Science.gov

Sample records for emission spectrometry icp-oes

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

    PubMed

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

    2008-01-01

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

  2. 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

  3. 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.

  4. Comparison method for uranium determination in ore sample by inductively coupled plasma optical emission spectrometry (ICP-OES).

    PubMed

    Sert, Şenol

    2013-07-01

    A comparison method for the determination (without sample pre-concentration) of uranium in ore by inductively coupled plasma optical emission spectrometry (ICP-OES) has been performed. The experiments were conducted using three procedures: matrix matching, plasma optimization, and internal standardization for three emission lines of uranium. Three wavelengths of Sm were tested as internal standard for the internal standardization method. The robust conditions were evaluated using applied radiofrequency power, nebulizer argon gas flow rate, and sample uptake flow rate by considering the intensity ratio of the Mg(II) 280.270 nm and Mg(I) 285.213 nm lines. Analytical characterization of method was assessed by limit of detection and relative standard deviation values. The certificated reference soil sample IAEA S-8 was analyzed, and the uranium determination at 367.007 nm with internal standardization using Sm at 359.260 nm has been shown to improve accuracy compared with other methods. The developed method was used for real uranium ore sample analysis. PMID:23816124

  5. 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.

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

    PubMed

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

    2007-02-01

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

  7. 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

  8. 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. PMID:21573840

  9. Determination of traces of As, B, Bi, Ga, Ge, P, Pb, Sb, Se, Si and Te in high-purity nickel using inductively coupled plasma-optical emission spectrometry (ICP-OES).

    PubMed

    Thangavel, S; Dash, K; Dhavile, S M; Sahayam, A C

    2015-01-01

    A method has been developed for the determination of traces of arsenic, boron, bismuth, gallium, germanium, phosphorus, lead, antimony, selenium, silicon and tellurium in nickel matrix. The sample was dissolved in HClO4 (~ 150°C) and nickel was settled as crystalline nickelperchlorate [Ni(ClO4)2] on cooling. The mixture was ultrasonicated and after the separation of Ni(ClO4)2, analytes of interest were determined in the supernatant using ICP-OES. Similarly, it was also found that, after the dissolution of nickel in perchloric acid, when the solution temperature was maintained at ~ 100°C, long needle like crystals of nickel perchlorate were formed. The crystals were separated from the mixture and trace elements in the supernatant were determined using ICP-OES. In both methods the matrix removal was >99% and the recoveries of analytes were in the range 92-97%. The limits of detection for As, B, Bi, Ga, Ge, P, Pb, Sb, Se, Si and Te were found to be 0.18, 0.21, 0.07, 0.06, 0.25, 0.11, 0.09, 0.10, 0.17, 0.20 and 0.07 μg g(-1) respectively. The procedure was applied for the analysis of a standard reference material nickel oxide (SRM 761, Nickel Oxide No.1, NBS, USA) and the values obtained are in close agreement with the certified values. PMID:25281133

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

    PubMed

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

    2016-12-01

    This study was aimed to establish the elemental profiling and provenance of coffee samples collected from eleven major coffee producing regions of Ethiopia. A total of 129 samples were analyzed for forty-five elements using inductively coupled plasma (ICP)-optical emission spectroscopy (OES), ICP-mass spectrometry (MS) and direct mercury analyzer (DMA). Among the macro elements, K showed the highest levels whereas Fe was found to have the lowest concentration values. In all the samples, Ca, K, Mg, P and S contents were statistically significant (p<0.05). Micro elements showed the concentrations order of: Mn>Cu>Sr>Zn>Rb>Ni>B. Contents of the trace elements were lower than the permissible standard values. Inter-regions differentiation by cluster analysis (CA), linear discriminant analysis (LDA) and principal component analysis (PCA) showed that micro and trace elements are the best chemical descriptors of the analyzed coffee samples. PMID:27374562

  11. 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

  12. 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.

  13. 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

  14. 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.

  15. 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.

  16. 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. PMID:24630410

  17. 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. PMID:26593498

  18. 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.

  19. Determination of heavy metals for the quality control in Argentinian herbal medicines by ETAAS and ICP-OES.

    PubMed

    Gomez, María R; Cerutti, Soledad; Sombra, Lorena L; Silva, María F; Martínez, Luis D

    2007-06-01

    The determination of trace elements in Hypericum perforatum leaves and flowers, their teas, tinctures and tablets was carried out by Electrothermal Atomic Absorption Spectrometry (ETAAS) and Ultrasonic Nebulization System coupled to Inductively Coupled Plasma Optical Emission Spectrometry (USN-ICP-OES). Hypericum perforatum (St. John's wort), is a phytomedicine used for the treatment of depression. Samples were collected from different sources in the argentinian market. Heavy metals contents in the investigated samples were found at different levels. Chromium and cobalt were undetectable above their limits of detection in both liquid and solid samples; while aluminum, cadmium, lead, iron and vanadium were present in the majority of samples. The analytical results obtained for all metals indicate that they were present at concentration well below the acceptable daily intake recommended by the World Health Organization. Based on the results obtained in the present work, it is concluded that the present techniques are suitable for the routine determination of heavy metals concentration in phytopharmaceuticals.

  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). PMID:24486318

  1. 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.

  2. 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.

  3. 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.

  4. 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. PMID:26939686

  5. 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. PMID:22608453

  6. 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...

  7. [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

  8. 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.

  9. 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.

  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. PMID:26610685

  11. Improvement of a sample preparation procedure for multi-elemental determination in Brazil nuts by ICP-OES.

    PubMed

    Welna, Maja; Szymczycha-Madeja, Anna

    2014-04-01

    Various sample preparation procedures, such as common wet digestions and alternatives based on solubilisation in aqua regia or tetramethyl ammonium hydroxide, were compared for the determination of the total Ba, Ca, Cr, Cd, Cu, Fe, Mg, Mn, Ni, P, Pb, Se, Sr and Zn contents in Brazil nuts using inductively coupled plasma optical emission spectrometry (ICP-OES). For measurement of Se, a hydride generation technique was used. The performance of these procedures was measured in terms of precision, accuracy and limits of detection of the elements. It was found that solubilisation in aqua regia gave the best results, i.e. limits of detection from 0.60 to 41.9 ng ml(-1), precision of 1.0-3.9% and accuracy better than 5%. External calibration with simple standard solutions could be applied for the analysis. The proposed procedure is simple, reduces sample handling, and minimises the time and reagent consumption. Thus, this can be a vital alternative to traditional sample treatment approaches based on the total digestion with concentrated reagents. A phenomenon resulting from levels of Ba, Se and Sr in Brazil nuts was also discussed.

  12. Development of cloud point extraction for simultaneous extraction and determination of gold and palladium using ICP-OES.

    PubMed

    Tavakoli, Laleh; Yamini, Yadollah; Ebrahimzadeh, Homeyra; Nezhadali, Azizollah; Shariati, Shahab; Nourmohammadian, Farahnaz

    2008-04-01

    Cloud point method was applied for the simultaneous extraction and preconcentration of trace amounts of gold and palladium. The extraction of analytes was performed in the presence of 1,8-diamino-4,5-dihydroxy anthraquinone as chelating agent and Triton X-114 as a non-ionic surfactant. After phase separation, the surfactant-rich phase was diluted with concentrated HNO(3) (65%, w/w) and the analytes concentrations were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES). The variables affecting the complexation and extraction conditions were optimized and under the optimum conditions (i.e. pH 6.5, 2.2 x 10(-4) mol l(-1) chelating agent, 0.15% (w/v) of Triton X-114, equilibration temperature 55 degrees C, centrifuge at 3500 rpm), quantitative extraction of Au(III) and Pd(II) from 100 ml of the aqueous solution was performed. The calibration curves were linear in the range of 0.5-1000 microg l(-1) with detection limits of 0.5 and 0.3 microg l(-1) and the enrichment factors were 8.6 and 20.2 for Au and Pd, respectively. Also the precision (%RSD) for eight replicate determinations of the analytes was better than 5%. Finally, the proposed method was successfully applied for the determination of Au and Pd in mine stones and standard reference materials (SRM).

  13. 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.

  14. 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. PMID:26452926

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

    PubMed

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

    2013-07-01

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

  16. 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.

  17. 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).

  18. 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.

  19. 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.

  20. 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. PMID:26005746

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

    PubMed

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

    2012-10-01

    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. PMID:22739429

  2. Dithizone modified magnetic nanoparticles for fast and selective solid phase extraction of trace elements in environmental and biological samples prior to their determination by ICP-OES.

    PubMed

    Cheng, Guihong; He, Man; Peng, Hanyong; Hu, Bin

    2012-01-15

    A fast and simple method for analysis of trace amounts of Cr(III), Cu(II), Pb(II) and Zn(II) in environmental and biological samples was developed by combining magnetic solid phase extraction (MSPE) with inductively coupled plasma-optical emission spectrometry (ICP-OES) detection. Dithizone modified silica-coated magnetic Fe(3)O(4) nanoparticles (H(2)Dz-SCMNPs) were prepared and used for MSPE of trace amounts of Cr(III), Cu(II), Pb(II) and Zn(II). The prepared magnetic nanoparticles were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). The factors affecting the extraction of the target metal ions such as pH, sample volume, eluent, and interfering ions had been investigated and the adsorption mechanism of the target metals on the self-prepared H(2)Dz-SCMNPs was investigated by FT-IR and X-ray photo electron spectroscopy (XPS). Under the optimized conditions, the detection limits of the developed method for Cr(III), Cu(II), Pb(II) and Zn(II) were 35, 11, 62, and 8ngL(-1), respectively, with the enrichment factor of 100. The relative standard deviations (RSDs, c=10μgL(-1), n=7) were in the range of 1.7-3.1% and the linear range was 0.1-100μgL(-1). The proposed method had been validated by two certified reference materials (GSBZ50009-88 environmental water and GBW07601 human hair), and the determined values were in good agreement with the certified values. The method was also applied for the determination of trace metals in real water and human hair samples with recoveries in the range of 85-110% for the spiked samples. The developed MSPE-ICP-OES method has the advantages of simplicity, rapidity, selectivity, high extraction efficiency and is suitable for the analysis of samples with large volume and complex matrix. PMID:22265534

  3. 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.

  4. 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. PMID:27016612

  5. 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%. PMID:23411174

  6. Solid phase extraction of gold(III) on attapulgite modified with triocarbohydrazide prior to its determination in environmental samples by ICP-OES.

    PubMed

    Zhang, Li; Li, Zhenhua; Hu, Zheng; Chang, Xijun

    2011-09-01

    The first study on the high efficiency of triocarbohydrazide modified attapulgite as solid-phase extractant for preconcentration of trace Au(III) prior to the measurement by inductively coupled plasma optical emission spectrometry (ICP-OES) has been reported. Experimental conditions for effective adsorption of trace levels of Au(III) were optimized with respect to different experimental parameters using batch and column procedures in detail. At pH 3, Au(III) could be quantitatively adsorbed on the new sorbent, and the adsorbed Au(III) could be completely eluted from the sorbent surface by 2.0mL 1.0molL(-1) of HCl+2% CS(NH(2))(2) solution. An enrichment factor of 150 was accomplished. Moreover, common interfering ions did not interfere in both separation and determination. The maximum adsorption capacity of the sorbent for Au(III) was found to be 66.7mgg(-1). The detection limit (3σ) of this method was 0.32μgL(-1) and the relative standard deviation (RSD) was 3.3% (n=8). The method, with high selectivity, sensitivity and reproducibility, was validated using certified reference materials, and had been applied for the determination of trace Au(III) with satisfactory results.

  7. 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. PMID:27260458

  8. 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.

  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). PMID:15702309

  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. 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. PMID:24607119

  12. 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).

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

    PubMed

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

    2016-09-01

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

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

    PubMed

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

    2016-09-01

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

  15. 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.

  16. Statistical design-principal component analysis optimization of a multiple response procedure using cloud point extraction and simultaneous determination of metals by ICP OES.

    PubMed

    Bezerra, Marcos A; Bruns, Roy E; Ferreira, Sergio L C

    2006-11-24

    A procedure has been developed for the simultaneous determination of traces amounts of Cd, Cr, Cu, Mn, Ni and Pb from saline oil-refinery effluents and digested vegetable samples using inductively coupled plasma optical emission spectrometry (ICP OES). The procedure is based on cloud point extraction (CPE) of these metals as 2-(bromo-2-pyridylazo)-5-diethyl-amino-phenol (Br-PADAP) complexes into a micellar phase of octylphenoxypolyethoxyethanol (Triton X-114). Optimization of the procedure was performed by response surface methodology (RSM) using a Doehlert design. Principal components (PC) were used to simplify the multiple response analysis. A response surface for the first PC score is useful in determining the optimum conditions for the Cd, Cr, Cu, Mn and Pb determinations whereas the second PC is highly correlated with the Ni response. Improvement factors of 22, 36, 46, 25, 65 and 39, along with limits of detection (3sigma(B)) of 0.081, 0.79, 0.38, 0.83, 0.28 and 0.69 microg L(-1), and precision expressed as relative standard deviation (%R.S.D., n=8, 20.0 microg L(-1)) of 1.5, 2.2, 3.5, 2.6, 2.5 and 2.5 were achieved for Cd, Cr, Cu, Mn, Ni and Pb, respectively. The accuracy was evaluated by spike tests in oil-refinery effluent samples and analysis of a vegetable certified reference material (NIST 1571, orchard leaves). Results found were in agreement with certified values.

  17. 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

  18. 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.

  19. 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

  20. Using SEM-EDX and ICP-OES to Investigate the Elemental Composition of Green Macroalga Vaucheria sessilis

    PubMed Central

    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.). PMID:25180212

  1. 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

    2016-06-01

    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.

  2. 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

    2016-06-01

    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. PMID:26994552

  3. 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).

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

    PubMed

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

    2016-04-01

    A method was developed for determining the concentrations of Cd, Co, Cr, Cu, Ni and Pb in lipstick samples intended to be used by adults and children using inductively coupled plasma optical emission spectrometry (ICP OES) and graphite furnace atomic absorption spectrometry (GF AAS) after treatment with dilute HNO3 and hot block. The combination of fractional factorial design and Desirability function was used to evaluate the ICP OES operational parameters and the regression models using Central Composite and Doehlert designs were calculated to stablish the best working condition for all analytes. Seventeen lipstick samples manufactured in different countries with different colors and brands were analyzed. Some samples contained high concentrations of toxic elements, such as Cr and Pb, which are carcinogenic and cause allergic and eczematous dermatitis. The maximum concentration detected was higher than the permissible safe limits for human use, and the samples containing these high metal concentrations were intended for use by children. Principal component analysis (PCA) was used as a chemometrics tool for exploratory analysis to observe the similarities between samples relative to the metal concentrations (a correlation between Cd and Pb was observed). PMID:26838401

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. 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.

  10. 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

  11. 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.

  12. Studies the alterations of biochemical and mineral contents in bone tissue of mus musculus due to aluminum toxicity and the protective action of desferrioxamine and deferiprone by FTIR, ICP-OES, SEM and XRD techniques

    NASA Astrophysics Data System (ADS)

    Sivakumar, S.; Khatiwada, Chandra Prasad; Sivasubramanian, J.

    The present study has attempt to analyze the changes in the biochemical and mineral contents of aluminum intoxicated bone and determine the protective action of desferrioxamine (DFO) and deferiprone (DFP) by using Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), inductively coupled plasma optical emission spectroscopy (ICP-OES), and scanning electron microscopy (SEM) techniques for four groups of animals such as control (Group I), aluminum intoxicated (Group II), Al + DFP (Group III) and Al + DFO + DFP (Group IV) treated groups respectively. The FTIR spectra of the aluminum intoxicated bone showed significant alteration in the biochemical constituents. The bands ratio at I1400/I877 significantly decreased from control to aluminum, but enhanced it by Al + DFP to Al + DFO + DFP treated bone tissue for treatments of 16 weeks. This result suggests that DFO and DFP are the carbonate inhibitor, recovered from chronic growth of bone diseases and pathologies. The alteration of proteins profile indicated by Amide I and Amide II, where peak area values decreased from control to aluminum respectively, but enhanced by treated with DFP (p.o.) and DFO + DFP (i.p.) respectively. The XRD analysis showed a decrease in crystallinity due to aluminum toxicity. Further, the Ca, Mg, and P contents of the aluminum exposed bone were less than those of the control group, and enhanced by treatments with DFO and DFP. The concentrations of trace elements were found by ICP-OES. Therefore, present study suggests that due to aluminum toxicity severe loss of bone minerals, decrease in the biochemical constituents and changes in the surface morphology.

