion and solid-phase extraction by P. eryngii immobilized on Amberlite XAD-16.

  9. Removal of uranium from soil sample digests for ICP-OES analysis of trace metals

    SciTech Connect

    Foust, R.D. Jr.; Bidabad, M.

    1996-10-01

    An analytical procedure has been developed to quantitatively remove uranium from soil sample digests, permitting ICP-OES analysis of trace metals. The procedure involves digesting a soil sample with standard procedures (EPA SW-846, Method 3050), and passing the sample digestate through commercially available resin (U/TEVA{sm_bullet}Spec, Eichrom Industries, Inc.) containing diarryl amylphosphonate as the stationary phase. Quantitative removal of uranium was achieved with soil samples containing up to 60% uranium, and percent recoveries averaged better than 85% for 9 of the 10 metals evaluated (Ag, As, Cd. Cr, Cu, Ni, Pb, Se and Tl). The U/TEVA{sm_bullet}Spec column was regenerated by washing with 200 mL of a 0.01 M oxalic acid/0.02 M nitric acid solution, permitting re-use of the column. GFAAS analysis of a sample spiked with 56.5% uranium, after treatment of the digestate with a U/TEVA{sm_bullet}Spec resin column, resulted in percent recoveries of 97% or better for all target metals.

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

    NASA Astrophysics Data System (ADS)

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

    2002-12-01

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

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

    PubMed

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

    2015-07-23

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

  12. Ornamental Planting Restoration at Jefferson's Poplar Forest Through XRF and ICP-OES Analysis of Disturbed Soils

    NASA Astrophysics Data System (ADS)

    Hatfield, M.; Low, P. C.; Devlin, S.

    2011-12-01

    Thomas Jefferson's Poplar Forest estate near Lynchburg, VA is currently attempting to restore the property to its Jeffersonian condition. Subsequent modifications to the property following its sale by Jefferson's heirs included the removal of the original trees in order to facilitate agricultural activity. One key facet of the restoration involves determining the precise location of the sixty-four paper mulberry trees that Jefferson reportedly had transplanted in 1815 from his on-site nursery to near the main house. At Monticello, it is well-documented that Jefferson used contextually innovative fertilizing techniques, including the addition of gypsum and lime "to restore the exhaustion of a single crop from the soil." Whether he used these methods in the nursery at Poplar Forest to the degree that decades of subsequent leaching, weathering, and other disturbances would not erase remains historically and analytically unclear. Since the transplantation process requires that large amounts of soil be moved with the trees, small areas of compositionally distinct soils in the suspected planting area could be used to establish the exact location of each tree through differentiating between nursery and in situ soils. Through X-ray fluorescence spectroscopy (XRF) and intercoupled plasma optical emission spectroscopy (ICP-OES) geochemical analysis, the specific composition of soil can be determined. Preliminary analysis shows slight differences in phosphorus and sulfur between the nursery and in situ soil; however, the property lies on three different distinct geological units: actinolite schist and feldspathic metagreywacke units of the Alligator Back formation, and biotite gneiss of the Ashe Formation (biotite gneiss). The location of the nursery where the sixty-four paper mulberry trees were originally grown lies on the feldspathic metagreywacke unit; whereas the relocation site where Jefferson had them planted rests on the actinolite schist unit. Percursory study

  13. Microwave digestion for the quantification of inorganic elements in coal and coal ash using ICP-OES.

    PubMed

    Low, Fiona; Zhang, Lian

    2012-11-15

    In this paper, microwave digestion conditions have been optimised to achieve complete recoveries for the ash-forming inorganic elements in coal and coal combustion fly ash, during the analysis by inductively coupled plasma optical emission spectroscopy (ICP-OES). The elements analysed include six major (Al, Ca, Fe, K, Mg and Na) and twelve trace (As, Ba, Be, Co, Cr, Cu, Li, Mn, Ni, Pb, Sr and V). Seven reference samples have been tested, including two standard coal references, SRM1632c and SARM19, their corresponding high-temperature ashes (HTAs), and three coal fly ash references, SRM1633c, SRM2690 and BCR38. The recoveries of individual elements in these samples have been examined intensively, as a function of the amount of hydrofluoric acid (HF, 0-2.0 ml), microwave power (900 W vs. 1200 W) and sample mass (0.05 g vs. 0.1 g). As have been confirmed, the recoveries of these individual elements varied significantly with the microwave digestion condition, elemental type and sample property. For the coal references and their HTAs, the use of HF can be ruled out for most of the elements, except K associated with feldspar, Pb and V. In particular, the recovery of Pb in coal is highly sample-specific and thus unpredictable. The majority of elements in fly ash references require the use of 0.1-0.2 ml HF for a complete recovery. Al in fly ash is the only exceptional element which gave incomplete recoveries throughout, suggesting the use of a complementary technique for its quantification. As has proven to be the only element inconsequential of sample type and digestion conditions, achieving complete recoveries for all cases. On the power parameter, using a higher power such as 1200 W is critical, which has proved to be an ultimatum for the recovery of certain elements, especially in fly ash. Halving sample mass from 0.1 g to 0.05 g was also found to be insignificant.

  14. A comparison of double-focusing sector field ICP-MS, ICP-OES and octopole collision cell ICP-MS for the high-accuracy determination of calcium in human serum.

    PubMed

    Simpson, Lorna A; Hearn, Ruth; Merson, Sheila; Catterick, Tim

    2005-02-28

    Human serum is routinely measured for total calcium content in clinical studies. A definitive high-accuracy and low-uncertainty method is required for reference measurements to underpin medical diagnoses. This study presents a novel octopole collision cell ICP-MS, high-accuracy, methodology and comparison of that technique with double-focusing sector field ICP-MS and an ICP-OES method. Double-matched isotope dilution mass spectrometry (IDMS) was employed for ICP-MS techniques and an exact matching bracketing technique using scandium as an internal standard was used for ICP-OES analysis. Medium resolution mode was utilised for double-focusing sector field ICP-MS analysis to resolve the dominant interferences on the (44)Ca/(42)Ca isotope pair. Hydrogen reaction gas was employed to chemically resolve a number of polyatomic interferences predominantly through charge transfer reactions in the octopole collision cell. Comparison data presented for NIST CRM 909b human serum analysis from all three techniques demonstrates highest accuracy (99.6%) and lowest uncertainty (1.1%) for octopole collision cell ICP-MS. Data from ICP-OES using a non-IDMS technique produces comparably accurate data and low-uncertainties. The much higher total expanded uncertainties for double-focusing sector field ICP-MS compared with octopole collision cell data are explained by lower precision on the measurement of the (44)Ca/(42)Ca isotope ratio. Data for octopole collision cell ICP-MS submitted for an international blind trial comparison (CCQM K-14) demonstrated excellent agreement with the mean of all participants with a low expanded uncertainty.

  15. Application of multivariate techniques in the optimization of a procedure for the determination of bioavailable concentrations of Se and As in estuarine sediments by ICP OES using a concomitant metals analyzer as a hydride generator.

    PubMed

    Lopes, Watson da Luz; Santelli, Ricardo Erthal; Oliveira, Eliane Padua; de Carvalho, Maria de Fátima Batista; Bezerra, Marcos Almeida

    2009-10-15

    A procedure has been developed for the determination of bioavailable concentrations of selenium and arsenic in estuarine sediments employing inductively coupled plasma optical emission spectrometry (ICP OES) using a concomitant metals analyzer device to perform hydride generation. The optimization of hydride generation was done in two steps: using a two-level factorial design for preliminary evaluation of studied factors and a Doehlert design to assess the optimal experimental conditions for analysis. Interferences of transition metallic ions (Cd(2+), Co(2+), Cu(2+), Fe(3+) and Ni(2+)) to selenium and arsenic signals were minimized by using higher hydrochloric acid concentrations. In this way, the procedure allowed the determination of selenium and arsenic in sediments with a detection limit of 25 and 30 microg kg(-1), respectively, assuming a 50-fold sample dilution (0.5 g sample extraction to 25 mL sample final volume). The precision, expressed as a relative standard deviation (% RSD, n=10), was 0.2% for both selenium and arsenic in 200 microg L(-1) solutions, which corresponds to 10 microg g(-1) in sediment samples after acid extraction. Applying the proposed procedure, a linear range of 0.08-10 and 0.10-10 microg g(-1) was obtained for selenium and arsenic, respectively. The developed procedure was validated by the analysis of two certified reference materials: industrial sludge (NIST 2782) and river sediment (NIST 8704). The results were in agreement with the certified values. The developed procedure was applied to evaluate the bioavailability of both elements in four sediment certified reference materials, in which there are not certified values for bioavailable fractions, and also in estuarine sediment samples collected in several sites of Guanabara Bay, an impacted environment in Rio de Janeiro, Brazil.

  16. Comparative analysis of ancient ceramics by neutron activation analysis, inductively coupled plasma-optical-emission spectrometry, inductively coupled plasma-mass spectrometry, and X-ray fluorescence.

    PubMed

    Tsolakidou, Alexandra; Kilikoglou, Vassilis

    2002-10-01

    The accurate measurement of the maximum possible number of elements in ancient ceramic samples is the main requirement in provenance studies. For this reason neutron activation analysis (NAA) and X-ray fluorescence (XRF) have been successfully used for most of the studies. In this work the analytical performance of inductively coupled plasma-optical-emission spectrometry (ICP-OES) and inductively coupled plasma-mass spectrometry (ICP-MS) has been compared with that of XRF and NAA for the chemical characterization of archaeological pottery. Correlation coefficients between ICP techniques and XRF or NAA data were generally better than 0.90. The reproducibility of data calculated on a sample prepared and analysed independently ten times was approximately 5% for most of the elements. Results from the ICP techniques were finally evaluated for their capacity to identify the same compositional pottery groups as results from XRF and NAA analysis, by use of multivariate statistics.

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

    PubMed

    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.

  18. Dissolution reaction and surface iron speciation of UICC crocidolite in buffered solution at pH 7.4: A combined ICP-OES, XPS and TEM investigation

    NASA Astrophysics Data System (ADS)

    Pacella, Alessandro; Fantauzzi, Marzia; Turci, Francesco; Cremisini, Carlo; Montereali, Maria Rita; Nardi, Elisa; Atzei, Davide; Rossi, Antonella; Andreozzi, Giovanni B.

    2014-02-01

    The dissolution reaction and the surface modifications of crocidolite asbestos fibres incubated for 0.5, 1, 24, 48, 168 and 1440 h in a phosphate buffered solution at pH 7.4 with and without hydrogen peroxide were investigated. Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) was used to monitor the ion release into solution, X-ray Photoelectron Spectroscopy (XPS) was performed to unveil the chemistry of the leached surface, and High Resolution Transmission Electron Microscopy (HR-TEM) was carried out to monitor the structural modifications of the fibres. No significant differences were observed between dissolution experiments carried out with and without H2O2 with the exception of results after the first hour, from which it may be inferred that the dissolution proceeds faster in the presence of H2O2 but only in its very early steps. Congruent mobilization of Si and Mg from crocidolite was observed, increasing with time especially in the range between 1 and 48 h, while Ca decreased after 48 h and Fe was not detected at any incubation time. In the undersaturated conditions (0-48 h), dissolution rate of UICC crocidolite fibres has been estimated to be d(Si)/dt = 0.079 μmol h-1. The fibre surface modification is continuous with time: XPS results showed a regular depletion of Si and Mg and enrichment of Fe along dissolution. The Fe2p3/2 signal on the surface was fitted with four components at 709.0, 710.5, 711.6 and 712.8 eV binding energy values corresponding to: (i) Fe(II)-O and (ii) Fe(III)-O surrounded by oxygen atoms in the silicate structure, (iii) Fe(III)-OOH as a product of the dissolution process, and (iv) Fe in a phosphate precipitate (Fe-P), respectively. The evolution of Fe speciation on the crocidolite surface was followed by integrating the four photoemission peaks, and results showed that the oxidative environment promotes the formation of Fe(III)-O (up to 37% Fetot) and of Fe-P species (up to 16% Fetot), which are found on the fibre

  19. [Simultaneous determination of germanium and some major ash forming elements in lignites using a dual-view ICP-OES].

    PubMed

    Zou, Ben-dong; Aodeng, Gao-wa; Shang, Hong-shan; Qi, Lu

    2005-09-01

    In this article, an ICP-OES method of simultaneous determination germanium and some major ash forming elements especially for Fe, Al, Ca, Mg, K, Na, Ti in lignites is described. An ICP-OES instrument equipped with a dual-view plasma torch and a simultaneous detector was used. This technology allows the simultaneous determination of trace elements and major components in the axial view along with in the radial view. The moderate operation condition of the instrument and analytical wavelength lack of interference from elements in the sample matrix was selected, the spectral background was automaticly eliminated. The obtained coal ashes were dissolved in mixtures of nitric acid, hydrofluoric acid and perchloric acid after coal samples were cinerated. The analytical results were in good agreement with those provided by national standard methods. The detection limit of the instrument is ranged between 0.00039-0.10 microg. x mL(-1), the precision of the method is in the range of 0.79%-2.84%, the average recovery of samples is 92.38%, the proposed method is well suitable for the determination germanium and some major ash forming elements in lignites.

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

    PubMed

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

    2016-04-01

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

  1. Comparing Compositions of Modern Cast Bronze Sculptures: Optical Emission Spectroscopy Versus x-Ray Fluorescence Spectroscopy

    NASA Astrophysics Data System (ADS)

    Young, M. L.; Dunand, D. C.

    2015-07-01

    Bulk elemental compositions of 74 modern cast bronze sculptures from the collection at the Art Institute of Chicago, the Philadelphia Museum of Art, and the Rodin Museum (Philadelphia, PA) were determined using inductively coupled plasma-optical emission spectroscopy (ICP-OES) and a handheld x-ray fluorescence (XRF) spectrometer. The elemental compositions of the cast sculptures as measured previously by ICP-OES and presently by XRF are compared: A good match is found between the two methods for the base metal (Cu) and the two majority alloying elements (Zn and Sn). For both ICP-OES and XRF data, when the Zn composition is plotted versus the Sn composition, three discernable clusters are found that are related to the artist, foundry, casting date, and casting method; they consist of (A) high-zinc brass, (B) low-zinc, low-tin brass, and (C) low-zinc, tin bronze. Thus, our study confirms that the relatively fast, nondestructive XRF spectrometry can be used effectively over slower and invasive, but more accurate, ICP-OES to help determine a sculpture's artist, foundry, date of creation, date of casting, and casting method.

  2. Fast method of elements determination in slim coffees by ICP OES.

    PubMed

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

    2014-03-01

    Six sample preparation procedures, i.e., the total decomposition in a HNO3 and H2O2 mixture by microwave-assisted or hot-plate heating, a partial decomposition by means of solubilisation in aqua regia or tetramethyl ammonium hydroxide and simple dissolution in diluted HNO3 or in H2O, for the determination of the total content of Ba, Ca, Cd, Cr, Cu, Fe, Mg, Mn, Ni, P, Pb, Sr and Zn in slim instant coffees using inductively coupled plasma optical emission spectrometry were compared. The performance of procedures was determined based on the precision and the accuracy of results and limits of detection of elements. It was found that the extraction with aqua regia provides the best results, i.e., limits of detection of elements within 0.11-108ngmL(-1), the precision of 0.6-5% and the accuracy better than 5%. Elements' concentrations agree with those after the wet digestion in the HNO3 and H2O2 mixture, therefore this procedure is a simple and fast alternative to complete sample decomposition procedures and can be easily applied for routine analyses. Six commercial slim coffee products were analysed with the proposed procedure. Copyright © 2013 Elsevier Ltd. All rights reserved.

  3. Elemental composition of edible nuts: fast optimization and validation procedure of an ICP-OES method.

    PubMed

    Tošić, Snežana B; Mitić, Snežana S; Velimirović, Dragan S; Stojanović, Gordana S; Pavlović, Aleksandra N; Pecev-Marinković, Emilija T

    2015-08-30

    An inductively coupled plasma-optical emission spectrometry method for the speedy simultaneous detection of 19 elements in edible nuts (walnuts: Juglans nigra; almonds: Prunus dulcis; hazelnuts: Corylus avellana; Brazil nuts: Bertholletia excelsa; cashews: Anacardium occidentalle; pistachios: Pistacia vera; and peanuts: Arachis hypogaea) available on the Serbian markets, was optimized and validated through the selection of instrumental parameters and analytical lines free from spectral interference and with the lowest matrix effects. The analysed macro-elements were present in the following descending order: Na > Mg > Ca > K. Of all the trace elements, the tested samples showed the highest content of Fe. The micro-element Se was detected in all the samples of nuts. The toxic elements As, Cd and Pb were either not detected or the contents were below the limit of detection. One-way analysis of variance, Student's t-test, Tukey's HSD post hoc test and hierarchical agglomerative cluster analysis were applied in the statistical analysis of the results. Based on the detected content of analysed elements it can be concluded that nuts may be a good additional source of minerals as micronutrients. © 2014 Society of Chemical Industry.

  4. In situ digestion for the determination of Ca in beverages by tungsten coil atomic emission spectrometry.

    PubMed

    Santos, Luana N; Gonzalez, Mário H; Moura, Monise F; Donati, George L; Nóbrega, Joaquim A

    2012-08-15

    Tungsten coil atomic emission spectrometry (WCAES) is employed for the determination of calcium in juice, mineral and coconut water samples. A sample aliquot of 20 μL is placed directly on the coil and a constant-voltage power source is used to dry and atomize the sample, as well as to promote Ca atomic emission. Analytical signals are resolved and detected using a Czerny-Turner spectrometer and a charge coupled device detector. Some experimental parameters such as coil position related to the spectrometer entrance slit and integration time are critically evaluated. A heating program with relatively constant drying temperatures is used in all measurements. An in situ digestion procedure is used to partially decompose organic matrices and improve WCAES precision and accuracy. By adding an oxidizing mixture to the sample and including a digestion step in the heating cycle, no statistical difference was observed between WCAES and ICP OES results for Ca in juice and coconut water samples. Mineral water samples were simply diluted with 1% vv(-1) HNO(3) before analysis and no significant interference was observed for concomitants such as Na and K. Despite severe positive interference caused by Mg, good agreement was obtained between WCAES and ICP OES results for Ca in several mineral water samples. Limits of detection and quantification obtained were 0.02 and 0.07 mg L(-1), respectively. The method precision, calculated as the relative standard deviation for 10 consecutive measurements of a 2.5 mg L(-1) Ca solution, is 3.8%.

  5. Development of a FI-HG-ICP-OES solid phase preconcentration system for inorganic selenium speciation in Argentinean beverages.

    PubMed

    Escudero, Luis A; Pacheco, Pablo H; Gasquez, José A; Salonia, José A

    2015-02-15

    A preconcentration system has been developed to determine inorganic selenium species. Selenium was retained by a column filled with polyvinyl chloride (PVC) with lanthanum hydroxide co-precipitation. Speciation was achieved by selective photoreduction previous Se preconcentration. The retention pH was optimized at 10.0. Two multivariate calibrations and a central composite design were employed for optimization of the system. Sample, reagents and acid flow rates are significant variables affecting the system. Employing HG-ICP-OES as detection, the optimized system reached a detection limit of 0.03μg/L, and an enhancement factor of 14875 (25 for preconcentration system, 595 for hydride generation). To verify the method' accuracy, two certified reference materials, BCR® 414 Plankton & IRMM-804 Rice Flour, were analysed. The system was applied to inorganic selenium speciation in several Argentinean beverages to estimate their selenium contribution to diet. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

    PubMed

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

    2015-07-23

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

  7. Determination of 28 selected elements in textiles by axially viewed inductively coupled plasma optical emission spectrometry.

    PubMed

    Rezić, Iva; Zeiner, Michaela; Steffan, Ilse

    2011-01-15

    A simple, robust and reliable analytical procedure for the determination of 28 selected elements, namely Al, As, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, K, Hg, Mg, Mn, Mo, Na, Ni, Pb, Sc, Si, Se, Sn, Sm, Sr, Tl, V, and Zn in textile materials by inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave digestion of samples was optimized and validated in this work. The total amount of elements present in textile samples was determined after microwave digestion of materials in 7 mol/L nitric acid within the optimal working program: 5 min at 150°C (power 250 W), 15 min 180°C (300 W) and 20 min at the maximum temperature of 200°C (350 W). For the quality control reasons, which were ascertained by analysis of the certified cotton trace elements reference material IAEA-V9, the ICP-OES method was optimized through several parameters: by comparing Meinhard and Gemcone Low Flow nebulizers efficiency, ranging nebulizer gas flows from 0.6 to 1.0 L/min, ranging sample flows from 0.8 to 1.2 mL/min, testing RF power from 1200 to 1400 W, detecting data acquisition time (read time) from 0 to 527 s, ranging washing (delay) time from 0 to 408 s, as well as by checking the occurring interferences for the optimal line selection. Validation included determination of linearity, selectivity, accuracy, reproducibility, precision and limits of detection calculated for all 28 selected elements of interest. The developed analytical procedure was successfully applied on textile fibers (cotton, flax and hemp) as well as on standard knitted textile sample materials (cotton and wool). Copyright © 2010 Elsevier B.V. All rights reserved.

  8. Determination of impurities in titanium nitride by slurry introduction axial viewed inductively coupled plasma optical emission spectrometry

    NASA Astrophysics Data System (ADS)

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

    2005-03-01

    A method of slurry nebulization for inductively coupled plasma optical emission spectrometry (ICP-OES) applied to the analysis of titanium niride(TiN) was reported. The TiN slurry sample was prepared with adding dispersant polyacrylate amine or polyethylene imine for the stabilization and homogenization of suspension, and the amount of additives was optimized. A Babington type cross-flow nebulizer with V-groove was used for nebulization of the slurry for avoidance of blockage from the particles. The stability of slurry was characterized via zeta potential measurement, scanning electron microscope observation, particle size distrbution measurement and signal stability testing. For nm size TiN, calibration curves could be established by aqueous standards and the analytical results were in good accordance with the alkaline fusion method. For μm size TiN, a negative deviation was observed for most of elements and this deviation can be corrected by using Ti intrinsic internal standard method.

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

    NASA Astrophysics Data System (ADS)

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

    2009-06-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2011-05-01

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

  11. Hybrid Sargassum-sand sorbent: a novel adsorbent in packed column to treat metal-bearing wastewaters from inductively coupled plasma-optical emission spectrometry.

    PubMed

    Vijayaraghavan, K; Joshi, U M

    2013-01-01

    Laboratory batch and column experiments were carried out to examine the efficiency of algal-based treatment technique to clean-up wastewaters emanating from inductively coupled plasma-optical emission spectrometry (ICP-OES). Chemical characterization revealed the extreme complexity of the wastewater, with the presence of 14 different metals under very low pH (pH = 1.1), high conductivity (6.98 mS/cm), total dissolved solid (4.46 g/L) and salinity (3.77). Batch experiments using Sargassum biomass indicated that it was possible to attain high removal efficiencies at optimum pH of 4.0. Efforts were also made to continuously treat ICP-OES wastewater using up-flow packed column. However, swelling of Sargassum biomass leads to stoppage of column. To address the problem, Sargassum was mixed with sand at a ratio of 40: 60 on volume basis. Remarkably, the hybrid Sargassum-sand sorbent showed very high removal efficiency towards multiple metal ions with the column able to operate for 11 h at a flow rate of 10 mL/min. Metal ions such as Cu, Cd, and Pb were only under trace levels in the treated water until 11 h. The results of the treatment process were compared with trade effluent discharge standards. Further the process evaluation and cost analysis were presented.

  12. Micro-scale flow system for on-line multielement preconcentration from saliva digests and determination by inductively coupled plasma optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    Menegário, Amauri A.; Fernanda Giné, Maria

    2001-10-01

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

  13. [Determination of life elements in hair and urine with brick-tea fluorosis in Inner Mongolia by ICP-OES].

    PubMed

    Hou, Kun; Ji, Hong-bing; Li, Hai-rong; Wang, Li-zhen; Wang, Wu-yi; Liu, Qing-bin; Wang, Ge; Liu, Xue-hui

    2009-04-01

    In brick-tea fluorosis affected areas XiLinHot city in Inner Mongolia, herdsmen who like drinking a large amount of brick tea in everyday life and Han habitants rarely drinking brick tea as control group were enrolled, and their hair and urine were sampled. The concentrations of Ca, Mg, K, Al, P, Cu, Zn and Fe in hair and urine were detected using ICP-OES. The RSDs of the method were between 2.32% and 8.03%, and the analytical results of the hair reference samples were consistent with the certified values. The results showed that the contents of Al, Mg and K in hair, and contents of Al and Ca in urine of herdsmen who were accustomed to drinking brick tea were obviously higher than those in control group (P<0.05), while the contents of K in urine of herdsmen who were accustomed to drinking brick tea was lower than those in control group (P<0.05), and other elements did not have statistic significance (P>0.05). Chronically drinking brick tea probably brings metabolic disorder of Ca and Al in human body, and the interaction mechanism of life elements in brick-tea fluorosis should be further studied.

  14. The combination of infrared and microwave radiation to quantify trace elements in organic samples by ICP OES.

    PubMed

    Dantas, A N S; Matos, W O; Gouveia, S T; Lopes, G S

    2013-03-30

    Sample-decomposition methods using microwave radiation in closed systems have been commonly used in the analysis of inorganic constituents; however, these methods are limited to small amounts of organic samples. This work proposes the combined use of infrared radiation and microwave radiation (IR-MW) to increase the amount of organic samples digested. The determination of Al, Ca, Cu, Fe, K, Mg, Mn, Na, P and Zn in human-feed samples was accomplished by ICP OES. The results were in agreement with those obtained from conventional decomposition by microwave radiation (closed system). The results obtained using the proposed IR-MW system for standard reference material (whole milk powder, NIST 8435) were also compared. Agreements of 85-100% were obtained for Al, Ca, Cu, Fe, K, Mg, Na, P and Zn in the standard reference material. The IR-MW system is simple to implement and cheap because it uses commercially available infrared lamps and allows the use of infrared radiation in the microwave-digestion vessel. Additionally, it is possible to reach better precision in the analysis of the human-feed samples using the IR-MW system. The proposed method also allows total digestion of large sample amounts or samples rich in organic compounds can also be performed in the IR-MW system using small volumes of nitric acid. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Determination of trace elements in biodiesel and vegetable oil by inductively coupled plasma optical emission spectrometry following alcohol dilution

    NASA Astrophysics Data System (ADS)

    Chaves, Eduardo S.; de Loos-Vollebregt, Margaretha T. C.; Curtius, Adilson J.; Vanhaecke, Frank

    2011-09-01

    A method for the simultaneous determination of Ca, Cu, Fe, K, Mg, Na, P, S and Zn in biodiesels and vegetable oils by inductively coupled plasma optical emission spectrometry (ICP-OES) has been developed. The method - based on the use of an ICP-OES instrument outfitted with a spectrometer in Paschen-Runge mount, equipped with linear charge coupled device detectors monitoring the entire spectrum from 130 to 770 nm - offers a high sample throughput as sample preparation is limited to dilution with alcohol, while all elements of interest are determined simultaneously. Ethanol is only suitable in the context of biodiesel analysis, whereas dilution with 1-propanol also allows application of the method, without any additional modification, to analysis of vegetable oils. As a result, the dilution with 1-propanol is preferable. Sample introduction was carried out with pneumatic nebulization and spectral interferences from carbon-containing compounds were reduced by cooling the cyclonic spray chamber to - 5 °C. The remaining spectral interferences in the low-UV region were efficiently corrected for by the background correction system offered in the software of the ICP-OES instrument used. Calibration was carried out against inorganic standards diluted in ethanol or 1-propanol, while Y was used as an internal standard, correcting for non-spectral interference and sensitivity drift. The accuracy of the method was verified through the analysis of the NIST SRMs 2772 and 2773 biodiesel reference materials. Additionally, as for most of the target elements only indicative concentration values are available for these reference materials, recovery tests have been performed using inorganic and organic standards. The results obtained were in good agreement with the values found on the certificate for both ethanol and 1-propanol sample dilution, while the recoveries were between 87 and 116% for biodiesel and between 95 and 106% for vegetable oils. The measurement precision expressed

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

    PubMed

    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.

  17. The determination of antimony and arsenic concentrations in fly ash by hydride generation inductively coupled plasma optical emission spectrometry.

    PubMed

    Ilander, Aki; Väisänen, Ari

    2011-03-18

    Hydride generation inductively coupled plasma optical emission spectrometry (HG-ICP-OES) was used in the determination of As and Sb concentrations in fly ash samples. The effect of sample pre-treatment reagents and measurement parameters used for hydride generation was evaluated. Due to memory effects observed, the appropriate read delay time was adjusted to 60s resulting in RSDs 0.6% and 2.3% for As and Sb, respectively. The most suitable volumes of pre-reduction reagents for 10 mL of sample were 4 mL of KI/ascorbic acid (5%) and 6 mL of HCl (conc.). The determination of Sb was significantly interfered by HF, but the interference could be eliminated by adding 2 mL of saturated boric acid and heating the samples to 60°C at least 45 min. The accuracy of the method was studied by analyses of SRM 1633b and two fly ash samples with the recovery test of added As and Sb. As high a recovery as 96% for SRM 1633b was reached for As using 193.696 nm with two-step ultrasound-assisted digestion. A recovery rate of 103% was obtained for Sb using 217.582 nm and the pre-reduction method with the addition of 2 mL of saturated boric acid and heating. The quantification limits for the determination of As and Sb in the fly ash samples using two-step ultrasound-assisted digestion followed with HG-ICP-OES were 0.89 and 1.37 mg kg(-1), respectively. Copyright © 2011 Elsevier B.V. All rights reserved.

  18. A fast method for apatite selective leaching from granitic rocks followed through rare earth elements and phosphorus determination by inductively coupled plasma optical emission spectrometry.

    PubMed

    Gásquez, José A; DeLima, Edmilson; Olsina, Roberto A; Martinez, Luis D; de la Guardia, Miguel

    2005-10-15

    Rare earth elements (REE) and phosphorus (P) in apatite were determined using inductively coupled plasma optical emission spectrometry (ICP-OES) after partial dissolution of the granitic rocks and pure apatite. The dissolution was performed with nitric acid in an open system and the matrix elements were separated by a cation exchange procedure. Samples of pure apatite from granitic rocks were dissolved with, 0.14 mol L(-1) nitric acid. The results showed that the release of REE is due to apatite leaching because it could be assessed by comparing the chondrite-normalised pattern corresponding to the rocks and the pure apatite. Similar results were found for absolute REE abundance from the partial dissolution of the rocks and pure apatite. This simple and rapid method can be applied for the determination of REE in apatite as an indicator for mineral exploration, although its use in petrology could be possible.

  19. 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

    NASA Astrophysics Data System (ADS)

    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

  20. The application of ICP-MS and ICP-OES in determination of micronutrients in wood ashes used as soil conditioners.

    PubMed

    Górecka, H; Chojnacka, K; Górecki, H

    2006-12-15

    In the present paper, the elemental composition of wood ashes obtained by the combustion of wood in a fireplace was determined with the use of ICP-MS and ICP-OES techniques. Wood ashes may find a potential application as deacidifying agents and soil conditioners, since they contain calcium (in the form of CaCO(3) and CaO), potassium (in the form of K(2)SO(4) and K(2)CO(3)) and significant levels of micronutrients. However, if applied to soil, it is important to assess the bioavailability of particular elements to plants. This process can be simulated by proper extraction procedures. Various species of wood were combusted in a firestove in a single-family house. The ashes underwent multielemental analyses with ICP-MS Varian Ultra Mass 700 (Australia) and ICP-OES Vista-MPX from Varian (Australia) in order to determine the content of macro- and micronutrients as well as toxic elements. Ashes were also extracted with solutions of 0.1M NaNO(3) and water in order to simulate the process of elemental transfer from ash (used as soil conditioner) to soil solution and consequently to plants. Also, the environmental impact of ash supplementation to soil was assessed in these experiments. Soil was supplemented with 0-20% of ash. After elution, the eluent underwent multielemental analysis by ICP-MS and ICP-OES techniques to determine the content of macronutrients (P, K, Mg), micronutrients (Fe, Mn, Co, Mo, Zn, Cu and Ti) and toxic elements (Hg, Pb, As and Cd). It was shown that fireplace ashes can be applied for deacidification of homestead gardens. Ash may be described as a valuable soil conditioner with N:P:K formula 0:1:3. It is concluded therefore that in order to achieve full fertilization, additional supplementation with nitrogen fertilizer would be necessary.

  1. [Determination of nine hazardous elements in textiles by inductively coupled plasma optical emission spectrometer after microwave-assisted dilute nitric acid extraction].

    PubMed

    Chen, Fei; Xu, Dian-dou; Tang, Xiao-ping; Cao, Jing; Liu, Ya-ting; Deng, Jian

    2012-01-01

    Textiles are easily contaminated by heavy metals in the course of processing. In order to monitor the quality of textiles, a new method was developed for simultaneous determination of arsenic, antimony, lead, cadmium, chromium, cobalt, copper, nickel and mercury in textiles by inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave-assisted dilute nitric acid extraction. After optimizing extraction conditions, we ultimately selected 5% nitric acid as extractant and 5 min as extraction time with the extraction temperature of 120 degrees C and instrument power of 400W in the microwave-assisted extraction procedure. Nine hazardous elements were detected sequentially by ICP-OES. The results showed that the detection limits were 0.3-15 microg x L(-1) and the recoveries 73.6%-105% with the RSDs (n = 3) of 0.1%-3%. The proposed method was successfully used to determine nine elements in cotton, wool, terylene and acrylic.

  2. On line vapor generation of osmium based on solution cathode glow discharge for the determination by ICP-OES.

    PubMed

    Zhu, Zhenli; Huang, Chunying; He, Qian; Xiao, Qing; Liu, Zhifu; Zhang, Suicheng; Hu, Shenghong

    2013-03-15

    A novel plasma induced vapor generation method is proposed to determine osmium in solutions. Without any chemical oxidizing agents, osmium ion can be readily converted to volatile osmium tetraoxide vapor in the solution cathode glow discharge (SCGD) system. The generated osmium vapor is then transported to inductively coupled plasma for determination by optical emission spectrometry. The influences of background electrolyte, carrier gas flow rate, sample flow rate, ICP power and discharge current were investigated. The analytical performances of this proposed technique were evaluated under optimized conditions. The detection limit of Os was calculated to be 0.51 ng mL(-1). The reproducibility, expressed as the relative standard deviation (n=11) of a 2.0 μg mL(-1) standard solution, was 1.9%. This SCGD induced vapor generation is sensitive and simple, oxidation reagents free, providing an alternative analytical method for measuring Os in geological or environmental water samples.

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

    NASA Astrophysics Data System (ADS)

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

    2015-03-01

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

  4. Tin content determination in canned fruits and vegetables by hydride generation inductively coupled plasma optical emission spectrometry.

    PubMed

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

    2012-01-01

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

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

    PubMed Central

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

    2012-01-01

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

  6. Study of the chemical composition of particulate matter from the Rio de Janeiro metropolitan region, Brazil, by inductively coupled plasma-mass spectrometry and optical emission spectrometry

    NASA Astrophysics Data System (ADS)

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

    2013-08-01

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

  7. Chlorine and sulfur determination in extra-heavy crude oil by inductively coupled plasma optical emission spectrometry after microwave-induced combustion

    NASA Astrophysics Data System (ADS)

    Pereira, Juliana S. F.; Mello, Paola A.; Moraes, Diogo P.; Duarte, Fábio A.; Dressler, Valderi L.; Knapp, Guenter; Flores, Érico M. M.

    2009-06-01

    In this study, microwave-induced combustion (MIC) of extra-heavy crude oil is proposed for further chlorine and sulfur determination by inductively coupled plasma optical emission spectrometry (ICP OES). Combustion was carried out under oxygen pressure (20 bar) in quartz vessels using ammonium nitrate (50 µl of 6 mol l - 1 solution) as ignition aid. Samples were wrapped with polyethylene film and placed on a quartz holder positioned inside the quartz vessels. The need for an additional reflux step after combustion and the type and concentration of absorbing solution (water, 0.02 to 0.9 mmol l - 1 H 2O 2, 10 to 100 mmol l - 1 (NH 4) 2CO 3 or 0.1 to 14 mol l - 1 HNO 3) were studied. The influence of sample mass, O 2 pressure and maximum pressure attained during the combustion process were investigated. Recoveries from 92 to 102% were obtained for Cl and S for all absorbing solutions. For comparison, Cl and S determination was also performed by ion chromatography (IC) using 25 mmol l - 1 (NH 4) 2CO 3 as absorbing solution. Using MIC with a reflux step the agreement was better than 95% for certified reference materials of similar composition (crude oil, petroleum coke, coal and residual fuel oil). Microwave-assisted digestion and water extraction in high pressure closed vessels were also evaluated. Using these procedures the maximum recoveries were 30 and 98% for Cl and S, respectively, using microwave-assisted digestion and 70% for Cl and less than 1% for S by water extraction procedure. Limits of detection by ICP OES were 12 and 5 µg g - 1 for Cl and S, respectively, and the corresponding values by IC were 1.2 and 8 µg g - 1 . Using MIC it was possible to digest simultaneously up to eight samples resulting in a solution suitable for the determination of both analytes with a single combustion step.