  13. 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.

  14. 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

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

    PubMed

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

    2016-01-01

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

  16. 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.

  17. 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.

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

    PubMed

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

    2010-10-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2009-06-01

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

  20. [Analysis of some nutrients and minerals in organic and traditional cherry tomato by ICP-OES method].

    PubMed

    Sheng, Ji-Ping; Liu, Can; Shen, Lin

    2009-08-01

    In the present study, the contents of nutritional elements such as Ca, Mg, K, Zn, Fe and Mn and heavy elements such as Cu, Cd and Pb in organic and traditional cherry tomato fruit were analyzed by ICP-OES, and the contents of some nutritional ingredients such as water, total soluble solid, soluble sugar and asorbic acid were also investigated. The results showed that the contents of K, Ca and Zn in organic cherry tomato were 1.62, 71.7 and 1.34 mg x g(-1), which were 4.52%, 129.81% and 65.43% respectively higher than those in traditional tomato. There were no significant differences in the contents of Mg and Fe, which showed 73.8 and 2.05 mg x g(-1) in organic cherry tomato. But the content of Mn in organic tomato was 0.475 mg x g(-1), 11.22% lower than that in traditional one (alpha = 0.05). The contents of Cu, Cd and Pb showed no significant differences in the two kinds of tomato, which were 0.457 mg x g(-1), 4.86 ng x g(-1) and 0.127 mg x g(-1) respectively in organic cherry tomato, and all the contents were lower than the national requirement. There were no significant differences in the contents of water, soluble sugar, and asorbic acid, but the total soluble solid and the content of soluble protein were significantly higher in organic cherry tomato. The differences in the nutritional ingredients and mineral elements and safety status in the two kinds of tomato provide academic data for the evaluation of organic vegetables and traditional ones.

  1. 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.

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

    PubMed

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

    2008-05-01

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

  3. 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.

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

    PubMed

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

    2016-09-01

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

  5. 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

  6. 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

  7. 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. PMID:23598105

  8. 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.

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

    PubMed

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

    2015-11-01

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

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

    PubMed

    Tirk, Paul; Wolfgang, Matthias; Wiltsche, Helmar

    2016-07-19

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

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

    PubMed

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

    2009-11-15

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

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

    PubMed

    Tirk, Paul; Wolfgang, Matthias; Wiltsche, Helmar

    2016-07-19

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

  13. 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).

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

    NASA Astrophysics Data System (ADS)

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

    2005-03-01

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

  15. Characterization of binary silver based alloys by nanosecond-infrared-laser-ablation-inductively coupled plasma-optical emission spectrometer

    NASA Astrophysics Data System (ADS)

    Márquez, Ciro; Sobral, Hugo

    2013-11-01

    A nanosecond infrared laser ablation (LA) system was examined to determine the composition of several silver-copper alloys through an inductively coupled plasma-optical emission spectrometer (ICP-OES). Samples with different concentrations were prepared and analyzed by atomic absorption, and ICP-OES after sample digestion, and compared with an energy-dispersive x-ray spectrometer-scanning electron microscopy (EDX-SEM). Elemental fractionation during the ablation process and within the ICP was investigated for different laser frequencies and fluences. Samples were used for optimizing and calibrating the coupling between LA to the ICP-OES system. Results obtained from the samples analysis were in agreement with those obtained by atomic absorption spectroscopy, ICP-OES and EDX-SEM, showing that fractionation was not significant for laser fluences higher than 55 J cm-2.

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

    PubMed

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

    2013-05-30

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

  17. 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.

  18. 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.

  19. 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).

  20. 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.

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

    PubMed

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

    2013-11-15

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

  2. 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.

  3. 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.

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

    PubMed

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

    2013-10-15

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

  5. Multi-element analysis of wines by ICP-MS and ICP-OES and their classification according to geographical origin in Slovenia.

    PubMed

    Selih, Vid S; Sala, Martin; Drgan, Viktor

    2014-06-15

    Inductively coupled plasma mass spectrometry and optical emission were used to determine the multi-element composition of 272 bottled Slovenian wines. To achieve geographical classification of the wines by their elemental composition, principal component analysis (PCA) and counter-propagation artificial neural networks (CPANN) have been used. From 49 elements measured, 19 were used to build the final classification models. CPANN was used for the final predictions because of its superior results. The best model gave 82% correct predictions for external set of the white wine samples. Taking into account the small size of whole Slovenian wine growing regions, we consider the classification results were very good. For the red wines, which were mostly represented from one region, even-sub region classification was possible with great precision. From the level maps of the CPANN model, some of the most important elements for classification were identified.

  6. Multielement plant tissue analysis using ICP spectrometry.

    PubMed

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

    2013-01-01

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

  7. 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

    2000-05-01

    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.

  8. Developments in glow discharge emission spectrometry

    NASA Astrophysics Data System (ADS)

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

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

  9. 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.

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

    PubMed

    Chen, Dahui; Hu, Bin; Huang, Chaozhang

    2009-04-30

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

  11. 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

  12. 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

  13. 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

  14. 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. PMID:27542497

  15. 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.

  16. Determination of trace elements in lithium niobate crystals by solid sampling and solution-based spectrometry methods.

    PubMed

    Bencs, László; György, Krisztina; Kardos, Márta; Osán, János; Alföldy, Bálint; Varga, Imre; Ajtony, Zsolt; Szoboszlai, Norbert; Stefánka, Zsolt; Széles, Eva; Kovács, László

    2012-05-13

    Solid sampling (SS) graphite furnace atomic absorption spectrometry (GFAAS) and solution-based (SB) methods of GFAAS, flame atomic absorption spectrometry (FAAS), inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) were elaborated and/or optimized for the determination of Cr, Fe and Mn trace elements used as dopants in lithium niobate optical crystals. The calibration of the SS-GFAAS analysis was possible with the application of the three-point-estimation standard addition method, while the SB methods were mostly calibrated against matrix-matched and/or acidic standards. Spectral and non-spectral interferences were studied in SB-GFAAS after digestion of the samples. The SS-GFAAS method required the use of less sensitive spectral lines of the analytes and a higher internal furnace gas (Ar) flow rate to decrease the sensitivity for crystal samples of higher (doped) analyte content. The chemical forms of the matrix produced at various stages of the graphite furnace heating cycle, dispensed either as a solid sample or a solution (after digestion), were studied by means of the X-ray near-edge absorption structure (XANES). These results revealed that the solid matrix vaporized/deposited in the graphite furnace is mostly present in the metallic form, while the dry residue from the solution form mostly vaporized/deposited as the oxide of niobium. PMID:22541007

  17. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry.

    PubMed

    Bentlin, Fabrina R S; Pozebon, Dirce; Mello, Paola A; Flores, Erico M M

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO3)2 was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 microg g(-1) of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES).

  18. Digital image-based flame emission spectrometry.

    PubMed

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

    2009-03-15

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

  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. 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). PMID:27026544

  1. Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Amberger, Martin A.; Höltig, Michael; Broekaert, José A. C.

    2010-02-01

    The use of slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL -1. As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL -1 of boron nitride were found suitable and were used for all further measurements. The limits of detection of SlS-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 μg g - 1 for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, SlS-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of SlS-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al 2O 3, powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by SlS-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective samples over a

  2. 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.

  3. 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.

  4. 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. PMID:25262949

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

    SciTech Connect

    Partridge, William P.

    2000-08-20

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

  6. 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.

  7. 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

    2007-01-01

    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. PMID:17386451

  8. A simple solution to expanding available reference materials for Laser Ablation Inductively Coupled Plasma Mass Spectrometry analysis: Applications to sedimentary materials

    NASA Astrophysics Data System (ADS)

    Shaheen, Mohamed E.; Fryer, Brian J.

    2011-08-01

    Analytical data on sediments are of great importance in understanding and documenting environmental issues. For laboratories interested in in-situ chemical analysis of sediments by LA-ICP-MS, a major issue is the lack of appropriate matrix matched sediment reference materials. Those available were largely designed for partial extractions which generally do not reflect the total elemental compositions. In this work we provide a comprehensive study on chemical compositions of seven currently available sediment reference materials (Lake sediments: LKSD-1, LKSD-2, LKSD-3, Stream sediments: STSD-2, STSD-3, and Marine sediments: PACS-2, MESS-3) as determined by Solution Nebulization Inductively Coupled Plasma Mass Spectrometry (SN-ICP-MS) and Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) after digestion in a mixture of concentrated HNO 3 and HF acids. We also report a simple method to prepare these sediment reference materials and more generally appropriate sediment cores for LA-ICP-MS analysis using epoxy resin. This sample preparation method maintains sediment integrity for high spatial resolution analysis which is required for tracing changes in environmental conditions over short time periods. This work also demonstrates the application of fs-LA-ICP-MS as a tool for direct, rapid and high spatial resolution analysis of sediments.

  9. 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.

  10. 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. PMID:26117893

  11. HPLC-ICP atomic emission spectrometry in environmental analysis

    SciTech Connect

    Frame, E.M.S.

    1996-10-01

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

  12. 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)…

  13. 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

  14. 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.

  15. 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.

  16. Atomic absorption spectrometry with a flame emission source

    NASA Astrophysics Data System (ADS)

    Calloway, Clifton P.; Jones, Bradley T.

    1994-12-01

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

  17. 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.

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

    SciTech Connect

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

    1995-10-01

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

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

    PubMed

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

    2003-04-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2002-06-01

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

  1. Narrowband emission line imaging spectrometry using Savart plates

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

  2. 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)

  3. 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

  4. Monitoring As and Hg variation in An-Gong-Niu-Huang Wan (AGNH) intermediates in a pilot scale blending process using laser-induced breakdown spectroscopy.

    PubMed

    Liu, Xiaona; Ma, Qun; Liu, Shanshan; Shi, Xinyuan; Zhang, Qiao; Wu, Zhisheng; Qiao, Yanjiang

    2015-01-01

    Laser-induced breakdown spectroscopy (LIBS) was used to assess the cinnabar and realgar blending of An-Gong-Niu-Huang Wan (AGNH) in a pilot-scale experiment, including the blending end-point. The blending variability of two mineral medicines, cinnabar and realgar, were measured by signal relative intensity changing rate (RICR) and moving window standard deviation (MWSD) based on LIBS. Meanwhile, relative concentration changing rate (RCCR) was obtained based on the reference method involving inductively coupled plasma optical emission spectrometry (ICP-OES). The LIBS result was consistent with ICP-OES at blending end-point determinations of both mineral medicines. Unlike the ICP-OES method, LIBS does not have an elaborate digestion procedure. LIBS is a promising and rapid technique to understand the blending process of Chinese Materia Medica (CMM) containing cinnabar and realgar. These results demonstrate the potential of LIBS in monitoring CMM pharmaceutical production. PMID:26162343

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

    NASA Astrophysics Data System (ADS)

    Montaser, A.

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

  6. 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.

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

    NASA Astrophysics Data System (ADS)

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

    1994-07-01

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

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

    PubMed

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

    1993-01-01

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

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

    NASA Astrophysics Data System (ADS)

    Kántor, Tibor; Bartha, András

    2015-11-01

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

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

    PubMed

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

    2014-05-01

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

  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

    NASA Astrophysics Data System (ADS)

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

    2016-01-01

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

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

    PubMed

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

    2016-01-01

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

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

    PubMed

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

    1999-08-01

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

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

    PubMed

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

    2016-01-01

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

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

    PubMed

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

    2016-01-01

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

  17. 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 ...

  18. 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…

  19. 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...

  20. 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.

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

    PubMed

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

    2006-12-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-01-01

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

  3. 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.

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

    PubMed

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

    2006-09-01

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

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

    PubMed

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

    2005-02-01

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

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

    PubMed

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

    2014-06-01

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

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

    PubMed

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

    2016-02-25

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

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

    DOEpatents

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

    2010-08-03

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

  9. 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.

  10. 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.

  11. 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

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

    PubMed

    Park, Jonghoo; Blick, Robert H

    2016-01-01

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

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

    PubMed

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

    2006-09-01

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

  14. 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.

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

    PubMed

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

    2015-11-01

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

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

    PubMed

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

    2015-11-01

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

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

    PubMed

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

    2011-04-15

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

  18. 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.

  19. 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.

  20. 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. PMID:27080872

  1. 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.

  2. Spectroscopic Characteristic and Analytical Capability of Ar-N₂ Inductively Coupled Plasma in Axially Viewing Optical Emission Spectrometry.

    PubMed

    Ohata, Masaki

    2016-01-01

    The spectroscopic characteristics and analytical capability of argon-nitrogen (Ar-N2) inductively coupled plasma (ICP) in axially viewing optical emission spectrometry (OES) were examined and figures of merit were determined in the present study. The spectroscopic characteristics such as the emission intensity profile and the excitation temperature observed from the analytical zone of Ar-N2 ICP in axially viewing ICPOES, in order to elucidate the enhancement of the emission intensity of elements obtained in our previous study, were evaluated and compared to those of the standard ICP. The background and emission intensities of elements as well as their excitation behavior for both atom and ion lines were also examined. As results, a narrower emission intensity profile and an increased excitation temperature as well as enhancements for both background and emission intensities of elements, which could be due to the ICP shrunken as well as the enhancement of the interaction between the central channel of the ICP and samples introduced, were observed for Ar-N2 ICP in axially viewing OES. In addition, the elements with relatively higher excitation and ionization energies such as As, Bi, Cd, Ni, P, and Zn revealed larger enhancements of the emission intensities as well as improved limits of detection (LODs), which were also attributed to the enhanced interaction between Ar-N2 ICP and the samples. Since the Ar-N2 ICP could be obtained easily only by the addition of a small amount of N2 gas to the Ar plasma gas of the standard ICP and no optimization on the alignment between Ar-N2 ICP and the spectrometer in commercially available ICPOES instruments was needed, it could be utilized as simple and optional excitation and ionization sources in axially viewing ICPOES. PMID:26860569

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

    NASA Astrophysics Data System (ADS)

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

    2000-08-01

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

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

    PubMed

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

    2013-01-01

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

  5. 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.

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

    PubMed

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

    2013-01-01

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

  7. 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.

  8. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2012-12-01

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

  10. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2012-12-01

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

  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. 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.

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

    PubMed

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

    2004-02-18

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

  15. 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...

  16. 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.

  17. 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)

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

    PubMed

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

    2015-01-01

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

  19. 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.

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

    NASA Astrophysics Data System (ADS)

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

    1999-07-01

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

  1. 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.

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

    SciTech Connect

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

    1993-02-01

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

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

    PubMed

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

    2015-01-01

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

  4. 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.

  5. 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.

  6. 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…

  7. 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.

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

    PubMed

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

    2015-11-01

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

  9. 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.

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

    PubMed

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

    2010-12-01

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

  11. 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.

  12. 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.

  13. 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.

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

    PubMed

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

    2015-12-17

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

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

    PubMed

    Gonzaga, Fabiano Barbieri; Pasquini, Celio

    2005-02-15

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

  16. 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)

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

    PubMed

    Lajunen, L H; Kubin, A

    1986-03-01

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

  18. 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

  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

    2014-01-01

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

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

    PubMed

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

    2012-05-01

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

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

    PubMed

    Shekhar, R

    2012-05-15

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

  2. 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.

  3. 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.

  4. 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).

  5. 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.

  6. Analytical performance of a low-gas-flow torch optimized for inductively coupled plasma atomic emission spectrometry

    USGS Publications Warehouse

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

    1984-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-12-01

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

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

    PubMed

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

    2016-04-19

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

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

    PubMed

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

    2009-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

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

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

    PubMed

    Smolik, Marek; Jakóbik-Kolon, Agata

    2009-04-01

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

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

    PubMed

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

    2014-01-01

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

  13. 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.

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

    NASA Astrophysics Data System (ADS)

    Daskalova, N.; Boevski, I. V.

    1999-07-01

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

  15. 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.

  16. 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.

  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. PMID:27154648

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

    SciTech Connect

    Montaser, A.

    1993-12-31

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

  19. [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

  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. 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.

  2. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2009-01-01

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

  4. 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

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

    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

  6. 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.

  7. A novel methodology for rapid digestion of rare earth element ores and determination by microwave plasma-atomic emission spectrometry and dynamic reaction cell-inductively coupled plasma-mass spectrometry.

    PubMed

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

    2016-11-01

    Short-wavelength infrared radiation has been successfully applied to accelerate the acid digestion of refractory rare-earth ore samples. Determinations were achieved with microwave plasma-atomic emission spectrometry (MP-AES) and dynamic reaction cell - inductively coupled plasma-mass spectrometry (DRC-ICP-MS). The digestion method developed was able to tackle high iron-oxide and silicate matrices using only phosphoric acid in a time frame of only 8min, and did not require perchloric or hydrofluoric acid. Additionally, excellent recoveries and reproducibilities of the rare earth elements, as well as uranium and thorium, were achieved. Digestions of the certified reference materials OREAS-465 and REE-1, with radically different mineralogies, delivered results that mirror those obtained by fusion processes. For the rare-earth CRM OKA-2, whose REE data are provisional, experimental data for the rare-earth elements were generally higher than the provisional values, often exceeding z-values of +2. Determined values for Th and U in this reference material, for which certified values are available, were in excellent agreement. PMID:27591646

  8. 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%.

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

    PubMed

    Schäfer, K; Haus, R; Heland, J

    1994-05-01

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

  10. 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…

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

    PubMed

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

    2016-02-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-01-01

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

  13. 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

  14. Effects of liquid chromatography mobile phases and buffer salts on phosphorus inductively coupled plasma atomic emission and mass spectrometries utilizing ultrasonic nebulization and membrane desolvation.

    PubMed

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

    2006-01-23

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

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

    PubMed

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

    1995-01-01

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

  16. 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. PMID:26384315

  17. 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.

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

    PubMed Central

    Chung, Yuen-Li

    2014-01-01

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

  19. Direct solid sampling system for electrothermal vaporization and its application to the determination of chlorine in nanopowder samples by inductively coupled plasma optical emission spectroscopy.

    PubMed

    Nakata, Kenichi; Hashimoto, Bunji; Uchihara, Hiroshi; Okamoto, Yasuaki; Ishizaka, Syoji; Fujiwara, Terufumi

    2015-06-01

    An electrothermal vaporization (ETV) system using a tungsten boat furnace (TBF) sample cuvette was designed for the direct determination of chlorine in metallic nanopowders and fine powder samples with detection by inductively coupled plasma optical emission spectroscopy (ICP-OES). A portion of a powder or particle sample was placed into a small tungsten sample cuvette and weighed accurately. A modifier solution of aqueous or alcoholic potassium hydroxide was added to it. Then, the cuvette was positioned on the TBF incorporated into the ETV apparatus. The analyte was vaporized and introduced into the ICP optical emission spectrometer with a carrier gas stream of argon and hydrogen. The metal samples were analyzed by using an external calibration curve prepared from aqueous standard solutions. Few chemical species including analyte and some chlorine-free species were introduced into the ICP, because the analyte has been separated from the matrix before introduction. Under such dry plasma conditions, the energy of plasma discharge was focused on the excitation of chlorine atoms, and as a result, lower detection limits were achieved. A detection limit of 170 ng g(-1) of chlorine in solid metal samples was established when 60 mg sample was used. The relative standard deviation for 16 replicate measurements obtained with 100 ng chlorine was 8.7%. Approximately 30 batches could be vaporized per hour. The analytical results for various nanopowders (iron (III) oxide, copper, silver, and gold) and metallic fine powder samples (silver and gold) are described. PMID:25863402

  20. 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

  1. 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.

  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. 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.

  4. 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.

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

    SciTech Connect

    Shen, Luan

    1995-10-06

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

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

    PubMed

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

    2014-07-01

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

  7. 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.

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

    SciTech Connect

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

    1983-11-01

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

  9. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2004-04-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-02-01

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

  12. 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.

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

    PubMed

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

    2003-01-01

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

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

    PubMed

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

    2012-12-01

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

  15. 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.

  16. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2005-03-01

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

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

    PubMed

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

    2000-10-01

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

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

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2016-06-01

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

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

    PubMed

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

    2013-12-01

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

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

    PubMed

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

    2016-08-01

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

  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. 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.

  4. 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.

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

    PubMed

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

    2015-01-01

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

  6. [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.

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

    PubMed

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

    2015-09-01

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

  8. Peat as a natural solid-phase for copper preconcentration and determination in a multicommuted flow system coupled to flame atomic absorption spectrometry.

    PubMed

    Gonzáles, A P S; Firmino, M A; Nomura, C S; Rocha, F R P; Oliveira, P V; Gaubeur, I

    2009-03-23

    The physical and chemical characteristics of peat were assessed through measurement of pH, percentage of organic matter, cationic exchange capacity (CEC), elemental analysis, infrared spectroscopy and quantitative analysis of metals by ICP OES. Despite the material showed to be very acid in view of the percentage of organic matter, its CEC was significant, showing potential for retention of metal ions. This characteristic was exploited by coupling a peat mini-column to a flow system based on the multicommutation approach for the in-line copper concentration prior to flame atomic absorption spectrometric determination. Cu(II) ions were adsorbed at pH 4.5 and eluted with 0.50 molL(-1) HNO(3). The influence of chemical and hydrodynamic parameters, such as sample pH, buffer concentration, eluent type and concentration, sample flow-rate and preconcentration time were investigated. Under the optimized conditions, a linear response was observed between 16 and 100 microgL(-1), with a detection limit estimated as 3 microgL(-1) at the 99.7% confidence level and an enrichment factor of 16. The relative standard deviation was estimated as 3.3% (n=20). The mini-column was used for at least 100 sampling cycles without significant variation in the analytical response. Recoveries from copper spiked to lake water or groundwater as well as concentrates used in hemodialysis were in the 97.3-111% range. The results obtained for copper determination in these samples agreed with those achieved by graphite furnace atomic absorption spectrometry (GFAAS) at the 95% confidence level. PMID:19264168

  9. [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.

  10. [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. PMID:25925077

  11. 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.

  12. 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.

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

    PubMed

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

    2015-05-01

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

  14. 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.

  15. 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.

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

    PubMed

    Zheng, Fei; Hu, Bin

    2007-09-15

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

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

    SciTech Connect

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

    2008-09-01

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

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

    PubMed

    Thiex, Nancy J

    2016-07-01

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

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

    PubMed

    Beiraghi, Assadollah; Babaee, Saeed

    2008-01-28

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

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

    NASA Astrophysics Data System (ADS)

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

    2002-02-01

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

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

    PubMed

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

    2016-02-01

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

  2. Determination of vanadium in petroleum and petroleum products using atomic spectrometric techniques.

    PubMed

    Amorim, Fábio A C; Welz, Bernhard; Costa, Antônio C S; Lepri, Fábio G; Vale, Maria Goreti R; Ferreira, Sérgio L C

    2007-04-30

    Vanadium is recognized worldwide as the most abundant metallic constituent in petroleum. It is causing undesired side effects in the refining process, and corrosion in oil-fired power plants. Consequently, it is the most widely determined metal in petroleum and its derivatives. This paper offers a critical review of analytical methods based on atomic spectrometric techniques, particularly flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ET AAS), inductively coupled plasma optical emission spectrometry (ICP OES), inductively coupled plasma mass spectrometry (ICP-MS). In addition an overview is provided of the sample pretreatment and preparation procedures for vanadium determination in petroleum and petroleum products. Also included are the most recent studies about speciation and fractionation analysis using atomic spectrometric techniques.

  3. 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.

  4. 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. PMID:26991383

  5. 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.

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

    PubMed

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

    2016-02-01

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

  7. 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

  8. Potential metal impurities in active pharmaceutical substances and finished medicinal products - A market surveillance study.

    PubMed

    Wollein, Uwe; Bauer, Bettina; Habernegg, Renate; Schramek, Nicholas

    2015-09-18

    A market surveillance study has been established by using different atomic spectrometric methods for the determination of selected elemental impurities of particular interest, to gain an overview about the quality of presently marketed drug products and their bulk drug substances. The limit tests were carried out with respect to the existing EMA guideline on the specification limits for residuals of metal catalysts or metal reagents. Also attention was given to the future implementation of two new chapters of the United States Pharmacopoeia (USP) stating limit concentrations of elemental impurities. The methods used for determination of metal residues were inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-optical emission spectrometry (ICP-OES), and atomic absorption spectrometry technologies (GFAAS, CVAAS, HGAAS). This article presents the development and validation of the methods used for the determination of 21 selected metals in 113 samples from drug products and their active pharmaceutical ingredients.

  9. 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. PMID:18280730

  10. Potential metal impurities in active pharmaceutical substances and finished medicinal products - A market surveillance study.

    PubMed

    Wollein, Uwe; Bauer, Bettina; Habernegg, Renate; Schramek, Nicholas

    2015-09-18

    A market surveillance study has been established by using different atomic spectrometric methods for the determination of selected elemental impurities of particular interest, to gain an overview about the quality of presently marketed drug products and their bulk drug substances. The limit tests were carried out with respect to the existing EMA guideline on the specification limits for residuals of metal catalysts or metal reagents. Also attention was given to the future implementation of two new chapters of the United States Pharmacopoeia (USP) stating limit concentrations of elemental impurities. The methods used for determination of metal residues were inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-optical emission spectrometry (ICP-OES), and atomic absorption spectrometry technologies (GFAAS, CVAAS, HGAAS). This article presents the development and validation of the methods used for the determination of 21 selected metals in 113 samples from drug products and their active pharmaceutical ingredients. PMID:26036232

  11. 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+).

  12. Fast digestion procedure for determination of catalyst residues in La- and Ni-based carbon nanotubes.

    PubMed

    Mortari, Sergio Roberto; Cocco, Carmem Regina; Bartz, Fabiane Regina; Dresssler, Valderi L; Flores, Erico Marlon de Moraes

    2010-05-15

    A procedure based on microwave-induced combustion (MIC) was applied for carbon nanotube (CNT) digestion and further determination of La and Ni by inductively coupled plasma optical emission spectrometry (ICP OES). Samples (up to 400 mg) were completely combusted at 20 bar of oxygen, and a reflux step was applied to improve the analyte absorption. Combustion was finished in less than 50 s, and analytes were absorbed in diluted acid solution. Absorbing solutions ranging from 1 to 12 mol L(-1) for HCl and from 1 to 14 mol L(-1) HNO(3) were tested. Accuracy for both analytes was evaluated using certified reference materials and analyte spikes. Neutron activation analysis was also used to check accuracy for La. Agreement was better than 96% for La and Ni using a 4 mol L(-1) absorbing solution of HNO(3) or HCl and 15 min of reflux. The residual carbon content was lower than 0.5%. Up to eight samples could be digested simultaneously in 36 min, that makes the throughput using MIC more suitable when it is compared to the digestion by dry ashing as recommended by other procedures. The obtained limits of detection using MIC were lower than those using dry ashing, and a single absorbing solution, e.g., diluted HNO(3), can be used for simultaneous determination of La and Ni by ICP OES. PMID:20405950

  13. 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.

  14. 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 ...

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  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. Toxic and nutrient elements in yerba mate (Ilex paraguariensis).

    PubMed

    Pozebon, Dirce; Dressler, Valderi Luiz; Marcelo, Marcelo Caetano Alexandre; de Oliveira, Tiago Charão; Ferrão, Marco Flores

    2015-01-01

    Toxic and nutrient elements were investigated in yerba mate (Ilex paraguariensis) from South America. Fifty-four brands of commercialised yerba mate from Argentina, Brazil, Paraguay and Uruguay were analysed for Al, Ba, Ca, Cu, Fe, K, Mg, Mn, P, Sr, and Zn, using inductively coupled plasma optical emission spectrometry (ICP-OES), and Li, Be, Ti, V, Cr, Ni, Co, As, Se, Rb, Mo, Ag, Cd, Sb, La, Ce, Pb, Bi and U using inductively coupled plasma mass spectrometry (ICP-MS). Antimony, Se, Ag and Bi were not detected in any sample whereas the limits of detection (LODs) of these elements were 0.19, 0.40, 0.003 and 0.001 μg g(-1), respectively. Analysis of variance (ANOVA) revealed that the concentrations of Cd, Ti, Ni, As, Mo, U, Li and Be in yerba mate were not statistically different with regard to the country of origin, while those of the other investigated elements differed.

  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. 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.

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

    USGS Publications Warehouse

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

    1996-01-01

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

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

    PubMed

    Lahl, H; Henke, G

    1997-11-01

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

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

    PubMed Central

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

    2013-01-01

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

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

    PubMed

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

    2014-07-11

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

  4. 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.

  5. Infrared Spectrometry.

    ERIC Educational Resources Information Center

    McDonald, Robert S.

    1984-01-01

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

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

    EPA Science Inventory

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

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

    EPA Science Inventory

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

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

    SciTech Connect

    Montaser, A.

    1994-09-01

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

  9. 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

  10. Silica-gel Particles Loaded with an Ionic Liquid for Separation of Zr(IV) Prior to Its Determination by ICP-OES.

    PubMed

    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

  11. Use of zirconium oxychloride to neutralize HF in the microwave-assisted acid dissolution of ceramic glazes for their chemical analysis by ICP-OES.

    PubMed

    Dondi, M; Fabbri, B; Mingazzini, C

    1998-04-01

    The use of a zirconium compound (ZrOCl(2)) to neutralize HF in the microwave-assisted acid dissolution of ceramic glazes for their chemical analysis was tested. Zr is a strong complexing agent for the fluorine ion and permits the determination of those elements which would form insoluble fluorides. The use of Zr implies strong spectral interferences and a high salt content; however, we found that at least 27 elements can be measured with low detection limits, and satisfactory precision and accuracy. In addition, the use of ZrOCl(2) would permit the complete analysis of a ceramic glaze with a single attack when acid-resistant mineral phases are not present. For potassium determinations in acid matrix, the addition of an ionization buffer was studied in order to increase sensitivity, avoiding ionization interferences and non-linear calibration curves. PMID:18967112

  12. 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. PMID:15081756

  13. 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

  14. 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.

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

    NASA Astrophysics Data System (ADS)

    Yassaa, Noureddine; Williams, Jonathan

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-01-01

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

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

    PubMed

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

    2009-04-01

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

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

    PubMed

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

    2015-08-01

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

  19. Heavy Metals in Soil and Salad in the Proximity of Historical Ferroalloy Emission

    PubMed Central

    Ferri, Roberta; Donna, Filippo; Smith, Donald R.; Guazzetti, Stefano; Zacco, Annalisa; Rizzo, Luigi; Bontempi, Elza; Zimmerman, Neil J.; Lucchini, Roberto G.

    2016-01-01

    Emissions of manganese (Mn), lead (Pb), iron (Fe), zinc (Zn), copper (Cu) from ferro-alloy operations has taken place in Valcamonica, a pre-Alp valley in the province of Brescia, Italy, for about a century until 2001. Metal concentrations were measured in the soil of local home gardens and in the cultivated vegetables. Soil analysis was carried out using a portable X-Ray Fluorescence (XRF) spectrometer in both surface soil and at 10 cm depth. A subset of soil samples (n = 23) additionally was analysed using the modified BCR sequential extraction method and ICP-OES for intercalibration with XRF (XRF Mn = 1.33 * total OES Mn – 71.8; R = 0.830, p < 0.0001). Samples of salads (Lactuca sativa and Chichorium spp.) were analyzed with a Total Reflection X-Ray Fluorescence (TXRF) technique. Vegetable and soil metal measurements were performed in 59 home gardens of Valcamonica, and compared with 23 gardens from the Garda Lake reference area. Results indicate significantly higher levels of soil Mn (median 986 ppm vs 416 ppm), Pb (median 46.1 ppm vs 30.2 ppm), Fe (median 19,800 ppm vs 13,100 ppm) in the Valcamonica compared to the reference area. Surface soil levels of all metals were significantly higher in surface soil compared to deeper soil, consistent with atmospheric deposition. Significantly higher levels of metals were shown also in lettuce from Valcamonica for Mn (median 53.6 ppm vs 30.2) and Fe (median 153 vs 118). Metals in Chichorium spp. did not differ between the two areas. Surface soil metal levels declined with increasing distance from the closest ferroalloy plant, consistent with plant emissions as the source of elevated soil metal levels. A correlation between Mn concentrations in soil and lettuce was also observed. These data show that historic ferroalloy plant activity, which ended nearly a decade before this study, has contributed to the persistence of increased Mn levels in locally grown vegetables. Further research is needed to assess whether this

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

    NASA Technical Reports Server (NTRS)

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

    2008-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2008-06-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2009-04-01

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

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

    USGS Publications Warehouse

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

    1984-01-01

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

  4. Extraction-spectrometric determination of lead in high-purity aluminium salts.

    PubMed

    Koksal, Jiří; Synek, Václav; Janos, Pavel

    2002-08-23

    Trace amounts of lead were determined in high purity aluminium salts (especially in ammonium aluminium sulfate) using inductively coupled plasma-optical emission spectrometry (ICP-OES) after extractive pre-concentration and matrix separation. Metals were extracted from the aluminium matrix in the form of chelates with ammonium pyrolidine dithoocarbamate into methyl isobutyketone. The organic extract was digested with nitric acid and hydrogen peroxide. The limit of detection for the determination of lead in crystalline ammonium aluminium sulfate was ca. 0.044 mug g(-1). The relative expanded uncertainty of the lead determination was ca. 23% at the level of 0.2 mug g(-1) and ca. 16% at the level of 1.0 mug g(-1). The main uncertainty contribution was associated with repeatability of the whole analytical procedure. PMID:18968757

  5. Heavy metals contamination of soils surrounding waste deposits in Romania

    NASA Astrophysics Data System (ADS)

    Matache, M.; Rozylowicz, L.; Ropota, M.; Patroescu, C.