  8. Application of cotton as a solid phase extraction sorbent for on-line preconcentration of copper in water samples prior to inductively coupled plasma optical emission spectrometry determination.

    PubMed

    Faraji, Mohammad; Yamini, Yadollah; Shariati, Shahab

    2009-07-30

    Copper, as a heavy metal, is toxic for many biological systems. Thus, the determination of trace amounts of copper in environmental samples is of great importance. In the present work, a new method was developed for the determination of trace amounts of copper in water samples. The method is based on the formation of ternary Cu(II)-CAS-CTAB ion-pair and adsorption of it into a mini-column packed with cotton prior applying inductively coupled plasma optical emission spectrometry (ICP-OES). The experimental parameters that affected the extraction efficiency of the method such as pH, flow rate and volume of the sample solution, concentration of chromazurol S (CAS) and cethyltrimethylammonium bromide (CTAB) as well as type and concentration of eluent were investigated and optimized. The ion-pair (Cu(II)-CAS-CTAB) was quantitatively retained on the cotton under the optimum conditions, then eluted completely using a solution of 25% (v/v) 1-propanol in 0.5 mol L(-1) HNO(3) and directly introduced into the nebulizer of the ICP-OES. The detection limit (DL) of the method for copper was 40 ng L(-1) (V(sample)=100mL) and the relative standard deviation (R.S.D.) for the determination of copper at 10 microg L(-1) level was found to be 1.3%. The method was successfully applied to determine the trace amounts of copper in tap water, deep well water, seawater and two different mineral waters, and suitable recoveries were obtained (92-106%).

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

    PubMed

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

    2016-01-01

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

  10. On-line dynamic extraction system hyphenated to inductively coupled plasma optical emission spectrometry for automatic determination of oral bioaccessible trace metal fractions in airborne particulate matter.

    PubMed

    Mohr, Victoria; Miró, Manuel; Limbeck, Andreas

    2017-04-01

    For a realistic evaluation of the potential hazard emanating from airborne particulate matter (APM), the determination of the total inhaled metal amounts associated with APM is insufficient in risk assessment. Additional information about metal fractions that can be mobilized by the human body is necessary, because only those soluble (also called bioaccessible) fractions can be absorbed by the human body, and thus potentially cause adverse health effects. In the present study, a dynamic flow-through approach as a front end to inductively coupled plasma optical emission spectrometry (ICP-OES) exploiting advanced flow analysis is employed for on-line handling of multiple APM samples and determination of bioaccessible trace metals under worst case extraction scenarios. The method is based on on-line continuous extraction of filter samples with synthetic gastric fluid followed by on-line ICP-OES measurement of the dissolved fraction of trace metals. The assembly permits an automated successive measurement of three sample replicates in less than 19 min. The on-line extraction procedure offers increased sample throughput and reduced risk of sample contamination and overcomes metal re-adsorption processes compared to the traditional batch-wise counterparts. Furthermore, it provides deeper information on the kinetics of the leaching process. The developed procedure was applied to the determination of bioaccessible metal fractions (Al, Ba, Cu, Fe and Mn as model analytes) in PM10 samples from Palma de Mallorca (Spain) and Vienna (Austria). Graphical Abstract On-line gastric bioaccessibility of elements in airborne particulate matter.

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

    PubMed

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

    2014-01-01

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

  12. Development of a model for characterizing pneumatically generated primary aerosols for inductively coupled plasma emission spectrometry

    SciTech Connect

    Msimanga, N.D.G.

    1992-01-01

    The study of aerosols plays a key role in the development of analytical atomic spectroscopy. While work has been carried out with Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) to improve transport efficiency, analyte signal, limits of detection, and to reduce matrix interferences, little study has focused on sample introduction processes. This study has focused on the characterization and optimization of pneumatic nebulizers used for liquid sample introduction to the ICP. Pneumatic nebulization is the most common means of sample introduction in atomic spectrometry. The pneumatic nebulizers most commonly used today for ICP spectrometry are the cross-flow type or all-glass concentric nebulizers. Aerosols undergo certain processes after the primary formation process before reaching the atomizer, the secondary and tertiary stages. In this work all three stages were looked at, focusing on the primary aerosols. The primary aerosol is the first stage in the formation of the aerosols and takes place at the tip of the nebulizer, as the liquid stream is shattered by the gas flow. The drop size diameters of primary aerosols were measured using a Fraunhofer Laser Diffraction instrument. The Sauter mean diameter (D3.2), which describes the volume of the aerosol with a given surface area, was determined for nebulizers at spray chambers operated under a variety of conditions. The characterization and optimization of sample introduction involved a study of aerosol technology, a study of different instruments for measuring the mean drop size, a description of the instrument, and the influence of some parameters on the D3.2. An empirical model summarizing the characteristics of the primary aerosols is proposed. Modeling is carried out using nonlinear software. The data for modelling were acquired using water, n-butanol, and methanol as the liquid solvents. The model was tested on data obtained from nebulizers with different cross-sectional areas.

  13. Validation of an inductively coupled plasma mass spectrometry (ICP-MS) method for the determination of cerium, strontium, and titanium in ceramic materials used in radiological dispersal devices (RDDs).

    PubMed

    Packer, Ana Paula; Larivière, Dominic; Li, Chunsheng; Chen, Michael; Fawcett, Amanda; Nielsen, Kathy; Mattson, Kristine; Chatt, Amares; Scriver, Christine; Erhardt, Lorne S

    2007-04-11

    In radiological dispersal device (RDD) studies, sintered ceramics made of CeO2 and SrTiO3 were used to simulate actinide oxides and (90)SrTiO3, respectively. Instrumental neutron activation analysis (INAA), inductively coupled plasma optical emission spectroscopy (ICP-OES), and inductively coupled plasma mass spectrometry (ICP-MS) were investigated as possible analytical techniques for the measurement of SrTiO3 and CeO2 constituents in powder forms, sintered ceramics, and air particulates collected following a detonation. For ICP-OES and ICP-MS analysis, new digestion procedures were developed using a closed-vessel microwave apparatus. Acid mixtures (HNO3:H2O2:HF (16:2:1) and HNO3:H2O2 (1:4)) were found to be effective for the digestion of SrTiO3 and CeO2, respectively. The intercomparison study confirmed that the results obtained by ICP-OES/MS are in good agreement with INAA results. This also confirms the efficiency of the digestion procedures for these refractory materials and the inter-exchangeability of the instrumentation tested. Comparison between the ICP-OES and the ICP-MS instrumentation for the determination of air particulates shows, that although the two methods are equivalent, ICP-MS provides better detection limits (0.11, 0.02, and 0.04 microg per filter for Ti, Sr, and Ce, respectively) and the possibility to determine isotopic fractionation as the result of an explosion.

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

    NASA Astrophysics Data System (ADS)

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

    2009-06-01

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

  15. Screening of TiO2 and Au nanoparticles in cosmetics and determination of elemental impurities by multiple techniques (DLS, SP-ICP-MS, ICP-MS and ICP-OES).

    PubMed

    de la Calle, Inmaculada; Menta, Mathieu; Klein, Marlène; Séby, Fabienne

    2017-08-15

    Cosmetics are part of the daily life of most of the people. Thus, a complete characterization of the products we applied in our skin is necessary. In this work, an analytical investigation of a wide variety of cosmetics from the point of view of total element content and metallic nanoparticles (NPs) has been performed. Firstly, we analyzed the total element content by ICP-MS and ICP-OES after acid digestion as an assessment of the presence of metal impurities. Prohibited elements in cosmetics, according to the European Commission regulation No 1223/2009, were not detected, and only elements mentioned in the label were found (e.g. Al, Fe, Ti and Si). Secondly, a screening of the presence of NPs has been performed by Dynamic Light Scattering (DLS) and Single Particle Inductively-Coupled Plasma Mass Spectrometry (SP-ICP-MS). Two sample preparation procedures were applied. The first protocol consisted in the preparation of suspensions in 0.1% w/v SDS and the second based on defatting with hexane followed by resuspension in water. DLS was employed as a routine method for a fast analysis of NPs, but this technique showed limitations due to the lack of specificity. SP-ICP-MS analyses were then performed, first as a screening technique to evaluate the presence of TiO2 and Au NPs in cosmetics suspensions prepared in SDS; and second, when a positive answer was obtained about the presence of NPs from the screening, SP-ICP-MS was used for particle size determination. Results showed that only TiO2 NPs were present in two sunscreens, one anti-wrinkle day cream, one lip balm protector labeled as 'nano' and in one brand of toothpaste not labeled as 'nano'. Sizes obtained for both sample preparations were compared and ranged from 30 to 120nm in most of the samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  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.

    PubMed

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

    NASA Astrophysics Data System (ADS)

    Li, Yingjie; Hu, Bin

    2007-10-01

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

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

    PubMed

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

    2016-09-06

    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%.

  19. Speciation analysis of Mn(II)/Mn(VII) using Fe3O4@ionic liquids-β-cyclodextrin polymer magnetic solid phase extraction coupled with ICP-OES.

    PubMed

    Chen, Songqing; Qin, Xingxiu; Gu, Weixi; Zhu, Xiashi

    2016-12-01

    Ionic liquids-β-cyclodextrin polymer (ILs-β-CDCP) was attached on Fe3O4 nanoparticles to prepare magnetic solid phase extraction agent (Fe3O4@ILs-β-CDCP). The properties and morphology of Fe3O4@ILs-β-CDCP were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction(XRD), size distribution and magnetic analysis. A new method of magnetic solid phase extraction (MSPE) coupled to ICP-OES for the speciation of Mn(II)/Mn(VII) in water samples was established. The results showed that Mn(VII) and total manganese [Mn(II)+Mn(VII)] were quantitatively extracted after adjusting aqueous sample solution to pH 6.0 and 10.0, respectively. Mn(II) was calculated by subtraction of Mn(VII) from total manganese. Fe3O4@ILs-β-CDCP showed a higher adsorption capacity toward Mn(II) and Mn(VII). Several factors, such as the pH value, extraction temperature and sample volume, were optimized to achieve the best extraction efficiency. Moreover, the adsorption ability of Fe3O4@ILs-β-CDCP would not be significantly lower after reusing of 10 times. The accuracy of the developed method was confirmed by analyzing certified reference materials (GSB 07-1189-2000), and by spiking spring water, city water and lake water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Dye-doped nanostructure polypyrrole film for electrochemically switching solid-phase microextraction of Ni(II) and ICP-OES analysis of waste water.

    PubMed

    Shamaeli, Ehsan; Alizadeh, Naader

    2012-01-01

    A nanostructure fiber based on conducting polypyrrole synthesized by an electrochemical method has been developed, and used for electrochemically switching solid-phase microextraction (ES-SPME). The ES-SPME was prepared by the doping of eriochrome blue in polypyrrole (PPy-ECB) and used for selectively extracting the Ni(II) cation in the presence of some transition and heavy metal ions. The cation-exchange behavior of electrochemically prepared polypyrrole on stainless-steel with and without eriochrome blue (ECB) dye was characterized using ICP-OES analysis. The effects of the scan rate for electrochemical synthesis, uptake and the release potential on the extraction behavior of the PPy-ECB conductive fiber were studied. Uptake and release time profiles show that the process of electrically switched cation exchange could be completed within 250 s. The results of the present study point concerning the possibility of developing a selective extraction process for Ni(II) from waste water was explored using such a nanostructured PPy-ECB film through an electrically switched cation exchange. 2012 © The Japan Society for Analytical Chemistry

  1. Use of a simplified generalized standard additions method for the analysis of cement, gypsum and basic slag by slurry nebulization ICP-OES.

    PubMed

    Marjanovic, Ljiljana; McCrindle, Robert I; Botha, Barend M; Potgieter, Herman J

    2004-05-01

    The simplified generalized standard additions method (GSAM) was investigated as an alternative method for the ICP-OES analysis of solid materials, introduced into the plasma in the form of slurries. The method is an expansion of the conventional standard additions method. It is based on the principle of varying both the sample mass and the amount of standard solution added. The relationship between the sample mass, standard solution added and signal intensity is assumed to be linear. Concentration of the analyte can be found either geometrically from the slope of the two-dimensional response plane in a three-dimensional space or mathematically from the ratio of the parameters estimated by multiple linear regression. The analysis of a series of certified reference materials (CRMs) (cement CRM-BCS No 353, gypsum CRM-Gyp A and basic slag CRM No 382/I) introduced into the plasma in the form of slurry is described. The slurries contained glycerol and hydrochloric acid and were placed in an ultrasonic bath to ensure good dispersion. "Table curve 3D" software was used to fit the data. Results obtained showed that the method could be successfully applied to the analysis of cement, gypsum and slag samples, without the need to dissolve them. In this way, we could avoid the use of hazardous chemicals (concentrated acids), incomplete dissolution and loss of some volatiles. The application of the simplified GSAM for the analysis did not require a CRM with similar chemical and mineralogical properties for the calibration of the instrument.

  2. Analysis of heavy metal distribution in superficial estuarine sediments (estuary of Bilbao, Basque Country) by open-focused microwave-assisted extraction and ICP-OES.

    PubMed

    Landajo, Amaia; Arana, Gorka; de Diego, Alberto; Etxebarria, Nestor; Zuloaga, Olatz; Amouroux, David

    2004-09-01

    Open-focused microwave-assisted extraction and ICP-OES determination of As, Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn from surface sediments of the estuary of Bilbao (Basque Country, North of Spain) was carried out. All the samples were collected at three different tributaries of the estuary (Asua, Galindo and Nerbioi-Ibaizabal) every two months during 1999. The digestion procedure was proposed from the conclusions of a fractionated factorial design, and the precision and accuracy of the method was verified using a certified reference sediment (RTC008-050). The results of the analysis were statistically treated by means of principal component analysis and correlation analysis. The principal component analysis of sediment data (32 samples x 9 metals) indicated different patterns of contamination regarding the tributary and sampling station. The two main patterns observed were a steady increment of the metal concentration along all the campaigns in the samples collected in the Galindo River and a seasonal variation in the Nerbioi-Ibaizabal River, with higher metallic content during summertime and lower content during wintertime.

  3. Comparison of dry, wet and microwave digestion methods for the multi element determination in some dried fruit samples by ICP-OES.

    PubMed

    Altundag, Huseyin; Tuzen, Mustafa

    2011-11-01

    The aim of this study was used to investigate the level of trace metals (Ba, Pb, Cd, Mn, Cr, Co, Ni, Cu, Mn, Zn, Sr and Fe) in some dried fruits (Prunus domestica L., Ficus carica L., Morus alba L., Vitis vinifera L., Prunus armeniaca L., and Malus domestica) samples from Turkey. Trace elements were determined by ICP-OES after dry, wet and microwave digestion methods in dried fruit samples. Validation of the proposed method was carried out by using a NIST-SRM 1515-Apple Leaves certified reference material. Element concentrations in dried fruit samples were 0.33-1.77 (Ba), 0.12-0.54 (Cd), 0.25-1.03 (Co), 0.45-2.30 (Cr), 0.43-2.74 (Cu), 0.56-4.87 (Mn), 0.61-2.54 (Ni), 0.40-2.14 (Pb), 2.16-6.54 (Zn), 0.83-12.02 (Al), 11.82-40.80 (Fe) and 0.16-6.34 (Sr) μg/g. The analytical parameters show that the microwave oven digestion procedure provided best results as compared to the wet and dry digestion procedures. The results were compared with the literature values.

  4. Determination of tungsten in tantalum-tungsten alloy by X-ray fluorescence spectrometry using fusion, thin layer, and pressed powder pellet techniques

    NASA Astrophysics Data System (ADS)

    Tian, Lunfu; Zou, Deshuang; Dai, Yichun; Tang, Guangping

    2015-08-01

    A method is described for the X-ray fluorescence (XRF) determination of tungsten in tantalum-tungsten alloy over the range of 10.5%-13.5%. The sample was prepared by three methods, namely, borate fusion, filter paper disk, and pressed powder pellet, respectively. We compared the feature of the three methods of specimen preparation and found that filter paper disk method was the most suitable technique for specimen preparation. Furthermore, the results were compared with those given by inductively coupled plasma optical emission spectrometry (ICP-OES), and the relative standard deviation was less than 2%, which could meet the requirement of this application.

  5. 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.

    PubMed

    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.

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

    PubMed Central

    Baytak, Sıtkı; Arslan, Zikri

    2015-01-01

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

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

    PubMed

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

    2012-11-15

    A dual-cloud point extraction (d-CPE) procedure has been developed for simultaneous pre-concentration and separation of heavy metal ions (Cd2+, Co2+, Ni2+, Pb2+, Zn2+, and Cu2+ ion) in water samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on forming complexes of metal ion with 8-hydroxyquinoline (8-HQ) into the as-formed Triton X-114 surfactant rich phase. Instead of direct injection or analysis, the surfactant rich phase containing the complexes was treated by nitric acid, and the detected ions were back extracted again into aqueous phase at the second cloud point extraction stage, and finally determined by ICP-OES. Under the optimum conditions (pH=7.0, Triton X-114=0.05% (w/v), 8-HQ=2.0×10(-4) mol L(-1), HNO3=0.8 mol L(-1)), the detection limits for Cd2+, Co2+, Ni2+, Pb2+, Zn2+, and Cu2+ ions were 0.01, 0.04, 0.01, 0.34, 0.05, and 0.04 μg L(-1), respectively. Relative standard deviation (RSD) values for 10 replicates at 100 μg L(-1) were lower than 6.0%. The proposed method could be successfully applied to the determination of Cd2+, Co2+, Ni2+, Pb2+, Zn2+, and Cu2+ ion in water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Multivariate optimization of an analytical method for the analysis of dog and cat foods by ICP OES.

    PubMed

    da Costa, Silvânio Silvério Lopes; Pereira, Ana Cristina Lima; Passos, Elisangela Andrade; Alves, José do Patrocínio Hora; Garcia, Carlos Alexandre Borges; Araujo, Rennan Geovanny Oliveira

    2013-04-15

    Experimental design methodology was used to optimize an analytical method for determination of the mineral element composition (Al, Ca, Cd, Cr, Cu, Ba, Fe, K, Mg, Mn, P, S, Sr and Zn) of dog and cat foods. Two-level full factorial design was applied to define the optimal proportions of the reagents used for microwave-assisted sample digestion (2.0 mol L(-1) HNO3 and 6% m/v H2O2). A three-level factorial design for two variables was used to optimize the operational conditions of the inductively coupled plasma optical emission spectrometer, employed for analysis of the extracts. A radiofrequency power of 1.2 kW and a nebulizer argon flow of 1.0 L min(-1) were selected. The limits of quantification (LOQ) were between 0.03 μg g(-1) (Cr, 267.716 nm) and 87 μg g(-1) (Ca, 373.690 nm). The trueness of the optimized method was evaluated by analysis of five certified reference materials (CRMs): wheat flour (NIST 1567a), bovine liver (NIST 1577), peach leaves (NIST 1547), oyster tissue (NIST 1566b), and fish protein (DORM-3). The recovery values obtained for the CRMs were between 80 ± 4% (Cr) and 117 ± 5% (Cd), with relative standard deviations (RSDs) better than 5%, demonstrating that the proposed method offered good trueness and precision. Ten samples of pet food (five each of cat and dog food) were acquired at supermarkets in Aracaju city (Sergipe State, Brazil). Concentrations in the dog food ranged between 7.1 mg kg(-1) (Ba) and 2.7 g kg(-1) (Ca), while for cat food the values were between 3.7 mg kg(-1) (Ba) and 3.0 g kg(-1) (Ca). The concentrations of Ca, K, Mg, P, Cu, Fe, Mn, and Zn in the food were compared with the guidelines of the United States' Association of American Feed Control Officials (AAFCO) and the Brazilian Ministry of Agriculture, Livestock, and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento-MAPA). Copyright © 2013 Elsevier B.V. All rights reserved.

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

    PubMed

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

    2009-08-15

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

  10. The use of silica-immobilized brown alga (Pilayella littoralis) for metal preconcentration and determination by inductively coupled plasma optical emission spectrometry.

    PubMed

    Carrilho, Elma Neide V M; Nóbrega, Joaquim A; Gilbert, Thomas R

    2003-08-29

    The brown alga Pilayella littoralis was used as a new biosorbent in an on-line metal preconcentration procedure in a flow-injection system. Al, Co, Cu and Fe were determined in lake water samples by inductively coupled plasma optical emission spectrometry (ICP-OES) after preconcentration in a silica-immobilized alga column. Like other algae, P. littoralis exhibited strong affinity for these metals proving to be an effective accumulation medium. Metals were bound at pH 5.5 and were displaced at pH<2 with diluted HCl. The enrichment factors for Cu(II), Fe(III), Al(III) and Co(II) were 13, 7, 16 and 11, respectively. Metal sorption efficiency ranged from 86 to 90%. The method accuracy was assessed by using drinking water certified reference material and graphite furnace atomic absorption spectrometry (GFAAS) as a comparison technique. The column procedure allowed a less time consuming, easy regeneration of the biomaterial and rigidity of the alga provided by its immobilization on silica gel.

  11. Determination of copper in liquid and solid insulation for large electrical equipment by ICP-OES. Application to copper contamination assessment in power transformers.

    PubMed

    Bruzzoniti, Maria Concetta; De Carlo, Rosa Maria; Sarzanini, Corrado; Maina, Riccardo; Tumiatti, Vander

    2012-09-15

    Copper is one of the main constituents of the components in power transformers and its presence both in liquid (mineral oil) and in solid (Kraft paper) insulators can lead to enhanced dielectric losses and to the subsequent deterioration of their insulating properties. Recently the latter have been correlated to plant failures which in turn may have severe impact on the environment. This paper describes the direct analysis of copper in insulating mineral oil by ICP-OES and how it was first optimized compared to the official American Society for Testing and Materials (ASTM) D7151 method. Detection and quantification limits of 8.8 μg kg(-1) and 29.3 μg kg(-1) were obtained. Secondly, copper determination was improved by coupling a microwave assisted dissolution procedure of the mineral oil which avoided the problems, in the real samples, due to the presence of solid species of copper which cannot be nebulized following traditional methods described in literature. Sixteen mineral insulating oils sampled from transformers in service were analyzed before and after dissolution. In order to evaluate copper speciation, size fractionation was performed by filtration on PTFE filters (0.45, 1 and 5 μm). This test was performed on all the oil samples. Finally, because of the key role of the solid insulator in failed transformers, the Authors applied the developed method to study the copper deposition tendency onto the insulating Kraft paper tapes exerted by two unused oils (a corrosive and a non-corrosive one) under defined ageing conditions.

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

    NASA Astrophysics Data System (ADS)

    Santelli, Ricardo Erthal; Oliveira, Eliane Padua; de Carvalho, Maria de Fátima Batista; Bezerra, Marcos Almeida; Freire, Aline Soares

    2008-07-01

    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 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 μg g - 1 , respectively. Precision values, expressed as the relative standard deviations (% RSD, n = 10) for 12 and 400 μg g - 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 Niterói/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 types of samples

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

    PubMed

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

    2015-11-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-06-01

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

  15. Determination of boron content and isotopic composition in gypsum by inductively coupled plasma optical emission spectroscopy and positive thermal ionization mass spectrometry using phase transformation.

    PubMed

    Ma, Yun-Qi; Peng, Zhang-Kuang; Yang, Jian; Xiao, Ying-Kai; Zhang, Yan-Ling

    2017-12-01

    As a stable isotope, boron plays an important role in hydrogeology, environmental geochemistry, ore deposit geochemistry and marine paleoclimatology. However, there is no report of boron isotopic composition in gypsum. This is mainly confined to complete dissolution of Gypsum by water or acid. In this study, gypsum was converted to calcium carbonate (CaCO3) with ammonium bicarbonate(NH4HCO3) by two steps at 50°C. In every step, the mass ratio of NH4HCO3/CaSO4·2H2O was twice, and conversion rate reached more than 98%. Converted CaCO3 was totally dissolved with hydrochloric acid (the dissolution rate was over 99%). In order to overcome the difficulties of the matrix interference and the detection limit of Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES), we use Amberlite IRA 743 resin to purify and enrichment the boron at first, then eluting boron from the resin with 10mL 0.1mol/L hydrochloric acid at 75°C. The boron isotopic composition of natural gypsum samples was determined using positive thermal ionization mass spectrometry (P-TIMS). The boron isotopic composition of gypsum may be an excellent indicator for the formation environment. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    PubMed

    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).

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

    PubMed

    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.

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

    PubMed

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

    2009-11-15

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

  19. Determination of platinum in waste platinum-loaded carbon catalyst samples using microwave-assisted sample digestion and ICP-OES

    NASA Astrophysics Data System (ADS)

    Ma, Yinbiao; Wei, Xiaojuan

    2017-04-01

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

  20. Liquid sample introduction in inductively coupled plasma atomic emission and mass spectrometry - Critical review

    NASA Astrophysics Data System (ADS)

    Bings, N. H.; Orlandini von Niessen, J. O.; Schaper, J. N.

    2014-10-01

    Inductively coupled plasma optical emission spectroscopy (ICP-OES) and mass spectrometry (ICP-MS) can be considered as the most important tools in inorganic analytical chemistry. Huge progress has been made since the first analytical applications of the ICP. More stable RF generators, improved spectrometers and detection systems were designed along with the achievements gained from advanced microelectronics, leading to overall greatly improved analytical performance of such instruments. In contrast, for the vast majority of cases liquid sample introduction is still based on the pneumatic principle as described in the late 19th century. High flow pneumatic nebulizers typically demand the use of spray chambers as “aerosol filters” in order to match the prerequisites of an ICP. By this, only a small fraction of the nebulized sample actually contributes to the measured signal. Hence, the development of micronebulizers was brought forward. Those systems produce fine aerosols at low sample uptake rates, but they are even more prone for blocking or clogging than conventional systems in the case of solutions containing a significant amount of total dissolved solids (TDS). Despite the high number of publications devoted to liquid sample introduction, it is still considered the Achilles' heel of atomic spectrometry and it is well accepted, that the technology used for liquid sample introduction is still far from ideal, even when applying state-of-the-art systems. Therefore, this review is devoted to offer an update on developments in the field liquid sample introduction that had been reported until the year 2013. The most recent and noteworthy contributions to this field are discussed, trends are highlighted and future directions are outlined. The first part of this review provides a brief overview on theoretical considerations regarding conventional pneumatic nebulization, the fundamentals on aerosol generation and discusses characteristics of aerosols ideally suited

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

    PubMed

    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%).

  2. Evaluation of the metal uptake of several algae strains in a multicomponent matrix utilizing inductively coupled plasma emission spectrometry.

    PubMed

    Mahan, C A; Majidi, V; Holcombe, J A

    1989-03-15

    Three freshwater heat-killed, lyophilized blue-green algae strains have been characterized as to their ability to accumulate heavy metals with a focus on the utilization of these algae as an analytical preconcentration technique. This study examines the metal uptake in several multicomponent mixtures by using inductively coupled plasma optical emission spectrometry (ICP-OES). Six milligrams of a pure strain of algae was added to 20-mL aliquots of buffered (pH 5.5-6.5) multielement solutions containing 0.1, 0.5, 1.0, 2.0, and 4.0 mg/L of K, Mg, Ca, Fe, Sr, Co, Cu, Mn, Ni, V, Zn, As, Cd, Mo, Pb, and Se. All three algae strains exhibit relatively high adsorption affinities for Fe, Pb, and Cu, with uptake between 70 and 98% at the 4 ppm concentration level. Biosorption occurs for essentially every element with the relative affinities decreasing in the order Pb greater than Fe greater than Cu greater than Cd greater than Zn greater than Mn greater than Mo greater than Sr greater than Ni greater than V greater than Se greater than As greater than Co for Chlorella pyrenoidosa at the 4 mg/L concentration level. Although some minor differences were seen, the other algae strains (Stichococcus bacillaris and Chlamydomonas reinharti) displayed similar adsorption behavior over the concentration range studied, indicating similar cell wall binding sites. Langmuirian isotherms exhibited a minimum of two slopes over the concentration range of 0.1-4.0 mg/L, indicating the probable existence of at least two adsorption mechanisms.

  3. Evaluation of the metal uptake of several algae strains in a multicomponent matrix utilizing inductively coupled plasma emission spectrometry

    SciTech Connect

    Mahan, C.A.; Majidi, V.; Holcombe, J.A.

    1989-03-15

    Three freshwater heat-killed, lyophilized blue-green algae strains have been characterized as to their ability to accumulate heavy metals with a focus on the utilization of these algae as an analytical preconcentration technique. This study examines the metal uptake in several multicomponent mixtures by using inductively coupled plasma optical emission spectrometry (ICP-OES). Six milligrams of a pure strain of algae was added to 20-mL aliquots of buffered (pH 5.5-6.5) multielement solutions containing 0.1, 0.5, 1.0, 2.0, and 4.0 mg/L of K, Mg, Ca, Fe, Sr, Co, Cu, Mn, Ni, V, Zn, As, Cd, Mo, Pb, and Se. All three algae strains exhibit relatively high adsorption affinities for Fe, Pb, and Cu, with uptake between 70 and 98% at the 4 ppm concentration level. Biosorption occurs for essentially every element with the relative affinities decreasing in the order Pb greater than Fe greater than Cu greater than Cd greater than Zn greater than Mn greater than Mo greater than Sr greater than Ni greater than V greater than Se greater than As greater than Co for Chlorella pyrenoidosa at the 4 mg/L concentration level. Although some minor differences were seen, the other algae strains (Stichococcus bacillaris and Chlamydomonas reinharti) displayed similar adsorption behavior over the concentration range studied, indicating similar cell wall binding sites. Langmuirian isotherms exhibited a minimum of two slopes over the concentration range of 0.1-4.0 mg/L, indicating the probable existence of at least two adsorption mechanisms.

  4. Determination of Zn in Dry Feeds for Cats and Dogs by Energy-Dispersive X-Ray Fluorescence Spectrometry.

    PubMed

    Ávila, Dayara Virgnía L; Souza, Sidnei O; Costa, Silvânio Silvério L; Araujo, Rennan Geovanny O; Garcia, Carlos Alexandre B; Alves, José do Patrocínio H; Passos, Elisangela A

    2016-11-01

    This work describes an analytical method for Zn determination in dry feeds for cats and dogs by energy-dispersive X-ray fluorescence (EDXRF). Samples of dry feed were powdered and prepared in the form of pellets for direct analysis by EDXRF. The LOQ (10σ) was 0.4 mg/kg. The samples were also analyzed by inductively coupled plasma-optical emission spectrometry (ICP-OES) as an independent comparative method. Application of a paired t-test showed no significant differences between Zn concentrations obtained by EDXRF and ICP-OES (at a 95% confidence level). Analysis of variance was also applied to the results and revealed no significant differences between the two techniques (at a 95% confidence level). The precision, expressed as the RSD (n = 3), was RSD < 4.55%. This analytical method provides a simple, rapid, accurate, and precise determination of Zn in dry feeds for cats and dogs by EDXRF as direct, solid-sample analysis.

  5. Tungsten coil atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

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

    2006-02-01

    A tungsten coil atomic emission spectrometer is described and evaluated. The system employs a single tungsten coil as a combined atomizer and excitation source for the determination of metals by atomic emission spectrometry. The tungsten coil is extracted from a 150 W, 15 V commercial slide projector light bulb. A simple, laboratory constructed, computer-controlled power supply provides a constant current to the coil. A high-resolution Czerny-Turner monochromator with a charge coupled device detector completes the system. Simultaneous, multi-element analyses are possible within a 4 nm spectral window. Eleven test elements are used to characterize the system: Al (396.1 nm), Co (353.0 nm), Cr (427.1 nm), Dy (404.6 nm), Ga (403.3 nm), K (404.4 nm), Mn (403.1 nm), Pb (405.8 nm), Rb (420.2 nm), Sc (404.8 nm), and Yb (398.7 nm). Tungsten coil atomic emission detection limits are reported for these elements for the first time: 0.02 ng Al, 0.7 ng Co, 0.003 ng Cr, 0.01 ng Dy, 0.7 ng Ga, 0.3 ng K, 0.04 ng Mn, 10 ng Pb, 0.07 ng Rb, 1 ng Sc, and 0.003 ng Yb. The precision for the new technique is better than 13% relative standard deviation for all metals at concentrations two orders of magnitude above the detection limit. Aluminum, Cr, Mn, and K are determined in a standard reference material (trace elements in water) after simple dilution with water, and found values varied from certified values by up to 26%. The average tungsten coil lifetime was found to be 265 heating cycles. The elimination of the external radiation source needed for atomic absorption measurements results in an emission system that could be quite portable.

  6. Determination of scandium in acid mine drainage by ICP-OES with flow injection on-line preconcentration using oxidized multiwalled carbon nanotubes.

    PubMed

    Jerez, Javier; Isaguirre, Andrea C; Bazán, Cristian; Martinez, Luis D; Cerutti, Soledad

    2014-06-01

    An on-line scandium preconcentration and determination system implemented with inductively coupled plasma optical emission spectrometry associated with flow injection was studied. Trace amounts of scandium were preconcentrated by sorption on a minicolumn packed with oxidized multiwalled carbon nanotubes, at pH 1.5. The retained analyte was removed from the minicolumn with 30% (v/v) nitric acid. A total enrichment factor of 225-fold was obtained within a preconcentration time of 300 s (for a 25 mL sample volume). The overall time required for preconcentration and elution of 25 mL of sample was about 6 min; the throughput was about 10 samples per hour. The value of the detection limit was 4 ng L(-1) and the precision for 10 replicate determinations at 100 ng L(-1) Sc level was 5% relative standard deviation, calculated from the peak heights obtained. The calibration graph using the preconcentration system was linear with a correlation coefficient of 0.9996 at levels near the detection limits up to at least 10 mg L(-1). After optimization, the method was successfully applied to the determination of Sc in an acid drainage from an abandoned mine located in the province of San Luis, Argentina.

  7. Determination of some traces metal levels in cheese samples packaged in plastic and tin containers by ICP-OES after dry, wet and microwave digestion.

    PubMed

    Bakircioglu, Dilek; Kurtulus, Yasemin Bakircioglu; Ucar, Gokhan

    2011-01-01

    The concentrations of Cd, Co, Cr, Cu, Mn, Ni, Pb, Se and Zn in cheese samples packaged in plastic and tin containers were analyzed using inductively coupled plasma-optical emission spectrometry after microwave, wet and dry digestion processes. In order to evaluate the best digestion method, the relationships between the concentrations of trace metals in cheese samples after microwave digestion was compared by wet and dry ashings. Microwave digestion was found fast, reliable, simple, and excellent procedure in comparison with dry and wet ashing methods. The accuracy of the digestion procedures was determined by using standard reference material (GBW 07605-Tea). The order of levels of the elements in the white cheese samples packaged in tin containers was determined to be Cd

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

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

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

  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.

    PubMed

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

    2013-11-15

    A novel restricted accessed material (RAM)-Cu(II) ion imprinted polymer (IIP) was synthesized by the surface imprinted-emulsion method, and possessed a high selectivity to Cu(II) and good macromolecules exclusion property. And a novel method of RAM-IIP packed microcolumn solid phase extraction (SPE) combined with inductively coupled plasma-optical emission spectrometry (ICP-OES) was developed for the determination of trace free Cu(II) in human body fluids. Under the optimized conditions, the adsorption capacity of RAM-IIP for Cu(II) was 15.9 mg g(-1). With a preconcentration factor of 30, the limit of detection was 0.17 µg L(-1), and the relative standard deviation was 2.2% (n=7, c=1 µg L(-1)). The developed method was validated by the analysis of two Certified Reference Materials, and the determined values were in good agreement with the certified values. This method was also successfully applied for the direct analysis of free Cu(II) in human urine and serum samples. While the total Cu can be determined by the proposed method after microwave digestion. The concentrations of free Cu(II) were much lower than that of total Cu, indicating that Cu is mainly coordinated with macromolecules in these biological samples. From this point of view, the developed method exhibits application potential in speciation of free metal ions and metallic complex molecules in biological samples. © 2013 Elsevier B.V. All rights reserved.

  11. [Determination of barium in natural curative waters by ICP-OES technique. Part I. Waters taken on the area of health resorts in Poland].

    PubMed

    Garboś, Sławomir; Swiecicka, Dorota

    2011-01-01

    Maximum admissible concentration level (MACL) of barium in natural mineral waters, natural spring waters and potable waters was set at the level of 1 mg/l, while MACL of this element in natural curative waters intended for drinking therapies and inhalations were set at the levels of 1.0 mg/l and 10.0 mg/l, respectively. Those requirements were related to therapies which are applied longer than one month. Above mentioned maximum admissible concentration levels of barium in consumed waters were established after taking into account actual criteria of World Health Organization which determined the guidelines value for this element in water intended for human consumption at the level of 0.7 mg/l. In this work developed and validated method of determination of barium by inductively coupled plasma emission spectrometry technique was applied for determination of this element in 45 natural curative waters sampled from 24 spa districts situated on the area of Poland. Concentrations of barium determined were in the range from 0.0036 mg/l to 24.0 mg/l. Natural curative waters characterized by concentrations of barium in the ranges of 0.0036 - 0.073 mg/l, 0.0036 - 1.31 mg/l and 0.0036 - 24.0 mg/l, were applied to drinking therapy, inhalations and balneotherapy, respectively (some of waters analyzed were simultaneously applied to drinking therapy, inhalations and balneotherapy). In the cases of 11 natural curative waters exceeding limit of 1 mg/l were observed, however they were classified mainly as waters applied to balneotherapy and in two cases to inhalation therapies (concentrations of barium - 1.08 mg/l and 1.31 mg/l). The procedure of classification of curative waters for adequate therapies based among other things on barium concentrations meets requirements of the Decree of Minister of Health from 13 April 2006 on the range of studies indispensable for establishing medicinal properties of natural curative materials and curative properties of climate, criteria of their

  12. Determination of low cadmium concentrations in wine by on-line preconcentration in a knotted reactor coupled to an inductively coupled plasma optical emission spectrometer with ultrasonic nebulization.