    2003-05-01

    Soils contamination with heavy metals is one of the most severe aspects of environmental pollution in Romania, independently of the origin sources (domestic or industrial activities) or type of disposal (organised landfill or hazardous deposits)[l-2]. This fact is the consequence of the poor state of the existing waste deposits in Romania and of the significant costs involved by the establishing of a new landfill according with the international regulations. The present study is trying to emphasise the contamination of soils surrounding different categories of waste deposits (sewage sludge ponds, domestic and industrial waste landfills, hillocks, sterile deposits) from various regions of Romania. Some case studies show a special interest being localise in a protected area (Iron Gates Natural Park). In order to quantify the concentration of metals like Cd, Cr, Cu, Pb, Zn, Ni, Mo in soil samples, analysis were performed using Inductively Coupled Plasma - Optical Emission Spectrometry (ICP-OES). Romanian standards were used as reference values[3].

  6. Metal concentrations of wild edible mushrooms from Turkey.

    PubMed

    Sarikurkcu, Cengiz; Tepe, Bektas; Solak, Mehmet Halil; Cetinkaya, Serap

    2012-01-01

    In the present study, the contents of Zn, Fe, Cu, Mn, Co, Ni, Pb, Cd, Cr, Al, Ca, Mg, and K in Agaricus campestris, Agrocybe cylindracea, Collybia dryophila, Helvella leucopus, Russula delica, Tricholoma auratum, Amanita ovoidea, Melanoleuca excissa, Rhizopogon roseolus, Russula chloroides, Volvoriella gloiocephala, Lyophyllum decastes, Morcella angusticeps, Morchella esculenta and Morcella eximia collected from Isparta, Mugla, and Osmaniye provinces (Turkey) were determined by inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave digestion. The intake of heavy metals (Pb, Cd) and other metals (Fe, Cu, Zn) by consumption of 30 g dry weight of mushrooms daily poses no risk at all except in A. cylindracea and H. leucopus (for Cd) for the consumer. PMID:22794131

  7. Pattern recognition applied to mineral characterization of Brazilian coffees and sugar-cane spirits

    NASA Astrophysics Data System (ADS)

    Fernandes, Andréa P.; Santos, Mirian C.; Lemos, Sherlan G.; Ferreira, Márcia M. C.; Nogueira, Ana Rita A.; Nóbrega, Joaquim A.

    2005-06-01

    Aluminium, Ca, Cu, Fe, K, Mg, Mn, Na, Pb, S, Se, Si, Sn, Sr, and Zn were determined in coffee and sugar-cane spirit (cachaça) samples by axial viewing inductively coupled plasma optical emission spectrometry (ICP OES). Pattern recognition techniques such as principal component analysis and cluster analysis were applied to data sets in order to characterize samples with relation to their geographical origin and production mode (industrial or homemade and organically or conventionally produced). Attempts to correlate metal ion content with the geographical origin of coffee and the production mode (organic or conventional) of cachaça were not successful. Some differentiation was suggested for the geographical origin of cachaça of three regions (Northeast, Central, and South), and for coffee samples, related to the production mode. Clear separations were only obtained for differentiation between industrial and homemade cachaças, and between instant soluble and roasted coffees.

  8. Lead and cadmium in wild boar (Sus scrofa) in the Sierra Nevada Natural Space (southern Spain).

    PubMed

    Mulero, Rocío; Cano-Manuel, Javier; Ráez-Bravo, Arián; Pérez, Jesús M; Espinosa, José; Soriguer, Ramón; Fandos, Paulino; Granados, José E; Romero, Diego

    2016-08-01

    The aims of the present study were to investigate Pb and Cd levels in tissues of wild boar (Sus scrofa) from the Sierra Nevada Natural Space (SNNS) (southern Spain). Heavy metal concentrations in livers, kidneys and bones from 111 animals were determined by inductively coupled plasma optical emission spectrometry (ICP-OES). Bones and kidneys were the most Pb- and Cd-contaminated tissues, respectively; Cd concentrations were 5.6 times higher in kidneys than in livers. This is the first biomonitoring study of these pollutants in wild boar tissues in the SNNS, and findings indicate that this population is chronically exposed to these heavy metals. The detected Pb and Cd concentrations were lower than those found in many studies performed in Europe on the same species. PMID:27178294

  9. Time-dependent biodistribution, clearance and biocompatibility of magnetic fibrin nanoparticles: an in vivo study.

    PubMed

    Prabu, Periyathambi; Vedakumari, Weslen S; Sastry, Thotapalli P

    2015-06-01

    Recently, bioretention and toxicity of injected nanoparticles in the body has drawn much attention in biomedical research. In the present study, 5 mg Fe per kg body weight of magnetic fibrin nanoparticles (MFNPs) were injected into mice intravenously and investigated for their blood clearance profile, biodistribution, haematology and pathology studies for a time period of 28 days. Moderately long circulation of MFNPs in blood was observed with probable degradation and excretion into the bloodstream via monoatomic iron forms. Inductively coupled plasma optical emission spectrometry (ICP-OES) and Prussian blue staining results showed increased accumulation of MFNPs in the liver, followed by spleen and other organs. Body weight, spleen/thymus indexes, haematology, serum biochemistry and histopathology studies demonstrated that MFNPs were biocompatible. These results suggest the feasibility of using MFNPs for drug delivery and imaging applications.

  10. Lead and cadmium in wild boar (Sus scrofa) in the Sierra Nevada Natural Space (southern Spain).

    PubMed

    Mulero, Rocío; Cano-Manuel, Javier; Ráez-Bravo, Arián; Pérez, Jesús M; Espinosa, José; Soriguer, Ramón; Fandos, Paulino; Granados, José E; Romero, Diego

    2016-08-01

    The aims of the present study were to investigate Pb and Cd levels in tissues of wild boar (Sus scrofa) from the Sierra Nevada Natural Space (SNNS) (southern Spain). Heavy metal concentrations in livers, kidneys and bones from 111 animals were determined by inductively coupled plasma optical emission spectrometry (ICP-OES). Bones and kidneys were the most Pb- and Cd-contaminated tissues, respectively; Cd concentrations were 5.6 times higher in kidneys than in livers. This is the first biomonitoring study of these pollutants in wild boar tissues in the SNNS, and findings indicate that this population is chronically exposed to these heavy metals. The detected Pb and Cd concentrations were lower than those found in many studies performed in Europe on the same species.

  11. Determining the geographical origin of Sechium edule fruits by multielement analysis and advanced chemometric techniques.

    PubMed

    Hidalgo, Melisa J; Fechner, Diana C; Marchevsky, Eduardo J; Pellerano, Roberto G

    2016-11-01

    This paper describes the determination and evaluation of the major and trace element composition (Al, As, Ba, Ca, Cd, Co, Cu, Fe, K, Mg, Mn, Na, Pb, Sr and Zn) of Sechium edule (Jacq) Swartz fruits collected from four different places of production in Corrientes province, Argentina. Element concentrations were determined by using inductively coupled plasma optical emission spectrometry (ICP OES) after microwave digestion. The accuracy was confirmed with standard reference material of spinach leaves (NIST, 1570a) and spiking tests. Principal component analysis (PCA), linear discriminant analysis (LDA), k-nearest neighbors (kNN), partial least square-discriminant analysis (PLS-DA) and support vector machine (SVM) were applied to the results for discriminating the geographical origin of S. edule fruits. Finally, the LDA method was found to perform best with up to 90% accuracy rate based on the following elements: Ca, Ba, Cu, Mn, Na, Sr, and Zn.

  12. Mineral profile of kaki fruits (Diospyros kaki L.).

    PubMed

    Mir-Marqués, Alba; Domingo, Ana; Cervera, M Luisa; de la Guardia, Miguel

    2015-04-01

    The main objective of this study was the determination of the mineral profile of 167 kaki fruit (Diospyros kaki L.) samples produced from different regions of Spain, including samples with the protected designation of origin (PDO) 'Kaki Ribera del Xúquer' Valencia (Spain). Samples were analysed by inductively coupled plasma optical emission spectroscopy (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). Consumption of one piece of kaki fruit (200-400 g) would give a mineral intake providing 1-10% of the recommended daily allowance (RDA) for calcium, 1-30% for copper and potassium, 1-15% from iron and magnesium, up to 1% of sodium, and up to 4% of zinc. ANOVA analysis indicates differences between samples from different Spanish region, thus offering a way for authentication of PDO sample origin.

  13. Time-dependent biodistribution, clearance and biocompatibility of magnetic fibrin nanoparticles: an in vivo study

    NASA Astrophysics Data System (ADS)

    Prabu, Periyathambi; Vedakumari, Weslen S.; Sastry, Thotapalli P.

    2015-05-01

    Recently, bioretention and toxicity of injected nanoparticles in the body has drawn much attention in biomedical research. In the present study, 5 mg Fe per kg body weight of magnetic fibrin nanoparticles (MFNPs) were injected into mice intravenously and investigated for their blood clearance profile, biodistribution, haematology and pathology studies for a time period of 28 days. Moderately long circulation of MFNPs in blood was observed with probable degradation and excretion into the bloodstream via monoatomic iron forms. Inductively coupled plasma optical emission spectrometry (ICP-OES) and Prussian blue staining results showed increased accumulation of MFNPs in the liver, followed by spleen and other organs. Body weight, spleen/thymus indexes, haematology, serum biochemistry and histopathology studies demonstrated that MFNPs were biocompatible. These results suggest the feasibility of using MFNPs for drug delivery and imaging applications.

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

    SciTech Connect

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

    2012-09-11

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

  15. 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

  16. Determination of inorganic pollutants in soil after volatilization using microwave-induced combustion

    NASA Astrophysics Data System (ADS)

    Picoloto, Rochele S.; Wiltsche, Helmar; Knapp, Günter; Mello, Paola A.; Barin, Juliano S.; Flores, Erico M. M.

    2013-08-01

    Microwave-induced combustion (MIC) was applied for analyte volatilization from soil and subsequent determination of As, Cd and Pb by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES), and Hg by cold vapor generation inductively coupled plasma mass spectrometry (CVG-ICP-MS). Soil samples (up to 300 mg) were mixed with microcrystalline cellulose, pressed as pellets and combusted in closed quartz vessels pressurized with 20 bar O2. Analytes were volatilized from soil during combustion and quantitatively absorbed in a suitable solution: nitric acid (1, 2, 4 or 6 mol L- 1) or a solution of nitric (2 mol L- 1) and hydrochloric (1, 2 or 4 mol L- 1) acids. Accuracy was evaluated using certified reference materials of soil (NIST 2709, San Joaquin Soil) and sediment (SUD-1, Sudbury sediment for trace elements). Agreement with certified values was better than 95% (t-test, 95% confidence level) for all analytes when 6 mL of a solution of 2 mol L- 1 HNO3 and 2 mol L- 1 HCl was used with a reflux step of 5 min. The limit of detection was 0.010, 0.002, 0.009 and 0.012 μg g- 1 for As, Cd, Hg and Pb, respectively using ICP-MS determination. A clear advantage of the proposed method over classical approaches is that only diluted solution is used. Moreover, a complete separation of the analytes from matrix is achieved minimizing potential interferences in ICP-MS or ICP-OES determination. Up to eight samples can be digested in a single run of only 25 min, resulting in a solution suitable for the determination of all analytes by both techniques.

  17. Elucidation of the binding sites of two novel Ru(II) complexes on bovine serum albumin.

    PubMed

    Nišavić, Marija; Masnikosa, Romana; Butorac, Ana; Perica, Kristina; Rilak, Ana; Korićanac, Lela; Hozić, Amela; Petković, Marijana; Cindrić, Mario

    2016-06-01

    Hyphenated mass spectrometry (MS) techniques have attained an important position in analysis of covalent and non-covalent interactions of metal complexes with peptides and proteins. The aim of the present study was to qualitatively and quantitatively determine ruthenium binding sites on a protein using tandem mass spectrometry and allied techniques, i.e. liquid chromatography (LC) and inductively coupled plasma optical emission spectrometry (ICP-OES). For that purpose, two newly synthesized Ru(II) complexes of a meridional geometry, namely mer-[Ru(4' Cl-tpy)(en)Cl](+) (1) and mer-[Ru(4' Cl-tpy)(dach)Cl](+) (2) (where 4' Cl-tpy=4'-chloro-2,2':6',2″-terpyridine, en=1,2-diaminoethane and dach=1,2-diaminocyclohexane), and bovine serum albumin were used. The binding of the complexes to the protein was investigated by means of size exclusion- and reversed phase-LC, ICP OES, matrix-assisted laser desorption ionization MS and MS/MS. Ruthenated peptide sequence and a binding target amino acid were revealed through accurate elucidation of MS/MS spectra. The results obtained in this study suggest a high binding capacity of the protein towards both complexes, with up to 5.77±0.14 and 6.95±0.43mol of 1 and 2 bound per mol of protein, respectively. The proposed binding mechanism for the selected complexes includes the release of Cl ligand, its replacement with water molecule and further coordination to electron donor histidine residue.

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

    PubMed

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

    2010-10-01

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

  19. Simultaneous determination of bromine and iodine in milk powder for adult and infant nutrition by plasma based techniques after digestion using microwave-induced combustion

    NASA Astrophysics Data System (ADS)

    Picoloto, Rochele S.; Doneda, Morgana; Flores, Eder L. M.; Mesko, Marcia F.; Flores, Erico M. M.; Mello, Paola A.

    2015-05-01

    In this work, bromine and iodine determination in milk powder for adult and infant nutrition was performed by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES) after digestion by microwave-induced combustion (MIC). Contrarily to previous works using MIC, a higher sample mass was digested (700 mg). Water and ammonium hydroxide (10 to 100 mmol L- 1) were investigated as absorbing solutions and accurate results were achieved using a 25 mmol L- 1 NH4OH solution. Moreover, the high stability of analytes after digestion (up to 30 days) using this solution was observed. The accuracy of the proposed MIC method was evaluated using certified and reference materials of milk powder (NIST 1549 and NIST 8435). No statistical difference was observed between results obtained by MIC-ICP-MS and reference values. Results for samples were also compared with those obtained by ICP-OES and no statistical difference was observed. Microwave-assisted alkaline extraction (MW-AE) was also evaluated for milk powder using NH4OH and tetramethylammonium hydroxide solutions. Solutions obtained after digestion by MIC (whole milk powder) presented low carbon content in digests (< 25 mg L- 1) while solutions obtained after alkaline extraction presented up to 10,000 mg L- 1 of C. MIC method was preferable in view of the possibility of obtaining solutions with low carbon content even using a relatively high sample mass (up to 700 mg) avoiding additional dilution prior to ICP-MS analysis, thus allowing better detection limits. Limits of detection obtained by MIC-ICP-MS were 0.007 and 0.003 μg g- 1 for Br and I, respectively, while for MW-AE were 0.1 and 0.05 μg g- 1 respectively for Br and I. Among the main advantages of the proposed method are the use of diluted alkaline solutions that is in agreement with green analytical chemistry recommendations, the high stability of analytes in solution and the suitability of digests for

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

    NASA Astrophysics Data System (ADS)

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

    2013-10-01

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

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

    PubMed

    Poitevin, Eric

    2012-01-01

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

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

    PubMed

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

    2006-09-29

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

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

    PubMed

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

    2006-09-29

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

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

    NASA Astrophysics Data System (ADS)

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

    2007-09-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1998-08-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2005-06-01

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

  7. Laser ablation in liquids as a new technique of sampling in elemental analysis of solid materials

    NASA Astrophysics Data System (ADS)

    Muravitskaya, E. V.; Rosantsev, V. A.; Belkov, M. V.; Ershov-Pavlov, E. A.; Klyachkovskaya, E. V.

    2009-02-01

    Laser ablation in liquid media is considered as a new sample preparation technique in the elemental composition analysis of materials using optical emission spectroscopy of inductively coupled plasma (ICP-OES). Solid samples are transformed into uniform colloidal solutions of nanosized analyte particles using laser radiation focused onto the sample surface. High homogeneity of the resulting solution allows performing the ICP-OES quantitative analysis especially for the samples, which are poorly soluble in acids. The technique is compatible with the conventional solution-based standards.

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

    NASA Astrophysics Data System (ADS)

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

    1996-01-01

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

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

    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.

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

    USGS Publications Warehouse

    Hopkins, D.M.

    1991-01-01

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

  11. Evaluation of sample preparation methods for elastomer digestion for further halogens determination.

    PubMed

    Moraes, Diogo P; Pereira, Juliana S F; Diehl, Liange O; Mesko, Márcia F; Dressler, Valderi L; Paniz, José Neri G; Knapp, Guenter; Flores, Erico M M

    2010-05-01

    In this work, three sample preparation methods were evaluated for further halogen determination in elastomers containing high concentrations of carbon black. Samples of nitrile-butadiene rubber, styrene-butadiene rubber, and ethylene-propylene-diene monomer elastomers were decomposed using oxygen flask combustion and microwave-induced combustion (MIC) for further Br and Cl determination by ion chromatography (IC), inductively coupled plasma optical emission spectrometry (ICP OES), and inductively coupled plasma mass spectrometry (ICP-MS). Extraction assisted by microwave radiation in closed vessels was also evaluated using water or alkaline solution. Digestion by MIC was carried out using 50 mmol l(-1) (NH(4))(2)CO(3) as the absorbing solution. The effect of the reflux step was also evaluated. Accuracy was evaluated using certified reference materials with polymeric matrix composition and by comparison of results using neutron activation analysis. Agreement for Br and Cl was better than 95% by MIC using 5 min of reflux, and no statistical difference was found using IC, ICP OES, and ICP-MS for determination of both analytes. For MIC, the relative standard deviation (RSD) was lower than 5%. Using extraction in closed vessels, a high amount of residues was observed, and recoveries were lower than 45% for both analytes. For oxygen flask combustion, the agreement was similar using MIC but RSD was higher (20%). The residual carbon content, an important parameter used to evaluate the digestion efficiency, was always below 1% for MIC. Using MIC, it was possible to digest elastomers with high efficiency, resulting in a single solution suitable for halogen determination by different techniques. PMID:20135306

  12. Evaluation of sample preparation methods for elastomer digestion for further halogens determination.

    PubMed

    Moraes, Diogo P; Pereira, Juliana S F; Diehl, Liange O; Mesko, Márcia F; Dressler, Valderi L; Paniz, José Neri G; Knapp, Guenter; Flores, Erico M M

    2010-05-01

    In this work, three sample preparation methods were evaluated for further halogen determination in elastomers containing high concentrations of carbon black. Samples of nitrile-butadiene rubber, styrene-butadiene rubber, and ethylene-propylene-diene monomer elastomers were decomposed using oxygen flask combustion and microwave-induced combustion (MIC) for further Br and Cl determination by ion chromatography (IC), inductively coupled plasma optical emission spectrometry (ICP OES), and inductively coupled plasma mass spectrometry (ICP-MS). Extraction assisted by microwave radiation in closed vessels was also evaluated using water or alkaline solution. Digestion by MIC was carried out using 50 mmol l(-1) (NH(4))(2)CO(3) as the absorbing solution. The effect of the reflux step was also evaluated. Accuracy was evaluated using certified reference materials with polymeric matrix composition and by comparison of results using neutron activation analysis. Agreement for Br and Cl was better than 95% by MIC using 5 min of reflux, and no statistical difference was found using IC, ICP OES, and ICP-MS for determination of both analytes. For MIC, the relative standard deviation (RSD) was lower than 5%. Using extraction in closed vessels, a high amount of residues was observed, and recoveries were lower than 45% for both analytes. For oxygen flask combustion, the agreement was similar using MIC but RSD was higher (20%). The residual carbon content, an important parameter used to evaluate the digestion efficiency, was always below 1% for MIC. Using MIC, it was possible to digest elastomers with high efficiency, resulting in a single solution suitable for halogen determination by different techniques.

  13. Single event mass spectrometry

    DOEpatents

    Conzemius, Robert J.

    1990-01-16

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

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

    PubMed

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

    2014-09-01

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

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

    PubMed

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

    2009-05-15

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

  16. Environmental impact of volcanic emissions at Nyiragongo (DRC)

    NASA Astrophysics Data System (ADS)

    Scaglione, Sarah; Calabrese, Sergio; Bobrowski, Nicole; Giuffrida, Giovanni; D'Alessandro, Walter; Brusca, Lorenzo; Bellomo, Sergio; Liotta, Marcello; Minani, Abel; Shamavu, Patient; Pandolfo, Francesco; Tedesco, Dario

    2015-04-01

    The large amount of trace elements emitted from volcanoes has a strong impact on the close surrounding areas. Nyiragongo Volcano (Democratic Republic of Congo) belongs to the Virunga volcanic chain and is one of the most active volcanoes in Africa. It is characterized by the presence of an active and permanent lava lake with a persistent degassing activity. During a field trip in October-November 2014, we investigated the impact of the volcanogenic deposition in the surrounding of the crater by using different sampling techniques. Rain-gauges were used to collect atmospheric bulk deposition. Active and passive biomonitoring techniques (moss-bags and leaves of endemic plants - Senecio spp. and Amarantus viridis) were applied in order to investigate the dispersion of volcanic gas and particle emissions. We collected daily rainfall events at various sites: seven samples at the crater rim (on the western and southern side, 3470 m a.s.l.), one sample at the village Kibati (south-eastern flank, 1955 m a.s.l.) located at the up-wind base of the volcano (representing the local background), and four samples in the city of Goma (southern flank of the volcano, 1500 m a.s.l.). In order to implement our dataset, several samples of rainwater, amaranth leaves, soils and atmospheric depositions (by moss-bags and filters exposition) were sampled after the field trip by the researchers of the Goma Volcano Observatory (GVO). Since, the prevalent wind direction was blowing the plume in westerly or southwesterly direction, we exposed the raingauges in the villages of Bulengo, Rusayo and Kingi in the southwestern side respect to the volcano, and Kibumba in the southesthern as a background site, at increasing distance from the rim. In the same sites, leaves of Amarantus viridis, which is one of the principal vegetables eaten by the local population, were collected. Rainwater, moss bags and plant samples were analyzed for major and trace elements by IC, ICP-OES and ICP-MS. The large

  17. Effect of gallium on growth of Streptococcus mutans NCTC 10449 and dental tissues.

    PubMed

    Valappil, S P; Owens, G J; Miles, E J; Farmer, N L; Cooper, L; Miller, G; Clowes, R; Lynch, R J M; Higham, S M

    2014-01-01

    Gallium-doped phosphate-based glasses (Ga-PBG) were assessed for their impact on Streptococcus mutans and dental mineralisation, firstly by disc diffusion assays followed by biofilms grown on nitrocellulose filter membrane (NFM) and constant-depth film fermentor (CDFF). Short-time exposure (10 min) effects of Ga-PBG on S. mutans biofilm were compared with that of 0.2% chlorhexidine. The effects of Ga-PBG on bovine enamel (which was investigated under pH-cycling condition) and dentine were analysed using transverse microradiography (TMR), profilometry and inductively coupled plasma optical-emission spectrometry (ICP-OES). The disc diffusion assays showed inhibition zones of 24.5 ± 0.5 mm for Ga-PBG compared with controls (C-PBG). Ga-PBG showed statistically significant growth inhibition of S. mutans biofilms on NFM (p = 0.001) and CDFF (p < 0.046) compared with hydroxyapatite (HA) and C-PBG. The CDFF assay revealed a maximum of 2.11 log colony-forming unit (CFU) reduction at 48 h, but short-time exposure effects were comparable with that of 0.2% chlorhexidine only on older biofilms (maximum of 0.59 vs. 0.69 log CFU reduction at 120 h). TMR analyses of the enamel revealed non-significant mineral loss (p = 0.37) only in the case of Ga-PBG samples compared with controls including sodium fluoride. ICP-OES analyses indicated transient gallium adsorption into dentine by calcium displacement. The results confirmed that gallium inhibited S. mutans growth and appears to have the potential to protect the enamel surface under conditions representative of the oral environment. Further work is needed to establish whether it has an application in daily oral hygiene procedures to prevent or reduce caries.

  18. A Practical Approach to Determination of Elements by ICP and ED-XRF in Coastal Waters and Processed Seawaters of East Sea in Korea

    NASA Astrophysics Data System (ADS)

    Yoon, H.; Shin, M.; Yoon, C.; Park, C.; Sim, Y.; Kim, S.; Lee, J.; Chung, K.

    2006-12-01

    A direct analytical technique has been extensively studied for the use as correct estimation of recoverable Eco-elements in seawater and three processed seawaters from East Sea of Korea and Hanjoo Co. Ltd. We have been developing techniques to retrieve valuable elements such as lithium, boron, bromine, strontium, magnesium...etc' from seawater. This is R&D project named "Recovering the Valuable Minerals from Seawater and Sand" has been supported for many years by the Ministry of Maritime Affairs & Fisheries (MOMAF) of Korea. Testing the reliability of recovery technique now has become a major interest and achieving low-level detection limits is requested before launching the commercial pilot plant. In this study, two kinds of analytical techniques, ICP-OES and ED-XRF were examined to develop a rapid and simple method in seawater analysis for commercial purposes. Inductively coupled plasma Optical Emission Spectrometry (ICP-OES, Ultima2C, Jobin Yvon) method is preferred for the analysis of the low levels of elements found in high matrix environmental samples such as seawater. High matrix solutions are frequently affected in analyte response during instrumental analysis as the concentration of major component changed drastically. To overcome such a complication during standard sample preparation and a better application in pilot plant, a modified matrix matching standard addition method was developed and the reliability was checked carefully. Along this, ED-XRF Spectrometer (Epsilon5, PANalytical) was used in this study. This Epsilon5 spectrometer implements the 3-dimensional polarizing technique. The primary Gd-anode X-ray tube, secondary targets and measuring position are arranged in 3- dimensional space. In this way it completely removes background that may arise from primary X-ray beam scattering and thus vastly improves signal to noise ratio during seawater analysis. We found this correction method is especially useful where there are difficulties in measuring

  19. Effect of gallium on growth of Streptococcus mutans NCTC 10449 and dental tissues.

    PubMed

    Valappil, S P; Owens, G J; Miles, E J; Farmer, N L; Cooper, L; Miller, G; Clowes, R; Lynch, R J M; Higham, S M

    2014-01-01

    Gallium-doped phosphate-based glasses (Ga-PBG) were assessed for their impact on Streptococcus mutans and dental mineralisation, firstly by disc diffusion assays followed by biofilms grown on nitrocellulose filter membrane (NFM) and constant-depth film fermentor (CDFF). Short-time exposure (10 min) effects of Ga-PBG on S. mutans biofilm were compared with that of 0.2% chlorhexidine. The effects of Ga-PBG on bovine enamel (which was investigated under pH-cycling condition) and dentine were analysed using transverse microradiography (TMR), profilometry and inductively coupled plasma optical-emission spectrometry (ICP-OES). The disc diffusion assays showed inhibition zones of 24.5 ± 0.5 mm for Ga-PBG compared with controls (C-PBG). Ga-PBG showed statistically significant growth inhibition of S. mutans biofilms on NFM (p = 0.001) and CDFF (p < 0.046) compared with hydroxyapatite (HA) and C-PBG. The CDFF assay revealed a maximum of 2.11 log colony-forming unit (CFU) reduction at 48 h, but short-time exposure effects were comparable with that of 0.2% chlorhexidine only on older biofilms (maximum of 0.59 vs. 0.69 log CFU reduction at 120 h). TMR analyses of the enamel revealed non-significant mineral loss (p = 0.37) only in the case of Ga-PBG samples compared with controls including sodium fluoride. ICP-OES analyses indicated transient gallium adsorption into dentine by calcium displacement. The results confirmed that gallium inhibited S. mutans growth and appears to have the potential to protect the enamel surface under conditions representative of the oral environment. Further work is needed to establish whether it has an application in daily oral hygiene procedures to prevent or reduce caries. PMID:24335164

  20. Facile synthesis of ultrasmall monodisperse ``raisin-bun''-type MoO3/SiO2 nanocomposites with enhanced catalytic properties

    NASA Astrophysics Data System (ADS)

    Wang, Jiasheng; Li, Xin; Zhang, Shufen; Lu, Rongwen

    2013-05-01

    We report the preparation of ultrasmall monodisperse MoO3/SiO2 nanocomposites in reverse microemulsions formed by Brij-58/cyclohexane/water. The nanocomposites are of ``raisin-bun''-type with 1.0 +/- 0.2 nm MoO3 homogeneously dispersed in 23 +/- 2 nm silica spheres. Characterization is carried out based on transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectrometry (EDS), X-ray powder diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma-optical emission spectrometry (ICP-OES), N2 sorption measurement, and NH3 temperature-programmed desorption (NH3-TPD). The as-prepared MoO3/SiO2 nanocomposites are microporous and exhibit enhanced catalytic activities for acetalization of benzaldehyde with ethylene glycol and can be repeatedly used 5 times without obvious deactivation. The catalytic performance improvement is attributed to the unique structure and ultrasmall size of the nanocomposites.We report the preparation of ultrasmall monodisperse MoO3/SiO2 nanocomposites in reverse microemulsions formed by Brij-58/cyclohexane/water. The nanocomposites are of ``raisin-bun''-type with 1.0 +/- 0.2 nm MoO3 homogeneously dispersed in 23 +/- 2 nm silica spheres. Characterization is carried out based on transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectrometry (EDS), X-ray powder diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma-optical emission spectrometry (ICP-OES), N2 sorption measurement, and NH3 temperature-programmed desorption (NH3-TPD). The as-prepared MoO3/SiO2 nanocomposites are microporous and exhibit enhanced catalytic activities for acetalization of benzaldehyde with ethylene glycol and can be repeatedly used 5 times without obvious deactivation. The catalytic performance improvement is attributed to the unique

  1. Nuclear Magnetic Resonance Spectrometry.

    ERIC Educational Resources Information Center

    Wasson, John R.; Salinas, Jorge E.

    1980-01-01

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

  2. Mass spectrometry in India.

    PubMed

    Vairamani, M; Prabhakar, S

    2012-01-01

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

  3. Method of trivalent chromium concentration determination by atomic spectrometry

    DOEpatents

    Reheulishvili, Aleksandre N.; Tsibakhashvili, Neli Ya.

    2006-12-12

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

  4. Plasma-based determination of inorganic contaminants in waste of electric and electronic equipment after microwave-induced combustion

    NASA Astrophysics Data System (ADS)

    Mello, Paola A.; Diehl, Lisarb O.; Oliveira, Jussiane S. S.; Muller, Edson I.; Mesko, Marcia F.; Flores, Erico M. M.