    PubMed

    Lara, R F; Wuilloud, R G; Salonia, J A; Olsina, R A; Martinez, L D

    2001-12-01

    An on-line cadmium preconcentration and determination system implemented with inductively coupled plasma optical emission spectrometry (ICP-OES) associated to flow injection (FI) with ultrasonic nebulization system (USN) was studied. The cadmium was retained as the cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol, Cd-(5-Br-PADAP), complex, at pH 9.5. The cadmium complex was removed from the knotted reactor (KR) with 3.0 mol/L nitric acid. A total enhancement factor of 216 was obtained with respect to ICP-OES using pneumatic nebulization (12 for USN and 18 for KR) with a preconcentration time of 60 s. The value of the detection limit for the preconcentration of 5 mL of sample solution was 5 ng/L. The precision for 10 replicate determinations at the 5 microg/L Cd level was 2.9% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for cadmium was linear with a correlation coefficient of 0.9998 at levels near the detection limits up to at least 1,000 microg/L. The method was successfully applied to the determination of cadmium in wine samples.

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

    PubMed

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

    2013-10-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2011-05-01

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

  15. A comparison of portable XRF and ICP-OES analysis for lead on air filter samples from a lead ore concentrator mill and a lead-acid battery recycler.

    PubMed

    Harper, Martin; Pacolay, Bruce; Hintz, Patrick; Andrew, Michael E

    2006-03-01

    Personal and area samples for airborne lead were taken at a lead mine concentrator mill, and at a lead-acid battery recycler. Lead is mined as its sulfidic ore, galena, which is often associated with zinc and silver. The ore typically is concentrated, and partially separated, on site by crushing and differential froth flotation of the ore minerals before being sent to a primary smelter. Besides lead, zinc and iron are also present in the airborne dusts, together with insignificant levels of copper and silver, and, in one area, manganese. The disposal of used lead-acid batteries presents environmental issues, and is also a waste of recoverable materials. Recycling operations allow for the recovery of lead, which can then be sold back to battery manufacturers to form a closed loop. At the recycling facility lead is the chief airborne metal, together with minor antimony and tin, but several other metals are generally present in much smaller quantities, including copper, chromium, manganese and cadmium. Samplers used in these studies included the closed-face 37 mm filter cassette (the current US standard method for lead sampling), the 37 mm GSP or "cone" sampler, the 25 mm Institute of Occupational Medicine (IOM) inhalable sampler, the 25 mm Button sampler, and the open-face 25 mm cassette. Mixed cellulose-ester filters were used in all samplers. The filters were analyzed after sampling for their content of the various metals, particularly lead, that could be analyzed by the specific portable X-ray fluorescence (XRF) analyzer under study, and then were extracted with acid and analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES). The 25 mm filters were analyzed using a single XRF reading, while three readings on different parts of the filter were taken from the 37 mm filters. For lead at the mine concentrate mill, all five samplers gave good correlations (r2 > 0.96) between the two analytical methods over the entire range of found lead mass

  16. Simultaneous preconcentrations of Co(2+), Cr(6+), Hg(2+) and Pb(2+) ions by Bacillus altitudinis immobilized nanodiamond prior to their determinations in food samples by ICP-OES.

    PubMed

    Ozdemir, Sadin; Kilinc, Ersin; Celik, Kadir Serdar; Okumus, Veysi; Soylak, Mustafa

    2017-01-15

    A novel solid phase extraction method was developed for simultaneous preconcentration-separation of Co(2+), Cr(6+), Hg(2+) and Pb(2+) ions prior to their determinations in food samples by ICP-OES. Thermophilic Bacillus altitudinis immobilized nanodiamond was used as a new biosorbent. SEM and FT-IR analysis were studied to characterize the biosorbent. The optimum pH values of quantitative biosorption for Co(2+), Cr(6+), Hg(2+) and Pb(2+) were found to be 5.0, 6.0, 6.0 and 6.0, respectively. A flow rate of 3.0mLmin(-1) was selected as optimum for all metal ions. 5mL of 1mol/L HCl was used as eluent. Preconcentration factor was achieved as 80. LODs were calculated as 0.071, 0.023, 0.016 and 0.034ngmL(-1), respectively for Hg(2+), Co(2+), Cr(6+) and Pb(2+). The biosorption capacities were calculated for Co(2+), Cr(6+), Hg(2+) and Pb(2+) as 26.4, 30.4, 19.5, and 35.2mg/g, respectively. The developed method was successfully applied to food samples to determine analyte concentrations.

  17. Heavy metals content by ICP-OES in Sarda sarda, Sardinella aurita and Lepidopus caudatus from the Strait of Messina (Sicily, Italy).

    PubMed

    Lo Turco, Vincenzo; Di Bella, Giuseppa; Furci, Patrizia; Cicero, Nicola; Pollicino, Gianmichele; Dugo, Giacomo

    2013-01-01

    In this study copper, nickel, lead, cadmium, arsenic, chromium and vanadium content was measured in the muscles and gills of 24 fishes (Sarda sarda, Sardinella aurita and Lepidopus caudatus) caught in the Strait of Messina, by inductively coupled plasma-optical emission spectroscopy with microwave digestion techniques. In general, it was found that arsenic was higher than other analytes in all fish species, particularly its content was much higher in S. aurita than in the other two exemplary species. Lead and cadmium were always detected with values below the legal limits (CE no. 1881/2006 and subsequent modification CE no. 629/2008).

  18. Inductively coupled plasma optical emission spectrometric determination of minerals in catfish frame.

    PubMed

    Losso, Jack N; Munene, Cate N; Moody, Michael W

    2003-10-01

    The concentration of 14 major and trace elements in catfish (Ictalurus punctatus) frames was determined and analyzed for differences. Three frames were obtained each week for five consecutive weeks in the spring and the fall of 2000. The frames were freed of remaining flesh, dried, treated by microwave dissolution technique and the minerals determined by inductively coupled plasma optical emission spectrometry (ICP-OES). The mean calcium concentration (mg/kg, dry basis) in the spring (140400) was not significantly (P > 0.05) different from that in fall (167000). Among the heavy metals (Cd, Pb, and Al) the concentration of Cd varied significantly (P < 0.05) from week to week but not from season to season. The concentration of all the above-mentioned heavy metals did not exceed the critical level for human consumption.

  19. Evaluation of PGE Liberation and Chromium Isolation in a Solid UG2 Chromitite Concentrates at Moderate Temperatures Using ICP-OES

    NASA Astrophysics Data System (ADS)

    Chiweshe, Trevor T.; Purcell, Walter; Venter, Johan A.

    2016-06-01

    Complete sample digestion is a prerequisite in achieving accurate and reproducible results in wet chemical analysis as well as effective element recovery in hydrometallurgical beneficiation processes. Inductively coupled plasma-optical emission spectroscopy was used to evaluate the efficiency of (NH4)2HPO4/(NH4)H2PO4, Na2HPO4/NaH2PO4·H2O (800°C), NH4F·HF flux (250°C), microwave dissolution using HCl and aqua regia acids (240°C) to dissolve and liberate the platinum group metals (PGE) in a Upper Group 2 (UG2) chromitite concentrate sample. Complete digestion of the UG2 chromitite ore was achieved using Na2HPO4/NaH2PO4·H2O and (NH4)2HPO4/(NH4)H2PO4 flux mixtures and average PGE (Ru, Os and Pt) yields of 1.90 g/kg (Ru), 0.88 g/kg (Os), 2.52 g/kg (Pt) were obtained using Sc as internal standard. Fusion with NH4F·HF yielded 0.85 g/kg (Ru), 0.72 g/kg (Os) and 0.95 g/kg (Pt) whilst microwave dissolution using HCl and aqua regia yielded an average of 0.77 g/kg (Ru), 0.08 g/kg (Os) and 0.35 g/kg (Pt). Sodium phosphate flux, however, introduced Na+ ions as easily ionised elements, which affected the emission intensities to yield slightly inflated PGE (Ru, Os and Pt) yields. The use of ammonium phosphate and sodium phosphate at 800°C (after the selective removal of Na+ ions) proved to better the fluxes and produced higher and consistent PGE yields. The use of ammonium phosphate flux was also shown to facilitate the isolation of a green chromium precipitate with a 98.9% purity, which may assist in a hydrometallurgical beneficiation process of the UG2 chromitite concentrate ore and may also have important implications for the ferro-chrome industry.

  20. TXRF and ICP-OES analysis of liquid-phase laser-ablated (LP-LA) nanoparticles of cryolite-alumina solutions

    NASA Astrophysics Data System (ADS)

    Castell, Ricardo; Greaves, Eduardo D.; Abdala, Lyzeth; Barros, Haydn

    2012-10-01

    A new procedure with minimum sample preparation has been developed for a fast and serial analysis of cryolite with varying concentrations of dissolved alumina by liquid-phase laser ablation followed by Total Reflection X-Ray Fluorescence and induced coupled plasma optical emission spectroscopy. The analysis supplies the sodium/aluminium ratio of bath samples taken from industrial Hall-Herault reduction cells, as well as trace element relative concentrations. Two different types of molten samples taken directly from the aluminium production plant were placed under distilled de-ionized water in a quartz cell and subjected to pulsed laser ablation using the beam from a third harmonic Nd:YAG laser. Scanning electron microscopy examination shows the nanoparticles nature of the ablated material. The water-suspension is deposited on quartz reflectors for Total Reflection X-ray Fluorescence analysis or directly aspirated to the induced coupled plasma yielding the aluminium and sodium signals. Instrument quantification of the elements is performed by the use of aqueous standards. Validation tests were done with cryolite sample digestion and standard methods of sample quantification. The procedure can provide the aluminium/sodium ratio with adequate precision for aluminium production plant cell diagnostics and reveals the trace elements that could be considered as contamination.

  1. Analysis of Zn, Cd, As, Cu, Pb, and Fe in snails as bioindicators and soil samples near traffic road by ICP-OES.

    PubMed

    Massadeh, Adnan M; Alomary, Ahmed A; Mir, Sayeeda; Momani, Fouad A; Haddad, Hazem I; Hadad, Yazen A

    2016-07-01

    Snails are used as biological indicators of the environment pollution for heavy metals. Living snail samples were collected from different sites at the city of Irbid-Jordan and classified according to their morphological features including Helix pelasga, Eobania vermiculata, Xeropicta derbentina, Oychilus, Xerocrassa seetzenii, Xerocrassa simulata, and Pila. Zn, Cd, As, Cu, Pb, and Fe levels were measured by inductively coupled plasma-optical emission spectroscopy. Results indicated that metal concentrations in all snail shell samples were with an average and range for Zn 22.4 (6.5-105.5) μg g(-1), Cd 7.8 (0.4-48.1) μg g(-1), As 25.9 (0.7-248.5) μg g(-1), Cu 15.1 (1.6-69.0) μg g(-1), Pb 0.4 (0.2-1.7) μg g(-1), and Fe 119.6 (14.0-1102.0) μg g(-1), whereas, in soil samples, the average and range for Zn 204.0 (12.0-709.0) μg g(-1), Cd 5.7 (0.2-39.5) μg g(-1), As 3.2 (1.8-5.2) μg g(-1), Cu 22.1 (2.3-77.4) μg g(-1), Pb 0.2 (0.1-0.3) μg g(-1), and Fe 242.4 (25.0-680.0) μg g(-1).

  2. Multielement plant tissue analysis using ICP spectrometry.

    PubMed

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

    2013-01-01

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

  3. Determination of selenium, zinc and cadmium in antidandruff shampoos by atomic spectrometry after microwave assisted sample digestion.

    PubMed

    Salvador, A; Pascual-Martí, M C; Aragó, E; Chisvert, A; March, J G

    2000-05-05

    Microwave assisted pre-treatments for atomic spectrometric determination (inductive coupled plasma-optical emission spectrometry, ICP-OES or flame atomic absorption spectrometry, FAAS) of metallic elements, usually present in antidandruff shampoos, are proposed. They are based on the digestion of the sample with HNO(3) into a closed reactor, which is irradiated at 800 W for a few minutes. Selenium was determined by ICP-OES. The limit of detection was 0.11 mg l(-1); the relative standard deviation (R.S.D.) for the selenium content in the samples was in the 0.6-3.6% range. The results obtained were in agreement with the label contents and the recovery of the proposed method was in the 100-106% range. Zinc and cadmium were determined by FAAS. The limit of detection for zinc determination was 0.078 mg l(-1); the R.S.D. for zinc contents was in the 0.8-8.6% range. A limit of detection of 0.09 mg l(-1) was obtained for cadmium determination; the R.S.D. for cadmium contents was in the 0.7-2.7% range. The determinations were performed after two different sample mineralization pre-treatments - dry ashing (in an electric furnace) and wet mineralization (in a microwave oven). Both methodologies provided comparable results for zinc and cadmium determination in shampoos. The proposed microwave assisted digestion procedures allow a precise and accurate determination of selenium, zinc and cadmium in commercial antidandruff shampoos, and the sample pre-treatment is less time-consuming than the classic methods.

  4. Analysis of whole blood samples with low gas flow inductively coupled plasma-optical emission spectrometry.

    PubMed

    Nowak, Sascha; Künnemeyer, Jens; Terborg, Lydia; Trümpler, Stefan; Günsel, Andreas; Wiesmüller, Gerhard A; Karst, Uwe; Buscher, Wolfgang

    2015-01-01

    Low gas flow ICP-OES with a total argon consumption below 0.7 L/min is introduced for the analysis of trace elements in blood samples to investigate the influence of samples containing an organic solvent in a demanding matrix on the performance of this plasma for the first time. Therefore, gadolinium was determined in human plasma samples and mercury in red blood cells, human plasma, and precipitated plasma protein fraction. Limits of detection (LOD) were determined to be in the low microgram per liter range for the analytes and the accuracy of the method was assessed by comparison with a conventional Fassel-type torch-based ICP-OES. It was proven that the low gas flow ICP-OES leads to comparable results with the instrument based on the Fassel-type torch.

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

    PubMed Central

    2012-01-01

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

  6. Analysis of Plant Leaves Using Laser Ablation Inductively Coupled Plasma Optical Emission Spectrometry: Use of Carbon to Compensate for Matrix Effects.

    PubMed

    Chirinos, José; Oropeza, Dayana; González, Jhanis; Zorba, Vassilia; Russo, Richard E

    2017-04-01

    Direct solid sampling by laser ablation into an inductively coupled plasma synchronous vertical dual view optical emission spectroscope (LA-SVDV-ICP-OES) was used for the elemental analysis of nutrient elements Ca, B, Mn, Mg, K, and Zn and essential (non-metallic) elements P and S in plant materials. The samples were mixed with paraffin as a binder, an approach that provides better cohesion of the particles in the pellets in addition to supplying carbon to serve as an internal standard (atomic line C I 193.027 nm) as a way to compensate for matrix effects, and/or variations in the ablation process. Precision was in the range of 1-8% relative standard deviation (RSD) with limit of detection in the range of 0.4-1 mg/kg(-1) and 25-640 mg/kg(-1) for metallic and non-metallic elements, respectively.

  7. Ultraviolet Absorption Spectrometry (UVAS) and Liquid Atomic Emission Spectrometry (LAES.

    DTIC Science & Technology

    1994-02-10

    salinity information. The system worked fairly well, although the flow rate was less than optimum. However, after a deep freeze in early January, the...significantly smaller heat sink. The absorbance flow cell system was modified to include two flow cells. Having two flow cells allows the operator to...excitation spectra. After the emission power supply, the emission flow cell is the second most critical component of the LAES system . A diagram of the

  8. Single-step microwave digestion with HNO(3) alone for determination of trace elements in coal by ICP spectrometry.

    PubMed

    Wang, Jie; Nakazato, Tetsuya; Sakanishi, Kinya; Yamada, Osamu; Tao, Hiroaki; Saito, Ikuo

    2006-02-28

    A microwave digestion method with HNO(3) alone was conducted at a temperature as high as 250 degrees C for determination of 19 trace elements (Li, Be, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Cd, Cs, Ba, Hg, and Pb) in coal jointly by inductively coupled plasma optical emission spectrometry (ICP-OES), inductively coupled plasma mass spectrometry (ICP-MS), and flow injection ICP-MS (FI-ICP-MS). The validity of determination was assessed by using three standard coals, SRM 1632c, BCR 180, and SARM 19. It was found that the high-temperature digestion led to an extensive decomposition of the organic matrix and clay in coal, and no dissolved and solid carbon remained in the final solution after evaporation. Good recoveries were observed for all trace elements in three coals, with the exception of V, Rb, and Cs in high-ash SARM 19. Additionally, FI-ICP-MS combined with the present digestion without evaporation pretreatment was proved to be a rapid and efficient approach for determination of ultra-trace elements such as Se, Cd, and Hg in coal.

  9. Comparison of Electron Spin Resonance Spectroscopy and Inductively-Coupled Plasma Optical Emission Spectroscopy for Biodistribution Analysis of Iron-Oxide Nanoparticles

    PubMed Central

    Chertok, Beata; Cole, Adam J.; David, Allan E.; Yang, Victor C.

    2010-01-01

    Magnetic nanoparticles (MNP) have been widely studied for use in targeted drug delivery. Analysis of MNP biodistribution is essential to evaluating the success of targeting strategies and the potential for off-target toxicity. This work compared the applicability of inductively-coupled plasma optical emission spectroscopy (ICP-OES) and electron spin resonance (ESR) spectroscopy in assessing MNP biodistribution. Biodistribution was evaluated in 9L-glioma bearing rats administered with MNP (12-25 mg Fe/kg) under magnetic targeting. Ex vivo analysis of MNP in animal tissues was performed with both ICP-OES and ESR. A cryogenic method was developed to overcome the technical hurdle of loading tissue samples into ESR tubes. Comparison of results from the ICP-OES and ESR measurements revealed two distinct relationships for organs accumulating high or low levels of MNP. In organs with high MNP accumulation such as liver and spleen, data were strongly correlated (r = 0.97, 0.94 for liver and spleen, respectively), thus validating equivalency of the two methods in this high concentration range (> 1000 nmol Fe/g tissue). The two sets of measurements, however, differed significantly in organs with lower levels of MNP accumulation such as brain, kidney, and the tumor. Whereas ESR resolved MNP to 10-55 nmol Fe/g tissue, ICP-OES failed to detect MNP due to masking by endogenous iron. These findings suggest that ESR coupled to cryogenic sample handling is more robust than ICP-OES, attaining better sensitivity in analyses. Such advantages render ESR the method of choice for accurate profiling of MNP biodistribution across tissues with high variability in nanoparticle accumulation. PMID:20039679

  10. Emission characterization of particulate matter in the ironmaking process.

    PubMed

    Li, Xiaoling; Sun, Wenqiang; Zhao, Liang; Cai, Jiuju

    2017-10-03

    The aim of this study is to provide a detailed physical and chemical characterization of particles collected in the ironmaking process from an integrated iron and steel factory. The samples collected from three measuring points includes a bunker system, a cast house and a pulverized coal feeding system. Using gravimetric, scanning electron microscope coupled with energy dispersive X-ray spectrometry (SEM-EDS), X ray fluorescence spectrometry (XRF), inductively coupled plasma optical emission spectrometry (ICP-OES) analyses, the size distribution, morphology, elemental composition and emission factor of particles were investigated. The contribution rates of cast house for emission factors of TSP, PM10 and PM2.5 are the largest, 57.0%, 75.5% and 83.3%, respectively. SEM-EDS analysis indicated that cast house particle shapes are mainly formed by polymerization from spherical particles and ultrafine particles, whose main component is Fe. But the particles of the bunker system or the pulverized coal feeding system are mainly the large ones of irregular block or powder particles and the main component is carbon. The highest content of the element in particles of the bunker system and cast house is Fe, followed by C, Si, Ca, Al. The main elements of particles in the pulverized coal feeding system are C, Si, Al and Ca, and their contents are 63.6%, 7.83%, 3.07% and 1.47%, respectively. These 'fingerprints' information of the particles can provide details for source apportionment studies at receptor sites and will be useful for the treatment of particulate matter in the steel industry.

  11. Critical evaluation of strategies for single and simultaneous determinations of As, Bi, Sb and Se by hydride generation inductively coupled plasma optical emission spectrometry.

    PubMed

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

    2017-05-15

    A systematic study of hydride generation (HG) of As, Bi, Sb and Se from solutions containing As(III), As(V), Bi(III), Sb(III), Sb(V), Se(IV) and Se(VI) was presented. Hydrides were generated in a gas-liquid phase separation system using a continuous flow vapor generation accessory (VGA) by mixing acidified aqueous sample, HCl and sodium borohydride reductant (NaBH4) solutions on-line. For detection, a simultaneous axially viewed inductively coupled plasma optical emission spectrometer (ICP-OES) was applied. Effects of the HCl concentration (related to sample and additional acid solutions) and type of the pre-reducing agents used for reduction of As(V), Sb(V) and Se(VI) into As(III), Sb(III) and Se(IV) on the analytical responses of As, Bi, Sb and Se were studied and discussed. Two compromised HG reaction conditions for simultaneous measurements of As+Bi+Sb (CC1) or As+Sb+Se (CC2) were established. It was found that choice of the pre-reductant prior to formation of the hydrides is critical in obtaining the dependable results of the analysis. Accordingly, for a As(III)+As(V)+Bi(III)+Sb(III)+Sb(V) mixture and using CC1, thiourea/thiourea-ascorbic acid interfered in Bi determination and hence, total As+Sb could be measured. If L-cysteine/L-cysteine-ascorbic acid were used, measurements of total Bi+Sb was possible in these HG reaction conditions. For a As(III)+As(V)+Sb(III)+Sb(V)+Se(IV)+Se(VI) mixture and using CC2, thiourea/thiourea-ascorbic acid and L-cysteine/L-cysteine-ascorbic acid influenced HG of Se but ensured total As+Sb determination. In contrast, heating a sample solution with HCl, although did not pre-reduce As(V) and Sb(V), assured quantitative reduction of Se(VI) to Se(IV). Finally, considering all favorable pre-reducing and HG conditions, methodologies for reliable determination of total As, Bi, Sb and Se by HG-ICP-OES were proposed. Strategies for single-, two- and three-element measurements were evaluated and validated, obtaining the detection limits

  12. Elemental profiling of Noah's Ark shell (Arca noae, Linnaeus, 1758) by plasma optical spectrometry and chemometric tools.

    PubMed

    Kobelja, Kristina; Nemet, Ivan; Župan, Ivan; Čulin, Jelena; Rončević, Sanda

    2016-12-01

    Determination of metal content in biominerals provides essential information with respect to relations between biomineralization processes and environmental status. Mussels are species that have a great potential as bio-marker species and therefore, they are in the focus of numerous biomineralization and ecological studies. In this study, elemental profile of mussel shell of Noah's Ark (Arca noe, Linnaeus, 1758), which inhabit eastern Adriatic Sea was obtained by determination of seventeen elements content using inductively coupled plasma optical emission spectrometry (ICP-OES). Shell samples were collected from marine protected area and from marine shipping route in eastern Adriatic Sea. The accuracy of applied analytical procedure based on microwave decomposition of shell samples was tested by use of reference materials of limestone and by matrix-matched standards. By aid of chemometric methods, the elemental profile along with variability of elements content of shell was obtained. The impact of different environment on elements content was established by use of multivariate statistical PCA method. Discernment between two groups of samples was manifested. Among results of main, minor and trace elements content, the last one which denoted to Cd, Co, Cu, Pb, and Mn was expressed as principal distinctive feature of shell samples collected from different sampling sites. Elemental profiling of mussel shell Noah's Ark provides novel insight in species status as well as in environmental status on the observed locations. Copyright © 2016 Elsevier GmbH. All rights reserved.

  13. Using bio-dispersive solution of chitosan for green dispersive liquid-liquid microextraction of trace amounts of Cu(II) in edible oils prior to analysis by ICP-OES.

    PubMed

    Limchoowong, Nunticha; Sricharoen, Phitchan; Techawongstien, Suchila; Chanthai, Saksit

    2017-09-01

    A green approach using chitosan solution as a novel bio-dispersive agent for the dispersive liquid-liquid microextraction (DLLME) of trace amounts of Cu(II) in edible oils is presented. An emulsion was formed by mixing the oil sample with 300µL of 0.25% (w/v) chitosan solution containing 200µL of 6molL(-1) HCl. Deionized water was used to induce emulsion breaking without centrifugation. The centrifuged Cu(II) extract was collected and analyzed using an inductively coupled plasma-optical emission spectrometer. The detection and quantitation limits were 2.1 and 6.8µgL(-1), respectively. Trace amounts of Cu(II) in six edible oil samples were tested under optimum conditions for DLLME, with a recovery ranging from 90.3% to 109.3%. Therefore, the new dispersive agent in DLLME offers superior performance owing to the non-toxic nature of the solvent, short extraction time, high sensitivity, and easy operation. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

    NASA Astrophysics Data System (ADS)

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

    1986-03-01

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

  15. Characterization of the Etna volcanic emissions through an active biomonitoring technique (moss-bags): part 1--major and trace element composition.

    PubMed

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

    2015-01-01

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

  16. Determination of Silicon in Gasoline by Directly Measuring under Organic Phase Using Inductively Coupled Plasma Optical Emission Spectroscopy.

    PubMed

    Zhang, Wen-mei; Wen, Huan; Lü, Huan-ming; Liu, Hui-qin; Lin, Zhi-sheng; Wang, Rong-hua

    2015-03-01

    A simple and accurate method was developed for determining silicon in gasoline using inductively coupled plasma optical emission spectroscopy (ICP-OES). For sample inroduction a Burgener nubulizer and a Cyclonic spray chamber were used. A gasoline sample was diluted with isooctane and then introduced into the cooled spray chamber of the ICP-OES. Good linearity was achieved in the silicon concentration range 0.1 - 10.0 mg x kg(-1), and the correlation coefficient was 0.999 96. The detection limit for silicon was 0.012 mg x kg(-1) and the silicon recoveries from gasoline samples were 95.8% - 98.4%, with relative standard deviations of less than 3.0% The method was proved to be simple, reliable and highly sensitive, and suitable for determining silicon in samples of motor gasoline, ethanol-gasoline and methanol-gasoline fuel mixtures those containing not more than 15% (V/V) oxygenates.

  17. Microwave-assisted extraction of rare earth elements from petroleum refining catalysts and ambient fine aerosols prior to inductively coupled plasma-mass spectrometry.

    PubMed

    Kulkarni, Pranav; Chellam, Shankararaman; Mittlefehldt, David W

    2007-01-09

    A robust microwave-assisted acid digestion procedure followed by inductively coupled plasma-mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM(2.5)). High temperature (200 degrees C), high pressure (200 psig), acid digestion (HNO(3), HF and H(3)BO(3)) with 20 min dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst and PM(2.5). This method was also employed to measure 27 non-REEs including Na, Mg, Al, Si, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Cd, Cs, Ba, Pb and U. Complete extraction of several REEs (Y, La, Ce, Pr, Nd, Tb, Dy and Er) required HF indicating that they were closely associated with the aluminosilicate structure of the zeolite FCC catalysts. Internal standardization using (115)In quantitatively corrected non-spectral interferences in the catalyst digestate matrix. Inter-laboratory comparison using ICP-optical emission spectroscopy (ICP-OES) and instrumental neutron activation analysis (INAA) demonstrated the applicability of the newly developed analytical method for accurate analysis of REEs in FCC catalysts. The method developed for FCC catalysts was also successfully implemented to measure trace to ultra-trace concentrations of La, Ce, Pr, Nd, Sm, Gd, Eu and Dy in ambient PM(2.5) in an industrial area of Houston, TX.

  18. Microwave-assisted Extraction of Rare Earth Elements from Petroleum Refining Catalysts and Ambient Fine Aerosols Prior to Inductively Coupled Plasma - Mass Spectrometry

    NASA Technical Reports Server (NTRS)

    Mittlefehldt, David W.; Kulkarni, Pranav; Chellam, Shankar

    2006-01-01

    In the absence of a certified reference material, a robust microwave-assisted acid digestion procedure followed by inductively coupled plasma - mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM2.5). High temperature (200 C), high pressure (200 psig), acid digestion (HNO3, HF, and H3BO3) with 20 minute dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst, and PM2.5. This method was also employed to measure 27 non-REEs including Na, Mg, Al, Si, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Cd, Cs, Ba, Pb, and U. Complete extraction of several REEs (Y, La, Ce, Pr, Nd, Tb, Dy, and Er) required HF indicating that they were closely associated with the aluminosilicate structure of the zeolite FCC catalysts. Internal standardization using 115In quantitatively corrected non-spectral interferences in the catalyst digestate matrix. Inter-laboratory comparison using ICP-optical emission spectroscopy (ICP-OES) and instrumental neutron activation analysis (INAA) demonstrated the applicability of the newly developed analytical method for accurate analysis of REEs in FCC catalysts. The method developed for FCC catalysts was also successfully implemented to measure trace to ultra-trace concentrations of La, Ce, Pr, Nd, Sm, Gd, Eu, and Dy in ambient PM2.5 in an industrial area of Houston, TX.

  19. Determination of verapamil in pharmaceutical formulations using atomic emission spectrometry.

    PubMed

    Khalil, Sabry; Kelzieh, Ahmed

    2002-01-01

    Ion-associate complexes of verapamil hydrochloride (VpCl) with (Cd(II), Co(II), Mn(II), and Zn(II)) thiocyanates, potassium ferricyanide, and ammonium reineckate are precipitated. The solubility of the solid complexes at the recommended optimum conditions of pH and ionic strength values have been studied. Saturated solutions of each ion associate at different temperatures under the optimum precipitation conditions were prepared and the metal ion contents in the supernatant were determined. The solubility products were thus calculated at different temperatures and the thermodynamic parameters DeltaH, DeltaG, and DeltaS were calculated. A new accurate and precise method based on direct coupled plasma atomic emission spectrometry for the determination of VpCl (1.96-62.86 microg ml(-1)) in pure solutions and pharmaceutical preparations is given.

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

    ERIC Educational Resources Information Center

    Horlick, Gary

    1984-01-01

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

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

    ERIC Educational Resources Information Center

    Horlick, Gary

    1984-01-01

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

  2. Determination of As, Cr, Mo, Sb, Se and V in agricultural soil samples by inductively coupled plasma optical emission spectrometry after simple and rapid solvent extraction using choline chloride-oxalic acid deep eutectic solvent.

    PubMed

    Matong, Joseph M; Nyaba, Luthando; Nomngongo, Philiswa N

    2017-01-01

    A rapid, simple and green ultrasound-assisted extraction method using deep eutectic solvents (DES) for extraction of As, Cr, Mo, Sb, Se and V in soil samples, has been developed. Choline chloride-oxalic acid based DES was used as a solvent. The target analytes were subsequently quantified using inductively coupled plasma optical emission spectrometer (ICP OES). The parameters that affect the extraction of the target analytes was optimized using standard reference material of San Joaquin soil (SRM 2709a). In the optimization step, a two-level full factorial experimental design was used. The factors under investigation include extraction time, sample mass and acid concentration. Under optimized conditions, limits of detection (LOD) and limits of quantification (LOQ) ranged from 0.009 to 0.1 and 0.03-0.3µgg(-1), respectively. The repeatability (n=20) estimated in terms of relative standard deviation (%RSD) ranged from 0.9% to 3.7%. The accuracy of the proposed method was carried out using SRM 2709a. The obtained and certified/ indicative values were statistically in good agreement at 95% confidence level. The proposed method applied for quantification of As, Cr, Mo, Sb, Se and V in real soil samples. For comparison, the analytes of interest were also determined using a conventional acid digestion method. According to the paired t-test, the analytical results were not significant differences at 95% confidence level. The method was found to be accurate, precise and environmentally friendly. Copyright © 2016 Elsevier Inc. All rights reserved.

  3. Determination of trace amounts of total dissolved cationic aluminium species in environmental samples by solid phase extraction using nanometer-sized titanium dioxide and atomic spectrometry techniques.

    PubMed

    Matús, Peter; Hagarová, Ingrid; Bujdos, Marek; Divis, Pavel; Kubová, Jana

    2009-11-01

    Nanometer-sized titanium dioxide was used as a solid-phase extractant for the separation and preconcentration of trace amounts of Al(III) prior to its determination by electrothermal atomic absorption spectrometry (ET AAS) and inductively coupled plasma optical emission spectrometry (ICP OES). The optimal conditions for the proposed solid phase extraction (SPE; 50mg TiO(2), 10 min extraction time, pH 6.0, HCl and HNO(3) as eluents) and ET AAS measurement (1500 degrees C pyrolysis and 2600 degrees C atomization temperatures, Mg(NO(3))(2) as matrix modifier) were obtained. The adsorption capacity of TiO(2) was 4.1mg Al g(-1) TiO(2). Two modes of the proposed procedure were compared, (I) batch and elution mode with the elution of Al from TiO(2) phase by nitric or hydrochloric acid, and (II) batch and slurry mode (without elution) with the direct TiO(2) phase-slurry sampling. Finally, the batch and slurry mode of nanometer-sized TiO(2) SPE with slurry ET AAS detection and quantification was preferred and used for the determination of trace amounts of total dissolved cationic Al species in synthetic and natural water samples. The method accuracy was checked by the analysis of lake water CRM TMDA-61 and by the technique of analyte addition (sample spiking). Under the optimal conditions, the calibration curve for batch and slurry TiO(2) SPE with a 10-fold preconcentration was linear up to 40 microg L(-1) Al. The limit of detection (LOD) and the limit of quantification (LOQ) was 0.11 microg L(-1) Al and 0.35 microg L(-1) Al, respectively, with a preconcentration factor of 20 and a relative standard deviation (RSD) lower than 5%.

  4. Resonance Ionization Laser Mass Spectrometry: New possibilities for on-line analysis of waste incinerator emissions

    SciTech Connect

    Zimmermann, Ralf; Rohwer, Egmont R.; Heger, Hans Joerg; Schlag, Edward W.; Kettrup, Antonius; Gilch, Gerhard; Lenoir, Dieter; Boesl, Ulrich

    1997-01-15

    A concept for the use of Resonance Ionization Laser Mass Spectrometry for on-line emission analysis of chlorinated aromatic compounds in waste incinerator flue gas is presented. New analytical results suggest that low chlorinated benzenes can be used as indicator parameter for dioxin emissions.

  5. Field-flow fractionation: An efficient approach for matrix removal of soil extract for inductively coupled plasma optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    Sangsawong, Supharart; Waiyawat, Weerawan; Shiowatana, Juwadee; Siripinyanond, Atitaya

    2011-06-01

    An on-line coupling between a continuous-flow sequential extraction (CFSE) unit and flow field-flow fractionation with cross flow matrix removal (FlFFF/CFM) with ICP-OES detection was developed for determination of metal leachability from soil. The use of high concentration of Mg(NO 3) 2 in exchangeable phase can cause undesirable matrix effects by shifting ionization equilibrium in the plasma, etc., resulting in a clear need for matrix removal. Therefore, the capability of FlFFF/CFM to remove Mg matrix ion from soil extract was evaluated. Poly(ethylene imine) (PEI) having molecular weight of 25,000 Da was added to form complexes with analyte elements (Cu, Mn, Pb, and Zn) but not the matrix element (Mg). The free Mg matrix ions were then removed by filtering off through the ultrafiltration membrane, having a 1000-Da molecular weight cut-off, inside the FlFFF channel. With the use of FlFFF/CFM, matrix removal efficiency was approximately 83.5%, which was equivalent to approximately 6-fold dilution of the matrix ion. The proposed hyphenated system of CFSE and FlFFF/CFM with ICP-OES detection was examined for its reliability by checking with SRM 2710 (a highly contaminated soil from Montana). The metal contents determined by the proposed method were not significantly different (at 95% confidence) from the certified values.

  6. Chemical composition and characteristics of ambient aerosols and rainwater residues during Indian summer monsoon: Insight from aerosol mass spectrometry

    NASA Astrophysics Data System (ADS)

    Chakraborty, Abhishek; Gupta, Tarun; Tripathi, Sachchida N.