    2015-03-01

    A systematic study was performed for the determination of inorganic contaminants in polymeric waste from electrical and electronic equipment (EEE) for achieving an efficient digestion to minimize interferences in determination using plasma-based techniques. The determination of As, Br, Cd, Co, Cr, Cu, Ni, Pb, Sb, and Zn by inductively coupled plasma mass spectrometry (ICP-MS) and also by inductively coupled plasma optical emission spectrometry (ICP OES) was carried out after digestion using microwave-induced combustion (MIC). Arsenic and Hg were determined by flow-injection chemical vapor generation inductively coupled plasma mass spectrometry (FI-CVG-ICP-MS). Dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) with ammonia was also used for Cr determination. The suitability of MIC for digestion of sample masses up to 400 mg was demonstrated using microcrystalline cellulose as aid for combustion of polymers from waste of EEEs that usually contain flame retardants that impair the combustion. The composition and concentration of acid solutions (HNO3 or HNO3 plus HCl) were evaluated for metals and metalloids and NH4OH solutions were investigated for Br absorption. Accuracy was evaluated by comparison of results with those obtained using high pressure microwave-assisted wet digestion (HP-MAWD) and also by the analysis of certified reference material (CRM) of polymer (EC680k-low-density polyethylene). Bromine determination was only feasible using digestion by MIC once losses were observed when HP-MAWD was used. Lower limits of detection were obtained for all analytes using MIC (from 0.005 μg g- 1 for Co by ICP-MS up to 3.120 μg g-1 for Sb by ICP OES) in comparison to HP-MAWD due to the higher sample mass that can be digested (400 mg) and the use of diluted absorbing solutions. The combination of HNO3 and HCl for digestion showed to be crucial for quantitative recovery of some elements, as Cr and Sb. In addition, suitable agreement of Cr to

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

    USGS Publications Warehouse

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

    2011-01-01

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

  6. Data on copper level in the blood of patients with normal and abnormal angiography.

    PubMed

    Amiri, Leila; Movahed, Ali; Iranpour, Dariush; Ostovar, Afshin; Raeisi, Alireza; Keshtkar, Mozhgan; Hajian, Najmeh; Dobaradaran, Sina

    2016-12-01

    In this data article, we measured the levels of copper in the blood of patients undergoing coronary angiography. The samples were taken from patients with cardiovascular disease in Bushehr׳s university hospital, Iran. Patients were divided in two groups: normal angiography and abnormal angiography. After the chemical digestion of samples, the concentration levels of Cu in both groups were determined by using inductively coupled plasma optical spectrometry (ICP-OES). PMID:27622204

  7. Forensic Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Hoffmann, William D.; Jackson, Glen P.

    2015-07-01

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

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

    PubMed

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

    2013-09-01

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

  9. Fourier transform mass spectrometry.

    PubMed

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

    2011-07-01

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

  10. Environmental Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Lebedev, Albert T.

    2013-06-01

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

  11. Fourier Transform Mass Spectrometry

    PubMed Central

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

    2011-01-01

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

  12. Ion Mobility Spectrometry (IMS) and Mass Spectrometry

    SciTech Connect

    Shvartsburg, Alexandre A.

    2010-04-20

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

  13. Ambient ionization mass spectrometry

    NASA Astrophysics Data System (ADS)

    Lebedev, A. T.

    2015-07-01

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

  14. Nanostructured inorganic materials: Synthesis and associated electrochemical properties

    NASA Astrophysics Data System (ADS)

    Yau, Shali Zhu

    Synthetic strategy for preparing potential battery materials at low temperature was developed. Magnetite (Fe3O4), silver hollandnite (AgxMn8O16), magnesium manganese oxide (MgxMnO 2˙yH2O), and silver vanadium phosphorous oxide (Ag 2VO2PO4) were studied. Magnetite (Fe3O4) was prepared by coprecipitation induced by triethylamine from aqueous iron(II) and iron(III) chloride solutions of varying concentrations. Variation of the iron(II) and iron(III) concentrations results in crystallite size control of the Fe3O4 products. Materials characterization of the Fe3O4 samples is reported, including Brunauer-Emmitt-Teller (BET) surface area, x-ray powder diffraction (XRD), transmission electron microscopy (TEM), particle size, and saturation magnetization results. A strong correlation between discharge capacity and voltage recovery behavior versus crystallite size was observed when tested as an electrode material in lithium electrochemical cells. Silver hollandite (AgxMn8O16) was successfully synthesized through a low temperature reflux reaction. The crystallite size and silver content of AgxMn8O16 by varying the reactant ratio of silver permanganate (AgMnO4) and manganese sulfate monohydrate (MnSO4˙H2O). Silver hollandite was characterized by Brunauer-Emmitt-Teller (BET) surface area, inductively coupled plasma-optical emission (ICP-OES) spectrometry, helium pycnometry, simultaneous thermogravimetric analysis/differential scanning calorimetry (TGA/DSC), and x-ray powder diffraction (XRD). The crystallite size showed a strong correlation with silver content, BET surface area, and particle sizes. The silver hollandite cathode showed good discharge capacity retention in 30 cycles of discharge-charge. There were a good relationship between crystallite size and rate capability and pulse ability. Magnesium manganese oxide (MgxMnO2˙yH 2O) was made by redox reaction by mixing sodium hydroxide (NaOH), manganese sulfate monohydrate (MnSO4˙HO2), and potassium persulfate (K2S2O8

  15. Analytical mass spectrometry

    SciTech Connect

    Not Available

    1990-01-01

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

  16. Analytical mass spectrometry. Abstracts

    SciTech Connect

    Not Available

    1990-12-31

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

  17. MASS SPECTROMETRY IN ENVIRONMENTAL SCIENCES

    EPA Science Inventory

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

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

    PubMed

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

    2012-03-16

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

  19. Synthesis of mesoporous Mn/TiO2 nanocomposites and investigating the photocatalytic properties in aqueous systems.

    PubMed

    Oseghe, Ekemena Oghenovoh; Ndungu, Patrick Gathura; Jonnalagadda, Sreekanth Babu

    2015-01-01

    Mesoporous 20 wt% Mn/TiO2 nanocomposites were synthesized adopting modified sol-gel method at different pH (pH = 2, 7 and 11) conditions and calcined at 400 °C. Based on the characteristics of the 20 wt% Mn/TiO2 nanocomposites synthesized at pH 11, same procedure was adopted for the synthesis of different wt% Mn/TiO2. The nanocomposite samples and their surface properties were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), mapping, inductively coupled plasma optical emission spectrometry (ICP-OES), Fourier transform infrared (FTIR), and fluorescence spectrometry. The nanocomposites existed in the anatase phase of TiO2 with no peak assigned to Mn on the diffractogram. The photocatalytic activities of the materials were evaluated by monitoring degradation of a model dye (methylene blue (MB)) in presence of visible light and ozone. The nanocomposite synthesized under neutral condition (pH = 7) exhibited the best photocatalytic activity resulting from its relatively smaller crystal size (5.98 nm) and larger pore volume (0.30 cm(3)/g). One percentage of weight Mn/TiO2 showed 100% decolouration of MB in the presence of O3 after 100 min.

  20. TiO2/SiO2 porous composite thin films: Role of TiO2 areal loading and modification with gold nanospheres on the photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Levchuk, Irina; Sillanpää, Mika; Guillard, Chantal; Gregori, Damia; Chateau, Denis; Parola, Stephane

    2016-10-01

    The aim of the work was to study photocatalytic activity of composite TiO2/Au/SiO2 thin films. Coatings were prepared using sol-gel technique. Physicochemical parameters of coatings were characterized using UV-vis spectrometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectrometry (XPS), inductively coupled plasma optical emission spectroscopy (ICP-OES), ellipsometry, tactile measurements, goniometry and diffuse reflectance measurements. The photocatalytic activity of the films was tested in batch mode using aqueous solution of formic acid. Changes of formic acid concentration were determined by means of high pressure liquid chromatography (HPLC). Increase of initial degradation rate of formic acid was detected for TiO2/Au/SiO2 films with gold nanoparticle's load 0.5 wt.% and 1.25 wt.%. However, deeper insights using more detailed characterization of these coatings demonstrated that the improvement of the photocatalytic activity is more probably attributed to an increase in the areal loading of TiO2.

  1. Assessing the suitability of Norway spruce wood as an environmental archive for sulphur.

    PubMed

    Barrelet, T; Ulrich, A; Rennenberg, H; Zwicky, C N; Krähenbühl, U

    2008-12-01

    The aim of this study was to assess the suitability of Norway spruces (Picea abies L. Karst.) as an environmental archive for sulphur. For this purpose spruce trees were sampled in two distinct regions of Switzerland: the Alps and the Swiss Plateau, which differ significantly with respect to S immission. Wood samples were measured using two methods: LASER Ablation high resolution inductively coupled plasma mass spectrometry (LA-HR-ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES) after acid digestion. Independently corroborated by previous measurements of sulphur in peat bogs, the rise and fall of sulphur dioxide pollution in Switzerland appears to be reflected in spruce wood sulphur content. While the wood sulphur content profile of trees sampled in the Alps is relatively flat, the profiles of trees located on the Swiss Plateau display a characteristic sulphur peak. This corresponds to air pollution data in the different regions and indicates that the trees reacted on the changing S supply and recorded a pollution signal in the wood.

  2. Determination of trace elements in petroleum products by inductively coupled plasma techniques: A critical review

    NASA Astrophysics Data System (ADS)

    Sánchez, Raquel; Todolí, José Luis; Lienemann, Charles-Philippe; Mermet, Jean-Michel

    2013-10-01

    The fundamentals, applications and latter developments of petroleum products analysis through inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are revisited in the present bibliographic survey. Sample preparation procedures for the direct analysis of fuels by using liquid sample introduction systems are critically reviewed and compared. The most employed methods are sample dilution, emulsion or micro-emulsion preparation and sample decomposition. The first one is the most widely employed due to its simplicity. Once the sample has been prepared, an organic matrix is usually present. The performance of the sample introduction system (i.e., nebulizer and spray chamber) depends strongly upon the nature and properties of the solution finally obtained. Many different devices have been assayed and the obtained results are shown. Additionally, samples can be introduced into the plasma by using an electrothermal vaporization (ETV) device or a laser ablation system (LA). The recent results published in the literature showing the feasibility, advantages and drawbacks of latter alternatives are also described. Therefore, the main goal of the review is the discussion of the different approaches developed for the analysis of crude oil and its derivates by inductively coupled plasma (ICP) techniques.

  3. Potential Health Risk of Herbal Distillates and Decoctions Consumption in Shiraz, Iran.

    PubMed

    Moore, F; Akhbarizadeh, R; Keshavarzi, B; Tavakoli, F

    2015-10-01

    Concentration of 26 elements in 16 different herbal distillates and 5 herbal decoctions, were determined using inductively coupled plasma-mass spectrometry (ICP-MS). The elemental content of five raw herbal materials used for making decoctions and seven distilled and boiled residues were also evaluated by inductively coupled plasma optical emission spectrometry (ICP-OES). The results indicated that herbal products display a wide range of elemental concentrations. Compared with world health regulations, the concentrations of the elements in herbal distillates and decoctions did not exceed the recommended limits. The analysis of herbal extracts did not show a significant transfer of toxic elements during decoction preparation. Comparison of elemental content among fresh herbal material and herbal distillate and decoction of the same herb showed that, besides the elemental abundance of herbal organs, the ionic potential of elements also play an important role in elemental content of herbal products. Based on the results of the research, it seems that most health benefits attributed to herbal products (especially herbal distillates) are more related to their organic compounds rather than elemental composition. Calculated hazard quotient (HQ) and hazard index (HI) were used to evaluate the noncarcinogenic health risk from individual and combined metals via daily consumption of 100 ml of herbal distillates and 250 ml of herbal decoctions. Both HQs and HI through consumption of herbal distillates and herbal decoctions (except Valerian) were below 1. Apparently, daily consumption of herbal distillates and decoctions at the indicated doses poses no significant health risk to a normal adult. PMID:25778835

  4. Methodological aspects of in vitro assessment of bio-accessible risk element pool in urban particulate matter.

    PubMed

    Sysalová, Jiřina; Száková, Jiřina; Tremlová, Jana; Kašparovská, Kateřina; Kotlík, Bohumil; Tlustoš, Pavel; Svoboda, Petr

    2014-11-01

    In vitro tests simulating the elements release from inhaled urban particulate matter (PM) with artificial lung fluids (Gamble's and Hatch's solutions) and simulated gastric and pancreatic solutions were applied for an estimation of hazardous element (As, Cd, Cr, Hg, Mn, Ni, Pb and Zn) bio-accessibility in this material. An inductively coupled plasma optical emission spectrometry (ICP-OES) and an inductively coupled plasma mass spectrometry (ICP-MS) were employed for the element determination in extracted solutions. The effect of the extraction agent used, extraction time, sample-to-extractant ratio, sample particle size and/or individual element properties was evaluated. Different patterns of individual elements were observed, comparing Hatch's solution vs. simulated gastric and pancreatic solutions. For Hatch's solution, a decreasing sample-to-extractant ratio in a PM size fraction of <0.063 mm resulted in increasing leached contents of all investigated elements. As already proved for other operationally defined extraction procedures, the extractable element portions are affected not only by their mobility in the particulate matter itself but also by the sample preparation procedure. Results of simulated in vitro tests can be applied for the reasonable estimation of bio-accessible element portions in the particulate matter as an alternative method, which, consequently, initiates further examinations including potential in vivo assessments.

  5. Pretreatment and integrated analysis of spectral data reveal seaweed similarities based on chemical diversity.

    PubMed

    Wei, Feifei; Ito, Kengo; Sakata, Kenji; Date, Yasuhiro; Kikuchi, Jun

    2015-03-01

    Extracting useful information from high dimensionality and large data sets is a major challenge for data-driven approaches. The present study was aimed at developing novel integrated analytical strategies for comprehensively characterizing seaweed similarities based on chemical diversity. The chemical compositions of 107 seaweed and 2 seagrass samples were analyzed using multiple techniques, including Fourier transform infrared (FT-IR) and solid- and solution-state nuclear magnetic resonance (NMR) spectroscopy, thermogravimetry-differential thermal analysis (TG-DTA), inductively coupled plasma-optical emission spectrometry (ICP-OES), CHNS/O total elemental analysis, and isotope ratio mass spectrometry (IR-MS). The spectral data were preprocessed using non-negative matrix factorization (NMF) and NMF combined with multivariate curve resolution-alternating least-squares (MCR-ALS) methods in order to separate individual component information from the overlapping and/or broad spectral peaks. Integrated analysis of the preprocessed chemical data demonstrated distinct discrimination of differential seaweed species. Further network analysis revealed a close correlation between the heavy metal elements and characteristic components of brown algae, such as cellulose, alginic acid, and sulfated mucopolysaccharides, providing a componential basis for its metal-sorbing potential. These results suggest that this integrated analytical strategy is useful for extracting and identifying the chemical characteristics of diverse seaweeds based on large chemical data sets, particularly complicated overlapping spectral data.

  6. Depleted uranium mobility across a weapons testing site: isotopic investigation of porewater, earthworms, and soils.

    PubMed

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

    2008-12-15

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

  7. Facile synthesis of ultrasmall monodisperse "raisin-bun"-type MoO3/SiO2 nanocomposites with enhanced catalytic properties.

    PubMed

    Wang, Jiasheng; Li, Xin; Zhang, Shufen; Lu, Rongwen

    2013-06-01

    We report the preparation of ultrasmall monodisperse MoO3/SiO2 nanocomposites in reverse microemulsions formed by Brij-58/cyclohexane/water. The nanocomposites are of "raisin-bun"-type with 1.0 ± 0.2 nm MoO3 homogeneously dispersed in 23 ± 2 nm silica spheres. Characterization is carried out based on transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectrometry (EDS), X-ray powder diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma-optical emission spectrometry (ICP-OES), N2 sorption measurement, and NH3 temperature-programmed desorption (NH3-TPD). The as-prepared MoO3/SiO2 nanocomposites are microporous and exhibit enhanced catalytic activities for acetalization of benzaldehyde with ethylene glycol and can be repeatedly used 5 times without obvious deactivation. The catalytic performance improvement is attributed to the unique structure and ultrasmall size of the nanocomposites. PMID:23613166

  8. In vitro permeation of platinum through African and Caucasian skin.

    PubMed

    Franken, A; Eloff, F C; du Plessis, J; Badenhorst, C J; Du Plessis, J L

    2015-02-01

    The majority of the South African workforce are Africans, therefore potential racial differences should be considered in risk and exposure assessments in the workplace. Literature suggests African skin to be a superior barrier against permeation and irritants. Previous in vitro studies on metals only included skin from Caucasian donors, whereas this study compared the permeation of platinum through African and Caucasian skin. A donor solution of 0.3 mg/ml of potassium tetrachloroplatinate (K₂PtCl₄) dissolved in synthetic sweat was applied to the vertical Franz diffusion cells with full thickness abdominal skin. Skin from three female African and three female Caucasian donors were included (n=21). The receptor solution was removed at various intervals during the 24 h experiment, and analysed with high resolution inductively coupled plasma-mass spectrometry (ICP-MS). Skin was digested and analysed by inductively coupled plasma-optical emission spectrometry (ICP-OES). Significantly higher permeation of platinum through intact African skin (p=0.044), as well as a significantly higher mass of platinum retention in African skin in comparison with Caucasian skin (p=0.002) occurred. Significant inter-donor variation was found in both racial groups (p<0.02). Results indicate that African workers have increased risk of dermal permeation and therefore possible sensitisation caused by dermal exposure to platinum salts. These results are contradictory to limited literature suggesting a superior barrier in African skin and further investigation is necessary to explain the higher permeation through African skin.

  9. A novel solid-state fractionation of naphthenic acid fraction components from oil sands process-affected water.

    PubMed

    Mohamed, Mohamed H; Wilson, Lee D; Shah, Jaimin R; Bailey, Jon; Peru, Kerry M; Headley, John V

    2015-10-01

    Various sorbent materials were evaluated for the fractionation of naphthenic acid fraction components (NAFCs) from oil sand process-affected water (OSPW). The solid phase materials include activated carbon (AC), cellulose, iron oxides (magnetite and goethite), polyaniline (PANI) and three types of biochar derived from biomass (BC-1; rice husks, BC-2; acacia low temperature and BC-3; acacia high temperature). NAFCs were semi-quantified using electrospray ionization high resolution Orbitrap mass spectrometry (ESI-MS) and the metals were assessed by inductively coupled plasma optical emission spectrometry (ICP-OES). The average removal efficacy of NAFCs by AC was 95%. The removal efficacy decreased in the following order: AC, BC-1>BC-2, BC-3, goethite>PANI>cellulose, magnetite. The removal of metals did not follow a clear trend; however, there was notable leaching of potassium by AC and biochar samples. The bound NAFCs by AC were desorbed efficiently with methanol. Methanol regeneration and recycling of AC revealed 88% removal on the fourth cycle; a 4.4% decrease from the first cycle. This fractionation method represents a rapid, cost-effective, efficient, and green strategy for NAFCs from OSPW, as compared with conventional solvent extraction. PMID:26042363

  10. Chemical Elemental Distribution and Soil DNA Fingerprints Provide the Critical Evidence in Murder Case Investigation

    PubMed Central

    Concheri, Giuseppe; Bertoldi, Daniela; Polone, Elisa; Otto, Stefan; Larcher, Roberto; Squartini, Andrea

    2011-01-01

    Background The scientific contribution to the solution of crime cases, or throughout the consequent forensic trials, is a crucial aspect of the justice system. The possibility to extract meaningful information from trace amounts of samples, and to match and validate evidences with robust and unambiguous statistical tests, are the key points of such process. The present report is the authorized disclosure of an investigation, carried out by Attorney General appointment, on a murder case in northern Italy, which yielded the critical supporting evidence for the judicial trial. Methodology/Principal Findings The proportional distribution of 54 chemical elements and the bacterial community DNA fingerprints were used as signature markers to prove the similarity of two soil samples. The first soil was collected on the crime scene, along a corn field, while the second was found in trace amounts on the carpet of a car impounded from the main suspect in a distant location. The matching similarity of the two soils was proven by crossing the results of two independent techniques: a) elemental analysis via inductively coupled plasma mass spectrometry (ICP-MS) and optical emission spectrometry (ICP-OES) approaches, and b) amplified ribosomal DNA restriction analysis by gel electrophoresis (ARDRA). Conclusions Besides introducing the novel application of these methods to forensic disciplines, the highly accurate level of resolution observed, opens new possibilities also in the fields of soil typing and tracking, historical analyses, geochemical surveys and global land mapping. PMID:21674041

  11. Methodological aspects of in vitro assessment of bio-accessible risk element pool in urban particulate matter.

    PubMed

    Sysalová, Jiřina; Száková, Jiřina; Tremlová, Jana; Kašparovská, Kateřina; Kotlík, Bohumil; Tlustoš, Pavel; Svoboda, Petr

    2014-11-01

    In vitro tests simulating the elements release from inhaled urban particulate matter (PM) with artificial lung fluids (Gamble's and Hatch's solutions) and simulated gastric and pancreatic solutions were applied for an estimation of hazardous element (As, Cd, Cr, Hg, Mn, Ni, Pb and Zn) bio-accessibility in this material. An inductively coupled plasma optical emission spectrometry (ICP-OES) and an inductively coupled plasma mass spectrometry (ICP-MS) were employed for the element determination in extracted solutions. The effect of the extraction agent used, extraction time, sample-to-extractant ratio, sample particle size and/or individual element properties was evaluated. Different patterns of individual elements were observed, comparing Hatch's solution vs. simulated gastric and pancreatic solutions. For Hatch's solution, a decreasing sample-to-extractant ratio in a PM size fraction of <0.063 mm resulted in increasing leached contents of all investigated elements. As already proved for other operationally defined extraction procedures, the extractable element portions are affected not only by their mobility in the particulate matter itself but also by the sample preparation procedure. Results of simulated in vitro tests can be applied for the reasonable estimation of bio-accessible element portions in the particulate matter as an alternative method, which, consequently, initiates further examinations including potential in vivo assessments. PMID:25123460

  12. Assessing the suitability of Norway spruce wood as an environmental archive for sulphur.

    PubMed

    Barrelet, T; Ulrich, A; Rennenberg, H; Zwicky, C N; Krähenbühl, U

    2008-12-01

    The aim of this study was to assess the suitability of Norway spruces (Picea abies L. Karst.) as an environmental archive for sulphur. For this purpose spruce trees were sampled in two distinct regions of Switzerland: the Alps and the Swiss Plateau, which differ significantly with respect to S immission. Wood samples were measured using two methods: LASER Ablation high resolution inductively coupled plasma mass spectrometry (LA-HR-ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES) after acid digestion. Independently corroborated by previous measurements of sulphur in peat bogs, the rise and fall of sulphur dioxide pollution in Switzerland appears to be reflected in spruce wood sulphur content. While the wood sulphur content profile of trees sampled in the Alps is relatively flat, the profiles of trees located on the Swiss Plateau display a characteristic sulphur peak. This corresponds to air pollution data in the different regions and indicates that the trees reacted on the changing S supply and recorded a pollution signal in the wood. PMID:18534728

  13. Final report of the key comparison CCQM-K88: Determination of lead in lead-free solder containing silver and copper

    NASA Astrophysics Data System (ADS)

    Hioki, Akiharu; Nonose, Naoko; Liandi, Ma; Jingbo, Chao; Liuxing, Feng; Chao, Wei; Haeng Cho, Kyung; Suh, Jung Ki; Min, Hyung Sik; Lim, Youngran; Recknagel, Sebastian; Koenig, Maren; Vogl, Jochen; Caciano de Sena, Rodrigo; dos Reis, Lindomar Augusto; Borinsky, Mónica; Puelles, Mabel; Hatamleh, Nadia; Acosta, Osvaldo; Turk, Gregory; Rabb, Savelas; Sturgeon, Ralph; Methven, Brad; Rienitz, Olaf; Jaehrling, Reinhard; Konopelko, L. A.; Kustikov, Yu A.; Kozyreva, S. B.; Korzh, A. A.

    2013-01-01

    The CCQM-K88 key comparison was organized by the Inorganic Analysis Working Group of CCQM to test the abilities of the national metrology institutes to measure the mass fraction of lead in lead-free solder containing silver and copper. National Metrology Institute of Japan (NMIJ), National Institute of Metrology of China (NIM) and Korea Research Institute of Standards and Science (KRISS) acted as the coordinating laboratories. The participants used different measurement methods, though most of them used inductively coupled plasma optical emission spectrometry (ICP-OES) or isotope-dilution inductively coupled plasma mass spectrometry (ID-ICP-MS). Accounting for relative expanded uncertainty, comparability of measurement results was successfully demonstrated by the participating NMIs for the measurement of the mass fraction of lead in lead-free solder at the level of 200 mg/kg. It is expected that metals at mass fractions greater than approximately 100 mg/kg in lead-free solder containing silver and copper can be determined by each participant using the same technique(s) employed for this key comparison to achieve similar uncertainties mentioned in the present report. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

  14. Long-term in vivo clearance of gadolinium-based AGuIX nanoparticles and their biocompatibility after systemic injection.

    PubMed

    Sancey, Lucie; Kotb, Shady; Truillet, Charles; Appaix, Florence; Marais, Arthur; Thomas, Eloïse; van der Sanden, Boudewijn; Klein, Jean-Philippe; Laurent, Blandine; Cottier, Michèle; Antoine, Rodolphe; Dugourd, Philippe; Panczer, Gérard; Lux, François; Perriat, Pascal; Motto-Ros, Vincent; Tillement, Olivier

    2015-03-24

    We previously reported the synthesis of gadolinium-based nanoparticles (NPs) denoted AGuIX (activation and guiding of irradiation by X-ray) NPs and demonstrated their potential as an MRI contrast agent and their efficacy as radiosensitizing particles during X-ray cancer treatment. Here we focus on the elimination kinetics of AGuIX NPs from the subcellular to whole-organ scale using original and complementary methods such as laser-induced breakdown spectroscopy (LIBS), intravital two-photon microscopy, inductively coupled plasma optical emission spectrometry (ICP-OES), transmission electron microscopy (TEM), and electrospray ionization mass spectrometry (ESI-MS). This combination of techniques allows the exact mechanism of AGuIX NPs elimination to be elucidated, including their retention in proximal tubules and their excretion as degraded or native NPs. Finally, we demonstrated that systemic AGuIX NP administration induced moderate and transient effects on renal function. These results provide useful and promising preclinical information concerning the safety of theranostic AGuIX NPs.

  15. XRF scanners as a quick screening tool for detecting toxic pollutant elements in sediments from Marín harbour in the Ría de Pontevedra (NW Spain).

    PubMed

    Rodríguez-Germade, I; Rubio, B; Rey, D

    2014-09-15

    X-ray fluorescence scanners, such as the Itrax™ Core Scanner (Itrax) (Cox Analytical Systems, Mölndal, Sweden), provide high-resolution geochemical data within several hours. However, the semi-quantitative nature of these analysers has hampered their use to study pollution. This study explores Itrax's capabilities to detect trace metals, such as Hg and Cd, in the Ría de Pontevedra harbour (NW Spain). A set of Itrax detection levels were proposed for each metal after comparison with quantitative measurements obtained from Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) and Vapour Atomic Absorption Spectrometry (CVAAS) analyses. These quantitative data obtained after a sequential extraction were used to evaluate pollutant bioavailability and to determine metal pollution levels exhibiting Hg pollution. The reliability of inc/coh and Br/Cl ratios to assess the total organic matter variability was also evaluated. The results indicated that the Itrax is an efficient and fast option to monitor contamination, thereby avoiding laborious discrete analyses and reducing analytical cost and time.

  16. Potential Health Risk of Herbal Distillates and Decoctions Consumption in Shiraz, Iran.

    PubMed

    Moore, F; Akhbarizadeh, R; Keshavarzi, B; Tavakoli, F

    2015-10-01

    Concentration of 26 elements in 16 different herbal distillates and 5 herbal decoctions, were determined using inductively coupled plasma-mass spectrometry (ICP-MS). The elemental content of five raw herbal materials used for making decoctions and seven distilled and boiled residues were also evaluated by inductively coupled plasma optical emission spectrometry (ICP-OES). The results indicated that herbal products display a wide range of elemental concentrations. Compared with world health regulations, the concentrations of the elements in herbal distillates and decoctions did not exceed the recommended limits. The analysis of herbal extracts did not show a significant transfer of toxic elements during decoction preparation. Comparison of elemental content among fresh herbal material and herbal distillate and decoction of the same herb showed that, besides the elemental abundance of herbal organs, the ionic potential of elements also play an important role in elemental content of herbal products. Based on the results of the research, it seems that most health benefits attributed to herbal products (especially herbal distillates) are more related to their organic compounds rather than elemental composition. Calculated hazard quotient (HQ) and hazard index (HI) were used to evaluate the noncarcinogenic health risk from individual and combined metals via daily consumption of 100 ml of herbal distillates and 250 ml of herbal decoctions. Both HQs and HI through consumption of herbal distillates and herbal decoctions (except Valerian) were below 1. Apparently, daily consumption of herbal distillates and decoctions at the indicated doses poses no significant health risk to a normal adult.

  17. Occurrence, distribution, and ecological risk assessment of potentially toxic elements in surface sediments of Lake Awassa and Lake Ziway, Ethiopia.

    PubMed

    Mekonnen, Kebede N; Ambushe, Abayneh A; Chandravanshi, Bhagwan S; Redi-Abshiro, Mesfin; McCrindle, Robert I

    2015-01-01

    Microwave-assisted acid digestion and modified aqua regia (HNO3:HCl:HF:H3BO3) leaching techniques were used for the determination of 15 potentially toxic elements (V, Cr, Fe, Mn, Co, Ni, Cu, Zn, As, Se, Ag, Cd, Sn, Hg and Pb) in sediment samples from Lake Awassa and Lake Ziway, Ethiopia. The digests were subsequently analyzed by inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-optical emission spectrometry (ICP-OES). Mercury was directly determined in the solid samples using an elemental mercury analyzer. The precision and accuracy of the digestion procedures were verified using certified reference materials. The experimental results were in good agreement with the certified values (P < 0.05) and the recoveries were quantitative (>90%). The average relative standard deviations were below 10%. There is significant correlation between the two lakes at the 0.01 level (2-tailed). Using the sediment quality guidelines, both lakes are heavily polluted with Zn and some of the sites are heavily polluted with Cu, Ni and Pb. Based on effect range low (ERL) - effect range medium (ERM), in both lakes for Ag were greater than the ERM, indicating that the areas could be toxic to aquatic organisms, while for Cr, Cu, As and Hg the values were less than ERL. PMID:25438135

  18. Toxic and nutrient elements in yerba mate (Ilex paraguariensis).

    PubMed

    Pozebon, Dirce; Dressler, Valderi Luiz; Marcelo, Marcelo Caetano Alexandre; de Oliveira, Tiago Charão; Ferrão, Marco Flores

    2015-01-01

    Toxic and nutrient elements were investigated in yerba mate (Ilex paraguariensis) from South America. Fifty-four brands of commercialised yerba mate from Argentina, Brazil, Paraguay and Uruguay were analysed for Al, Ba, Ca, Cu, Fe, K, Mg, Mn, P, Sr, and Zn, using inductively coupled plasma optical emission spectrometry (ICP-OES), and Li, Be, Ti, V, Cr, Ni, Co, As, Se, Rb, Mo, Ag, Cd, Sb, La, Ce, Pb, Bi and U using inductively coupled plasma mass spectrometry (ICP-MS). Antimony, Se, Ag and Bi were not detected in any sample whereas the limits of detection (LODs) of these elements were 0.19, 0.40, 0.003 and 0.001 μg g(-1), respectively. Analysis of variance (ANOVA) revealed that the concentrations of Cd, Ti, Ni, As, Mo, U, Li and Be in yerba mate were not statistically different with regard to the country of origin, while those of the other investigated elements differed. PMID:26125226

  19. Long-term in vivo clearance of gadolinium-based AGuIX nanoparticles and their biocompatibility after systemic injection.