    2016-07-01

    Real time composition of non-refractory submicron aerosol (NR-PM1) is measured via Aerosol mass spectrometer (AMS) for the first time during Indian summer monsoon at Kanpur, a polluted urban location located at the heart of Indo Gangetic Plain (IGP). Submicron aerosols are found to be dominated by organics followed by nitrate. Source apportionment of organic aerosols (OA) via positive matrix factorization (PMF) revealed several types of secondary/oxidized and primary organic aerosols. On average, OA are completely dominated by oxidized OA with a very little contribution from biomass burning OA. During rain events, PM1 concentration is decreased almost by 60%, but its composition remains nearly the same. Oxidized OA showed slightly more decrease than primary OAs, probably due to their higher hygroscopicity. The presence of organo nitrates (ON) is also detected in ambient aerosols. Apart from real-time sampling, collected fog and rainwater samples were also analyzed via AMS in offline mode and in the ICP-OES (Inductively coupled plasma - Optical emission spectrometry) for elements. The presence of sea salt, organo nitrates and sulfates has been observed. Rainwater residues are also dominated by organics but their O/C ratios are 15-20% lower than the observed values for ambient OA. Alkali metals such as Ca, Na, K are found to be most abundant in the rainwater followed by Zn. Rainwater residues are also found to be much less oxidized than the aerosols present inside the fog water, indicating presence of less oxidized organics. These findings indicate that rain can act as an effective scavenger of different types of pollutants even for submicron particle range. Rainwater residues also contain organo sulfates which indicate that some portion of the dissolved aerosols has undergone aqueous processing, possibly inside the cloud. Highly oxidized and possibly hygroscopic OA during monsoon period compared to other seasons (winter, post monsoon), indicates that they can act

  7. Electron cyclotron emission spectrometry on the Tokamak a Configuration Variable

    SciTech Connect

    Klimanov, I.; Porte, L.; Alberti, S.; Blanchard, P.; Fasoli, A.; Goodman, T.P.

    2005-09-15

    Electron cyclotron emission (ECE) measurements are an important component of the diagnostic suite on the Tokamak a Configuration Variable (TCV) [F. Hoffman et al., Plasma Phys. Controlled Fusion 36, B277 (1994)]. A recently installed, 24-channel dual-conversion heterodyne radiometer covering the radio frequency range 65-100 GHz and viewing from the low-field side (LFS) of the tokamak greatly enhances the system and, in combination with an existing radiometer viewing from the high-field side (HFS), allows simultaneous measurements of emission from the HFS and LFS. In addition, the new radiometer has multiple lines of sight that can receive the emission perpendicular to the toroidal magnetic field as well as with a finite k{sub parallel} (wave vector parallel to magnetic field). Such flexibility allows the LFS radiometer to make standard measurements of thermal emission and nonstandard measurements of nonthermal, anisotropic emission. The toroidal line of sight allows access to overdense plasma via mode converted emission. The enhanced ECE diagnostic is described and examples of measurements made in various configurations are presented.

  8. Pulsed, atmospheric pressure plasma source for emission spectrometry

    DOEpatents

    Duan, Yixiang; Jin, Zhe; Su, Yongxuan

    2004-05-11

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

  9. Characterization of the General Electric CID-17 as a Detector for Plasma Emission Spectrometry.

    DTIC Science & Technology

    1985-11-25

    multiwavelength disreteetectors. All tnToes oF detectors ’or plasma emission snectroscopv must mntil there o eapresetutisemhas. been, byes ereounu ai!- numer...photomultiplier tubes. With almost 100,000 channels, true multiwavelength detection is obtained making a new wealth of information available to the analytical...of complex mixtures by optical emission spectrometry requires sensitive simultaneous multiwavelength detection. Until the present, this has been

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

    NASA Astrophysics Data System (ADS)

    Spencer, Kathleen M.

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

  11. Apparatus and method for transient thermal infrared emission spectrometry

    DOEpatents

    McClelland, John F.; Jones, Roger W.

    1991-12-24

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

  12. Solid sampling electrothermal vaporization for sample introduction in inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry

    NASA Astrophysics Data System (ADS)

    Moens, L.; Verrept, P.; Boonen, S.; Vanhaecke, F.; Dams, R.

    1995-06-01

    Solid sampling using electrothermal vaporization is an attractive sample introduction method for atomic absorption spectrometry (AAS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). For AAS, the method is well established. The techniques needed to apply SS-ETV in ICP-based methods are described, with the emphasis on the coupling of different types of ETV-devices to the inductively coupled plasma torch and on the requirements for the spectrometer and the data acquisition and handling system. Though standardization is not straightforward, it is shown that standard addition and external calibration with solid standards yield accurate results. The latter is demonstrated by the analysis of standard reference materials. Figures of merit for SS-ETV-ICP-AES and SS-ETV-ICP-MS are presented. The literature concerning ICP-AES and ICP-MS (methods and applications) is briefly reviewed and new results of SS-ETV-ICP-MS analysis of SRMs are presented.

  13. Analytical control of wollastonite for biomedical applications by use of atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry.

    PubMed

    De Aza, P N; Guitián, F; De Aza, S; Valle, F J

    1998-04-01

    Preliminary in vitro experiments revealed that wollastonite (CaSiO3) is a potentially highly bioactive material that forms a hyroxyapatite (HA) surface layer on exposure to simulated body fluid with an ion concentration, pH and temperature virtually identical with those of human blood plasma. The formation of the HA layer is an essential requirement for an artificial material to be used as bioactive bone substitute. This finding opens up a wide field for biomedical applications of wollastonite. Biomaterials used as implants in the human body require strict control of trace elements and of the toxic species specified in American Society for Testing and Materials F-1185-88 (As, Cd, Hg and Pb) in ceramic hydroxyapatite for surgical implantation. In this work, two types of pseudowollastonite, the high temperature form of wollastonite, were analysed by using cold vapour atomic absorption spectrometry and hydride generation atomic absorption spectrometry, in order to determine the elements stated in the above-mentioned norm, and inductively coupled plasma atomic emission spectrometry to establish the SiO2/CaO ratio of the two materials and analyse for all other impurities introduced by the raw materials and by the processes of synthesis, sintering and grinding. Barium and Mg were especially prominent in raw materials, and Zr, Y, Mg, W, Co and Ni come mainly from the processing.

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

    SciTech Connect

    Montaser, A.

    1992-01-01

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

  15. Online coupling of fully automatic in-syringe dispersive liquid-liquid microextraction with oxidative back-extraction to inductively coupled plasma spectrometry for sample clean-up in elemental analysis: A proof of concept.

    PubMed

    Horstkotte, Burkhard; Fikarová, Kateřina; Cocovi-Solberg, David J; Sklenářová, Hana; Solich, Petr; Miró, Manuel

    2017-10-01

    A proof of concept of a novel automatic sample cleanup approach for metal assays in troublesome matrixes as a front-end sample pre-treatment to inductively coupled plasma optical emission spectroscopy - ICP-OES - is herein presented. Target metals, namely, copper, lead, and cadmium were complexed in-system quantitatively using ammonium pyrrolidine dithiocarbamate (APDC) and transferred into a minute volume of toluene as extractant employing lab-in-syringe magnetic stirring-assisted dispersive liquid-liquid microextraction (LIS-MSA-DLLME). After discharge of the sample, the analytes were back-extracted into nitric acid and injected on-line into ICP-OES. To promote and expedite this process in-syringe, advantage was taken from oxidative decomposition of the chelate by potassium iodate, reported in this article for the first time. Experimental conditions for LIS-MSA-DLLME were optimized by Box-Benkhen multivariate analysis using the geometric mean of analyte recoveries as the desirability function. Times of extraction and back-extraction of 300s and 100s, respectively, pH 5.5 at 30mmol/L acetate, 300µL of extraction solvent, and 600µmol/L of APDC were finally applied. Online interfacing to ICP-OES for back-extract analysis yielded average repeatabilities for Cd, Cu, and Pb of 2.9%, 3.5%, and 3.5% with limits of detections (3s) of 1.9, 1.4, and 5.6ng/mL, respectively. Oxidative back-extraction was proven reliable for the determination of metal species in coastal seawater, surrogate digestive fluids and soil leachates with recovery values for Cd, Cu, and Pb ranging from 90% to 118%, 68% to 104%, and 86% to 112%, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Rapid total sulphur reduction in coal samples using various dilute alkaline leaching reagents under microwave heating: preventing sulphur emissions during coal processing.

    PubMed

    Mketo, Nomvano; Nomngongo, Philiswa Nosizo; Ngila, Jane Catherine

    2017-07-07

    Currently in South Africa, online flue gas desulphurisation (FGD) is being utilized as one of the most effective methods for total sulphur reduction in coal samples during the combustion process. However, the main disadvantage associated with FGD is the formation of its by-products (FGD gypsum). The latter is mostly formed in low grade quality, thereby bringing secondary pollution problems and extra disposal costs. Therefore, the current study describes the development of total sulphur extraction in coal under microwave heating using different dilute alkaline solutions such as NaOH, NaOH-H2O2, NH4OH, and NH4OH-H2O2. The experimental conditions were as follows: 150 °C, 5 min and 10% (m/v or v/v) for temperature, extraction time and reagent concentration, respectively. The most effective alkaline reagent for coal desulphurisation was observed to be NaOH-H2O2 with total sulphur reduction of 55% (from the inductively coupled plasma-optical emission spectrometry (ICP-OES) results). The NaOH-H2O2 reagent also showed significant morphological changes in coal as observed from the SEM images and effective demineralisation as revealed by the powder X-ray diffractometer (P-XRD) results. Additionally, desulphurisation results obtained from the developed microwave-assisted dilute alkaline extraction (MW-ADAE) method were quite comparable with the published work. The proposed total sulphur reduction method is advantageous as compared to some of the literature reported coal desulphurisation methods as it requires a short period (5 min) of time to reach its completion. Additionally, the proposed method shows excellent reproducibility (% RSD from 0.5 to 1); therefore, it can be utilized for routine analysis. Graphical abstract ᅟ.

  17. Direct determination of Cu by liquid cathode glow discharge-atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Lu, Quanfang; Yang, Shuxiu; Sun, Duixiong; Zheng, Jidong; Li, Yun; Yu, Jie; Su, Maogen

    2016-11-01

    In this study, a novel liquid cathode glow discharge-atomic emission spectrometry was developed for the direct determination of Cu in aqueous solutions, in which the glow discharge plasma was produced in the solution between the needle-like Pt cathode and the electrolyte around it. The effects of discharge voltage, solution pH, and the ionic surfactant cetyltrimethylammonium chloride (CTAC) on emission intensities were investigated. The limit of detection (LOD) of Cu was compared with those measured by closed-type electrolyte cathode discharge-atomic emission spectrometry (ELCAD-AES). The results showed that the optimal operation conditions are voltage of 135 V, a pH of 1, and addition of 0.15% CTAC. CTAC can enhance the emission intensity and lower the LOD of Cu I. The net intensity of atomic emission lines of Cu I at 324.8 nm with 0.15% CTAC improved by 1.5 fold, and the LODs of the Cu at 135 V with 0.15% CTAC and without CTAC are 0.019 and 0.234 mg L- 1, respectively. The analytical capability of Cu in this study is comparable to the closed-type ELCAD-AES, and it satisfied the recommended levels of Cu in the WHO standards for drinking-water quality. This technique can be effectively used for on-line monitoring of metal ions in aqueous samples.

  18. Evaluation of a new optic-enabled portable X-ray fluorescence spectrometry instrument for measuring toxic metals/metalloids in consumer goods and cultural products

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

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

    SciTech Connect

    Montaser, A.

    1990-01-01

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

  20. Particulate PAH emissions from residential biomass combustion: time-resolved analysis with aerosol mass spectrometry.

    PubMed

    Eriksson, A C; Nordin, E Z; Nyström, R; Pettersson, E; Swietlicki, E; Bergvall, C; Westerholm, R; Boman, C; Pagels, J H

    2014-06-17

    Time-resolved emissions of particulate polycyclic aromatic hydrocarbons (PAHs) and total organic particulate matter (OA) from a wood log stove and an adjusted pellet stove were investigated with high-resolution time-of-flight aerosol mass spectrometry (AMS). The highest OA emissions were found during the addition of log wood on glowing embers, that is, slow burning pyrolysis conditions. These emissions contained about 1% PAHs (of OA). The highest PAH emissions were found during fast burning under hot air starved combustion conditions, in both stoves. In the latter case, PAHs contributed up to 40% of OA, likely due to thermal degradation of other condensable species. The distribution of PAHs was also shifted toward larger molecules in these emissions. AMS signals attributed to PAHs were found at molecular weights up to 600 Da. The vacuum aerodynamic size distribution was found to be bimodal with a smaller mode (Dva ∼ 200 nm) dominating under hot air starved combustion and a larger sized mode dominating under slow burning pyrolysis (Dva ∼ 600 nm). Simultaneous reduction of PAHs, OA and total particulate matter from residential biomass combustion may prove to be a challenge for environmental legislation efforts as these classes of emissions are elevated at different combustion conditions.

  1. [Determination of trace elements in shark cartilage by inductively coupled plasma atomic emission spectrometry].

    PubMed

    Deng, B; Zhang, Z

    1998-10-01

    Semiquantitative estimation of all elements in shark cartilage was investigated by inductively coupled plasma mass spectrometry (ICP-MS). The determination of trace elements, namely Fe, Zn, Se, Cu, Mn, Mo, Ti and Sr in shark cartilage, was carried out using inductively coupled plasma atomic emission spectrometry (ICP-AES). The matrix effects were overcome by using yttrium as an internal standard element. The recoveries are in the range of 81.6 to 100.7%. The determination limits of Fe, Zn, Se, Cu, Mn, Mo, Ti and Sr are 0.60, 0.55, 0.21, 0.39, 0.042, 0.27, 0.038 and 0.48 microg x g(-1), respectively. The results showed that the shark cartilage contains higher amount of Fe, Zn, Se, Cu, Mn, Mo, Ti and Sr than those in other fishes and in other animal bones.

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

    NASA Astrophysics Data System (ADS)

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

    1994-07-01

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

  3. Searching the most appropriate sample pretreatment for the elemental analysis of wines by inductively coupled plasma-based techniques.

    PubMed

    Gonzálvez, A; Armenta, S; Pastor, A; de la Guardia, M

    2008-07-09

    Different sample preparation methods were evaluated for the simultaneous multielement analysis of wine samples by inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). Microwave-assisted digestion in closed vessel, thermal digestion in open reactor, and direct sample dilution were considered for the determination of Li, Be, Na, Mg, Al, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Sr, Y, Mo, Cd, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Tl, Pb, and Bi in 12 samples of red wine from Valencia and Utiel-Requena protected designation of origin. ICP-MS allows the determination of 17 elements in most of the samples, and using ICP-OES, a maximum of 15 elements were determined. On comparing the sample pretreatment methodology, it can be concluded that the three assayed procedures provide comparable results for the concentration of Li, Na, Mg, Al, K, Ca, Mn, Fe, Zn, and Sr by ICP-OES. Furthermore, ICP-MS data found for Cu, Pb, and Ba were comparable. Digestion treatment provides comparable values using both total decomposition in open system and microwave-assisted treatment for Cu by ICP-OES and for Cr, Ni, and Zn by ICP-MS. Open vessel total digestion provides excess values for Cr, Mn, Fe, and Zn by ICP-OES and defect values for Se. However, direct measurement of diluted wine samples provided uncomparable results with the digestion treatment for Mn, Cu, Pb, Zn, Ba, and Bi by ICP-OES and for Mg, Cr, Fe, Ni, and Zn by ICP-MS. Therefore, it can be concluded that microwave-assisted digestion is the pretreatment procedure of choice for elemental analysis of wine by ICP-based techniques.

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

    PubMed

    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%.

  5. Determination of selenium in foods by inductively-coupled plasma atomic emission spectrometry and hydride generation.

    PubMed

    Kardos, J; Zimmer, K; Coni, E; Caroli, S; Stacchini, A

    1989-01-01

    Within the framework of a survey launched by the Istituto Superiore di Sanità to assess the average daily intake of Se with food in the Italian population, a preliminary study was carried out to develop an analytical procedure for the quantification of the element in food products. The method implies the use of a hydride generation system in combination with inductively-coupled plasma atomic emission spectrometry (ICP-AES) and exploits the inherent advantages of this last also for the analysis of non-metals. The overall approach was tested in some Hungarian and Italian foods, adequately lending itself to routine and reliable Se assay.

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

    PubMed

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

    1993-01-01

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

  7. [Determination of trace niobium and tantalum in rock sample by atomic emission spectrometry].

    PubMed

    Li, Hui-zhi; Zhou, Chang-li; Luo, Chuan-nan

    2002-10-01

    This paper describes the determination of trace Nb and Ta in sample using carbon powder and hafnium oxide as buffer by atomic emission spectrometry (AES). Hafnium has been selected as internal standard, since it has scinilar evaporation curve as those of Nb and Ta. Samples can be analyzed without chemical pretreatment. The sample was directly loaded onto the ordinary electrode. The method is simple, rapid and accurate. The range of determination for Nb and Ta are 0%-0.25% and 0%-0.125% respectively, and the detection limits are found to be 0.003% and 0.001%, respectively. Satisfactory results are obtained.

  8. Effect of microstructure of graphite on the nonreductive thermal ion emission in thermal ionization mass spectrometry.

    PubMed

    Wei, H Z; Jiang, S Y; Xiao, Y K

    2010-02-25

    The emission behavior of polyatomic ions in the ionization source of thermal ionization mass spectrometry (TIMS) was investigated. The results suggest that the presence of a graphite promoter plays a key role for the formation and stable emission of polyatomic ions, such as M(2)X(+), M(2)BO(2)(+), Cs(2)NO(2)(+), and Cs(2)CNO(+). Our data further implied that the intensity of M(2)X(+) and M(2)BO(2)(+) increases and the emission temperature decreases with increasing cationic and anionic radius. During the boron isotopic measurement using the Cs(2)BO(2)(+)-graphite-PTIMS method, the isobaric interference ion Cs(2)CNO(+) cannot be transformed from nitrate or organic compounds containing an amide group but can be induced by the existence of trace amounts of boron because of its special electron-deficiency property (B(3+)). Characterization on the planar crystalline structure of various graphite samples with SEM, TEM, and Raman spectroscopy confirmed the relationship of the emission capacity of polyatomic ions and the crystal microstructure of graphite and provides direct evidence that graphite with a perfect parallel and equidistant layer orientation shows a beneficial effect on the emission of polyatomic ions in TIMS. The mechanism study on the formation of polyatomic ions opens the possibility to establish high precision methods for isotopic composition analysis of more nonmetal elements with the TIMS technique.

  9. Resonance ionization mass spectrometry and its application to trace analysis of emissions from combustion engines

    NASA Astrophysics Data System (ADS)

    Boesl, Ulrich; Nagel, Holger; Zimmermann, Ralf; Frey, Ruediger

    1997-05-01

    The principle of resonance-ionization mass spectrometry with lasers is the combination of two analytical tools, UV- spectroscopy in the gas phase and time-of-flight mass selection. The special features of this combination are: very high selectivity, high speed, multicomponent ability, and adaptability to many different problems. Examples for the latter are on-line trace analysis of emissions from combustion processes, such as from combustion engines as well as from municipal incinerators. But also monitoring of industrial procedures, e.g. food processing, are interesting applications of REMPI-MS. In this paper the principles will be shortly explained and results for the analysis of exhaust emissions from motorized vehicles presented.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed Central

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

    2016-01-01

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

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

    PubMed

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

    2016-01-14

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

  13. Evaluation of FTIR emission spectrometry for the determination of turbine exhaust composition in test beds

    NASA Astrophysics Data System (ADS)

    Schaefer, Klaus; Heland, Joerg; Lister, Dave H.; Lindermeir, Erwin; Hilton, Moira; Bishop, Gary; Wiesen, Peter; Bernard, Marc

    1999-09-01

    The capability of taking non-intrusive species measurements in a jet plume of a modified mid-size low by-pass aero-engine running on a sea level test bed at several thrust levels was demonstrated. Also conventional intrusive measurements were performed with a spatially resolved method using a traversing single-point sampling probe which fulfills ICAO standards. The FTIR spectrometry measurements included both emission and absorption mode with a multi-path reflection compartment as well as the single emission mode. Due to the lack of a common/unique definition for the exhaust plume diameter it was found that the column density was the best measure to compare the different techniques. The FTIR engine measurement results for CO2, CO, and NO have been proven to be in agreement with the intrusive data within plus or minus 30%. Several error sources during the radiometric radiance calibration were identified which lead to uncertainties in the FTIR retrievals, namely (1) incomplete knowledge of the optical surface emissivities, (2) incomplete knowledge and inhomogeneities of the optical surface temperature, and (3) undefined instrumental drifts and non-linearities during the calibration.

  14. Differentiation of two Canary DO red wines according to their metal content from inductively coupled plasma optical emission spectrometry and graphite furnace atomic absorption spectrometry by using Probabilistic Neural Networks.

    PubMed

    Moreno, Isabel M; González-Weller, Dailos; Gutierrez, Valerio; Marino, Marino; Cameán, Ana M; González, A Gustavo; Hardisson, Arturo

    2007-04-15

    The metal content of 54 commercialized wines (30 samples from Tacoronte-Acentejo DO (class T) and 24 Valle de la Orotava DO (class O) wines) was performed by ICP-OES (Al, Ba, Cu, Fe, Mn, Sr, Zn, Ca, K, Na and Mg) and GF-AAS (Ni and Pb). Wine samples were processed by dry ashing followed by solution with 5% nitric acid. Metals were considered as suitable descriptors to differentiate between T and O classes. Supervised learning pattern recognition procedures were applied. Linear discriminant analysis (LDA) led to good results up to about 90% of correct classification. In order to improve the results, another kind of algorithms able to model non-linear separation between classes was considered: Probabilistic Neural Networks. Accordingly, excellent results were obtained, leading to sensitivities and specificities higher than 95% for the two classes.

  15. [The possibilities for determining the shooting distance by means of inductively coupled plasma optical emission spectrometry].

    PubMed

    Svetlolobov, D Yu; Luzanova, I S; Zorin, Yu V; Makarov, I Yu; Lorents, A S

    The objective of the present study was to evaluate the possibilities for determining the shooting distance for the MR-79-9 Makarych non-lethal pistol (diameter 9 mm, rubber bullet, shot energy 50 J) by means of inductively coupled plasma optical emission spectrometry. The experiments were carried under the conditions of a ballistic shooting range making the shots from a distance of 0 to 120 cm. The 15×15 cm pieces of muslin fabric and biomaterials (leather) were used as the targets. The morphological signs of the damages inflicted to the targets were evaluated either with the unassisted eye, a criminalistical magnifying glass or the SMT-4 binocular stereoscopic microscope (Germany). The shot products, the area and boundaries of their dispersion were determined in reflected IR and filtered UV rays. Inductively coupled plasma optical emission spectrometry was applied for the qualitative and quantitative analysis of various shot products from the entry hole zone with the contamination (wipedown) bands and contusion collars being 0.2-0.5 cm (group 1) and 2-3 cm (group 2) in width, with special reference to the identification of Ba, Cu, Cr, Fe, K, Ni, Pb, Sb, Sn and Zn. The results of the study give evidence that the detection of Ba, Pb, and Sb among the products of a shot fired from the MR-79-9 Makarych non-lethal pistol is of especially high informative value for determining the shooting distance whereas the detection of Cr, K, Sn and Ni is of a minimum value for this purpose.

  16. Laser ablation inductively coupled plasma mass spectrometry for direct analysis of the spatial distribution of trace elements in metallurgical-grade silicon.

    PubMed

    Pisonero, Jorge; Kroslakova, Ivana; Günther, Detlef; Latkoczy, Christopher

    2006-09-01

    The spatial distribution and concentration of impurities in metallurgical-grade silicon (MG-Si) samples (97-99% w/w Si) were investigated by use of laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The spatial resolution (120 mum) and low limits of detection (mg kg(-1)) for quality assurance of such materials were studied in detail. The volume-dependent precision and accuracy of non-matrix-matched calibration for quantification of minor elements, using NIST SRM 610 (silicate standard), indicates that LA-ICP-MS is well suited to rapid process control of such materials. Quantitative results from LA-ICP-MS were compared with previously reported literature data obtained by use of ICP-OES and rf-GD-OES. In particular, the distribution of element impurities and their relationship to their different segregation coefficients in silicon is demonstrated.

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

    ERIC Educational Resources Information Center

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

    2007-01-01

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

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

    EPA Science Inventory

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

  19. The determination of samarium, europium, gadolinium and dysprosium in uranium products by direct-current plasma emission spectrometry.

    PubMed

    Flavelle, F; Westland, A D

    1986-05-01

    Samarium, europium, gadolinium and dysprosium were separated from uranium-containing materials by means of solvent extraction with Alamine 336, followed by cation-exchange. The elements were determined in the sub-ppm range by means of direct-current plasma atomic-emission spectrometry.

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

    EPA Science Inventory

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

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

    EPA Science Inventory

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

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

    ERIC Educational Resources Information Center

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

    2007-01-01

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

  3. Methylmercury determination in seafood by photochemical vapor generation capacitively coupled plasma microtorch optical emission spectrometry.

    PubMed

    Covaci, Eniko; Senila, Marin; Ponta, Michaela; Darvasi, Eugen; Petreus, Dorin; Frentiu, Maria; Frentiu, Tiberiu

    2017-08-01

    A non-chromatographic method based on double liquid-liquid extraction and measurements by UV photochemical vapor generation capacitively coupled plasma microtorch optical emission spectrometry was developed and characterized for methylmercury determination in seafood. Samples were prepared following the procedure recommended in JRC Technical Report of European Commission formerly proposed for the determination of methylmercury in seafood by thermal decomposition atomic absorption spectrometry, namely confinement of Hg species in 47% HBr solution, extraction of CH3Hg(+) in toluene and back-extraction in 1% l-cysteine aqueous solution. Mercury cold vapor was generated by flow injection UV photo-reduction from CH3Hg(+) in 0.6molL(-1) HCOOH, while quantification was performed against external Hg(2+) aqueous standards and measuring Hg 253.652nm emission using a low power/Ar consumption plasma microtorch (15W, 100mLmin(-1)) and a low resolution microspectrometer (Ocean Optics). The figures of merit and analytical capability were assessed by analyzing certified reference materials and test samples of fish fillet and discussed in relation with requirements for Hg determination in seafood in European legislation (Decisions 2007/333/EC and 2002/657/EC) as well as compared to performances achieved in thermal decomposition atomic absorption spectrometry. The limit of detection and quantification of 2µgkg(-1) and 6µgkg(-1) respectively, precision of 2.7-9.4% and accuracy of 99±8% of the proposed method for the determination of CH3Hg(+) fulfill the demands of European legislation for Hg quantification. The limit of detection and quantification were better than those in the used reference method or other non-/chromatographic methods taken for comparison. The analysis of certified reference materials and the Bland and Altman test performed on 12 test samples confirmed trueness of the proposed method and its reliability for the determination of traces of CH3Hg(+) with 95

  4. Laser-Ablation Sampling for Accurate Analysis of Sulfur in Edible Salts.

    PubMed

    Lee, Yonghoon; Chirinos, Jose; Gonzalez, Jhanis; Oropeza, Dayana; Zorba, Vassilia; Mao, Xianglei; Yoo, Jonghyun; Russo, Richard E

    2017-04-01

    We evaluated the performance of laser ablation analysis techniques such as laser-induced breakdown spectroscopy (LIBS), laser ablation inductively coupled optical emission spectrometry (LA-ICP-OES), and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), in comparison with that of ICP-OES using aqueous solutions for the quantification of sulfur (S) in edible salts from different geographical origins. We found that the laser ablation based sampling techniques were not influenced by loss of S, which was observed in ICP-OES with aqueous solutions for a certain salt upon their dissolution in aqueous solutions, originating from the formation of volatile species and precipitates upon their dilution in water. Although detection of S using direct laser sampling with LA-ICP-MS has well-known isobaric and polyatomic interferences, LIBS and LA-ICP-OES showed good accuracy in the detection of S for all salts. LIBS also provided the ability to identify the dominant chemical form in which S is present in salts. Correlation between S and oxygen, observed in LIBS spectra, provided chemical information about the presence of S(2-) or [Formula: see text], which are associated with the origin and quality of edible salts.

  5. EVALUATION OF A MATRIX INTERFERENCE IN GROUND WATER ARSENIC MEASUREMENT BY ICP-OES

    EPA Science Inventory

    Arsenic enters ground water systems by either the weathering of naturally occurring subsurface materials or human activities such as mining and pesticide manufacturing. The current EPA drinking water limit for arsenic is set at 50 ug/L, with the reduction to 10 ug/L in 2006. The...

  6. EVALUATION OF A MATRIX INTERFERENCE IN GROUND WATER ARSENIC MEASUREMENT BY ICP-OES

    EPA Science Inventory

    Arsenic enters ground water systems by either the weathering of naturally occurring subsurface materials or human activities such as mining and pesticide manufacturing. The current EPA drinking water limit for arsenic is set at 50 ug/L, with the reduction to 10 ug/L in 2006. The...

  7. Extraction of trace elements in coal for determination by inductively coupled plasma-optical emission spectrometry using N,N-dimethylformamide and ultrasound

    NASA Astrophysics Data System (ADS)

    Mujuru, Munyaradzi; Moyo, Stanley; McCrindle, Robert I.; Mokgalaka-Matlala, Ntebogeng

    2012-10-01

    Coal usage continues to increase due to global energy demands. Increasing environmental monitoring and concern means that better methods of trace element determination are always required. This study investigated the use of N,N-dimethylformamide (DMF), Triton X-100, HNO3 and ultrasound to extract trace elements (Cr, Mn, Pb, Sr and V) from coal prior to analysis using ICP-OES and ICP-MS. It was found that the proportion extracted was lowest for V (17%) and highest for Pb (100%). Partial dissolution of the coal particles used in the slurries was demonstrated using scanning electron microscopy studies. Trace element determination of two reference material coal samples demonstrated that this method of extraction is effective. Trace elements in three bituminous coals from different seams being mined in South Africa were determined.

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

    USGS Publications Warehouse

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

    1987-01-01

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

  9. Inductively coupled plasma optical emission spectroscopy determination of trace element composition of argan oil.

    PubMed

    Gonzálvez, A; Ghanjaoui, M E; El Rhazi, M; de la Guardia, M

    2010-02-01

    A methodology based on inductively coupled plasma optical emission spectroscopy (ICP-OES) after microwave assisted acid digestion has been developed to determine the trace element content of Moroccan argan oil. Limit of detection values equal or lower than few mg/kg were obtained for all elements under study. To assure the accuracy of the whole procedure, recovery studies were carried out on argan oil samples spiked at different concentration levels from 10 to 200 µg/L. Quantitative average recovery values were obtained for all elements evaluated, demonstrating the suitability of this methodology for the determination of trace elements in argan oil samples. Aluminum, calcium, chromium, iron, potassium, lithium, magnesium, sodium, vanadium and zinc were quantitatively determined in Moroccan argan oils being found that their concentration is different of that found in other edible oils thus offering a way for authentication and for the evaluation of possible adulterations.

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

    DOEpatents

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

    2010-08-03

    A method for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry (ICP-AES). ICP-AES analysis is performed across a plurality of selected locations in the plasma on an unknown sample, collecting the light intensity at one or more selected wavelengths of one or more sought-for analytes, creating a first dataset. The first dataset is then calibrated with a calibration dataset creating a calibrated first dataset curve. If the calibrated first dataset curve has a variability along the location within the plasma for a selected wavelength, errors are present. Plasma-related errors are then corrected by diluting the unknown sample and performing the same ICP-AES analysis on the diluted unknown sample creating a calibrated second dataset curve (accounting for the dilution) for the one or more sought-for analytes. The cross-over point of the calibrated dataset curves yields the corrected value (free from plasma related errors) for each sought-for analyte.

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

    PubMed

    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.

  12. Investigations on laser ablation microwave induced plasma atomic emission spectrometry using polymer samples

    NASA Astrophysics Data System (ADS)

    Leis, F.; Bauer, H. E.; Prodan, L.; Niemax, K.

    2001-01-01

    The potential of laser ablation-microwave induced plasma-atomic emission spectrometry (LA-MIP-AES) for the analysis of plastic materials has been investigated. A Nd/YAG laser, operated in its fundamental mode at 1064 nm, was used to ablate small amounts of various plastics. The sample atoms were transported and excited in a closely neighbored continuously running microwave induced plasma (MIP) operated in argon or helium at reduced pressure. A 0.5-m échelle spectrometer, equipped with an intensified charge coupled device (ICCD) as a detector was used for recording the spectra. The amount of ablated material was found to be strongly dependent on the matrix (10-190 ng/shot). Signals for some metals often used as additives in polymers (Al, Ca, Cu, Sb, Ti) and for the elements F, Cl, Br, J, and P in various polymers were recorded in the spectral range 250-840 nm. The estimated detection limits were found to be in the range 0.001-0.08% for metals and 0.05-0.7% for non-metals. Spectral lines of fluorine and iodine could only be measured in the helium MIP. For high concentrations of chlorine and carbon in the samples (polyvinylchloride), a memory effect was observed.

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

    PubMed

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

    2016-02-25

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

  14. Composition of Renaissance paint layers: simultaneous particle induced X-ray emission and backscattering spectrometry.

    PubMed

    de Viguerie, L; Beck, L; Salomon, J; Pichon, L; Walter, Ph

    2009-10-01

    Particle induced X-ray emission spectroscopy (PIXE) is now routinely used in the field of cultural heritage. Various setups have been developed to investigate the elemental composition of wood/canvas paintings or of cross-section samples. However, it is not possible to obtain information concerning the quantity of organic binder. Backscattering spectrometry (BS) can be a useful complementary method to overcome this limitation. In the case of paint layers, PIXE brings the elemental composition (major elements to traces) and the BS spectrum can give access to the proportion of pigment and binder. With the use of 3 MeV protons for PIXE and BS simultaneously, it was possible to perform quantitative analysis including C and O for which the non-Rutherford cross sections are intense. Furthermore, with the use of the same conditions for PIXE and BS, the experiment time and the potential damage by the ion beam were reduced. The results obtained with the external beam of the Accélérateur Grand Louvre pour l'Analyse Elementaire (AGLAE) facility on various test painting samples and on cross sections from Italian Renaissance masterpieces are shown. Simultaneous combination of PIXE and BS leads to a complete characterization of the paint layers: elemental composition and proportion of the organic binder have been determined and thus provide useful information about ancient oil painting recipes.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed Central

    Park, Jonghoo; Blick, Robert H.

    2016-01-01

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

  17. Method 200.7: Determination of Metals and Trace Elements in Water and Wastes by Inductively Coupled Plasma-Atomic Emission Spectrometry

    EPA Pesticide Factsheets

    SAM lists this method for preparation and analysis of aqueous liquid and drinking water samples. This method will determine metal-containing compounds as the total metal (e.g., total arsenic), using inductively coupled plasma-atomic emission spectrometry.

  18. Coupling dispersive liquid-liquid microextraction to inductively coupled plasma atomic emission spectrometry: An oxymoron?

    PubMed

    Martínez, David; Torregrosa, Daniel; Grindlay, Guillermo; Gras, Luis; Mora, Juan

    2018-01-01

    Coupling dispersive liquid-liquid micro-extraction (DLLME) to inductively coupled plasma atomic emission spectrometry (ICP-AES) is usually troublesome due to the limited plasma tolerance to the organic solvents usually employed for metal extraction. This work explores different coupling strategies allowing the multi-element determination by ICP-AES of the solutions obtained after DLLME procedures. To this end, three of the most common extractant solvents in DLLME procedures (1-undecanol, 1-butyl-3-methyl-imidazolium hexafluorophosphate and chloroform) have been selected to face most of the main problems reported in DLLME-ICP-AES coupling (i.e., those arising from the high solvent viscosity and volatility). Results demonstrate that DLLME can be successfully coupled to ICP-AES after a careful optimization of the experimental conditions. Thus, elemental analysis in 1-undecanol and 1-butyl-3-methyl-imidazolium hexafluorophosphate extracts can be achieved by ICP-AES after a simple dilution step with methanol (1:0.5). Chloroform can be directly introduced into the plasma with minimum changes in the ICP-AES configuration usually employed when operating with aqueous solutions. Diluted inorganic acid solutions (1% w w(-1) either nitric or hydrochloric acids) have been successfully tested for the first time as a carrier for the introduction of organic extractants in ICP-AES. The coupling strategies proposed have been successfully applied to the multi-element analysis (Al, Cu, Fe, Mn, Ni and Zn) of different water samples (i.e. marine, tap and river) by DLLME-ICP-AES. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    PubMed

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

    2007-09-01

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

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

    PubMed

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

    2014-06-01

    An inductively coupled plasma optical emission spectrometry method for the quantitative simultaneous determination of Al, Ca, Co, Cu, Cr, Fe, K, Mg, Mn, Na, Ni, P and Zn in Cuban laterite and serpentine minerals has been developed. Additionally, V and Ti can be quantitatively determined in laterite mineral; Li, Sr, and Zr can be detected in both mineral types and Pb can be detected just in laterite mineral. The microwave-assisted total acid digestion of samples was achieved with HCl+HNO3+HF and HNO3+HClO4+HF acid mixtures for laterite and serpentine samples, respectively. In non-robust plasma operating conditions, the matrix effect characteristics of the laterite sample were dictated by the principal component Fe; while the character of the Mg principal component matrix effect was some how modified by the concomitants Fe and Ni in serpentine sample. The selection of robust conditions decreased the matrix effect. Additionally, the simulation of the matrix samples by introducing the principal component Fe or Mg, correspondingly, in calibration dissolutions was needed to overcome completely the matrix effect over the analysis accuracy. Precision of analysis was very near or lower than 10% for most elements, except Sr (15%) in L-1; and K (15%) and Li (15%) in SNi sample. Accuracy of analysis was around or lowers than 10% for most elements, except K (15%), Na (19%), P (19%) and V (19%) in L-1 sample; and Ca (14%) and P (20%) in SNi sample. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

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

    2004-12-01

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

  3. Determination of silver in nano-plastic food packaging by microwave digestion coupled with inductively coupled plasma atomic emission spectrometry or inductively coupled plasma mass spectrometry.

    PubMed

    Lin, Q-B; Li, B; Song, H; Wu, H-J

    2011-08-01

    The detection of silver in nano-plastic food packaging by microwave digestion coupled with either inductively coupled plasma atomic emission spectrometry (ICP-AES) or inductively coupled plasma mass spectrometry (ICP-MS) was investigated. Microwave digestion was optimised by trialling different acid mixtures. Both ICP-AES and ICP-MS showed good reproducibility, repeatability and recovery. For ICP-AES the limit of detection of the method (LODm) was 25.0 µg g(-1), the limit of detection of the instrument (LODi) was 30.0 ng ml(-1), the linear range was 0.10-10.0 µg ml(-1). The average recoveries for blank samples spiked with silver at 100, 250 and 500 µg g(-1) ranged from 82.53% to 87.60%, and the relative standard deviations (RSDs) were from 1.79% to 8.30%. For ICP-MS analysis the LODm was 0.75 µg g(-1), the LODi was 0.04 ng ml(-1), the linear range was 0.20-500.0 ng ml(-1), the RSDs were 2.26-4.79%, and the recoveries were 78.09-92.72% (spiked concentrations of 2.5, 5.0 and 10.0 µg g(-1)). These results indicate that the proposed method could be employed to analyse silver in nano-plastic food packaging.

  4. Carbon-, sulfur-, and phosphorus-based charge transfer reactions in inductively coupled plasma-atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

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

    2016-01-01

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

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

    USGS Publications Warehouse

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

    1991-01-01

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

  6. Classification of Antarctic algae by applying Kohonen neural network with 14 elements determined by inductively coupled plasma optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    Balbinot, L.; Smichowski, P.; Farias, S.; Arruda, M. A. Z.; Vodopivez, C.; Poppi, R. J.

    2005-06-01

    Optical emission spectrometers can generate results, which sometimes are not easy to interpret, mainly when the analyses involve classifications. To make simultaneous data interpretation possible, the Kohonen neural network is used to classify different Antarctic algae according to their taxonomic groups from the determination of 14 analytes. The Kohonen neural network architecture used was 5×5 neurons, thus reducing 14-dimension input data to two-dimensional space. The input data were 14 analytes (As, Co, Cu, Fe, Mn, Sr, Zn, Cd, Cr, Mo, Ni, Pb, Se, V) with their concentrations, determined by inductively coupled plasma optical emission spectrometry in 11 different species of algae. Three taxonomic groups ( Rhodophyta, Phaeophyta and Cholorophyta) can be differentiated and classified through only their Cu content.

  7. Background correction in atomic emission spectrometry using repetitive harmonic wavelength scanning and applying Fourier analysis—I. Theory

    NASA Astrophysics Data System (ADS)

    Matthee, T.; Visser, K.

    1995-07-01

    Repetitive wavelength scanning can be used as a means of detecting and correcting for unwanted background in atomic emission spectrometry (AES). This paper deals with the theory underlying such harmonic wavelength scanning in time and stresses the relative importance of the relevant parameters. A set of integrated Turbo Pascal programs for an IBM PC was developed to provide a numerical simulation for the deconvolution of a detected spectral profile during repetitive harmonic wavelength scanning. By applying this numerical analysis the theory for separating the net spectral emission signal and the background radiation by filtering specific frequency components is investigated. It is concluded that, barring the dc component, repetitive scanning over a symmetric spectral profile leads to the generation of even-numbered Fourier harmonics at the modulation frequency, while an asymmetric spectral profile generates odd-numbered Fourier harmonics.

  8. Validation and comparable analysis of aluminum in the popular Chinese fried bread youtiao by wavelength dispersive XRF.

    PubMed

    Hua, Hongying; Jiang, Xiaofei; Wu, Shimin

    2016-09-15

    Aluminum (Al) is an element in alum commonly used as a raising agent for Chinese flour products, especially for a typical fried food youtiao. In the present study, the feasibility of wavelength dispersive X-ray fluorescence spectrometry (WDXRF) for analysis of aluminum levels in youtiao was examined. Youtiao samples spiked with known amounts of aluminum were used for calibration. Linearity, accuracy, precision, and detection and quantification limits were tested, based on three calibration curves. For further validation, test youtiao samples were analyzed by both WDXRF and inductively coupled plasma optical emission spectrometry (ICP-OES). Comparison of the two methods showed that measurement performance was not significantly different. Taken together, these results indicate that WDXRF can form the basis of a rapid and simple methodology for measuring the aluminum content of youtiao, and that it is a good candidate for replacing ICP-OES for analyzing Al-containing flour products. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

    PubMed

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

    2013-05-15

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

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

    SciTech Connect

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

    2014-05-15

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

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

    PubMed

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

    2012-12-01

    A cloud-point extraction process coupled to ICP-OES by using 3-nitro benzaldehyde thiosemicarbazone (3-NBT) as complexing agent was developed for the simultaneous preconcentration and determination of copper and mercury in water samples. The variables affecting the complexation and extraction steps were optimized. Under the optimum conditions (i.e. 1.5×10(-5) mol L(-1) ligand, 0.3% (v/v) Triton X-114, 55 °C equilibrium temperature, incubation time of 30 min) the calibration graphs were linear in the range of 5-120 and 10-100 ng mL(-1) with enhancement factor of 82.7 and 51.3 for Cu(2+) and Hg(2+), respectively. The preconcentration factors were 28.6 in both cases and detection limits were obtained 0.48 for Cu and 1.1 ng mL(-1) for Hg. The precisions (R.S.D.%) for five replicate determinations at 50 ng mL(-1) of copper and mercury were better than 1.8% and 3.2%, respectively. The accuracy of the proposed method is validated by analyzing a certified reference material of water (RTC-QCI-049) with satisfactory results. Finally, the proposed method was utilized successfully for the determination of copper and mercury in surface water (river), tap water and bottled mineral water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Determination of antimony and tin in beverages using inductively coupled plasma-optical emission spectrometry after ultrasound-assisted ionic liquid dispersive liquid-liquid phase microextraction.

    PubMed

    Biata, N Raphael; Nyaba, Luthando; Ramontja, James; Mketo, Nomvano; Nomngongo, Philiswa N

    2017-12-15

    The aim of this study was to develop a simple and fast ultrasound-assisted ionic liquid dispersive liquid-liquid phase microextraction (UA-IL-DLLME) method for preconcetration of trace antimony and tin in beverage samples. The novelty of this study was based on the application of ligandless UA-IL-DLLME using low-density ionic liquid and organic solvents for preconcentration of Sb and Sn. The concentration of Sb and Sn were quantified using ICP-OES. Under the optimum conditions, the calibration graph was found to be LOQ-250µgL(-1) (r(2)=0.9987) for Sb and LOQ-350µgL(-1) for Sn. The LOD and LOQ of Sb and Sn ranged from 1.2to 2.5ngL(-1) and 4.0 to 8.3ngL(-1), respectively, with high preconcentration factors. The precisions (%RSD) of the proposed method ranged from 2.1% to 2.5% and 3.9% to 4.7% for Sb and Sn, respectively. The proposed method was successfully applied for determination of Sb and Sn in beverages. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

    SciTech Connect

    JURGENSEN, AR

    2004-04-20

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

  14. Flow field-flow fractionation-inductively coupled optical emission spectrometric investigation of the size-based distribution of iron complexed to phytic and tannic acids in a food suspension: implications for iron availability.

    PubMed

    Purawatt, Sopon; Siripinyanond, Atitaya; Shiowatana, Juwadee

    2007-10-01

    Flow field-flow fractionation-inductively coupled plasma optical emission spectrometry (FlFFF-ICP-OES) was applied to achieve the size-based fractionation of iron in a food suspension in order to gain insights into iron availability. The binding of iron with phytic and tannic acids, employed as model inhibitors of iron availability in foods, was investigated at pH 2.0 (representing stomach fluid), pH 5.0 (the transition stage in the upper part of the duodenum), and pH 7.0 (the small intestine). In the presence of phytic acid, iron was found as a free ion or it was associated with molecules smaller than 1 kDa at pH 2.0. Iron associated with molecules larger than 1 kDa when the pH of the mixture was raised to 5.0 and 7.0. In the presence of tannic acid, iron was again mostly associated with molecules smaller than 1 kDa at pH 2.0. However, at pH 5.0, iron and tannic acid associated in large molecules (approximately 25 kDa), while at pH 7.0, most of the iron was associated with macromolecules larger than 500 kDa. Iron size-based distributions of kale extract and tea infusion containing phytic and tannic acids, respectively, were also examined at the three pH values, with and without enzymatic digestion. Without enzymatic digestion of the kale extract and the tea infusion at pH 2.0, most of the iron was released as free ions or associated with molecules smaller than 1 kDa. At other pH values, most of the iron in the kale extract and the tea infusion was found to bind with ~2 kDa and >500 kDa macromolecules, respectively. Upon enzymatic gastrointestinal digestion, the iron was not observed to bind to macromolecules >1 kDa but <500 kDa, due to the enzymatic breakdown of large molecules to smaller ones (<1 kDa).

  15. Flagging and correcting non-spectral matrix interferences with spatial emission profiles and gradient dilution in inductively coupled plasma-atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Cheung, Yan; Schwartz, Andrew J.; Chan, George C.-Y.; Hieftje, Gary M.

    2015-08-01

    Matrix interference remains one of the most daunting challenges commonly encountered in inductively coupled plasma-atomic emission spectrometry (ICP-AES). In the present study, a method is described that enables identification and correction of matrix interferences in axial-viewed ICP-AES through a combination of spatial mapping and on-line gradient dilution. Cross-sectional emission maps of the plasma are used to indicate the presence of non-spectral (plasma-related and sample-introduction-related) matrix interferences. In particular, apparent concentrations of an analyte species determined at various radial locations in the plasma differ in the presence of a matrix interference, which allows the interference to be flagged. To correct for the interference, progressive, on-line dilution of the sample, performed by a gradient high-performance liquid-chromatograph pump, is utilized. The spatially dependent intensities of analyte emission are monitored at different levels of sample dilution. As the dilution proceeds, the matrix-induced signal variation is reduced. At a dilution where the determined concentrations become independent of location in the plasma, the matrix interference is minimized.

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

    PubMed

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

    2015-02-01

    The aim of the work was to establish a method for emission control of biogas plants especially the observation of fugitive methane emissions. The used method is in a developmental stage but the topic is crucial to environmental and economic issues. A remote sensing measurement method was adopted to determine methane emission rates of a biogas plant in Rhineland-Palatinate, Germany. An inverse dispersion model was used to deduce emission rates. This technique required one concentration measurement with an open path tunable diode laser absorption spectrometer (TDLAS) downwind and upwind the source and basic wind information, like wind speed and direction. Different operating conditions of the biogas plant occurring on the measuring day (December 2013) could be represented roughly in the results. During undisturbed operational modes the methane emission rate averaged 2.8 g/s, which corresponds to 4% of the methane gas production rate of the biogas plant. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

    PubMed

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

    2004-02-18

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

  18. Continuous Liquid-Sample Introduction for Bunsen Burner Atomic Emission Spectrometry.

    ERIC Educational Resources Information Center

    Smith, Gregory D.; And Others

    1995-01-01

    Describes a laboratory-constructed atomic emission spectrometer with modular instrumentation components and a simple Bunsen burner atomizer with continuous sample introduction. A schematic diagram and sample data are provided. (DDR)

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    Bradley, Eliza Swan

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

  1. Environmental biomonitoring of essential and toxic elements in human scalp hair using accelerated microwave-assisted sample digestion and inductively coupled plasma optical emission spectroscopy.

    PubMed

    Kumakli, Hope; Duncan, A'ja V; McDaniel, Kiara; Mehari, Tsdale F; Stephenson, Jamira; Maple, Lareisha; Crawford, Zaria; Macemore, Calvin L; Babyak, Carol M; Fakayode, Sayo O

    2017-05-01

    Human scalp hair samples were collected and used to assess exposure to toxic elements and essential elements in the state of North Carolina, USA using accelerated microwave assisted acid digestion and inductively coupled plasma optical emission spectroscopy (ICP-OES). The figures-of-merit of the ICP-OES were appropriate for elemental analysis in scalp hair with detection limits as low as 0.0001 mg/L for Cd, good linearity (R(2) > 0.9978), and percent recoveries that ranged from 96 to 106% for laboratory-fortified-blanks and 88-112% for sample spike recovery study. The concentrations of essential elements in scalp hair were larger than those of toxic elements, with Ca having the highest average concentration (3080 μg/g, s = 14,500, n = 194). Some of the maximum concentrations observed for As (65 μg/g), Ni (331 μg/g), Cd (2.96 μg/g), and Cr (84.6 μg/g) in individual samples were concerning, however. Samples were statistically analyzed to determine the influence of race, gender, smoking habits, or age on the elemental concentrations in scalp hair. Higher concentrations of essential elements were observed in the scalp hair of Caucasians, females, and non-smokers, and the differences were often significant at a 90% confidence level. Several pairs of essential elements, for example Ca-K, Ca-Mg, and Ca-Zn, were strongly correlated in Caucasian hair but uncorrelated in African-American hair. Similarly, essential elements were strongly correlated in female hair but weakly correlated in male hair. Toxic element pairs (As-Cd, As-Se, Pb-As, and Se-Cd) were strongly correlated in the hair of smokers but uncorrelated in that of non-smokers, suggesting that cigarette smoke is a common source of toxic elements in humans.

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

    NASA Astrophysics Data System (ADS)

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

    2003-03-01

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

  3. Field measurement of nitromethane from automotive emissions at a busy intersection using proton-transfer-reaction mass spectrometry

    NASA Astrophysics Data System (ADS)

    Inomata, Satoshi; Fujitani, Yuji; Fushimi, Akihiro; Tanimoto, Hiroshi; Sekimoto, Kanako; Yamada, Hiroyuki

    2014-10-01

    Field measurements of seven nitro-organic compounds including nitromethane and ten related volatile organic compounds were carried out using proton-transfer-reaction mass spectrometry at a busy intersection of an urban city, Kawasaki, Japan from 26th February to 6th March, 2011. Among the nitro-organic compounds, nitromethane was usually observed along with air pollutants emitted from automobiles. The mixing ratios of nitromethane varied substantially and sometimes clearly varied at an approximately constant interval. The interval corresponded to the cycle of the traffic signals at the intersection and the regular peaks of nitromethane concentrations were caused by emissions from diesel trucks running with high speed. In addition to the regular peaks, sharp increases of nitromethane concentrations were often observed irregularly from diesel trucks accelerating in front of the measurement site. For other nitro-organic compounds such as nitrophenol, nitrocresol, dihydroxynitrobenzene, nitrobenzene, nitrotoluene, and nitronaphthalene, most of the data fluctuated within the detection limits.

  4. Analysis of trace metals in water by inductively coupled plasma emission spectrometry using sodium dibenzyldithiocarbamate for preconcentration

    USGS Publications Warehouse

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

    1984-01-01

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

  5. Determination of major and trace elements in glycol-based fluids by inductively coupled plasma atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Beckwith, Paul M.

    The development of an analysis based on inductively coupled plasma atomic emission spectrometry (ICP-AES) is reported for the determination of 14 major and trace elements in coolant/antifreeze solutions to provide information on composition of new solutions and wear metals in used solutions. The evaluation of new coolant/antifreeze formulations for aluminum cooling systems has indicated that corrosion protection and stability are strongly dependent on the concentrations of the various components of the solution. The inhibitors include inorganic salts, such as silicates, borates, phosphates and molybdates, and these components are now determined by traditional analytical methods based on gravimetric and titrimetric techniques, spectrophotometry, atomic absorption spectrometry, and ion chromatography. The ICP-AES method may be used to replace these techniques with a simultaneous determination of four inhibitors as well as wear metals in used coolant/antifreeze solutions. The total time for analysis is reduced from several hours to approximately 15 min per sample. The relative standard deviation for the determination of the inhibitors is typically 2%. The detection limit for most of the wear metals is on the order of 0.1 mg l -1.

  6. Detection of trace gas emissions from point sources using shortwave infrared imaging spectrometry

    NASA Astrophysics Data System (ADS)

    Thorpe, A. K.; Roberts, D. A.; Dennison, P. E.; Bradley, E. S.; Funk, C. C.

    2011-12-01

    Existing spaceborne remote sensing provides an effective means of detecting continental-scale variation in trace gas concentrations, but does not permit mapping of local emissions from point sources. Point source emissions of methane (CH4), nitrous oxide (N2O) and particulates, often associated with combustion and carbon dioxide (CO2) emissions, have significant impacts on air quality. Using Airborne Visible InfraRed Imaging Spectrometer (AVIRIS) data and a cluster-tuned matched filter technique, we have mapped local CH4, N2O and CO2 emissions from terrestrial sources in the Los Angeles basin. CH4 anomalies were in close proximity to known and probable emission sources, including hydrocarbon storage tanks and gas flares. Multiple N2O and CH4 anomalies were detected at a wastewater treatment facility, while CH4 and CO2 anomalies were also identified at a large oil refinery. We discuss ongoing efforts to estimate CH4 concentrations using radiative transfer modeling and potential application of this technique to additional trace gasses with distinct absorption features. This method could be applied to data from existing airborne sensors and planned satellite missions like HyspIRI, thereby improving high resolution mapping of trace gasses and better constraining local sources.

  7. Ground-based aircraft exhaust measurements of a Lufthansa Airbus A340 using FTIR emission spectrometry

    NASA Astrophysics Data System (ADS)

    Schaefer, Klaus; Heland, Joerg

    1999-01-01

    The emission inventories of aircraft emissions are being set up using flight routing data and test rig measurements of the engine manufacturers for certification purposes which have to be extrapolated with respect to the actual parameters at cruise altitude. Precise data from in-service engines are not existing. FTIR-emission-spectroscopy as a remote sensing multi-component exhaust gas analysis method has been further developed to specify the traceable molecules in aircraft exhausts, to determine the detection limits, and to obtain reliable statements concerning its accuracy. The first measurement with the Airbus A340 engine CFM56-5C2 during run up tests at ground level showed the overall ability of the FTIR-emission system to analyze the exhausts of modern gas turbines with high bypass ratio and mixing of fan air into the exhausts before the nozzle exit. Good quality spectra were measured and analyzed with respect to the mixing rations of CO2, H2O, CO, NO, and N2O, and the emission indices of CO, NO, and N2O. Total measurement times at one thrust level should be about 15 minutes to obtain reliable result which can be compared to the ICAO data of this engine.

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

    PubMed

    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.

  9. New method for removal of spectral interferences for beryllium assay using inductively coupled plasma atomic emission spectrometry.

    PubMed

    Maxwell, Sherrod L; Bernard, Maureen A; Nelson, Matthew R; Youmans, Linda D

    2008-07-15

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

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

    PubMed

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

    2015-01-01

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

  11. Mass spectrometry.

    NASA Technical Reports Server (NTRS)

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

    1972-01-01

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

  12. Mass spectrometry.

    NASA Technical Reports Server (NTRS)

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

    1972-01-01

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

  13. Comparison of several analytical methods for the determination of tin in geochemical samples as a function of tin speciation

    USGS Publications Warehouse

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

    1989-01-01

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

  14. Endogenous and exogenous hydrogen influence on amorphous silicon thin films analysis by pulsed radiofrequency glow discharge optical emission spectrometry.

    PubMed

    Sánchez, Pascal; Alberts, Deborah; Fernández, Beatriz; Menéndez, Armando; Pereiro, Rosario; Sanz-Medel, Alfredo

    2012-02-10

    During the last decade the photovoltaic industry has been growing rapidly. One major strategy to reduce the production costs is the use of thin film solar cells based on hydrogenated amorphous silicon (a-Si:H). The potential of pulsed radiofrequency glow discharge coupled to optical emission spectrometry (rf-PGD-OES) for the analysis of such type of materials has been investigated in this work. It is known that when hydrogen is present in the argon discharge, even in small quantities, significant changes can occur in the emission intensities and sputtering rates measured. Therefore, a critical comparison has been carried out by rf-PGD-OES, in terms of emission intensities, penetration rates and depth resolution for two modes of hydrogen introduction in the discharge, manually external hydrogen in gaseous form (0.2% H(2)-Ar) or internal hydrogen, sputtered as a sample constituent. First, a comparative optimisation study (at 600 Pa and 50 W) was performed on conducting materials and on a silicon wafer varying the pulse parameters: pulse frequency (500 Hz-20 kHz) and duty cycle (12.5-50%). Finally, 600 Pa, 50 W, 10 kHz and 25% duty cycle were selected as the optimum conditions to analyse three types of hydrogenated samples: an intrinsic, a B-doped and a P-doped layer based on a-Si:H. Enhanced emission intensities have been measured for most elements in the presence of hydrogen (especially for silicon) despite the observed reduced sputtering rate. The influence of externally added hydrogen and that of hydrogen sputtered as sample constituent from the analysed samples has been evaluated. Copyright © 2011 Elsevier B.V. All rights reserved.

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

    USGS Publications Warehouse

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

    1990-01-01

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

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

    ERIC Educational Resources Information Center

    Hindy, Kamal T.; And Others

    1992-01-01

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

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

    ERIC Educational Resources Information Center

    Hindy, Kamal T.; And Others

    1992-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-09-01

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

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

    NASA Astrophysics Data System (ADS)

    Luc, Paul

    1995-07-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

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

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

    PubMed

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

    2015-11-01

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

  2. Volatile organic compound emissions from dairy cows and their waste as measured by proton-transfer-reaction mass spectrometry.

    PubMed

    Shaw, Stephanie L; Mitloehner, Frank M; Jackson, Wendi; Depeters, Edward J; Fadel, James G; Robinson, Peter H; Holzinger, Rupert; Goldstein, Allen H

    2007-02-15

    California dairies house approximately 1.8 million lactating and 1.5 million dry cows and heifers. State air regulatory agencies view these dairies as a major air pollutant source, but emissions data are sparse, particularly for volatile organic compounds (VOCs). The objective of this work was to determine VOC emissions from lactating and dry dairy cows and their waste using an environmental chamber. Carbon dioxide and methane were measured to provide context for the VOCs. VOCs were measured by proton-transfer-reaction mass spectrometry (PTR-MS). The compounds with highest fluxes when cows plus waste were present were methanol, acetone + propanal, dimethylsulfide, and m/z 109 (likely 4-methyl-phenol). The compounds with highest fluxes from fresh waste (urine and feces) were methanol, m/z 109, and m/z 60 (likely trimethylamine). Ethanol fluxes are reported qualitatively, and several VOCs that were likely emitted (formaldehyde, methylamine, dimethylamine) were not detectable by PTR-MS. The sum of reactive VOC fluxes measured when cows were present was a factor of 6-10 less than estimates historically used for regulatory purposes. In addition, ozone formation potentials of the dominant VOCs were -10% those of typical combustion or biogenic VOCs. Thus dairy cattle have a comparatively small impact on ozone formation per VOC mass emitted.

  3. Metal carbonyl vapor generation coupled with dielectric barrier discharge to avoid plasma quench for optical emission spectrometry.

    PubMed

    Cai, Yi; Li, Shao-Hua; Dou, Shuai; Yu, Yong-Liang; Wang, Jian-Hua

    2015-01-20

    The scope of dielectric barrier discharge (DBD) microplasma as a radiation source for optical emission spectrometry (OES) is extended by nickel carbonyl vapor generation. We proved that metal carbonyl completely avoids the extinguishing of plasma, and it is much more suitable for matching the DBD excitation and OES detection with respect to significant DBD quenching by concomitant hydrogen when hydride generation is used. A concentric quartz UV reactor allows sample solution to flow through the central channel wherein to efficiently receive the uniformly distributed UV irradiation in the confined cylindrical space between the concentric tubes, which facilitates effective carbonyl generation in a nickel solution. The carbonyl is transferred into the DBD excitation chamber by an argon stream for nickel excitation, and the characteristic emission of nickel at 232.0 nm is detected by a charge-coupled device (CCD) spectrometer. A 1.0 mL sample solution results in a linear range of 5-100 μg L(-1) along with a detection limit of 1.3 μg L(-1) and a precision of 2.4% RSD at 50 μg L(-1). The present DBD-OES system is validated by nickel in certified reference materials.

  4. Spectroscopic characteristics of spiral flow ICP for axially viewing ICP optical emission spectrometry.

    PubMed

    Ohata, Masaki; Kurosawa, Satoru; Shinoduka, Isao; Takaku, Yuichi; Kishi, Yoko

    2015-01-01

    Spectroscopic characteristics of a spiral flow inductively coupled plasma (ICP), which could be sustained stably at 9 L min(-1) of Ar plasma gas flow rate with 1.5 kW RF forward power, were studied for axially viewing ICPOES. The emission intensity profile, excitation temperature and plasma robustness were evaluated, and were similar to those of the standard ICP. The background and emission intensities of elements as well as the excitation behavior for both atom and ion lines were also examined and compared to those of the standard ICP. Since the spectroscopic characteristics of the spiral flow ICP were similar to those of the standard ICP, it could be used as a new low gas flow ICP in axially viewing ICPOES.

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

    SciTech Connect

    Caridi, F.

    2015-02-15

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

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

    PubMed

    Wagatsuma, Kazuaki

    2009-04-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-05-01

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

  8. On-line complexation/cloud point preconcentration for the sensitive determination of dysprosium in urine by flow injection inductively coupled plasma-optical emission spectrometry.

    PubMed

    Ortega, Claudia; Cerutti, Soledad; Olsina, Roberto A; Silva, María F; Martinez, Luis D

    2003-01-01

    An on-line dysprosium preconcentration and determination system based on the hyphenation of cloud point extraction (CPE) to flow injection analysis (FIA) associated with ICP-OES was studied. For the preconcentration of dysprosium, a Dy(III)-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex was formed on-line at pH 9.22 in the presence of nonionic micelles of PONPE-7.5. The micellar system containing the complex was thermostated at 30 degrees C in order to promote phase separation, and the surfactant-rich phase was retained in a microcolumn packed with cotton at pH 9.2. The surfactant-rich phase was eluted with 4 mol L(-1) nitric acid at a flow rate of 1.5 mL min(-1), directly in the nebulizer of the plasma. An enhancement factor of 50 was obtained for the preconcentration of 50 mL of sample solution. The detection limit value for the preconcentration of 50 mL of aqueous solution of Dy was 0.03 microg L(-1). The precision for 10 replicate determinations at the 2.0 microg L(-1)Dy level was 2.2% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for dysprosium was linear with a correlation coefficient of 0.9994 at levels near the detection limits up to at least 100 microg L(-1). The method was successfully applied to the determination of dysprosium in urine.

  9. Analysis of barium and strontium in sediments by dc plasma emission spectrometry

    USGS Publications Warehouse

    Bowker, P.C.; Manheim, F. T.

    1982-01-01

    The dc plasma are is suited to analysis of barium and strontium in a wide range of sedimentary rock matrices, from sands, shales, and carbonates, to ferromanganese nodules. Samples containing 10 ppm to more than 3000 ppm barium and strontium were studied. Both alkali (3500 ppm lithium borate, from a preliminary fusion) and lanthanum salts (1%) in the final solution are needed to achieve freedom from systematic effects due to extreme variation in matrix. In the absence of La, neither Li, Na, K, nor Cs totally eliminated effects of Al and other constituents on emission. Silica addition to the fusion helps achieve proper flux viscosity to aid removal of fused beads from graphite crucibles. The effect of refractory-substance formers such as aluminum with calcium can be reduced or removed by selection of a portion of the are for emission measurement. However, it was decided not to pursue this approach because of loss in analytical sensitivity and need for greater precision in optical adjustment. Analysis of standard rock samples showed generally satisfactory agreement with precision methods of analysis, and some new standard rock data are reported.

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

    NASA Astrophysics Data System (ADS)

    Miller, Dennis D.; Rutzke, Michael A.

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

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

    PubMed

    Lajunen, L H; Kubin, A

    1986-03-01

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

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

    SciTech Connect

    Montaser, A.

    1992-09-01

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

  13. A comparison of reliability of soil Cd determination by standard spectrometric methods

    PubMed Central

    McBride, M.B.

    2015-01-01

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

  14. Study of uranium matrix interference on ten analytes using inductively coupled plasma atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Ghazi, A. A.; Qamar, Sajid; Atta, M. A.

    1993-08-01

    Maximum allowable concentrations of 12 elements in uranium hexafluoride feed for enrichment to reactor grade material (about 3%), vary from 1 to 100 ppm ( μg/g). Using an inductively coupled plasma atomic emission spectrometer, 51 lines of ten of these elements (B, Cr, Mo, P, Sb, Si, Ta, Ti, V and W) have been studied with a uranium matrix to investigate the matrix interference on the basis of signal to background (SBR), and background to background ratios (BBR). Detection limits and limits of quantitative determination (LQDs) were calculated for these elements in a uranium matrix using SBR and relative standard deviation of the background signal (RSD B) approach. In almost all cases, the uranium matrix interference reduces the SBRs to the extent that direct trace analysis is impossible. A uranium sample having known concentrations of impurities (around LQDs) was directly analysed with results that showed reasonable accuracy and precision.

  15. Rapid Analysis of Inorganic Species in Herbaceous Materials Using Laser-Induced Breakdown Spectroscopy.

    PubMed

    Westover, Tyler L; Emerson, Rachel M

    2015-12-01

    Inorganic compounds in biomass, often referred to as ash, are known to be problematic in the thermochemical conversion of biomass to bio-oil or syngas and, ultimately, hydrocarbon fuels because they negatively influence reaction pathways, contribute to fouling and corrosion, poison catalysts, and impact waste streams. The most common ash-analysis methods, such as inductively coupled plasma-optical emission spectrometry/mass spectrometry (ICP-OES/MS), require considerable time and expensive reagents. Laser-induced breakdown spectroscopy (LIBS) is emerging as a technique for rapid analysis of the inorganic constituents in a wide range of biomass materials. This study compares analytical results using LIBS data to results obtained from three separate ICP-OES/MS methods for 12 samples, including six standard reference materials. Analyzed elements include aluminum, calcium, iron, magnesium, manganese, phosphorus, potassium, sodium, and silicon, and results show that concentrations can be measured with an uncertainty of approximately 100 parts per million using univariate calibration models and relatively few calibration samples. These results indicate that the accuracy of LIBS is comparable to that of ICP-OES methods and indicate that some acid-digestion methods for ICP-OES may not be reliable for Na and Al. These results also demonstrate that germanium can be used as an internal standard to improve the reliability and accuracy of measuring many elements of interest, and that LIBS can be used for rapid determination of total ash in biomass samples. Key benefits of LIBS include little sample preparation, no reagent consumption, and the generation of meaningful analytical data instantaneously.

  16. Rapid Analysis of Inorganic Species in Herbaceous Materials Using Laser-Induced Breakdown Spectroscopy

    PubMed Central

    Emerson, Rachel M.

    2015-01-01

    Abstract Inorganic compounds in biomass, often referred to as ash, are known to be problematic in the thermochemical conversion of biomass to bio-oil or syngas and, ultimately, hydrocarbon fuels because they negatively influence reaction pathways, contribute to fouling and corrosion, poison catalysts, and impact waste streams. The most common ash-analysis methods, such as inductively coupled plasma-optical emission spectrometry/mass spectrometry (ICP-OES/MS), require considerable time and expensive reagents. Laser-induced breakdown spectroscopy (LIBS) is emerging as a technique for rapid analysis of the inorganic constituents in a wide range of biomass materials. This study compares analytical results using LIBS data to results obtained from three separate ICP-OES/MS methods for 12 samples, including six standard reference materials. Analyzed elements include aluminum, calcium, iron, magnesium, manganese, phosphorus, potassium, sodium, and silicon, and results show that concentrations can be measured with an uncertainty of approximately 100 parts per million using univariate calibration models and relatively few calibration samples. These results indicate that the accuracy of LIBS is comparable to that of ICP-OES methods and indicate that some acid-digestion methods for ICP-OES may not be reliable for Na and Al. These results also demonstrate that germanium can be used as an internal standard to improve the reliability and accuracy of measuring many elements of interest, and that LIBS can be used for rapid determination of total ash in biomass samples. Key benefits of LIBS include little sample preparation, no reagent consumption, and the generation of meaningful analytical data instantaneously. PMID:26733765

  17. Characterization of Croatian Rape (Brassica sp.) Honey by Pollen Spectrum, Physicochemical Characteristics, and Multielement analysis by ICP-OES.

    PubMed

    Rajs, Blanka Bilić; Flanjak, Ivana; Mutić, Jelena; Vukojević, Vesna; Đurđić, Slađana; Primorac, Ljiljana

    2017-07-01

    Rape (Brassica sp.) unifloral honey from Croatia was characterized by certain physicochemical parameters, micro- and macroelement content, and pollen spectrum, as determined in 21 honey samples. The Brassica sp. pollen type was predominant in the analyzed samples and ranged between 60 and 98%, with Trifolium spp., Robinia pseudoacacia, Rosaceae, Helianthus annuus, Salix spp., and Taraxacum officinale as the main accompanying pollen types. The electrical conductivity mean value was 0.22 ± 0.05 mS/cm and the glucose/fructose ratio mean value was 1.1 ± 0.07, whereas sucrose was absent in the samples. The most abundant macroelement was potassium (K) (268.49 mg/kg), followed by phosphorus (P) (60.23 mg/kg), calcium (Ca) (54.02 mg/kg), sodium (Na) (22.52 mg/kg), sulfur (S) (15.79 mg/kg), and magnesium (Mg) (12.58 mg/kg). Toxic elements were mainly bellow the LODs; only arsenic (As) concentration was detectable in higher amount (0.233 mg/kg), which may be related to the high arsenic concentration in the soil and groundwater of eastern Croatia. The differences between the two harvesting seasons observed in a large number of elements could be related to climatic and soil conditions and different nectar yields originating from the associated plant species.

  18. Highly Simple Deep Eutectic Solvent Extraction of Manganese in Vegetable Samples Prior to Its ICP-OES Analysis.

    PubMed

    Bağda, Esra; Altundağ, Hüseyin; Soylak, Mustafa

    2017-02-23

    In the present work, simple and sensitive extraction methods for selective determination of manganese have been successfully developed. The methods were based on solubilization of manganese in deep eutectic solvent medium. Three deep eutectic solvents with choline chloride (vitamin B4) and tartaric/oxalic/citric acids have been prepared. Extraction parameters were optimized with using standard reference material (1573a tomato leaves). The quantitative recovery values were obtained with 1.25 g/L sample to deep eutectic solvent (DES) volume, at 95 °C for 2 h. The limit of detection was found as 0.50, 0.34, and 1.23 μg/L for DES/tartaric, DES/oxalic, and DES/citric acid, respectively. At optimum conditions, the analytical signal was linear for the range of 10-3000 μg/L for all studied DESs with the correlation coefficient >0.99. The extraction methods were applied to different real samples such as basil herb, spinach, dill, and cucumber barks. The known amount of manganese was spiked to samples, and good recovery results were obtained.

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

    PubMed

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

    2014-01-02

    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.

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

    PubMed

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

    2011-10-15

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

  1. Hydrodemetallation and Hydrodesulfurization Spent Catalysts Elemental Analysis: Comparison of Wavelength Dispersive X-ray Fluorescence and Atomic Emission Spectrometries.

    PubMed

    Garoux, Laetitia; Gourhand, Sébastien; Hébrant, Marc; Schneider, Michel; Diliberto, Sébastien; Meux, Eric

    2017-08-01

    Petroleum industries continuously consume catalysts on very large scales. The recycling of spent catalysts is thus of major economic and environmental importance and its first step consists of the characterization of the valuable metal content. Wavelength dispersive X-ray fluorescence (WDXRF) analysis is compared with inductively coupled plasma atomic emission spectrometry (ICP-AES) for the analysis of five samples of spent hydrodesulphurization (HDS) and hydrodemetallization (HDM) catalysts. The elements are considered for their economic interest (Co, Ni, Mo, and V) or for the problems that can arise when they are present in the sample in significant quantities (Al, As, P, Fe). First, the systematic comparison of the analysis of known synthetic samples was performed. The originality here is that the samples were first beaded with lithium tetraborate (Li2B4O7) for WDXRF analysis and then dissolved in hot HCl 6M for ICP-AES measurements. With this processing, we were able to clearly identify the origin of analytical problems when they arose. Second, the semi-quantitative protocol of WDXRF is compared with the quantitative procedure. Finally, the analysis of the spent catalysts is presented and the information gained by the systematic comparison of ICP-AES and WDXRF is shared. The interest of the simultaneous determination by the two techniques when such complicated heterogeneous matrices are involved is clearly demonstrated.

  2. Determination of trace bismuth in human serum by cloud point extraction coupled flow injection inductively coupled plasma optical emission spectrometry.

    PubMed

    Sun, Mei; Wu, Qianghua

    2011-09-15

    A cloud point extraction method for the preconcentration of ultra-trace bismuth in human serum prior to its determination by inductively coupled plasma optical emission spectrometry had been developed in this paper. The cloud point extraction method was based on the complex of Bi(III) with 8-hydroxyquinoline and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time were investigated in detail. An enrichment factor of 81 was obtained for the preconcentration of Bi(III) with 25 mL solution. Under the optimal conditions, the detection limit of Bi(III) is 0.12 μg L(-1). The relative standard deviation (n = 7) of determination was 2.3%, values of recovery of bismuth were from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination trace bismuth in human serum. Copyright © 2010 Elsevier B.V. All rights reserved.

  3. Determination of metal impurities in advanced lead zirconate titanate ceramics by axial view mode inductively coupled plasma optical emission spectrometry.

    PubMed

    Villanueva Tagle, M E; Larrea Marín, M T; Martin Gavilán, O; Durruthy Rodríguez, M D; Calderón Piñar, F; Pomares Alfonso, M S

    2012-05-30

    An inductively coupled plasma optical emission spectrometry quantification method for the determination of Al, Ca, Cr Cu, Fe, Mn, Mg, Ni, Zn, Ba, K, In and Co in lead zirconate-titanate (PZT) ceramics, modified with strontium and chromium, was developed. Total digestion of ceramics was achieved with a HNO(3), H(2)O(2) and HF (ac) mixture by using a microwave furnace. The sensitivity of the net signal intensity respect to radiofrequency power (P) and nebulizer argon flow (F(N)) variations was strongly dependent of the total excitation energy of line (TEE). For lines with TEE near metastable atoms and ions of argon, an increment of the sensitivities to P and F(N) variation was observed. At robust plasma conditions the matrix effect was reduced for all matrices and analytes considered. The precision of analysis ranged from 3 to 13%, whereas the analytes recoveries in the spiked samples varied, mostly, from 90 to 110%. The detection limits of studied elements were from 0.004 to 10 mg kg(-1).

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

    NASA Astrophysics Data System (ADS)

    Tyburska, Anna; Jankowski, Krzysztof; Rodzik, Agnieszka

    2011-07-01

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

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

    SciTech Connect

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

    2008-01-14

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

  6. Microplasma source based on a dielectric barrier discharge for the determination of mercury by atomic emission spectrometry.

    PubMed

    Zhu, Zhenli; Chan, George C-Y; Ray, Steven J; Zhang, Xinrong; Hieftje, Gary M

    2008-11-15

    A low-power, atmospheric-pressure microplasma source based on a dielectric barrier discharge (DBD) has been developed for use in atomic emission spectrometry. The small plasma (0.6 mm x 1 mm x 10 mm) is generated within a glass cell by using electrodes that do not contact the plasma. Powered by an inexpensive ozone generator, the discharge ignites spontaneously, can be easily sustained in Ar or He at gas flow rates ranging from 5 to 200 mL min(-1), and requires less than 1 W of power. The effect of operating parameters such as plasma gas identity, plasma gas flow rate, and residual water vapor on the DBD source performance has been investigated. The plasma can be operated without removal of residual water vapor, permitting it to be directly coupled with cold vapor generation sample introduction. The spectral background of the source is quite clean in the range from 200 to 260 nm with low continuum and structured components. The DBD source has been applied to the determination of Hg by continuous-flow, cold vapor generation and offers detection limits from 14 (He-DBD) to 43 pg mL(-1) (Ar-DBD) without removal of the residual moisture. The use of flow injection with the He-DBD permits measurement of Hg with a 7.2 pg limit of detection, and with repetitive injections having an RSD of <2% for a 10 ng mL(-1) standard.

  7. Determination of impurities in magnesium niobate by slurry introduction axially viewed inductively coupled plasma optical emission spectrometry.

    PubMed

    Wu, Dongmei; Qu, Haiyun; Dong, Min; Wang, Anbao; He, Pingang; Fang, Yuzhi

    2007-11-01

    A simple preparation scheme is described for the quantitative analysis of a magnesium niobate sample using slurry introduction axially viewed inductively coupled plasma optical emission spectrometry. Relationships between the stability of slurries and the conditions, such as particle size, pH, dispersant and amount of dispersant, were investigated experimentally. The MgNb(2)O(6) slurry sample was prepared by adding the dispersant sodium polyacrylate and agitation in an ultrasonic bath to ensure good dispersion. Under optimization of pH and amount of dispersant, an analysis of minor and trace impurities (Ba, Ca, Cr, Cu, Fe, Mn, Ni, Pb) in magnesium niobate was accomplished. Applying a paired t test, we showed that the results were in agreement at a 95% confidence level with the reference values obtained by a fusion method for a magnesium niobate sample, which verified that the calibration curves could be established by aqueous standards. Analytical results demonstrate that the factors that affected the accuracy of determination for MgNb(2)O(6) are mainly the particle size of the sample and the stability of slurry.

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

    PubMed

    Shekhar, R

    2012-05-15

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

  9. Simultaneous multielemental analysis of some environmental and biological samples by inductively coupled plasma atomic emission spectrometry

    SciTech Connect

    Hee, S.S.Q.; Boyle, J.R.

    1988-05-15

    The Parr bomb technique is found to be the preferred acid digestion method for multielemental analysis by simultaneous inductively coupled plasma atomic emission spectroscopy (ICP-AES) when compared with microwave and hot plate methods for many environmental and biological specimens, but especially for the latter. One digestion alone often did not produce quantitative results compared with a sequential digestion scheme. The digestions were then refined to be as similar as possible for the various substrates studied. The interference of carbon on As and Se had to be corrected at less than or equal to 3000 ..mu..g of C/mL in the analysis solution, and thus the C content had to be monitored to assess the efficiency of the digestions and to determine if interelemental correction for C presence was required. The C correction was adequate in the range 3000-10,000 ..mu..g of C/ml. The use of modified k values was demonstrated to provide accuracy and had to be used for ICP-AES spectrometers where background corrections were performed first for fixed channels. The results on Cincinnati soils and feces of Cincinnati children showed that Si and Ti were possible tracer elements for soil ingestion by the children.

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

    PubMed

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

    2016-04-19

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

  11. Determination of barium, chromium, cadmium, manganese, lead and zinc in atmospheric particulate matter by inductively coupled plasma atomic emission spectrometry (ICP-AES)

    NASA Astrophysics Data System (ADS)

    Boevski, I. V.; Daskalova, N.; Havezov, I.

    2000-11-01

    The present paper has shown that the Q concept, as proposed by P.W.J.M. Boumans, J.J.A.M. Vrakking, Spectrochim. Acta Part B 43 (1988) 69, can be used as a basic methodology in the determination of Ba, Cr, Cd, Mn, Pb and Zn in pairs of atmospheric particles by inductively coupled plasma atomic emission spectrometry (ICP-AES). The data base of Q values for line interference [ QIj(λ a)] and Q values for wing background interference [ QWJ(Δλ a)] were obtained in our former work [N. Daskalova, Iv. Boevski, Spectral interferences in the determination of trace elements in environmental materials by inductively coupled plasma atomic emission spectrometry, Spectrochim. Acta Part B 54 (1999) 1099-1122]. The samples of atmospheric particles were collected by the Bergerhoff method. The ICP-AES determination was performed after sample digestion with aqua regia. Q values were used for the calculation of both the total interfering signal under the analysis lines and the true detection limits, depending on the matrix constituents in the different samples. Comparative data for the concentration of analytes were obtained by flame atomic absorption spectrometry (FAAS) and direct current arc atomic emission spectrographic method (dc arc-AES).

  12. Modelling of the evaporation behaviour of particulate material for slurry nebulization inductively coupled plasma atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Merten, D.; Heitland, P.; Broekaert, J. A. C.

    1997-11-01

    This paper is an electronic publication in Spectrochimica Acta Electronica (SAE), the electronic section of Spectrochimica Acta, Part B (SAB). This hardcopy text, comprising the main body and an appendix, is accompanied by a disk with programs, data files and a brief manual. The main body discusses purpose, design principle and usage of the computer software for modelling the evaporation behaviour of particles in inductively coupled plasma atomic emission spectrometry (ICP-AES). Computer software has been developed in FORTRAN 77 language in order to simulate the evaporation behaviour of particles of refractory materials such as encountered in the analysis of advanced ceramic powders by slurry nebulization inductively coupled argon plasma atomic spectrometry. The program simulates the evaporation of single particles in the inductively coupled plasma and also enable it to calculate on the base of a given particle size distribution the evaporation behaviour of all the particles contained in a sample. In a so-called "intensity concept", the intensity is calculated as a function of the observation height in order to determine recovery rates for slurries compared with aqueous solutions. This yields a quick insight whether a calibration with aqueous solutions can be used for analysis of slurries of a given powder by slurry nebulization ICP-AES and also is a help in determining the optimal parameters for analyses of powders by means of slurry nebulization ICP-AES. Applications for the evaporation of Al 2O 3 and SiC powders document the usefulness of the model for the case of a 1.5 kW argon ICP of which the temperature at 8 mm above the load coil has been determined to be 6100 K. The model predicts the maximum particle size for SiC and Al 2O 3 that can be transported (10-15 μm) and evaporated for a given efficiency under given experimental conditions. For both Al 2O 3 and SiC, two ceramic powders of different grain size were investigated. The median particle sizes cover

  13. A Multi-Pumping Flow System for In Situ Measurements of Dissolved Manganese in Aquatic Systems

    PubMed Central

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

    2016-01-01

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

  14. A Multi-Pumping Flow System for In Situ Measurements of Dissolved Manganese in Aquatic Systems.

    PubMed

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

    2016-11-30

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

  15. Simple methods for characterization of metals in historical textile threads.

    PubMed

    Rezić, Iva; Curković, Lidija; Ujević, Magdalena

    2010-06-30

    Characterization of metal threads on historical textile materials is important for preservation of valuable cultural heritage. Obtained results dictate decisions on cleaning, conservation and restoration steps. The most important part of characterization is chemical analysis of originally applied materials, since this enables understanding the nature of chemical and physical degradation and determines the cleaning methods. Methods applied should be non-destructive and sensitive enough to detect trace elements in small sample amounts. The goal of this research was to describe the most useful procedures for fast and simple determination of specific metals of interest. Therefore we propose application of scanning electron microscopy equipped with EDS detector (SEM-EDS) for sample surface analysis and inductively coupled plasma-optical emission spectroscopy (ICP-OES) for chemical analysis of metals threads. For quality insurance reasons, a comparative method applied for chemical analysis was atomic absorption spectrometry (AAS). This combination of methods has proven to be very useful in analysis of historical samples, since SEM-EDS was a simple and non-destructive method which provided information on chemical composition of sample surfaces, while ICP-OES and AAS enabled the full insight into the average chemical composition of samples. Nevertheless, both ICP-OES and AAS were destructive methods which demanded dissolving of samples prior to the analysis. In this work nine different metal fibers collected from historical textile materials were characterized. Proposed methods enabled obtaining information on sample constitution, morphology, topology and chemical composition. Copyright 2010 Elsevier B.V. All rights reserved.

  16. Elemental analysis of gunshot residue to differentiate bullet type and firing distance

    NASA Astrophysics Data System (ADS)

    Hay, Christine Ella

    Gunshot residue (GSR) was deposited on porcine tissue with hand loaded non-jacketed (NJ) and full-jacketed (FJ) ammunition at two different firing distances. Fresh tissue samples, as well as samples collected throughout decomposition were microwave digested in nitric acid and analyzed by inductively coupled plasma-optical emission spectroscopy (ICP-OES) and inductively coupled plasma-mass spectrometry (ICP-MS) to determine the elemental composition of the GSR. Element concentrations for lead (Pb), antimony (Sb), barium (Ba), copper (Cu), iron (Fe), and zinc (Zn) were statistically compared in order to investigate differentiation of bullet type and firing distance based on chemical concentrations in the GSR. Control (unshot) samples were collected in order to assess for environmental contaminants. Results of this study demonstrated that ICP-OES was adequate to detect the characteristic elements of GSR in fresh tissue, but was not sensitive enough to detect all elements throughout decomposition. Lead and Sb were significantly greater in NJ samples. Barium was useful in differentiating firing distance for both bullet types, while Cu was used to differentiate firing distance in FJ ammunition only. Analysis using ICP-MS, which has detection limits up to three orders of magnitude lower compared to ICP-OES, demonstrated the persistence of Pb, Sb, and Ba on porcine tissue throughout decomposition at a firing distance of 5 cm for both NJ and FJ ammunition.

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

    PubMed

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

    2016-07-01

    An Inductively Coupled Plasma Optical Emission Spectrometry method for simultaneous determination of Al, Ca, Cu, Fe, In, Mn, Ni, Si, Sr, Y, Zn, Zr and rare earth elements (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu) in magnesium alloys, including the new rare earth elements-alloyed magnesium, has been developed. Robust conditions have been established as nebulizer argon flow rate of 0.5mLmin(-1) and RF incident power of 1500W, in which matrix effects were significantly reduced around 10%. Three acid digestion procedures were performed at 110°C in closed PFA vessels heated in an oven, in closed TFM vessels heated in a microwave furnace, and in open polypropylene tubes with reflux caps heated in a graphite block. The three digestion procedures are suitable to put into solution the magnesium alloys samples. From the most sensitive lines, one analytical line with lack or low spectral interferences has been selected for each element. Mg, Rh and Sc have been studied as internal standards. Among them, Rh was selected as the best one by using Rh I 343.488nm and Rh II 249.078nm lines as a function of the analytical lines. The trueness and precision have been established by using the Certified Reference Material BCS 316, as well as by means of recovery studies. Quantification limits were between 0.1 and 9mgkg(-1) for Lu and Pr, respectively, in a 2gL(-1) magnesium matrix solution. The method developed has been applied to the commercial alloys AM60, AZ80, ZK30, AJ62, WE54 and AE44. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    NASA Astrophysics Data System (ADS)

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

    2014-06-01

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

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

    PubMed

    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 <20μm), prepared in 10% m/v HCl through the application of ultrasonic agitation, was used with calibration by the standard addition 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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-12-01

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

  1. A novel approach for reducing toxic emissions during high temperature processing of electronic waste.

    PubMed

    Saini, R; Khanna, R; Dutta, R K; Cayumil, R; Ikram-Ul-Haq, M; Agarwala, V; Ellamparuthy, G; Jayasankar, K; Mukherjee, P S; Sahajwalla, V

    2017-03-09

    A novel approach is presented to capture some of the potentially toxic elements (PTEs), other particulates and emissions during the heat treatment of e-waste using alumina adsorbents. Waste PCBs from mobile phones were mechanically crushed to sizes less than 1mm; their thermal degradation was investigated using thermo-gravimetric analysis. Observed weight loss was attributed to the degradation of polymers and the vaporization of organic constituents and volatile metals. The sample assembly containing PCB powder and adsorbent was heat treated at 600°C for times ranging between 10 and 30min with air, nitrogen and argon as carrier gases. Weight gains up to ∼17% were recorded in the adsorbent thereby indicating the capture of significant amounts of particulates. The highest level of adsorption was observed in N2 atmosphere for small particle sizes of alumina. SEM/EDS results on the adsorbent indicated the presence of Cu, Pb, Si, Mg and C. These studies were supplemented with ICP-OES analysis to determine the extent of various species captured as a function of operating parameters. This innovative, low-cost approach has the potential for utilization in the informal sector and/or developing countries, and could play a significant role in reducing toxic emissions from e-waste processing towards environmentally safe limits.

  2. Emission mechanism of polyatomic ions Cs2Cl+ and Cs2BO2(+) in thermal ionization mass spectrometry with various carbon materials.

    PubMed

    Wei, Hai-Zhen; Jiang, Shao-Yong; Hemming, Gary N; Yang, Jing-Hong; Xiao, Ying-Kai; Yang, Tao; Yan, Xiong; Yan, Yan

    2011-12-29

    The emission behavior of polyatomic ions Cs(2)Cl(+) and Cs(2)BO(2)(+) in the presence of various carbon materials (Graphite, Carbon, SWNTs, and Fullerenes) in the ionization source of thermal ionization mass spectrometry (TIMS) has been investigated. The emission capacity of various carbon materials are remarkably different as evidenced by the obvious discrepancy in signal intensity of polyatomic ions and accuracy/precision of boron and chlorine isotopic composition determined using Cs(2)Cl(+)-graphite-PTIMS/Cs(2)BO(2)(+)-graphite-PTIMS methods. Combined with morphology and microstructure properties of four selected carbon materials, it could be concluded that the emission behavior of the polyatomic ions strongly depends on the microstructure of the carbon materials used. A surface-induced collision mechanism for formation of such kinds of polyatomic ions in the ionization source of TIMS has been proposed based on the optimized configuration of Cs(2)BO(2)(+) and Cs(2)Cl(+) ions in the gas phase using a molecular dynamics method. The combination of the geometry of the selected carbon materials with the configuration of two polyatomic ions explains the structure effect of carbon materials on the emission behavior of polyatomic ions, where graphite samples with perfect parallels and equidistant layers ensure the capacity of emission to the maximum extent, and fullerenes worsen the emission of polyatomic ions by blocking their pathway.

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

    SciTech Connect

    Ombaba, J.M.

    1992-01-01

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

  4. [Pretreatment of Aluminum-Lithium Alloy Sample and Determination of Argentum and Lithium by Spectral Analysis].

    PubMed

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

    2015-10-01

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

  5. Energy-dispersive X-ray spectrometry combined with directly suspended droplet microextraction for determination of dissolved silicate in surface water via silicomolybdenum blue complex.

    PubMed

    Pytlakowska, Katarzyna

    2014-10-01

    Energy-dispersive X-ray fluorescence spectrometry (EDXRF) is a well-established analytical technique successfully applied with good precision and accuracy to determination of many elements. However, in the case of elements of low atomic number, such as silicon, direct determination is hampered due to low fluorescence yield and relatively low energy easily absorbed by sample matrix. An indirect method for determining surface water silicate is thus proposed. The method is based on silicate determination via molybdenum present in silicomolybdenum blue complex. Determination follows directly suspended droplet microextraction. Optimum conditions for both microextraction and EDXRF measurement were studied. A good ratio of silicon to molybdenum (1-41) and a sensitive Kα line of molybdenum make it possible to determine low concentrations of silicate. Under optimized conditions, good linearity, up to 3 μg mL(-1) (r=0.9990), and good detection limit (6 ng mL(-1)) were achieved. The total RSD for the EDXRF determination of silicate following DSDME was 6.7%. Taking into account all steps preceding the determination and the uncertainty of XRF measurements, the proposed method can be recognized as precise. The enrichment factor was 140. The developed method was used to determine dissolved silicate content in surface water samples. The accuracy and repeatability of the proposed procedure were checked by standard addition method and compared to the results obtained using ICP-OES technique. The recovery (92.2-96%) was satisfactory and indicates usefulness of the developed procedure.

  6. Investigations on the conditional kinetic and thermodynamic stability of aquatic humic substance-metal complexes by means of EDTA exchange, ultrafiltration and atomic spectrometry.

    PubMed

    Van den Bergh, J; Jakubowski, B; Burba, P

    2001-09-13

    The conditional metal availability and the kinetic stability of humic substance-metal species in humic-rich waters (e.g. bog water) was characterized by means of EDTA exchange. For this purpose a combined procedure consisting of time-controlled ligand exchange by EDTA, species differentiation by a fast single-stage tangential-flow ultrafiltration (TF-UF) technique (cut-off 1 kDa) and sensitive atomic spectrometry methods (e.g. AAS, ICP-OES, TXRF) was developed. The kinetics and the yield of the EDTA exchange served as operational parameters for assessing the kinetic stability and EDTA availability of HS-metal species, respectively. Considerable fractions of natural HS-metal species studied were shown to be EDTA-inert (e.g. 31% of the total Fe, 44% of the total Al) even after long reaction times (48 h), in contrast to artificial ones formed in solutions of isolated HS. Moreover, the conditional thermodynamic stability of HS-metal complexes formed by successive loading of an aquatic reference HS (HO14) with a number of heavy metal ions (e.g. Cr(III), Cu(II), Fe(III), Mn(II), Zn(II)) was also evaluated discriminating the free metal concentrations by means of TF-UF. In addition, from the loading isotherms obtained conditional complexation capacities could be derived for the studied HS exhibiting the order Fe(III)>Cu(II)>Cr(III)>Co(II)>Mn(II).

  7. Simultaneous determination of trace heavy metals in ambient aerosols by inductively coupled plasma atomic emission spectrometry after pre-concentration with sodium diethyldithiocarbamate.

    PubMed

    Talebi, S M; Malekiha, M

    2008-07-01

    The simultaneous determination of heavy metals associated with airborne particulate matter in the atmosphere of the city Isfahan (Iran) was performed by inductively coupled plasma atomic emission spectrometry (ICP-AES) after pre-concentration with sodium diethyldithiocarbamate. The preconcentration procedure developed found instrumental to determine the trace heavy metals associated with ambient aerosols collected at a short sampling period or collected from rural areas where the concentrations of these metals are much less than those in urban areas. Several samples were analyzed by both flame atomic absorption spectrometry (FAAS) as a conventional method and the proposed method. The results obtained by the two methods were found in good agreement. The method was applied to the determination of atmospheric level of heavy metals in rural area and also for study of variation in levels of heavy metals in urban atmosphere during the days and nights.

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

    NASA Astrophysics Data System (ADS)

    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

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

    PubMed

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

    2016-03-01

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

  10. On-line monitoring of pine needles combustion emissions in the presence of fire retardant using a "thermogravimetry (TG)-bridge/mass spectrometry method".

    PubMed

    Tzamtzis, N; Karma, S; Pappa, A; Statheropoulos, M

    2006-07-28

    In this work a new method called TG-bridge/mass spectrometry is presented, for the on-line monitoring of the pine needles combustion emissions in a common lab furnace. The TG-bridge (thermogravimetry-bridge) system has been developed in-house as a TG-MS (thermogravimetry-mass spectrometry) interface, for TG-MS analysis. In this work, TG-bridge was used for directly sampling of the combustion emissions from the inside of the furnace and transferring them into the mass spectrometer (MS), without disturbing the sub-pressure conditions inside the MS ion source. The effect of Fire-Trol 931 (a long-term fire retardant) on the emissions, produced during the combustion of pine needles, is tested in the lab for future application in the field. It was shown that in treated samples, increased evolution of ammonia and aromatic compounds took place, compared to untreated samples. Maximum concentrations of specific compounds, such as benzene and toluene, evolved during the combustion experiments in the furnace, were determined.

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

    PubMed

    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.

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

    NASA Astrophysics Data System (ADS)

    Ombaba, Jackson M.

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

  13. Comparison of ultrasonic and thermospray systems for high performance sample introduction to inductively coupled plasma atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Conver, Timothy S.; Koropchak, John A.

    1995-06-01

    This paper describes detailed work done in our lab to compare analytical figures of merit for pneumatic, ultrasonic and thermospray sample introduction (SI) systems with three different inductively coupled plasma-atomic emission spectrometry (ICP-AES) instruments. One instrument from Leeman Labs, Inc. has an air path echelle spectrometer and a 27 MHz ICP. For low dissolved solid samples with this instrument, we observed that the ultrasonic nebulizer (USN) and fused silica aperture thermospray (FSApT) both offered similar LOD improvements as compared to pneumatic nebulization (PN), 14 and 16 times, respectively. Average sensitivities compared to PN were better for the USN, by 58 times, compared to 39 times for the FSApT. For solutions containing high dissolved solids we observed that FSApT optimized at the same conditions as for low dissolved solids, whereas USN required changes in power and gas flows to maintain a stable discharge. These changes degraded the LODs for USN substantially as compared to those utilized for low dissolved solid solutions, limiting improvement compared to PN to an average factor of 4. In general, sensitivities for USN were degraded at these new conditions. When solutions with 3000 μg/g Ca were analyzed, LOD improvements were smaller for FSApT and USN, but FSApT showed an improvement over USN of 6.5 times. Sensitivities compared to solutions without high dissolved solids were degraded by 19% on average for FSApT, while those for USN were degraded by 26%. The SI systems were also tested with a Varian Instruments Liberty 220 having a vacuum path Czerny-Turner monochromator and a 40 MHz generator. The sensitivities with low dissolved solids solutions compared to PN were 20 times better for the USN and 39 times better for FSApT, and LODs for every element were better for FSApT. Better correlation between relative sensitivities and anticipated relative analyte mass fluxes for FSApT and USN was observed with the Varian instrument. LOD

  14. Analytical capability of a medium power capacitively coupled plasma for the multielemental determination in multimineral/multivitamin preparations by atomic emission spectrometry.

    PubMed

    Frentiu, Tiberiu; Ponta, Michaela; Darvasi, Eugen; Frentiu, Maria; Cordos, Emil

    2012-10-15

    A method for multielemental (Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P and Zn) determination in multimineral/multivitamins by atomic emission spectrometry in a medium power radiofrequency capacitively coupled plasma (275 W) and low Ar consumption (0.4 L min(-1)) is proposed. Determinations were performed on commercially available tablets and a standard reference material after acidic high-pressure microwave assisted digestion and using the standard additions procedure. The detection limits (mg g(-1)) were in the range 0.003 (Na)-1.5 (P) and were not depreciated by the non-spectral interference of mineral matrices of K, Ca, Mg and Na excepting Zn and P. Found concentrations corresponded generally to the labelled contents with recovery in the range of 90-107% and 1.0-13.0% repeatability. The proposed technique could be an advantageous alternative to the more expensive inductively coupled plasma atomic emission spectrometry in the quality control of multimineral/multivitamin preparations. Copyright © 2012 Elsevier Ltd. All rights reserved.

  15. Lithium loss in the solid electrolyte interphase: Lithium quantification of aged lithium ion battery graphite electrodes by means of laser ablation inductively coupled plasma mass spectrometry and inductively coupled plasma optical emission spectroscopy

    NASA Astrophysics Data System (ADS)

    Schwieters, Timo; Evertz, Marco; Mense, Maximilian; Winter, Martin; Nowak, Sascha

    2017-07-01

    In this work we present a new method using LA-ICP-MS to quantitatively determine the lithium content in aged graphite electrodes of a lithium ion battery (LIB) by performing total depth profiling. Matrix matched solid external standards are prepared using a solid doping approach to avoid elemental fractionation effects during the measurement. The results are compared and matched to the established ICP-OES technique for bulk quantification after performing a microwave assisted acid digestion. The method is applied to aged graphite electrodes in order to determine the lithium immobilization (= ;Li loss;) in the solid electrolyte interphase after the first cycle of formation. For this, different samples including a reference sample are created to obtain varying thicknesses of the SEI covering the electrode particles. By applying defined charging voltages, an initial lithiation process is performed to obtain specific graphite intercalation compounds (GICs, with target stoichiometries of LiC30, LiC18, LiC12 and LiC6). Afterwards, the graphite electrode is completely discharged to obtain samples without mobile, thus active lithium in its lattice. Taking the amount of lithium into account which originates from the residues of the LiPF6 (dissolved in the carbon components containing electrolyte), it is possible to subtract the amount of lithium in the SEI.

  16. Efficiency of macroporous poly(vinylphosphoramidic acid) resin adsorbing of selected elements and determination of trace dysprosium, holmium, erbium, and ytterbium in waste water by inductively coupled plasma optical emission spectrometry

    SciTech Connect

    Zhan Guangyao; Su Zhixing; Lou Xingyin; Chang Xijun )

    1992-03-01

    A macroporous poly(vinylphosphoramidic acid) resin is synthesized through the reaction of macroporous poly(vinylethylenediamine) resin with formaldehyde and phosphorus acid. The adsorption efficiency of the resin to selected elements is determined. An ICP-OES method has been established for the resin enrichment and separation of trace Dy, Ho, Er and Yb ions in waste water. The ability of the Na-form resin to adsorb Dy, Ho, Er, and Yb ions is far better than the H-form resin. The IR spectra of the resin before and after adsorbing Dy are shown. The mechanism of resin adsorption of Dy is explored. The results of resin enriched waste water analysis from a smelter plant are 31.0 ng/ml for dy, 41.1 ng/ml for Hl, 20.6 ng/ml for Er and 20.2 ng/ml for Yb ions. The recovery of standard additions of Dy, Ho, Er, and Yb to the waste water is in the range of 97.0-98.5%.

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

    PubMed

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

    2016-02-02

    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.

  18. Development and fundamental investigation of Laser Ablation Glow Discharge Time-Of-Flight Mass Spectrometry (LA-GD-TOFMS)

    NASA Astrophysics Data System (ADS)

    Tarik, Mohamed; Lotito, Giovanni; Whitby, James A.; Koch, Joachim; Fuhrer, Katrin; Gonin, Marc; Michler, Johann; Bolli, Jean-Luc; Günther, Detlef

    2009-03-01

    Glow Discharge (GD) spectroscopy is a well known and accepted technique for the bulk and surface composition analysis, while laser ablation (LA) provides analysis with high spatial-resolution analysis in LIBS (laser-induced breakdown spectroscopy) or when coupled to inductively coupled plasma spectrometry (ICP-OES or ICP-MS). This work concerns the construction of a Laser Ablation Glow Discharge Time-Of-Flight Mass Spectrometry (LA-GD-TOFMS) instrument to study the analytical capabilities resulting from the interaction of a laser-generated sample plume with a pulsed glow discharge. Two ablation configurations were studied in detail. In a first approach, the laser-generated plume was introduced directly into the GD, while the second approach generated the plume inside the GD. The ablated material was introduced at different times with respect to the discharge pulse in order to exploit the efficient ionization in the GD plasma. For both LA-GD configurations, direct ablation into the afterglow of the pulsed glow discharge leads to an ion signal enhancement of up to a factor of 7, as compared to the ablation process alone under the same experimental conditions. The LA-GD enhancement was found to occur exclusively in the GD afterglow, with a maximum ablation S/N occurring in a few hundred microseconds after the termination of the glow discharge. The duration of the enhanced signal is about two milliseconds. Both the laser pulse energy and the position of the ablation plume (with respect to the sampling orifice) were found to affect the amount of mass entering the afterglow region and consequently, the enhancement factor of ionization.

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

    PubMed

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

    2014-01-02

    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.

  20. A novel methodology for rapid digestion of rare earth element ores and determination by microwave plasma-atomic emission spectrometry and dynamic reaction cell-inductively coupled plasma-mass spectrometry.

    PubMed

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

    2016-11-01

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

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

    PubMed Central

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

    2014-01-01

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

  2. Light emission of a polyfluorene derivative containing complexed europium ions.

    PubMed

    Turchetti, Denis Augusto; Nolasco, Mariela Martins; Szczerbowski, Daiane; Carlos, Luís Dias; Akcelrud, Leni Campos

    2015-10-21

    The photophysical properties of a new alternating copolymer containing fluorene, terpyridine, and complexed sites with trivalent europium (Eu(3+)) ions (LaPPS66Eu) were investigated, using the non-complexed backbone (LaPPS66) and a low molecular weight compound of similar chemical structure of the ligand/Eu(3+) site (LaPPS66M) as a model compound. The analogous gadolinium complex (LaPPS66Gd) was also synthesized to determine the triplet state of the complex. (1)H and (13)C nuclear magnetic resonance (NMR) analysis, Fourier transform infrared (FT-IR) spectroscopy, inductively coupled plasma optical emission spectroscopy (ICP-OES), elemental analyses, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA) characterized the chemical structure and thermal properties of the synthesized materials. A level of Eu(3+) insertion of 37% (molar basis) in the polymer backbone was achieved. The photoluminescence studies were performed in the solid state showing the occurrence of polymer-to-Eu(3+) energy transfer brought about by the spectral overlap between the absorption spectra of the Eu(3+) complex and the emission of the polymer backbone. A detailed theoretical photoluminescence study performed using time-dependent DFT (TD-DFT) calculations and the recently developed LUMPAC luminescence package is also presented. The high accuracy of the theoretical calculations was achieved on comparison with the experimental values. Aiming at a deeper level of understanding of the photoluminescence process, the ligand-to-Eu(3+) intramolecular energy transfer and back-transfer rates were predicted. The complexed materials showed a dominant pathway involving the energy transfer between the triplet of the dbm (dibenzoylmethane) ligand and the (5)D1 and (5)D0 Eu(3+) levels.

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

    NASA Astrophysics Data System (ADS)

    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.

  4. Lanthanoides in Glass and Glass Ceramics

    NASA Astrophysics Data System (ADS)

    Meinhardt, Jürgen; Kilo, Martin; Somorowsky, Ferdinand; Hopp, Werner

    2017-03-01

    Many types of glass contain lanthanoides; among them, special glass for optical applications is the one with the highest content of lanthanoides. The precise determination of the lanthanoides' concentration is performed by inductively coupled plasma-optical emission spectrometry (ICP-OES). However, up to now, there are no established standard processes guaranteeing a uniform approach to the lanthanoide analysis. The knowledge of the lanthanoides' concentrations is necessary on the microscale in some cases, especially if a suitable separation and recycling procedure is to be applied. Here, the analysis is performed by energy-dispersive X-ray (EDX) or wavelength-dispersive X-ray (WDX) analytics in the scanning electron microscope.

  5. Determination of non-metallic elements by capacitively coupled helium microwave plasma atomic emission spectrometry with capillary gas chromatography.

    PubMed

    Uchida, H; Berthod, A; Winefordner, J D

    1990-07-01

    A capacitively coupled microwave helium plasma with a tubular tantalum electrode was evaluated as an element selective detector for gas chromatography (GC). The end of a 10-m bonded fused capillary column was directly inserted into the tubular electrode without any switching system. A heated copper tube was used to house the part of the GC column that protruded from the oven. The optimisation of operating parameters, line selection, background emission and horizontal and vertical observation position is described. Analytical figures of merit including sensitivity, reproducibility, signal to background ratio, selectivity, dynamic range and limit of detection (LOD), were evaluated for carbon, hydrogen, chlorine and bromine emission. Limits of detection in the low ng range (20 pmol) were obtained for halogenated compounds using carbon emission, whereas LODs in the 0.1 micrograms range (2 nmol) were obtained using chlorine or bromine emission lines.

  6. Capacitively coupled microplasma for on-column detection of chromatographically separated inorganic gases by optical emission spectrometry.

    PubMed

    Guchardi, Renato; Hauser, Peter C

    2004-04-16

    Two tubular electrodes placed on a capillary tubing are used to couple an electrical ac field of high voltage (20 kV) but low frequency (20 kHz) and about 8 W power inside for generation of the plasma. The emitted radiation is passed to a spectrometer via an optical fibre butted to the side of the capillary. The excitation temperature of the plasma determined from helium emission lines is about 4000 K. It was found possible to detect oxygen from its emission at 777 and 845 nm, hydrogen at 656 nm and sulfur containing species from emission at 923 nm. The carbon-containing species CH4, CO, and CO2 could be determined from an emission band at 385 nm due to CN. Detection limits in the range between about 1 and 10 ng were obtained using a miniature diode array spectrometer.

  7. X-ray Spectrometry.

    ERIC Educational Resources Information Center

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

    1984-01-01

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

  8. X-ray Spectrometry.

    ERIC Educational Resources Information Center

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

    1984-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2006-07-01

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

  10. Use of gradient dilution to flag and overcome matrix interferences in axial-viewing inductively coupled plasma-atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Cheung, Yan; Schwartz, Andrew J.; Hieftje, Gary M.

    2014-10-01

    Despite the undisputed power of inductively coupled plasma-atomic emission spectrometry (ICP-AES), its users still face serious challenges in obtaining accurate analytical results. Matrix interference is perhaps the most important challenge. Dilution of a matrix-containing sample is a common practice to reduce matrix interference. However, determining the optimal dilution factor requires tedious and time-consuming offline sample preparation, since emission lines and the effect of matrix interferences are affected differently by the dilution. The current study exploits this difference by employing a high-performance liquid chromatography gradient pump prior to the nebulizer to perform on-line mixing of a sample solution and diluent. Linear gradient dilution is performed on both the calibration standard and the matrix-containing sample. By ratioing the signals from two emission lines (from the same or different elements) as a function of dilution factor, the analyst can not only identify the presence of a matrix interference, but also determine the optimal dilution factor needed to overcome the interference. A ratio that does not change with dilution signals the absence of a matrix interference, whereas a changing ratio indicates the presence of an interference. The point on the dilution profile where the ratio stabilizes indicates the optimal dilution factor to correct the interference. The current study was performed on axial-viewing ICP-AES with o-xylene as the solvent.

  11. Determination of heavy metals in bee honey with connected and not connected metal wires using inductively coupled plasma atomic emission spectrometry (ICP-AES).

    PubMed

    Özcan, Mehmet Musa; Al Juhaimi, Fahad Y

    2012-04-01

    Two honey samples are taken from two parts of the same honeycomb: one that contacts to the surface of the wire and the other taken from the surface that does not contact the wires. Heavy metal contents of these two samples were determined by inductively coupled plasma atomic emission spectrometry). The Mo, Cd, Cr, Fe, Mn, Ni and Zn contents of the honey in contact with wire is higher when compared to the other. Especially, Fe and Zn contents of honey in contact with wire is much higher than the non-contact one. These values are, respectively, 190.21 and 112.76 ppm. Besides, Ni content of honey in contact with wire is approximately 50% higher.

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

    NASA Astrophysics Data System (ADS)

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

    2002-08-01

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

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

    PubMed

    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.

  14. [On-line determination of niobium and tantalum in soil and geochemical exploration samples by inductively coupled plasma atomic emission spectrometry with solvent extraction flow injection].

    PubMed

    Ai, J; Tang, Z Y

    2001-10-01

    A new method for the determination of trace niobium and tantalum in soil and geochemical exploration samples by inductively coupled plasma atomic emission spectrometry with solvent extraction flow injection was proposed. The niobium and tantalum were extracted with the mixed solvent of MIBK and TBP at 1 mol.L-1 HF and 4 mol.L-1 H2SO4. Experiment conditions and manifold parameters were investigated in detail. The detection limits were 0.5 x 10(-12) g.L-1 and 0.8 x 10(-12) g.L-1. The proposed method was rapid, simple and accurate, it has been applied to the determination of trace niobium and tantalum in national standard samples. The results were in good agreement with certified values with precisions of 4.5% and 5.1% RSD (n = 10). The sample throughput for niobium and tantalum is 20.h-1.

  15. Electrothermal vaporization — inductively coupled plasma-atomic emission spectrometry for trace metal determination in uranium and thorium compounds without prior matrix separation

    NASA Astrophysics Data System (ADS)

    Purohit, Paru J.; Goyal, Neelam; Thulasidas, S. K.; Page, A. G.; Sastry, M. D.

    2000-08-01

    The electrothermal vaporization (ETV) mode of sample introduction into inductively coupled plasma (ICP) has been examined for its suitability for the analysis of trace metals in uranium and thorium compounds without prior chemical separation of the matrices using atomic emission spectrometry (AES). The ETV interfaced with an ICP torch adapted for glove box operation, has led to determination of sub-nanogram amounts of Al, Be, Ca, Cd, Co, Cr, Cu, Mg, Mn, Na, Ni, Zn, Dy, Eu, Gd and Sm using 10 μl of the sample aliquot containing 200 μg of U/Th matrix with a precision of 1-2%RSD. The results obtained here especially for rare earths in the presence of the matrix are of significance.

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

    PubMed

    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.

  17. Direct determination of trace elements in niobium, tantalum and their oxides by inductively coupled plasma atomic emission spectrometry after microwave dissolution

    NASA Astrophysics Data System (ADS)

    Grebneva, O. N.; Kubrakova, I. V.; Kudinova, T. F.; Kuz'min, N. M.

    1997-07-01

    Analytical schemes for the determination of trace elements in high-purity niobium, tantalum and their oxides are proposed. The schemes are based on microwave dissolution of the metals and oxides followed by inductively coupled plasma atomic emission spectrometry (ICP-AES) determination of impurities in the solutions. The possibilities of interelement and off-peak background corrections in ICP-AES analysis are discussed. The accuracy of the results obtained is confirmed by the determination of trace elements after a matrix sorption separation procedure. For a number of elements, a comparison of the results obtained by ICP-AES without and with the matrix separation procedure and by electrothermal atomic absorption spectrometry (ETAAS) shows good agreement. The limits of detection for direct ICP-AES determination are in the range 0.4*1.0 μg g -1 for Ba, Ca, Fe, Mg, Mn, Y and La; between 2.0 and 10.0 μ g -1 for B, Cd, Co, Cr, Cu, Hf, Mo, Na, Nb, Ni, Pb, Sr, Ti, Zr and Ta; and for K, Sb and W a detection limit of 20 μ g -1 is achieved. The schemes proposed are intended for rapid routine analysis.

  18. Development and Characterization of a 9-mm Inductively Coupled Argon Plasma (ICP) Source for Atomic Emission Spectrometry.

    DTIC Science & Technology

    1980-09-30

    plus inter- fereni (S.,0:l ol; raio Pal :Ca). Rcati\\,e :;talcs X , 10" V. I0(’ V - ,. ’::ire tO. lffect of P0,, on Ca 11 (393.4 tin) emission profiles...mL- I of Ca while 10 curve B is from tile same solution but with phosphate added at a molar ratio of 50 to 1 (P0 4 : Ca). Profile X was obtained at...emission profiles with changing rf power levels klramne X , 500 W; Y, 750 W). Curve A represcnts amalytc (50 jig mLŕ Ca) signal and curve B awi ]ytc

  19. Determination of calcium by inductively coupled plasma-atomic emission spectrometry, and lead by graphite furnace atomic absorption spectrometry, in calcium supplements after microwave dissolution or dry-ash digestion: method trial.

    PubMed

    Siitonen, P H; Thompson, H C

    1998-01-01

    A 3-laboratory method trial was conducted to evaluate 2 sample digestion procedures and instrumental determination parameters for analysis of calcium and lead in Ca supplements. Calcium supplements were treated by dry-ash digestion or microwave dissolution prior to spectrometric analysis. In each case, Pb was determined by graphite furnace atomic absorption spectrometry and Ca by inductively coupled plasma-atomic emission spectrometry. Blind duplicates of 6 Ca supplement samples were analyzed after each sample treatment procedure. Matrix pairs contained dissimilar Pb levels to cover the analyte range encountered during method development. Calcium content of the Ca supplement samples also reflected the range seen during method development. Stock solutions of Ca and Pb were supplied to collaborators for preparation of quantitation standards to remove a variable external to the method. National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1486, bone meal, was included to assess method accuracy and recovery at NIST certificate Ca and Pb levels for this material (26.58 +/- 0.24% Ca and 1.335 +/- 0.014 micrograms Pb/g). Analyses of the NIST SRM yielded 25.9 +/- 1.1 and 27.2 +/- 2.3% Ca and 1.53 +/- 0.19 and 1.26 +/- 0.19 micrograms Pb/g for dry-ash and microwave procedures, respectively. Statistical analyses of data indicated acceptable repeatability and reproducibility for determination of Pb and Ca in various Ca supplements. With either sample preparation technique, the method is appropriate for determining Pb or Ca in Ca supplements.

  20. Evolution of In-Cylinder Diesel Engine Soot and Emission Characteristics Investigated with Online Aerosol Mass Spectrometry.

    PubMed

    Malmborg, V B; Eriksson, A C; Shen, M; Nilsson, P; Gallo, Y; Waldheim, B; Martinsson, J; Andersson, Ö; Pagels, J

    2017-02-07

    To design diesel engines with low environmental impact, it is important to link health and climate-relevant soot (black carbon) emission characteristics to specific combustion conditions. The in-cylinder evolution of soot properties over the combustion cycle and as a function of exhaust gas recirculation (EGR) was investigated in a modern heavy-duty diesel engine. A novel combination of a fast gas-sampling valve and a soot particle aerosol mass spectrometer (SP-AMS) enabled online measurements of the in-cylinder soot chemistry. The results show that EGR reduced the soot formation rate. However, the late cycle soot oxidation rate (soot removal) was reduced even more, and the net effect was increased soot emissions. EGR resulted in an accumulation of polycyclic aromatic hydrocarbons (PAHs) during combustion, and led to increased PAH emissions. We show that mass spectral and optical signatures of the in-cylinder soot and associated low volatility organics change dramatically from the soot formation dominated phase to the soot oxidation dominated phase. These signatures include a class of fullerene carbon clusters that we hypothesize represent less graphitized, C5-containing fullerenic (high tortuosity or curved) soot nanostructures arising from decreased combustion temperatures and increased premixing of air and fuel with EGR. Altered soot properties are of key importance when designing emission control strategies such as diesel particulate filters and when introducing novel biofuels.

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

    NASA Astrophysics Data System (ADS)

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

    2004-12-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

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

    NASA Astrophysics Data System (ADS)

    Vieira de Souza, Carolina; Corrêa, Sergio Machado

    2015-02-01

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

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

    USGS Publications Warehouse

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

    1982-01-01

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

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

    USGS Publications Warehouse

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

    1978-01-01

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

  6. Surface modification of hexatriacontane by CF_4 plasmas studied by optical emission and threshold ionization mass spectrometries

    NASA Astrophysics Data System (ADS)

    Poncin-Epaillard, F.; Wang, W.; Ausserré, D.; Scharzenbach, W.; Derouard, J.; Sadeghi, N.

    1998-11-01

    The behavior of tetrafluoromethane microwave plasma (2% argon included) has been studied by emission spectroscopy during the treatment of hexatriacontane, a model for high density polyethylene. The evolution of the densities of F* atoms, and CF, CF^*2, radicals has been followed by using the actinometric technique with 2% argon added to the gas. The surface properties, such as surface energy and surface roughness were correlated to the emission intensity of reactives species in the plasma gas phase. We found that the evolution of the fluorinated species emissions in the plasma gas phase can be a direct indication of the surface modifications by the plasma. A mild exposure to the plasma can result in a great decrease of surface energy corresponding to the fluorination. The surface roughness only changes under drastic plasma conditions. Threshold ionization mass spectroscopy is applied to detect the fluorine atoms and CFx radicals. Time resolved measurements in pulsed plasma, give access to the decay rate of F atoms concentration in the afterglow, and to their sticking coefficient on different surfaces. The influences of the discharge parameters and of the surfaces (metal, silicon or hexatriacontane) in contact with the plasma are investigated. The results show that the plasma generated ions and/or UV radiations highly enhance the reactivity of the F atoms on polymer surface.

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

    SciTech Connect

    Luan, Shen

    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.

  8. Signal enhancement in solution-cathode glow discharge — optical emission spectrometry via low molecular weight organic compounds

    NASA Astrophysics Data System (ADS)

    Doroski, Todd A.; Webb, Michael R.

    2013-10-01

    HCOOH, CH3COOH, and CH3CH2OH were used as chemical modifiers in a solution-cathode glow discharge. Emission was measured directly from the discharge, without a gas-liquid separator or a secondary excitation source. Emission from Ag, Se, Pb, and Hg was strongly enhanced, and the detection limits (DL) for these elements were improved by up to an order of magnitude using a combination of HCOOH and HNO3 compared to using HNO3 alone. The DL was measured for Mg (1 μg/L), Fe (10 μg/L), Ni (6 μg/L), Cu (6 μg/L), Pb (1 μg/L), Ag (0.1 μg/L), Se (300 μg/L), and Hg (2 μg/L). Coefficients of determination (R2) were between 0.9986 and 0.9999. A voltage of 1 kV was used, which produced a current of approximately 70 mA.

  9. A Comparative Analysis of Caries Inhibitory Effect of Remineralizing Agents on Human Enamel Treated With Er:YAG Laser: An In-vitro Atomic Emission Spectrometry Analysis

    PubMed Central

    Nair, Aswin Saseendran; Kumar, R Krishna; Ahameed, Syed Shaheed; Punnathara, Sairaj; Peter, Joby

    2016-01-01

    Introduction The tug of war to maintain tooth integrity is dependent on a ratio between demineralization and remineralization. Hence, demineralization should be retarded and remineralization should be enhanced to maintain a natural equilibrium in the oral cavity. Aim To compare in-vitro acid resistance of human enamel when using Casein Phosphopeptides Amorphous Calcium Phosphate (CPP-ACP) [GC Tooth mousse] cream, Casein Phosphopeptide Amorphous Calcium Fluoride Phosphate (CPP-ACFP) [GC Tooth mousse plus] cream, Er:YAG laser alone, combination of CPP-ACP with Er:YAG laser, CPP-ACFP with Er:YAG laser. Materials and Methods An in-vitro study was done on 100 specimens which were prepared from 50 human premolars to investigate the caries inhibitory effect of remineralizing agents and laser on enamel using an atomic emission spectrometry analysis. The enamel specimens were randomly allocated into 6 groups: Untreated (control); CPP-ACP (GC Tooth mousse); CPP-ACFP (GC Tooth mousse plus); Er:YAG laser treatment alone; CPP-ACP with Er:YAG laser; CPP-ACFP with Er: YAG laser. Then specimens were immersed individually in 5ml of acetate buffer solution (0.1mol/L, pH 4.5) and incubated at 37°C for 24 hours, to determine the acid resistance by analyzing the calcium release using atomic emission spectrometry. An ANOVA model was constructed (p-value 0.05), followed by post-hoc Tukey’s test for multiple pair wise comparisons of mean values. Results There was a significant difference among the various groups with respect to amount of calcium released (p<0.001). The lowest mean score of calcium release was observed for CPP-ACFP with Er:YAG laser followed by CPP-ACFP but the differences between these groups were statistically not significant (p>0.05). Similarly the differences between CPP-ACP with Er:YAG laser and CPP-ACP also were not significant (p>0.05). The highest mean score of calcium release was for Er:YAG laser and no significant statistical difference was noticed in

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

    NASA Astrophysics Data System (ADS)

    Salewski, M.; Nocente, M.; Jacobsen, A. S.; Binda, F.; Cazzaniga, C.; Ericsson, G.; Eriksson, J.; Gorini, G.; Hellesen, C.; Hjalmarsson, A.; Kiptily, V. G.; Koskela, T.; Korsholm, S. B.; Kurki-Suonio, T.; Leipold, F.; Madsen, J.; Moseev, D.; Nielsen, S. K.; Rasmussen, J.; Schneider, M.; Sharapov, S. E.; Stejner, M.; Tardocchi, M.; Contributors, JET

    2017-05-01

    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-resolution γ-ray spectrometer detecting the γ-rays released in two reactions. The tomographic inversion based on these five spectra is in excellent agreement with numerical simulations with the ASCOT-RFOF and the SPOT-RFOF codes. The length of the measured fast-ion tail corroborates the prediction that very few particles are accelerated above 2 MeV due to the weak wave-particle interaction at higher energies.

  11. Investigation of charge transfer with non-argon gaseous species in mixed-gas inductively coupled plasma atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

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

    2007-03-01

    Potential charge-transfer reactions with non-argon gaseous species in a mixed-gas inductively coupled plasma were probed by means of two different experimental methodologies, namely the plasma-related matrix-effect approach and the relative-intensity technique. The foreign gases, introduced one by one into the central channel, were oxygen, hydrogen, nitrogen, krypton, methane and carbon dioxide at volumetric concentrations of 15%, 10%, 5%, 100%, 3% and 3%, respectively. Both matrix effects and relative intensities showed no change in behavior for emission lines with excitation energies in the vicinity of the ionization potentials of the foreign gases. This pattern suggests that the contribution of charge transfer from the foreign-gas ion is not important to the overall ionization and excitation of the analyte, in the normal analytical zone of the plasma and at the concentration of foreign gases used here.

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

    PubMed

    Roelandts, I; Robaye, G; Delbrouck-Habaru, J M; Weber, G

    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 40, 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.

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

    NASA Astrophysics Data System (ADS)

    Matusiewicz, Henryk; Barnes, Ramon M.

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

  14. Emission pattern of semi-volatile organic compounds from recycled styrenic polymers using headspace solid-phase microextraction gas chromatography-mass spectrometry.

    PubMed

    Vilaplana, Francisco; Martínez-Sanz, Marta; Ribes-Greus, Amparo; Karlsson, Sigbritt

    2010-01-15

    The emission of low molecular weight compounds from recycled high-impact polystyrene (HIPS) has been investigated using headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). Four released target analytes (styrene, benzaldehyde, acetophenone, and 2-phenylpropanal) were selected for the optimisation of the HS-SPME sampling procedure, by analysing operating parameters such as type of SPME fibre (polarity and operating mechanism), particle size, extraction temperature and time. 26 different compounds were identified to be released at different temperatures from recycled HIPS, including residues of polymerisation, oxidated derivates of styrene, and additives. The type of SPME fibre employed in the sampling procedure affected the detection of emitted components. An adsorptive fibre such as carbowax/polydimethylsiloxane (CAR/PDMS fibre) offered good selectivity for both non-polar and polar volatile compounds at lower temperatures; higher temperatures result in interferences from less-volatile released compounds. An absorptive fibre as polydimethylsiloxane (PDMS) fibre is suitable for the detection of less-volatile non-polar molecules at higher temperatures. The nature and relative amount of the emitted compounds increased with higher exposure temperature and smaller polymeric particle size. HS-SPME proves to be a suitable technique for screening the emission of semi-volatile organic compounds (SVOCs) from polymeric materials; reliable quantification of the content of target analytes in recycled HIPS is however difficult due to the complex mass-transfer processes involved, matrix effects, and the difficulties in equilibrating the analytical system. 2009 Elsevier B.V. All rights reserved.

  15. Comparative determination of Ba, Cu, Fe, Pb and Zn in tea leaves by slurry sampling electrothermal atomic absorption and liquid sampling inductively coupled plasma atomic emission spectrometry.

    PubMed

    Mierzwa, J; Sun, Y C; Chung, Y T; Yang, M H

    1998-12-01

    The comparative determination of barium, copper, iron, lead and zinc in tea leaf samples by two atomic spectrometric techniques is reported. At first, slurry sampling electrothermal atomization atomic absorption spectrometry (ETAAS) was applied. The results of Ba and Pb determination were calculated using the method of standard additions, and results of Cu, Fe and Zn from the calibration graphs based on aqueous standards. These results were compared with the results obtained after microwave-assisted wet (nitric+hydrochloric+hydrofluoric acids) digestion in closed vessels followed by inductively coupled plasma-atomic emission spectrometric (ICP-AES) determination with the calibration by means of aqueous standards. The exception was lead determined after a wet digestion procedure by ETAAS. The accuracy of the studied methods was checked by the use of the certified reference material Tea GBW-07605. The recoveries of the analytes varied in the range from 91 to 99% for slurry sampling ETAAS, and from 92.5 to 102% for liquid sampling ICP-AES. The advantages of slurry sampling ETAAS method are simplicity of sample preparation and very good sensitivity. Slurry sampling ETAAS method is relatively fast but if several elements must be determined in one sample, the time of the whole microwave-assisted digestion procedure and ICP-AES determination will be shorter. However, worse detection limits of ICP-AES must also be taken into the consideration in a case of some analytes.

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

    PubMed

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

    2014-08-01

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

  17. Multi-element analysis using inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectroscopy for provenancing of animals at the continental scale.

    PubMed

    Kreitals, Natasha M; Watling, R John

    2014-11-01

    Chemical signatures within the environment vary between regions as a result of climatological, geochemical and anthropogenic influences. These variations are incorporated into the region's geology, soils, water and vegetation; ultimately making their way through the food chain to higher level organisms. Because the variation in chemical signatures between areas is significant, a specific knowledge of differences in elemental distribution patterns between, and within populations, could prove beneficial for provenancing animals or animal related products when applied to indigenous and feral faunal populations. The domestic pig (Sus scrofa domestica) was used as an investigative model to determine the feasibility of using a chemical traceability method for the provenance determination of animal tissue. Samples of pig muscle, tongue, stomach, heart, liver and kidney were collected from known farming areas around Australia. Samples were digested in 1:3 H2O2:HNO3 and their elemental composition determined using solution based Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Pigs from different growing regions in Australia could be distinguished based on the chemical signature of each individual tissue type. Discrimination was possible at a region, state and population level. This investigation demonstrates the potential for multi-element analysis of low genetic variation native and feral species of forensic relevance.

  18. 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.

    PubMed

    Patole, Shashikant P; Simões, Filipa; Yapici, Tahir F; Warsama, Bashir H; Anjum, Dalaver H; Costa, Pedro M F J

    2016-02-01

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

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

    PubMed

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

    2012-12-01

    Volatile Organic Compounds (VOCs) formed during anaerobic digestion of aerobically pre-treated Organic Fraction of Municipal Solid Waste (OFMSW), have been monitored over a 30 day period by a direct injection mass spectrometric technique: Proton Transfer Reaction Time-of-Flight Mass Spectrometry (PTR-ToF-MS). Most of the tentatively identified compounds exhibited a double-peaked emission pattern which is probably the combined result from the volatilization or oxidation of the biomass-inherited organic compounds and the microbial degradation of organic substrates. Of the sulfur compounds, hydrogen sulfide had the highest accumulative production. Alkylthiols were the predominant sulfur organic compounds, reaching their maximum levels during the last stage of the process. H(2)S formation seems to be influenced by the metabolic reactions that the sulfur organic compounds undergo, such as a methanogenesis induced mechanism i.e. an amino acid degradation/sulfate reduction. Comparison of different batches indicates that PTR-ToF-MS is a suitable tool providing information for rapid in situ bioprocess monitoring. Copyright © 2012 Elsevier Ltd. All rights reserved.

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

    PubMed

    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).

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

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2016-06-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2006-09-01

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

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

    NASA Astrophysics Data System (ADS)

    Matusiewicz, Henryk; Golik, Bartosz

    2004-05-01

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

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

    SciTech Connect

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

    1982-11-01

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

  5. X-ray photoelectron emission microscopy and time-of-flight secondary ion mass spectrometry analysis of ultrathin fluoropolymer coatings for stent applications.

    PubMed

    Hale, Penelope; Turgeon, Stéphane; Horny, Paula; Lewis, François; Brack, Narelle; Van Riessen, Grant; Pigram, Paul; Mantovani, Diego

    2008-08-05

    Fluoropolymer plasma coatings have been investigated for application as stent coatings due to their chemical stability, conformability, and hydrophobic properties. The challenge resides in the capacity for these coatings to remain adherent, stable, and cohesive after the in vivo stent expansion, which can generate local plastic deformation of up to 25%. Plasma-coated samples have been prepared by a multistep process on 316L stainless steel substrates, and some coated samples were plastically deformed to mimic a stent expansion. Analyses were then performed by X-ray photoelectron spectroscopy (XPS), X-ray photoelectron emission microscopy (X-PEEM), and time-of-flight secondary ion mass spectrometry (TOF-SIMS) to determine the chemical and physical effects of such a deformation on both the coating and the interfacial region. While XPS analyses always showed a continuous coating with no significant effect of the deformation, TOF-SIMS and near-edge X-ray absorption fine structure (derived from X-PEEM) data indicated the presence of a certain density of porosity and pinholes in all coatings as well as sparse fissures and molecular fragmentation in the deformed ones. The smallness of the area fraction affected by the defects and the subtlety of the chemical changes could only be evidenced through the higher chemical sensitivity of these latter techniques.

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

    PubMed

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

    2015-01-01

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

  7. Development and validation of an analytical method for quantification of arsenic and antimony in liposomes using inductively coupled plasma-optical emission spectrometry.

    PubMed

    Reis, Priscila G; Abreu, Adriana T; Guimarães, Andrea G; Teixeira, Mônica C; de Souza, Jacqueline; Silva-Barcellos, Neila M

    2013-01-01

    Arsenic and antimony compounds are used to treat endemic diseases, such as cancer, leishmaniasis, and schistosomiasis, in spite of their toxicity. Several studies seeking the development and characterization of nanocarrier systems such as liposomes are being carried out with the aim of developing new drug delivery systems and minimizing the toxicity of these drugs. However, the lack of reference methods to quantify these semimetals within a liposomal matrix hinders the QC of these formulations. Therefore, the validation of an analytical method for arsenic and antimony quantification in liposomal matrix by inductively coupled plasma-optical emission spectrometry is presented here. The linearity, specificity, LOD, LOQ, accuracy, and precision were determined according to the International Conference on Harmonization norms and the Brazilian Health Surveillance Agency (Resolution 899). The LOD values were 0.02 and 0.06 mg/L for antimony and arsenic, respectively. The LOQ for both was 3.0 mg/L, with an adequate accuracy within 98.26 and 101.32% for different levels of antimony and 99.98 and 100.36% for arsenic. Precision (CV) was lower than 5.0%. The developed and validated method was shown to be reproducible for quantification of arsenic and antimony in liposome pharmaceutical dosage forms.

  8. Beryllium Limits of Detection and Spectral Interferences in 2 Per Cent Nitric Acid, Digested Air Filter Paper, and GHOSTWIPETM Matrices by Inductively Coupled Plasma Emission Spectrometry

    SciTech Connect

    Jurgensen, A.R.

    2004-02-13

    The Analytical Development Section (ADS) of the Savannah River Technology Center (SRTC) has been requested to perform beryllium (Be) analysis on digested Air Filter Paper and GHOSTWIPE (Trade Mark) samples by Inductively Coupled Plasma Emission Spectrometry (ICP-ES). One of the important figures of merit for this analysis is the detection limit (LOD), the smallest concentration of an element that can be detected with a defined certainty. To meet the site Industrial Hygiene (IH) requirements, an instrument LOD of 0.03 mg per Air Filter Paper (1 hr sample) and 0.2 mg per GHOSTWIPE (Trade Mark) must be demonstrated. Another important analytical parameter is the effect on the Be quantization from potential spectral interfering matrix elements. Any existing spectral overlaps could give false positives or increase the measured Be concentrations in these matrices. The purpose of this study was to document the Analytical Development Sections' s contained ICP-ES performance in these two areas. In addition, other Quality Control recommendations will be discussed.

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

    NASA Astrophysics Data System (ADS)

    Masson, Pierre

    2014-12-01

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

  10. 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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

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

    2013-12-01

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

  12. 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.

    PubMed

    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.

  13. Determination of rare earth elements in geological samples by inductively coupled plasma atomic emission spectrometry with flow injection liquid-liquid extraction.

    PubMed

    Xu, Zhifang; Liu, Congqiang; Zhang, Hongxiang; Ma, Yingjun; Lin, Soulin

    2003-12-01

    A direct sampling with organic solvent extracts for simultaneous multi-element determination implemented with inductively coupled plasma atomic emission spectrometry (ICP-AES) associated with a flow injection liquid-liquid extraction (FI-LLE) sample preconcentration method was studied. The "robustness" of the plasma discharge with tributyl phosphate (TBP) loading was diagnosed by using the Mg II 279.55 nm and Mg I 285.21 nm lines intensity ratio. A FI-LLE preconcentration system for rare earth elements (REEs)-nitrate-TBP was established by using a laboratory-designed phase separator. For these elements, an average sensitivity enhancement factor of 64 was obtained with respect to ICP-AES sampling with aqueous solutions. The precision of the method was characterized by a relative standard deviation (%RSD) of 1.8 - 5.2%. A throughput of 27 samples per hour can be achieved with an organic solvent consumption of less than 200 microl per determination. Good results were obtained for the analysis of standard reference materials.

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

    PubMed

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

    2005-02-01

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

  15. [Interlaboratory study on migration test of antimony and germanium for food-contact polyethylene terephthalate].

    PubMed

    Murakami, Ryo; Mutsuga, Motoh; Abe, Takashi; Abe, Yutaka; Ohsaka, Ikue; Ohno, Haruka; Ohno, Hiroyuki; Ohno, Yuichiro; Ozaki, Asako; Kakihara, Yoshiteru; Kawasaki, Hiromi; Kobayashi, Hisashi; Shibata, Hiroshi; Shirono, Katsuhiro; Sekido, Haruko; Sonobe, Hironori; Takasaka, Noriko; Tajima, Yoshiyasu; Tanaka, Aoi; Tanaka, Hideyuki; Nomura, Chie; Haneishi, Nahoko; Hikida, Akinori; Miura, Toshihiko; Watanabe, Kazunari; Akiyama, Hiroshi

    2015-01-01

    An interlaboratory study was performed to evaluate a migration test method of antimony (Sb) and germanium (Ge), based on the Japanese Food Sanitation Law for food- contact polyethylene terephthalate. Eighteen laboratories participated, and quantified Sb and Ge in three test solutions as blind duplicates using graphite furnace atomic absorption spectrometry (GF-AAS), inductively coupled plasma-optical emission spectrometry (ICP-OES) or induced coupled plasma-mass spectrometry (ICP-MS). Statistical analysis revealed that the trueness, repeatability and reproducibility were 98-107%, 1.7-7.5% and 2.0-18.8% by using GF-AAS and ICP-OES. The performance of these methods is sufficient for testing the specifications. The performance parameters of ICP-MS were 99-106%, 0.7-2.2% and 2.2-10.5%, respectively. ICP-MS is available as an alternative measuring method. However, in some laboratories, the quantitative values of Sb were higher than the addition levels. We found that Sb in working solutions is absorbed on glass vessels. Careful control of concentration in working solutions is required for Sb analysis.

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

    PubMed

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

    2014-11-01

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

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

    SciTech Connect

    Urasa, I.T.

    1991-09-20

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

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

    PubMed

    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. A comparison of benthic foraminiferal Mn / Ca and sedimentary Mn / Al as proxies of relative bottom-water oxygenation in the low-latitude NE Atlantic upwelling system

    NASA Astrophysics Data System (ADS)

    McKay, C. L.; Groeneveld, J.; Filipsson, H. L.; Gallego-Torres, D.; Whitehouse, M. J.; Toyofuku, T.; Romero, O. E.

    2015-09-01

    Trace element incorporation into foraminiferal shells (tests) is governed by physical and chemical conditions of the surrounding marine environment, and therefore foraminiferal geochemistry provides a means of palaeo-oceanographic reconstructions. With the availability of high-spatial-resolution instrumentation with high precision, foraminiferal geochemistry has become a major research topic over recent years. However, reconstructions of past bottom-water oxygenation using foraminiferal tests remain in their infancy. In this study we explore the potential of using Mn / Ca determined by secondary ion mass spectrometry (SIMS) as well as by flow-through inductively coupled plasma optical emission spectroscopy (FT-ICP-OES) in the benthic foraminiferal species Eubuliminella exilis as a proxy for recording changes in bottom-water oxygen conditions in the low-latitude NE Atlantic upwelling system. Furthermore, we compare the SIMS and FT-ICP-OES results with published Mn sediment bulk measurements from the same sediment core. This is the first time that benthic foraminiferal Mn / Ca is directly compared with Mn bulk measurements, which largely agree on the former oxygen conditions. Samples were selected to include different productivity regimes related to Marine Isotope Stage 3 (35-28 ka), the Last Glacial Maximum (28-19 ka), Heinrich Event 1 (18-15.5 ka), Bølling Allerød (15.5-13.5 ka) and the Younger Dryas (13.5-11.5 ka). Foraminiferal Mn / Ca determined by SIMS and FT-ICP-OES is comparable. Mn / Ca was higher during periods with high primary productivity, such as during the Younger Dryas, which indicates low-oxygen conditions. This is further supported by the benthic foraminiferal faunal composition. Our results highlight the proxy potential of Mn / Ca in benthic foraminifera from upwelling systems for reconstructing past variations in oxygen conditions of the sea floor environment as well as the need to use it in combination with other proxy records such as faunal

  20. Biomonitoring of boron: Development and characterization of a simple, reliable and quality controlled biomonitoring method.

    PubMed

    Michalke, Bernhard

    2017-03-01

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

  1. Determination of lithium and transition metals in Li1 Ni1/3 Co1/3 Mn1/3 O2 (NCM) cathode material for lithium-ion batteries by capillary electrophoresis.

    PubMed

    Vortmann-Westhoven, Britta; Lürenbaum, Constantin; Winter, Martin; Nowak, Sascha

    2017-02-01

    In this work, we present a novel electrophoretic method that was developed for the determination of lithium and transition metals in LiNi1/3 Co1/3 Mn1/3 O2 cathode material after microwave digestion. The cations in the digested LiNi1/3 Co1/3 Mn1/3 O2 material were separated by CE and the element content was determined by UV/Vis detection. To characterize the precision of the measurements, the RSDs and concentrations were calculated and compared to those obtained with ICP-optical emission spectrometry (ICP-OES). Furthermore, a certified reference material (BCR 176R-fly ash) was investigated for all techniques. For active material components, the LOD and LOQ were determined. The LODs and LOQs for the metals determined by CE were as follows: lithium (LOD/LOQ): 17.41/62.70 μg/L, cobalt (LOD/LOQ): 348.4/1283 μg/L, manganese (LOD/LOQ): 540.2/2095 μg/L, and nickel (LOD/LOQ): 838.0/2982 μg/L. Recovery rates for lithium were in the range of 95-103%. It could be proven that with the new technique, the results for the determination of the lithium content of active material were comparable with those obtained by ICP-OES and ion chromatography. Furthermore, the recovery rates of the transition metals were determined to be between 96 and 110% by CE and ICP-OES.

  2. Silica-gel Particles Loaded with an Ionic Liquid for Separation of Zr(IV) Prior to Its Determination by ICP-OES

    PubMed Central

    Marwani, Hadi M.; Alsafrani, Amjad E.; Asiri, Abdullah M.; Rahman, Mohammed M.

    2016-01-01

    A new ionic liquid loaded silica gel amine (SG-APTMS-N,N-EPANTf2) was developed, as an adsorptive material, for selective adsorption and determination of zirconium, Zr(IV), without the need for a chelating intermediate. Based on a selectivity study, the SG-APTMS-N,N-EPANTf2 phase showed a perfect selectivity towards Zr(IV) at pH 4 as compared to other metallic ions, including gold [Au(III)], copper [Cu(II)], cobalt [Co(II)], chromium [Cr(III)], lead [Pb(II)], selenium [Se(IV)] and mercury [Hg(II)] ions. The influence of pH, Zr(IV) concentration, contact time and interfering ions on SG-APTMS-N,N-EPANTf2 uptake for Zr(IV) was evaluated. The presence of incorporated donor atoms in newly synthesized SG-APTMS-N,N-EPANTf2 phase played a significant role in enhancing its uptake capacity of Zr(IV) by 78.64% in contrast to silica gel (activated). The equilibrium and kinetic information of Zr(IV) adsorption onto SG-APTMS-N,N-EPANTf2 were best expressed by Langmuir and pseudo second-order kinetic models, respectively. General co-existing cations did not interfere with the extraction and detection of Zr(IV). Finally, the analytical efficiency of the newly developed method was also confirmed by implementing it for the determination of Zr(IV) in several water samples. PMID:27367692

  3. Analysis of human serum and whole blood for mineral content by ICP-MS and ICP-OES: development of a mineralomics method.

    PubMed

    Harrington, James M; Young, Daniel J; Essader, Amal S; Sumner, Susan J; Levine, Keith E

    2014-07-01

    Minerals are inorganic compounds that are essential to the support of a variety of biological functions. Understanding the range and variability of the content of these minerals in biological samples can provide insight into the relationships between mineral content and the health of individuals. In particular, abnormal mineral content may serve as an indicator of illness. The development of robust, reliable analytical methods for the determination of the mineral content of biological samples is essential to developing biological models for understanding the relationship between minerals and illnesses. This paper describes a method for the analysis of the mineral content of small volumes of serum and whole blood samples from healthy individuals. Interday and intraday precision for the mineral content of the blood (250 μL) and serum (250 μL) samples was measured for eight essential minerals--sodium (Na), calcium (Ca), magnesium (Mg), potassium (K), iron (Fe), zinc (Zn), copper (Cu), and selenium (Se)--by plasma spectrometric methods and ranged from 0.635 to 10.1% relative standard deviation (RSD) for serum and 0.348-5.98% for whole blood. A comparison of the determined ranges for ten serum samples and six whole blood samples provided good agreement with literature reference ranges. The results demonstrate that the digestion and analysis methods can be used to reliably measure the content of these minerals and potentially of other minerals.

  4. Determination of mercury, cadmium, lead, zinc, selenium and iron by ICP-OES in mushroom samples from around thermal power plant in Muğla, Turkey.

    PubMed

    Kula, Ibrahim; Solak, M Halil; Uğurlu, Mehmet; Işıloğlu, Mustafa; Arslan, Yasin

    2011-09-01

    Scleroderma verrucosum, Stropharia coronilla, Lactarius deterrimus, Chroogomphus rutilus, Russula delica, Laccaria laccata, Clitocybe odora var. alba, Lyophyllum decastes, Coprinus comatus, Helvella leucomelaena, Melanoleuca cognata, Melanoleuca cognata, Paxina acetabulum, Clitocybe vermicularis, Sarcosphaera crassa, Rhizopogon roseolu and Thelephora caryophyllea were collected from different localities in Muğla-Yatağan region of Turkey. Their trace metals concentrations were determined by ICPOES after microwave digestion. The results were 0.37 ± 0.01-5.28 ± 0.21 for cadmium, 467 ± 19-3,280 ± 131 for iron, 0.69 ± 0.03-9.15 ± 0.37 for lead, 18.70 ± 0.75-67.10 ± 2.68 for selenium, 75 ± 3-213 ± 8 for zinc and 0.15 ± 0.01-0.55 ± 0.01 for mercury (as μg/g). The detection limits for ICPOES were found as 0.25 for Cadmium, 0.2 for iron, 0.1 for lead, 0.5 for selenium, 0.2 for zinc and 0.03 for mercury (as mg L(-1)). The Relatively Standard Deviations (R.S.D.) were found below 4.0%. The accuracy of procedure was confirmed by certified reference material.

  5. Cadmium uptake and translocation in tumbleweed (Salsola kali), a potential Cd-hyperaccumulator desert plant species: ICP/OES and XAS studies.

    PubMed

    de la Rosa, Guadalupe; Peralta-Videa, Jose R; Montes, Milka; Parsons, Jason G; Cano-Aguilera, Irene; Gardea-Torresdey, Jorge L

    2004-06-01

    Cadmium is a heavy metal, which, even at low concentrations, can be highly toxic to the growth and development of both plants and animals. Plant species vary extensively in their tolerance to excess cadmium in a growth medium and very few cadmium-tolerant species have been identified. In this study, tumbleweed plants (Salsola kali) grown in an agar-based medium with 20 mgl(-1) of Cd(II) did not show phytotoxicity, and their roots had the most biomass (4.5 mg) (P < 0.05) compared to the control plants (2.7 mg) as well as other treated plants. These plants accumulated 2696, 2075, and 2016 mg Cd kg(-1) of dry roots, stems, and leaves, respectively. The results suggest that there is no restricted cadmium movement in tumbleweed plants. In addition, the amount of Cd found in the dry leaf tissue suggests that tumbleweed could be considered as potential cadmium hyperaccumulating species. X-ray absorption spectroscopy studies demonstrated that in roots, cadmium was bound to oxygen while in stems and leaves, the metal was attached to oxygen and sulfur groups. This might imply that some small organic acids are responsible for Cd transport from roots to stems and leaves. In addition, it might be possible that the plant synthesizes phytochelatins in the stems, later coordinating the absorbed cadmium for transport and storage in cell structures. Thus, it is possible that in the leaves, Cd either exists as a Cd-phytochelatin complex or bound to cell wall structures. Current studies are being performed in order to elucidate the proposed hypothesis.

  6. Analysis of Human Serum and Whole Blood for Mineral Content by ICP-MS and ICP-OES: Development of a Mineralomics Method

    PubMed Central

    Harrington, James M.; Young, Daniel J.; Essader, Amal S.; Sumner, Susan J.; Levine, Keith E.

    2014-01-01

    Minerals are inorganic compounds that are essential to the support of a variety of biological functions. Understanding the range and variability of the content of these minerals in biological samples can provide insight into the relationships between mineral content and the health of individuals. In particular, abnormal mineral content may serve as an indicator of illness. The development of robust, reliable analytical methods for the determination of the mineral content of biological samples is essential to developing biological models for understanding the relationship between minerals and illnesses. This manuscript describes a method for the analysis of the mineral content of small volumes of serum and whole blood samples from healthy individuals. Interday and intraday precision for the mineral content of the blood (250 μl) and serum (250 μl) samples was measured for eight essential minerals, sodium (Na), calcium (Ca), magnesium (Mg), potassium (K), iron (Fe), zinc (Zn), copper (Cu), and selenium (Se) by plasma spectrometric methods and ranged from 0.635 – 10.1% relative standard deviation (RSD) for serum and 0.348 – 5.98% for whole blood. A comparison of the determined ranges for ten serum samples and six whole blood samples provided good agreement with literature reference ranges. The results demonstrate that the digestion and analysis methods can be used to reliably measure the content of these minerals, and potentially to add other minerals. PMID:24917052

  7. The Levels of Trace Elements in Honey and Molasses Samples That Were Determined by ICP-OES After Microwave Digestion Method.

    PubMed

    Altundag, Huseyin; Bina, Emel; Altıntıg, Esra

    2016-04-01

    The aim of this study is determining the amount of Al, Cu, Fe, Mn, Ni, Pb and Zn in samples of molasses and honey which were gathered from the Sakarya and Istanbul regions. In this study, trace elements in 8 honey and 20 molasses samples with different botanic features were evaluated. The sample preparation phase was performed via wet decomposition method and microwave digestion system. The accuracy of the method was checked by the standard reference material; tea leaves (INCY-TL-1) and NIST-SRM 1515-apple. The concentrations of essential trace elements (TEs) were observed in the range of 1.61 ± 0.01-287.03 ± 1.07; 0.21 ± 0.01-11.04 ± 0.12; 0.35 ± 0.03-21.71 ± 0.02 and 1.19 ± 0.01-60.90 ± 1.09 μg g(-1) for iron, copper, manganese and zinc ions, respectively, while the toxic element contents were observed in the range of 0.82 ± 0.17-3.06 ± 0.03; 0.04 ± 0.05-1.96 ± 0.03 and 0.62 ± 0.01-120.52 ± 0.10 μg g(-1) for lead, nickel and aluminum ions, respectively. The concentrations of basic TEs iron, copper, manganese and zinc were determined as 3.87 ± 0.04-16.76 ± 0.06; 0.45 ± 0.03-2.15 ± 0.01; 0.13 ± 0.01-15.02 ± 0.14 and 0.80 ± 0.09-12.03 ± 0.19 for honey samples. Also, toxic metal, lead, nickel and aluminum values in the honey samples were determined as 1.21 ± 0.12-2.46 ± 0.21; 0.28 ± 0.14-0.88 ± 0.43 and 2.11 ± 0.02-8.04 ± 0.08. A comparison between gathered data and literature values has performed and it is determined that such findings are suitable with the literature.

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

    PubMed

    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.

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

    PubMed

    Masuck, Ines; Hutzler, Christoph; Luch, Andreas

    2010-04-30

    In the revised European toy safety directive 2009/48/EC the application of fragrance allergens in children's toys is restricted. The focus of the present work lies on the instrumental analytics of 13 banned fragrance allergens, as well as on 11 fragrance allergens that require declaration when concentrations surpass 100 microg per gram material. Applying a mixture of ethyl acetate and toluene solid/liquid extraction was performed prior to quantitative analysis of mass contents of fragrances in scented toys. In addition, an easy-to-perform method for the determination of emitted fragrances at 23 degrees C (handling conditions) or at 40 degrees C (worst case scenario) has been worked out to allow for the evaluation of potential risks originating from inhalation of these compounds during handling of or playing with toys. For this purpose a headspace solid-phase microextraction (HS-SPME) technique was developed and coupled to subsequent gas chromatography-mass spectrometry (GC-MS) analysis. Fragrance allergens were adsorbed (extracted) from the gas phase onto an 85 microm polyacrylate fiber while incubating pieces of the scented toys in sealed headspace vials at 23 degrees C and 40 degrees C. Quantification of compounds was performed via external calibration. The newly developed headspace method was subsequently applied to five perfumed toys. As expected, the emission of fragrance allergens from scented toys depends on the temperature and on the content of fragrance allergens present in those samples. In particular at conditions mimicking worst case (40 degrees C), fragrance allergens in toys may pose a risk to children since considerable amounts of compound might be absorbed by lung tissue via breathing of contaminated air. 2010 Elsevier B.V. All rights reserved.

  10. 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.

    PubMed

    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.

  11. Sensitive Determination of Cd in Small-Volume Samples by Miniaturized Liquid Drop Anode Atmospheric Pressure Glow Discharge Optical Emission Spectrometry.

    PubMed

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

    2017-06-06

    A novel liquid drop anode (LDA) direct current atmospheric pressure glow discharge (dc-APGD) system was applied for direct determination of Cd in liquid microsamples (50 μL) by optical emission spectrometry (OES). The microdischarge was generated in open-to-air atmosphere between a solid pin type tungsten cathode and a liquid drop placed on a graphite disk anode. The arrangement of the graphite disk placed on a PTFE chip platform as well as the solid pin type cathode was simple and robust. The limit of detection (LOD) of Cd for the developed LDA-APGD-OES method was 0.20-0.40 μg L(-1), while precision (as the relative standard deviation for the repeated measurements) was within 2-5%. By using the liquid drop of 50 μL, the linearity range of 1-1000 μg L(-1) was achieved. The effect of addition of the low-molecular weight (LMW) organic compounds, easily ionized elements (EIEs), i.e., Ca, K, Mg, and Na, as well as the foreign ions (Al, Cu, Fe, Mn, Zn) to the solution on the in situ atomization and excitation processes occurred during operation of the LDA-APGD system, and the response of Cd was studied. Validation of the proposed method was demonstrated by analysis of Lobster hepatopancreas (TORT-2), pig kidney (ERM-BB186), and groundwater (ERM-CA615) certified reference materials (CRMs) and recoveries of Cd from water samples spiked with 25 μg L(-1) of Cd. Very good agreement between the found and certified values of Cd in the CRMs (the recoveries were within the range of 96.3-99.6%) indicated trueness of the method and its reliability for determination of traces of Cd. In the case of the spiked water samples, the recoveries obtained were in the range from 95.2 to 99.5%.

  12. Optimized microwave-assisted decomposition method for multi-element analysis of glass standard reference material and ancient glass specimens by inductively coupled plasma atomic emission spectrometry.

    PubMed

    Zachariadis, G; Dimitrakoudi, E; Anthemidis, A; Stratis, J

    2006-02-28

    A novel microwave-assisted wet-acid decomposition method for the multi-element analysis of glass samples using inductively coupled plasma atomic emission spectrometry (ICP-AES) was developed and optimized. The SRM 621 standard reference glass material was used for this purpose, because it has similar composition with either archaeological glass specimens or common modern glasses. For the main constituents of SRM 621 (Ca, Na, Al, Fe, Mg, Ba and Ti), quality control data are given for all the examined procedures. The chemical and instrumental parameters of the method were thoroughly optimized. Thirteen acid mixtures of hydrochloric, nitric, and hydrofluoric acids in relation to two different microwave programs were examined in order to establish the most efficient protocol for the determination of metals in glass matrix. For both microwave programs, an intermediate step was employed with addition of H(3)BO(3) in order to compensate the effect of HF, which was used in all protocols. The suitability of the investigated protocols was evaluated for major (Ca, Na, Al), and minor (Fe, Mg, Ba, Ti, Mn, Cu, Sb, Co, Pb) glass constituents. The analytes were determined using multi-element matrix matched standard solutions. The analytical data matrix was processed chemometrically in order to evaluate the examined protocols in terms of their accuracy, precision and sensitivity, and eventually select the most efficient method for ancient glass. ICP-AES parameters such as spectral line, RF power and sample flow rate were optimized using the proposed protocol. Finally, the optimum method was successfully applied to the analysis of a number of ancient glass fragments.

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

    PubMed

    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.

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

    PubMed

    Thiex, Nancy J

    2016-07-01

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

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

    NASA Astrophysics Data System (ADS)

    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.

  16. Evaluation and application of argon and helium microstrip plasma for the determination of mercury by the cold vapor technique and optical emission spectrometry.

    PubMed

    Jiménez Zapata, Israel; Pohl, Pawel; Bings, Nicolas H; Broekaert, José A C

    2007-08-01

    The suitability of a 2.45-GHz atmospheric pressure, low-power microwave microstrip plasma (MSP) operated with Ar and He for the determination of Hg by continuous-flow cold vapor (CV) generation, using SnCl2/HCl as the reducing agent, and optical emission spectrometry (OES) using a small CCD spectrometer was studied. The areas of stability for a discharge in the Ar and in the He MSP enclosed in a cylindrical channel in a quartz wafer were investigated. The excitation temperatures as measured for discharge gas atoms (Ar I, He I), and the electron number densities at 35-40 W and 15-400 mL min(-1) were found to be at the order of 3,200-5,500 K and 0.8x10(14)-1.6x10(14) cm(-3), respectively. The relative intensity of the Hg I 253.6-nm line and the signal-to-background ratio as a function of the forward power (35-40 W) as well as of the flow rate of the working gas (15-400 mL min(-1)) were evaluated and discussed. For the selected measurement conditions, the Ar MSP was established to have the lower detection limit for Hg (0.6 ng mL(-1)) compared with the He MSP. The linearity range is up to 300 ng mL(-1) and the precision is on the order of 1-3%. With the optimized CV Ar MSP-OES method a determination of Hg in spiked domestic and natural waters at concentration levels of 20-100 microg L(-1) and an accuracy of 1-4% could be performed. In an NIST domestic sludge standard reference material, Hg (3.64 microg g(-1)) could be determined with a relative standard deviation of 4% and an agreement better than 4%.

  17. (10)B/(11)B isotopic ratio and atomic composition of boron carbide: Determination by proton induced γ-ray emission and proton elastic backscattering spectrometry.

    PubMed

    Sunitha, Y; Kumar, Sanjiv

    2017-10-01

    The (10)B/(11)B isotopic ratio and the atomic composition of boron carbide, an important non-metallic ceramic, have been determined non-destructively by the particle induced γ-ray emission (PIGE) and elastic backscattering spectrometry (EBS) techniques with proton beams. The analysis has been performed on powder as well as sintered ceramics containing boron in natural or (10)B enriched composition. The PIGE technique, performed at a 4.0-4.2MeV proton energy, utilizes the (10)B(p,αγ)(7)Be, (10)B(p,p'γ)(10)B and (11)B(p, p'γ)(11)B nuclear reactions for (a) the isotopic analysis of boron and (b) the determination of total boron, and the (13)C(p,p'γ)(13)C nuclear reaction for the determination of carbon. The irradiation conditions were optimized by determining the thick targets yields of prompt γ-rays, characteristic of these reactions, in the 3.0-4.2MeV proton energy range. The quantitative analysis was performed by comparison with standards taking into account the attenuation of γ-rays in the specimens. The uncertainty in the determination of the (10)B/(11)B isotopic ratio and the B/C atomic ratio is about 2% and about 5% respectively. The analysis by EBS, on the other hand, involves the (10)B(p,p)(10)B, (11)B(p,p)(11)B and (12)C(p,p)(12)C elastic scatterings at the 2.0MeV proton energy. This method too yields satisfactory results. Between the two, PIGE is the method of choice for bulk analysis while EBS is useful in discerning compositional variations in surface regions. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

    PubMed

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

    2016-03-01

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

  19. Extraction of trace amounts of mercury with sodium dodecyle sulphate-coated magnetite nanoparticles and its determination by flow injection inductively coupled plasma-optical emission spectrometry.

    PubMed

    Faraji, Mohammad; Yamini, Yadollah; Rezaee, Mohammad

    2010-05-15

    A new method for solid-phase extraction and preconcentration of trace amounts Hg(II) from environmental samples was developed by using sodium dodecyle sulphate-coated magnetite nanoparticles (SDS-coated Fe(3)O(4) NPs) as a new extractant. The procedure is based on the adsorption of the analyte, as mercury-Michler's thioketone [Hg(2)(TMK)(4)](2+) complex on the negatively charged surface of the SDS-coated Fe(3)O(4) NPs and then elution of the preconcentrated mercury from the surface of the SDS-coated Fe(3)O(4) NPs prior to its determination by flow injection inductively coupled plasma-optical emission spectrometry. The effects of pH, TMK concentration, SDS and Fe(3)O(4) NPs amounts, eluent type, sample volume and interfering ions on the recovery of the analyte were investigated. Under optimized conditions, the calibration curve was linear in the range of 0.2-100ngmL(-1) with r(2)=0.9994 (n=8). The limit of detection for Hg(II) determination was 0.04ngmL(-1). Also, relative standard deviation (R.S.D.) for the determination of 2 and 50ngmL(-1) of Hg(II) was 5.2 and 4.7% (n=6), respectively. Due to the quantitative extraction of Hg(II) from 1000mL of the sample solution an enhancement factor as large as 1230-fold can be obtained. The proposed method has been validated using a certified reference materials, and also the method has been applied successfully for the determination of Hg(II) in aqueous samples.

  20. Rapid Analysis of Ash Composition Using Laser-Induced Breakdown Spectroscopy (LIBS)

    SciTech Connect

    Tyler L. Westover

    2013-01-01

    Inorganic compounds are known to be problematic in the thermochemical conversion of biomass to syngas and ultimately hydrocarbon fuels. The elements Si, K, Ca, Na, S, P, Cl, Mg, Fe, and Al are particularly problematic and are known to influence reaction pathways, contribute to fouling and corrosion, poison catalysts, and impact waste streams. Substantial quantities of inorganic species can be entrained in the bark of trees during harvest operations. Herbaceous feedstocks often have even greater quantities of inorganic constituents, which can account for as much as one-fifth of the total dry matter. Current methodologies to measure the concentrations of these elements, such as inductively coupled plasma-optical emission spectrometry/mass spectrometry (ICP-OES/MS) are expensive in time and reagents. This study demonstrates that a new methodology employing laser-induced breakdown spectroscopy (LIBS) can rapidly and accurately analyze the inorganic constituents in a wide range of biomass materials, including both woody and herbaceous examples. This technique requires little or no sample preparation, does not consume any reagents, and the analytical data is available immediately. In addition to comparing LIBS data with the results from ICP-OES methods, this work also includes discussions of sample preparation techniques, calibration curves for interpreting LIBS spectra, minimum detection limits, and the use of internal standards and standard reference materials.

  1. Rapid methodology to screen flame retardants in upholstered furniture for compliance with new California labeling law (SB 1019).

    PubMed

    Petreas, Myrto; Gill, Ranjit; Takaku-Pugh, Sayaka; Lytle, Eric; Parry, Emily; Wang, Miaomiao; Quinn, John; Park, June-Soo

    2016-06-01

    In response to concerns regarding the widespread use of flame retardants, the California Legislature passed a law (SB1019) requiring labels on furniture products to indicate whether they do or do not contain flame retardants. To support the enforcement of the new law, our laboratory developed a step-wise, screening approach to test for brominated (BFR) and phosphorus-based flame retardants (OPFRs) in several types of furniture components (foam, fabric, batting, plumage, etc.). We used X-Ray Fluorescence (XRF) to screen for the presence of Br (and other elements) and Inductively Coupled Plasma - Optical Emission Spectrometry (ICP-OES) to identify and measure the concentration of P (and other elements). The same samples were also extracted by dichloromethane using sonication and analyzed by a single injection into a Gas Chromatograph - Tandem Mass Spectrometer to obtain concentrations of specific BFRs and OPFRs. Our approach showed excellent screening potential for Br and Sb by XRF and for P by ICP-OES, with both tests having predictive values of a negative equal to 1. To explore and screen for flame retardants in products not included in our current list of target chemicals, we used Liquid Chromatography/Time-of-Flight Mass Spectrometry operated with electrospray ionization, to identify additional flame retardants to be incorporated in quantitative methods. We are making all our methodologies public to facilitate simple and low cost methods that can help manufacturers and suppliers have their products tested and correctly labeled, ultimately benefitting the consumer.

  2. Assessment of the Effects Exerted by Acid and Alkaline Solutions on Bone: Is Chemistry the Answer?

    PubMed

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

    2017-09-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-05-01

    Volcanoes are well known as an impressive large natural source of trace elements into the troposphere. Among others, Etna (Italy) and Nyiragongo (D.R. Congo), two noteworthy emitters on Earth, are two stratovolcanoes located in different geological settings, both characterized by persistent passive degassing from their summit craters. Here, we present some results on trace element composition in volcanic plume emissions, atmospheric bulk deposition (rainwater) and their uptake of the surrounding vegetation, with the aim to compare and identify differences and similarities between this these two volcanoes. Volcanic emissions were sampled by using active filter-pack for acid gases (sulfur and halogens) and specific teflon filters for particulates (major and trace elements). The impact of the volcanogenic deposition in the surrounding of the crater rims was investigated by using different sampling techniques: bulk rain collectors gauges were used to collect atmospheric bulk deposition, and biomonitoring technique was carried out to collect gases and particulates by using endemic plant species. Concentrations of major and trace elements of volcanic plume emissions (gases and particulates) were obtained by elution and microwave digestion of the collected filters: sulfur and halogens were determined by ion chromatography and ICP-MS, and untreated filters for particulate were acid digested and analysed by ICP-OES and ICP-MS. Rain water and plant samples were also analysed for major and trace elements by using ICP-OES and ICP-MS. In total 55 elements were determined. The estimates of the trace element fluxes confirm that Etna and Nyiragongo are large sources of metals to the atmosphere, especially considering their persistent state of passive degassing. In general, chemical composition of the volcanic aerosol particles of both volcanoes is characterized by two main components: one is related to the silicic component produced by magma bursting and fragmentation, enriching

  4. Evaluation of laser induced breakdown spectroscopy for multielemental determination in soils under sewage sludge application.

    PubMed

    Ferreira, Edilene Cristina; Milori, Débora Marcondes Bastos Pereira; Ferreira, Ednaldo José; Dos Santos, Larissa Macedo; Martin-Neto, Ladislau; Nogueira, Ana Rita de Araújo

    2011-07-15

    Laser induced breakdown spectroscopy (LIBS) is an atomic emission spectroscopy technique for simple, direct and clean analysis, with great application potential in environmental sustainability studies. In a single LIBS spectrum it is possible to obtain qualitative information on the sample composition. However, quantitative analysis requires a reliable model for analytical calibration. Multilayer perceptron (MLP), an artificial neural network, is a multivariate technique that is capable of learning to recognize features from examples. Therefore MLP can be used as a calibration model for analytical determinations. Accordingly, the present study proposes to evaluate the traditional linear fit and MLP models for LIBS calibration, in order to attain a quantitative multielemental method for contaminant determination in soil under sewage sludge application. Two sets of samples, both composed of two kinds of soils were used for calibration and validation, respectively. The analyte concentrations in these samples, used as reference, were determined by a reference analytical method using inductively coupled plasma optical emission spectrometry (ICP OES). The LIBS-MLP was compared to a LIBS-linear fit method. The values determined by LIBS-MLP showed lower prediction errors, correlation above 98% with values determined by ICP OES, higher accuracy and precision, lower limits of detection and great application potential in the analysis of different kinds of soils. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. 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)

    USGS Publications Warehouse

    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.

  6. A combined accelerator mass spectrometry-positron emission tomography human microdose study with 14C- and 11C-labelled verapamil

    PubMed Central

    Wagner, Claudia C; Simpson, Marie; Zeitlinger, Markus; Bauer, Martin; Karch, Rudolf; Abrahim, Aiman; Feurstein, Thomas; Schütz, Matthias; Kletter, Kurt; Müller, Markus; Lappin, Graham; Langer, Oliver

    2013-01-01

    Background and Objective In microdose studies, the pharmacokinetic (PK) profile of a drug in blood after administration of a dose up to 100 μg is measured with sensitive analytical techniques, such as accelerator mass spectrometry (AMS). As most drugs exert their effect in tissue rather than blood, methodology is needed for extending PK analysis to different tissue compartments. In the present study, we combined, for the first time, AMS analysis with positron emission tomography (PET) in order to determine the PK profile of the model drug verapamil in plasma and brain of humans. In order to assess PK dose-linearity of verapamil, data were acquired and compared after administration of an intravenous (iv) microdose and an iv microdose dosed concomitantly with an oral therapeutic dose. Methods Six healthy male volunteers received an iv microdose (0.05 mg) (period 1) and an iv microdose dosed concomitantly with an oral therapeutic dose (80 mg) of verapamil (period 2) in a randomized, cross-over, two-period study design. The iv dose was a mixture of (R/S)-[14C]verapamil and (R)-[11C]verapamil and the oral dose was unlabelled racemic verapamil. Brain distribution of radioactivity was measured with PET whereas plasma PK of (R)- and (S)-verapamil was determined with AMS. PET data were analyzed by kinetic modeling to estimate the rate constants for transfer of radioactivity across the blood-brain barrier. Results Most PK parameters of (R)- and (S)-verapamil as well as parameters describing exchange of radioactivity between plasma and brain (K1=0.030±0.003 and 0.031±0.005 mL·mL−1·min−1 and k2=0.099±0.006 and 0.095±0.008 min−1 for period 1 and 2, respectively) were not statistically different between the two periods although there was a trend for non-linear kinetics for the (R)-enantiomer. On the other hand, all PK parameters (except for t1/2) differed significantly between the (R)- and (S)-enantiomers for both periods. Cmax, AUC(0-24) and AUC(0-inf) were higher

  7. Investigation on the heavy-metal content of zinc-air button cells.

    PubMed

    Richter, Andrea; Richter, Silke; Recknagel, Sebastian

    2008-01-01

    Within the framework of a German government project (initiated by the Federal Environment Agency) to check the compliance of commercially available batteries with the German Battery Ordinance concerning their heavy metal contents, 18 different types of commercially available zinc-air button cells were analysed for their cadmium, lead and mercury contents. After microwave assisted dissolution with aqua regia, Cd and Pb were determined using inductively coupled plasma mass spectrometry (ICP-MS), and Hg was determined using inductively coupled plasma optical emission spectrometry (ICP OES) and atomic absorption spectrometry. Cd contents were found to be much lower than the permitted limits; Pb contents were also found to be below the limits. Hg contents were found to be near the limits, and in one case the limit was exceeded.

  8. Assessment of the Bioaccessibility of Micronized Copper Wood on Simulated Stomach Fluid

    EPA Pesticide Factsheets

    The widespread use of copper-treated lumber has increased the potential for human exposure. Moreover, there is a lack of information on the fate and behavior of copper-treated wood particles following oral ingestion. In this study, the in vitro bioaccessibility of copper from copper-treated wood dust in simulated stomach fluid and DI water was determined. Three copper-treated wood products, liquid alkali copper quaternary and two micronized copper quarternary from different manufacturers, were incubated in the extraction media then fractionated by centrifugation and filtration through 0.45 ?m and 10 kDa filters. The copper concentrations from isolated fractions were measured using Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). Total amounts of copper from each wood product were also determined using microwave-assisted acid digestion of dried wood samples and quantification using ICP-OES. The percent in vitro bioaccessible copper was between 83 and 90 % for all treated wood types. However, the percent of copper released in DI water was between 14 and 25 % for all wood products. This data suggests that copper is highly bioaccessible at low pH and may pose a potential human exposure risk upon ingestion. This dataset is associated with the following publication:Santiago-Rodrigues, L., J.L. Griggs, K. Bradham , C. Nelson , T. Luxton , W. Platten , and K. Rogers. Assessment of the bioaccessibility of micronized copper wood in synthetic stomach flu

  9. Fe3O4/salicylic acid nanoparticles versatility in magnetic mediated vascular nanoblockage

    NASA Astrophysics Data System (ADS)

    Mîndrilă, I.; Buteică, S. A.; Mihaiescu, D. E.; Badea, G.; Fudulu, A.; Mărgăritescu, D. N.

    2016-01-01

    An aqueous dispersion of Fe3O4/salicylic acid magnetic nanoparticles (SaMNPs) was synthesized by a modified Massart method, characterized by Inductively Coupled Plasma-Optic Emission Spectrometry (ICP-OES), High-Resolution Transmission Electron Microscopy (HRTEM) and Dynamic Light Scattering (DLS) methods, and tested on the chick chorioallantoic membrane (CAM) model to evaluate biocompatibility, biodistribution, intravascular time persistence, and ability to be magnetically target driven in order to block the blood supply into a tumor xenograft. ICP-OES, DLS, and HRTEM SaMNPs sample analyses showed a 0.356 mg/mL Fe concentration, a good stability in water (average Zeta potential of 39.3 mV), a hydrodynamic diameter around 52 nm and a core diameter in the 7-15 nm range for the Fe3O4 nanoparticles. In vivo CAM assay showed that SaMNPs were biocompatible with the chick embryo, were fixed almost completely by the liver, had no embolic potential, and a threshold-dose-dependent intravascular magnetic targeting time. Study on the CAM tumor model showed that SaMNPs could be used for long-term magnetically mediated nanoblocking of the capillary networks and 70-µm smaller arterioles.

  10. Quantitative analysis of oxide materials by laser-induced breakdown spectroscopy with argon as an internal standard

    NASA Astrophysics Data System (ADS)

    Lasheras, R. J.; Bello-Gálvez, C.; Anzano, J. M.

    2013-04-01

    Laser-induced breakdown spectroscopy (LIBS) is demonstrated as a quantitative technique for geochemical analysis. This study demonstrates the applicability of LIBS to multielemental analysis of minerals using argon as an internal standard. Laser-induced breakdown spectroscopy has been applied to measure elements in oxide form. In the present study, the contents of several oxides, such as Fe2O3, CaO and MgO, in geological samples from the Tierga Mine (Zaragoza, Spain) were analyzed by LIBS. An argon environment was used to eliminate interference from air at atmospheric pressure. Furthermore, argon was used as an internal standard. The result was enhanced signal and enhanced linearity of the calibration curves. The Fe2O3, CaO and MgO concentrations determined by LIBS were compared with the results obtained using another analytical technique, inductively coupled plasma optical emission spectrometry (ICP-OES). The concentrations found using LIBS were in good agreement with the values obtained by ICP-OES.

  11. Effect of acid concentration on closed-vessel microwave-assisted digestion of plant materials

    NASA Astrophysics Data System (ADS)

    Araújo, Geórgia C. L.; Gonzalez, Mário H.; Ferreira, Antônio G.; Nogueira, Ana Rita A.; Nóbrega, Joaquim A.

    2002-12-01

    The efficiency of microwave-assisted acid digestion of plants using different concentrations of nitric acid (2.0, 3.0, 5.0, 7.0 and 14 mol l -1) with hydrogen peroxide (30% v/v) was evaluated by measuring the residual carbon content (RCC) using inductively coupled plasma optical emission spectrometry (ICP-OES) with axial viewing. Certified reference materials were used for evaluating the accuracy attained when 2 mol l -1 HNO 3 was employed for digestion. Under all experimental conditions RCC values were always lower than 13% w/v, and even the highest concentration did not cause any interference with element recovery. It seems that the high pressure reached for closed-vessel operation improved the oxidative action of nitric acid due to consequent temperature increase, even when this reagent was not used at high concentrations. According to acid-base titration data, residual acid in the digestates varied from 1.2 to 4.0 mol l -1, depending on the acid concentration initially added. It can be concluded that for plant materials, microwave-assisted acid digestion can be carried out under mild conditions, which implies that digestates do not need extensive dilution before introduction by pneumatic nebulization to ICP-OES. An additional advantage is the lower amount of residue generated when working with less concentrated acid solutions.

  12. Preparation and characterization of modified starch granules with high hydrophobicity and flowability.

    PubMed

    Chang, Fengdan; He, Xiaowei; Fu, Xiong; Huang, Qiang; Qiu, Yaofang

    2014-01-01

    Normal cornstarch (NC) was chemically modified by octenylsuccinic anhydride (OSA) and Al2(SO4)3. The effects of the concentration of NaOH, OSA, and Al2(SO4)3 on the properties of modified starch(OS-starch-Al) were investigated. The OS-starch-Al was characterized by repose angle, activation index, inductively coupled plasma-atomic emission spectrometry (ICP-OES), light microscopy, SEM, FT-IR, and (27)Al NMR. The results showed that pH 4 was the optimum condition for Al(3+) cross-linking with OS-starch and for obtaining high flowability and hydrophobicity. When the concentration of OSA and Al2(SO4)3 was 2%, the OS-starch-Al was characterized by high flowability. A concentration of 4% OSA and Al2(SO4)3 yielded the highest activation index. The moisture content affected the flowability of native NC, but had a minor effect on OS-starch-Al. SEM and polarized microscopy revealed that the modification had slight effects on the crystalline structure and morphology of NC. During the preparation, some dust particles functioning as flow additives were produced on the surface of starch granules. The results of FT-IR, ICP-OES, and (27)Al NMR confirmed the formation of ester group and the cross-link with Al(3+). Copyright © 2013 Elsevier Ltd. All rights reserved.

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

    EPA Science Inventory

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

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

    USDA-ARS?s Scientific Manuscript database

    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...

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

    EPA Science Inventory

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

  16. On-line detection of metal pollutant spikes in MSW incinerator flue gases prior to clean-up

    SciTech Connect

    Poole, D. Sharifi, V.; Swithenbank, J.; Argent, B.; Ardelt, D.

    2007-07-01

    SUWIC's unique mobile metals emissions monitoring laboratory has been used to measure metal pollutant spikes in the flue gas from a municipal solid waste incinerator, prior to gas clean-up. The laboratory has a heated sampling probe that extends into the plant, allowing the simultaneous on-line measurement of the concentrations of more than 30 metals by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). As little is known about temporal variation in metal concentrations, this capability is seen as a major advance. The graphs of continuous measurements show that the elemental loading is far from uniform, and that concentrations fluctuate far more than may have been conventionally expected. There are occasional significant spikes in the emission profiles for cadmium and mercury, which are believed to be due to specific items in the waste feed material. Continuous monitoring measurements are of significant value for those seeking to model metal behaviour in combustion and in pollution control devices.

  17. In vitro study of thimerosal reactions in human whole blood and plasma surrogate samples.

    PubMed

    Trümpler, Stefan; Meermann, Björn; Nowak, Sascha; Buscher, Wolfgang; Karst, Uwe; Sperling, Michael

    2014-04-01

    Because of its bactericidal and fungicidal properties, thimerosal is used as a preservative in drugs and vaccines and is thus deliberately injected into the human body. In aqueous environment, it decomposes into thiosalicylic acid and the ethylmercury cation. This organomercury fragment is a potent neurotoxin and is suspected to have similar toxicity and bioavailability like the methylmercury cation. In this work, human whole blood and physiological simulation solutions were incubated with thimerosal to investigate its behaviour and binding partners in the blood stream. Inductively coupled plasma with optical emission spectrometry (ICP-OES) was used for total mercury determination in different blood fractions, while liquid chromatography (LC) coupled to electrospray ionisation time-of-flight (ESI-TOF) and inductively coupled plasma-mass spectrometry (ICP-MS) provided information on the individual mercury species in plasma surrogate samples. Analogous behaviour of methylmercury and ethylmercury species in human blood was shown and an ethylmercury-glutathione adduct was identified.

  18. Clean Chemistry for Elemental Impurities Analysis of Pharmaceuticals in Compliance with USP 232.

    PubMed

    Jin, Chunguang

    2016-10-01

    United States Pharmacopeia updated its 100 years old metal analysis method with inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES). These sensitive instruments require that sample preparation be at least as sophisticated as the instrumentation used in the analysis. Sample contamination during sample preparation has to be controlled to an acceptable level given the low detection limit of these instruments and the ubiquitous presence of elements. This article focused on sample contamination during sample preparation. Contaminations from environment, reagents, and lab apparatus were investigated for their impact on trace element analysis. Advice on clean lab practice was offered to the pharmaceutical industry in regard to contamination control in elemental analysis labs at a time when the industry is preparing for compliance with elemental impurities in drug products.

  19. Multielemental fingerprinting as a tool for authentication of organic wheat, barley, faba bean, and potato.

    PubMed

    Laursen, Kristian H; Schjoerring, Jan K; Olesen, Jørgen E; Askegaard, Margrethe; Halekoh, Ulrich; Husted, Søren

    2011-05-11

    The multielemental composition of organic and conventional winter wheat, spring barley, faba bean, and potato was analyzed with inductively coupled plasma-optical emission spectrometry (ICP-OES) and -mass spectrometry (ICP-MS). The crops were cultivated in two years at three geographically different field locations, each accommodating one conventional and two organic cropping systems. The conventional system produced the highest harvest yields for all crops except the nitrogen-fixing faba bean, whereas the dry matter content of each crop was similar across systems. No systematic differences between organic and conventional crops were found in the content of essential plant nutrients when statistically analyzed individually. However, chemometric analysis of multielemental fingerprints comprising up to 14 elements allowed discrimination. The discrimination power was further enhanced by analysis of up to 25 elements derived from semiquantitative ICP-MS. It is concluded that multielemental fingerprinting with semiquantitative ICP-MS and chemometrics has the potential to enable authentication of organic crops.

  20. Standardisation of elemental analytical techniques applied to provenance studies of archaeological ceramics: an inter laboratory calibration study.

    PubMed

    Hein, A; Tsolakidou, A; Iliopoulos, I; Mommsen, H; Buxeda i Garrigós, J; Montana, G; Kilikoglou, V

    2002-04-01

    Chemical analysis is a well-established procedure for the provenancing of archaeological ceramics. Various analytical techniques are routinely used and large amounts of data have been accumulated so far in data banks. However, in order to exchange results obtained by different laboratories, the respective analytical procedures need to be tested in terms of their inter-comparability. In this study, the schemes of analysis used in four laboratories that are involved in archaeological pottery studies on a routine basis were compared. The techniques investigated were neutron activation analysis (NAA), X-ray fluorescence analysis (XRF), inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). For this comparison series of measurements on different geological standard reference materials (SRM) were carried out and the results were statistically evaluated. An attempt was also made towards the establishment of calibration factors between pairs of analytical setups in order to smooth the systematic differences among the results.

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

    NASA Astrophysics Data System (ADS)

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

    2006-11-01

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

  2. Novel method for the fast preconcentration and monitoring of a ppt level of lead and copper with a modified hexagonal mesoporous silica compound and inductively coupled plasma atomic emission spectrometry.

    PubMed

    Ganjali, Mohammad Reza; Babaei, Leila Hajiagha; Badiei, Alireza; Ziarani, Ghodsi Mohammadi; Tarlani, Aliakbar

    2004-04-01

    A novel method for the rapid extraction and determination of a ppt level of Pb2+ and Cu2+ ions using partial silylated MCM-41 modified by a new salophen and inductively coupled plasma atomic emission spectrometry (ICP-AES) is introduced. The preconcentration factor of the method is 500, and the detection limits of Pb2+ and Cu2+ are 335 and 34 ng L(-1), respectively. The time and efficiency of extraction, the pH and flow rate, the type and minimum amount of acid for stripping of Pb2+ and Cu2+ from modified MCM-41 and the break-through volume were investigated. The maximum capacity of 4 mg of silylated MCM-41 modified by salophen used was found to be 150 +/- 4 and 117 +/- 3 microg of Pb2+ and Cu2+, respectively.

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

    USGS Publications Warehouse

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

    1996-01-01

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

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

    PubMed

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

    2017-02-15

    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.

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

    PubMed Central

    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

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

    PubMed

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

    1993-06-01

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

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

    PubMed

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

    2013-04-01

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

  8. Raman Spectrometry.

    ERIC Educational Resources Information Center

    Gardiner, Derek J.

    1980-01-01

    Reviews mainly quantitative analytical applications in the field of Raman spectrometry. Includes references to other reviews, new and analytically untested techniques, and novel sampling and instrument designs. Cites 184 references. (CS)

  9. Raman Spectrometry.

    ERIC Educational Resources Information Center

    Gardiner, Derek J.

    1980-01-01

    Reviews mainly quantitative analytical applications in the field of Raman spectrometry. Includes references to other reviews, new and analytically untested techniques, and novel sampling and instrument designs. Cites 184 references. (CS)

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

    NASA Astrophysics Data System (ADS)

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

    2015-01-01

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