    PubMed

    Sancey, Lucie; Kotb, Shady; Truillet, Charles; Appaix, Florence; Marais, Arthur; Thomas, Eloïse; van der Sanden, Boudewijn; Klein, Jean-Philippe; Laurent, Blandine; Cottier, Michèle; Antoine, Rodolphe; Dugourd, Philippe; Panczer, Gérard; Lux, François; Perriat, Pascal; Motto-Ros, Vincent; Tillement, Olivier

    2015-03-24

    We previously reported the synthesis of gadolinium-based nanoparticles (NPs) denoted AGuIX (activation and guiding of irradiation by X-ray) NPs and demonstrated their potential as an MRI contrast agent and their efficacy as radiosensitizing particles during X-ray cancer treatment. Here we focus on the elimination kinetics of AGuIX NPs from the subcellular to whole-organ scale using original and complementary methods such as laser-induced breakdown spectroscopy (LIBS), intravital two-photon microscopy, inductively coupled plasma optical emission spectrometry (ICP-OES), transmission electron microscopy (TEM), and electrospray ionization mass spectrometry (ESI-MS). This combination of techniques allows the exact mechanism of AGuIX NPs elimination to be elucidated, including their retention in proximal tubules and their excretion as degraded or native NPs. Finally, we demonstrated that systemic AGuIX NP administration induced moderate and transient effects on renal function. These results provide useful and promising preclinical information concerning the safety of theranostic AGuIX NPs. PMID:25703068

  20. Pretreatment and integrated analysis of spectral data reveal seaweed similarities based on chemical diversity.

    PubMed

    Wei, Feifei; Ito, Kengo; Sakata, Kenji; Date, Yasuhiro; Kikuchi, Jun

    2015-03-01

    Extracting useful information from high dimensionality and large data sets is a major challenge for data-driven approaches. The present study was aimed at developing novel integrated analytical strategies for comprehensively characterizing seaweed similarities based on chemical diversity. The chemical compositions of 107 seaweed and 2 seagrass samples were analyzed using multiple techniques, including Fourier transform infrared (FT-IR) and solid- and solution-state nuclear magnetic resonance (NMR) spectroscopy, thermogravimetry-differential thermal analysis (TG-DTA), inductively coupled plasma-optical emission spectrometry (ICP-OES), CHNS/O total elemental analysis, and isotope ratio mass spectrometry (IR-MS). The spectral data were preprocessed using non-negative matrix factorization (NMF) and NMF combined with multivariate curve resolution-alternating least-squares (MCR-ALS) methods in order to separate individual component information from the overlapping and/or broad spectral peaks. Integrated analysis of the preprocessed chemical data demonstrated distinct discrimination of differential seaweed species. Further network analysis revealed a close correlation between the heavy metal elements and characteristic components of brown algae, such as cellulose, alginic acid, and sulfated mucopolysaccharides, providing a componential basis for its metal-sorbing potential. These results suggest that this integrated analytical strategy is useful for extracting and identifying the chemical characteristics of diverse seaweeds based on large chemical data sets, particularly complicated overlapping spectral data. PMID:25647718

  1. Essential metals profile of the hair and nails of patients with laryngeal cancer.

    PubMed

    Golasik, Magdalena; Przybyłowicz, Agnieszka; Woźniak, Anna; Herman, Małgorzata; Gawęcki, Wojciech; Golusiński, Wojciech; Walas, Stanisław; Krejpcio, Zbigniew; Szyfter, Krzysztof; Florek, Ewa; Piekoszewski, Wojciech

    2015-01-01

    Trace elements have an impact on numerous physiological processes. The monitoring of their levels in the organism allows you to detect not only their deficiencies, but also several illnesses. The aim of this study was to compare the levels of essential elements (calcium, magnesium, zinc, copper, iron, manganese) in hair, nails and serum of both patients with laryngeal cancer and healthy people. The determination of six metals was performed by an inductively coupled plasma mass spectrometry (ICP-MS) and an inductively coupled plasma optical emission spectrometry (ICP-OES). The concentration of essential elements in hair and nails of the control group was statistically significantly higher than in the group of patients with laryngeal cancer. In the case of serum, differences were found between the patients and controls in respect of the level of three metals. The results of principal component analysis (PCA) revealed the strong and similar clustering behavior of essential elements in hair and nails. The metals did not correlate between two alternative materials. The present study indicated that, using the level of essential elements in hair and nails as a basis, it is possible to distinguish cancer patients from healthy people. The alternative materials are independent of homeostasis and therefore seem to be more useful in the detection of diseases and mineral deficiencies in human than the classical biological materials, such as blood.

  2. Depleted uranium mobility across a weapons testing site: isotopic investigation of porewater, earthworms, and soils.

    PubMed

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

    2008-12-15

    The mobility and bioavailability of depleted uranium (DU) in soils at a UK Ministry of Defence (UK MoD) weapons testing range were investigated. Soil and vegetation were collected near a test-firing position and at eight points along a transect line extending approximately 200 m down-slope, perpendicular to the firing line, toward a small stream. Earthworms and porewaters were subsequently separated from the soils and both total filtered porewater (<0.2 microm) and discrete size fractions (0.2 microm-100 kDa, 100-30 kDa, 30-3 kDa, and <3 kDa)obtainedvia centrifugal ultrafiltration were examined. Uranium concentrations were determined by inductively coupled plasma optical emission spectrometry (ICP-OES) for soils and ICP-mass spectrometry (MS) for earthworms and porewaters, while 235U:238U atom ratios were determined by multicollector (MC)-ICP-MS. Comparison of the porewater and earthworm isotopic values with those of the soil solids indicated that DU released into the environment during weapons test-firing operations was more labile and more bioavailable than naturally occurring U in the soils at the testing range. Importantly, DU was shown to be present in soil porewater even at a distance of approximately 185 m from the test-firing position and, along the extent of the transect was apparently associated with organic colloids. PMID:19174886

  3. A new technique for trace elemental analysis of speleothems using microbeam xrf

    NASA Astrophysics Data System (ADS)

    Buckles, J.; Rowe, H.; Gao, Y.; Cheng, H.; Edwards, R. L.; Springer, G.; Hardt, B.

    2012-04-01

    Trace element ratios in speleothems (Sr/Ca, Mg/Ca, Ba/Ca) have been used to interpret the hydrogeochemical processes in the epikarst zone as well as the partitioning that occurs at the calcite-water interface. During periods of low rainfall, trace element ratios generally increase as a result of the longer residence time of water in the soil and epikarst zones. High-resolution time series analyses of these elements in speleothems provide evidence for changing paleohydrological and geochemical conditions over time. The conventional methods of trace metal analysis of speleothems- Laser Ablation Inductively-Coupled Plasma Mass Spectrometry (LA-ICPMS) and Inductively-Coupled Plasma Optical Emission Spectroscopy (ICP-OES) have yielded many high-quality data sets. However, these methods can be expensive, time-consuming, and require the destruction - either by ablation, micro-milling, or powdering of speleothem samples. The many caveats of these conventional methods have led to the search for a viable alternative - one that will provide the same high-resolution result, but that is affordable, rapid, and non-destructive. Presented here are trace element analysis results using microbeam X-ray Fluorescence Spectrometry. The Brüker-AXS ARTAX microbeam XRF spectrometer permits a multi-element analysis from Na to U with a spatial resolution of 70 µm. The method is non-contact and non-destructive, therefore preserving the sample for additional analyses (e.g. stable isotopes). A simple calibration method for Sr/Ca using pressed mixed powders will be described. It will be demonstrated that microbeam XRF is an important tool in trace element analysis of speleothems and a viable alternative to conventional methods. Sr/Ca ratios were obtained for multiple speleothems and serve as a preliminary test of microbeam XRF suitability. Analyses of variable count times, temporal and spatial reproducibility along transects, and a comparison between microbeam XRF spectra and ICP-OES spectra

  4. Laser ablation in liquids: an efficient sample preparation technique in ICP elemental analysis of art materials

    NASA Astrophysics Data System (ADS)

    Klyachkovskaya, E. V.; Kozhukh, N. M.; Muravitskaya, E. V.; Rosantsev, V. A.; Belkov, M. V.; Ershov-Pavlov, E. A.

    2007-06-01

    Laser ablation in liquid media is proposed as a new sample preparation technique in elemental composition analysis of art pigments using inductively coupled plasma optical emission spectroscopy (ICP-OES). Solid samples are transformed to colloidal solutions of nanosized analyte particles. This makes the technique compatible with convevtional solutionbased standardization. The dissociation of particles in solution is improved, which increases the accuracy of quantitative ICP measurements.

  5. Hydrogen Exchange Mass Spectrometry.

    PubMed

    Mayne, Leland

    2016-01-01

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

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

    USGS Publications Warehouse

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

    1997-01-01

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

  7. Micro-PIXE mapping of mineral distribution in mature grain of two pearl millet cultivars

    NASA Astrophysics Data System (ADS)

    Minnis-Ndimba, R.; Kruger, J.; Taylor, J. R. N.; Mtshali, C.; Pineda-Vargas, C. A.

    2015-11-01

    Micro-proton-induced X-ray emission (micro-PIXE) was used to map the distribution of several nutritionally important minerals found in the grain tissue of two cultivars of pearl millet (Pennisetum glaucum (L.) R. Br.). The distribution maps revealed that the predominant localisation of minerals was within the germ (consisting of the scutellum and embryo) and the outer grain layers (specifically the pericarp and aleurone); whilst the bulk of the endosperm tissue featured relatively low concentrations of the surveyed minerals. Within the germ, the scutellum was revealed as a major storage tissue for P and K, whilst Ca, Mn and Zn were more prominent within the embryo. Fe was revealed to have a distinctive distribution pattern, confined to the dorsal end of the scutellum; but was also highly concentrated in the outer grain layers. Interestingly, the hilar region was also revealed as a site of high accumulation of minerals, particularly for S, Ca, Mn, Fe and Zn, which may be part of a defensive strategy against infection or damage. Differences between the two cultivars, in terms of the bulk Fe and P content obtained via inductively coupled plasma optical emission spectrometry (ICP-OES), concurred with the average concentration data determined from the analysis of micro-PIXE spectra specifically extracted from the endosperm tissue.

  8. Electrical and gas sensing properties of self-aligned copper-doped zinc oxide nanoparticles

    SciTech Connect

    Sonawane, Yogesh S.; Kanade, K.G.; Kale, B.B. Aiyer, R.C.

    2008-10-02

    Electrical and gas sensing properties of nanocrystalline ZnO:Cu, having Cu X wt% (X = 0.0, 0.5, 1.0, and 1.5) in ZnO, in the form of pellet were investigated. Copper chloride and zinc acetate were used as precursors along with oxalic acid as a precipitating reagent in methanol. Material characterization was done by X-ray diffraction (XRD), scanning electron microscopy (SEM), field emission scanning electron microscopy (FE-SEM) and inductive coupled plasma with optical emission spectrometry (ICP-OES). FE-SEM showed the self-aligned Cu-doped ZnO nano-clusters with particles in the range of 40-45 nm. The doping of 0.5% of copper changes the electrical conductivity by an order of magnitude whereas the temperature coefficient of resistance (TCR) reduces with increase in copper wt% in ZnO. The material has shown an excellent sensitivity for the H{sub 2}, LPG and CO gases with limited temperature selectivity through the optimized operating temperature of 130, 190 and 220 deg. C for H{sub 2}, LPG and CO gases, respectively at 625 ppm gas concentration. The %SF was observed to be 1460 for H{sub 2} at 1% Cu doping whereas the 0.5% Cu doping offered %SF of 950 and 520 for CO and LPG, respectively. The response and recovery time was found to be 6 to 8 s and 16 s, respectively.

  9. Mass spectrometry with accelerators.

    PubMed

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

    2011-01-01

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

  10. Spectrometry of nebulae

    NASA Astrophysics Data System (ADS)

    Acker, A.

    2011-04-01

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

  11. Chemometric evaluation of trace metals in Prunus persica L. Batech and Malus domestica from Minićevo (Serbia).

    PubMed

    Alagić, Slađana Č; Tošić, Snežana B; Dimitrijević, Mile D; Petrović, Jelena V; Medić, Dragana V

    2017-02-15

    The samples of spatial soils and different organs of Prunus persica L. Batech and Malus domestica were analyzed by methods such as inductively coupled plasma optical emission spectroscopy (ICP-OES), Hierarchical Cluster Analysis (HCA), One-way ANOVA, and calculation of biological accumulation factors (BAFs) with the aim of investigating whether these methods may help in the evaluation of trace metals in plants, as well as in the estimation of plant bioaccumulation potentials. ICP-OES provided accurate data on present concentrations of Cu, Zn, Pb, As, Cd, and Ni which showed that most concentrations were in normal ranges, except in some cases for Cu, Zn, and As. HCA illustrated nicely various specifics in the distribution of metals in both investigated systems plant-soil. One-way ANOVA pointed successfully on the existing statistical differences between metal concentrations. Calculated BAFs showed that both plants had very low accumulation rates for all elements; they acted as metal excluders.

  12. Chemometric evaluation of trace metals in Prunus persica L. Batech and Malus domestica from Minićevo (Serbia).

    PubMed

    Alagić, Slađana Č; Tošić, Snežana B; Dimitrijević, Mile D; Petrović, Jelena V; Medić, Dragana V

    2017-02-15

    The samples of spatial soils and different organs of Prunus persica L. Batech and Malus domestica were analyzed by methods such as inductively coupled plasma optical emission spectroscopy (ICP-OES), Hierarchical Cluster Analysis (HCA), One-way ANOVA, and calculation of biological accumulation factors (BAFs) with the aim of investigating whether these methods may help in the evaluation of trace metals in plants, as well as in the estimation of plant bioaccumulation potentials. ICP-OES provided accurate data on present concentrations of Cu, Zn, Pb, As, Cd, and Ni which showed that most concentrations were in normal ranges, except in some cases for Cu, Zn, and As. HCA illustrated nicely various specifics in the distribution of metals in both investigated systems plant-soil. One-way ANOVA pointed successfully on the existing statistical differences between metal concentrations. Calculated BAFs showed that both plants had very low accumulation rates for all elements; they acted as metal excluders. PMID:27664673

  13. Instrumental comparison of the determination of Cr³+ uptake by human transferrin.

    PubMed

    Quarles, C Derrick; Brumaghim, Julia L; Marcus, R Kenneth

    2010-12-01

    UV-VIS absorbance, inductively coupled plasma-optical emission spectroscopy (ICP-OES), and particle beam/hollow cathode-optical emission spectroscopy (PB/HC-OES) are presented as techniques for determining Cr³+ loading into transferrin (Tf), with and without Fe³+. The methods are compared based on loading percentages (i.e. 100% loading would be equal to 2 M(n+): 1 Tf) determined for Cr³+ loading into apo-transferrin. Spectral interferences and overlapping LMCT bands cause inaccurate chromium (qualitative) and iron (qualitative and quantitative) results for the UV-VIS absorbance method. The ICP-OES and PB/HC-OES methods are in good agreement providing evidence that the PB/HC-OES method is a valid technique for investigating metal-protein complexes. Maximum Cr³+ loading into apo-transferrin over a 24 h period was determined to be 26.8 3.5% by the ICP-OES method and 25.3 2.2% by the PB/HC-OES method. Loading percentages were increased to 49.7 1.9% (ICP-OES) and 55.7 3.2% (PB/HC-OES) when the metal-transferrin solution was allowed to incubate for up to 10 days. Under non-excess carbonate conditions the Cr³+ loading is elevated over a 24 h incubation time, but under physiological conditions the loading is inhibited. Equal loading of Fe³+ and Cr³+ into apo-transferrin was achieved when chromium was at a level more than 5 times in excess of iron. Inhibition of Cr³+ loading was only observed when an excess of Fe³+ was available to bind into apo-transferrin. The ability for Cr³+ to displace Fe3+ from holo-transferrin was observed as small amounts of Cr³+ were loaded into the once occupied metal binding site.

  14. "Magic" Ionization Mass Spectrometry.

    PubMed

    Trimpin, Sarah

    2016-01-01

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

  15. "Magic" Ionization Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Trimpin, Sarah

    2016-01-01

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

  16. "Magic" Ionization Mass Spectrometry.

    PubMed

    Trimpin, Sarah

    2016-01-01

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

  17. Concurrent Sr/Ca Ratios and Bomb Test 14C Records from a Porites evermanni Colony on Kure Atoll: SST, Climate Change, Ocean Circulation and Management Applications

    NASA Astrophysics Data System (ADS)

    Covarrubias, S.; Potts, D.; Siciliano, D.; Andrews, A.; Franks, R.

    2013-12-01

    Coral reefs near their latitudinal and ecological limits may be affected disproportionately by global climate changes, especially by changing sea surface temperatures (SST's). One such reef is Kure Atoll, the northernmost reef in the Hawaiian chain. Kure Atoll experiences dramatic temperature and seasonal differences throughout the year. Tracking these fluctuations is important for understanding recent physical forces affecting coral growth in such marginal reefs, and for predicting likely responses to future climate and oceanic changes. We used Sr/Ca ratios of a 50cm Porites evermanni coral core collected in Kure (September 2002) as a SST proxy for reconstructing a temperature timescale spanning the length of the core (~62 years). After cutting a 5 mm thick slab through the center growth axis and X-raying it to identify annual density banding, we extracted 4 equally-spaced samples from each annual increment to quantify, seasonal, inter-annual, and decadal SST patterns. We measured Sr and Ca concentrations by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). We then converted Sr/Ca ratios (mmol/mol) to SST using published equations, and calibrated the more recent SST estimates against satellite-based SST imagery and instrumental records from Midway Atoll (ca. 90 km to SE). We coupled the ICP-OES data with Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) scans along the core to provide higher temporal resolution for interpreting intra-seasonal and inter-seasonal trends. Higher resolution of temperature dating can help us interpret strong inter-seasonal changes not readily seen with low resolution measurements, giving us the ability to track temperature anomalies at interannual and decadal timescales, such as El Niño/Southern Oscillation or La Niña/North Pacific Decadal Oscillation. Further, the SST signature from the Sr/Ca analyses are being used in conjunction with bomb radiocarbon signals in order to establish a complete

  18. Characterization and determination of 28 elements in fly ashes collected in a thermal power plant in Argentina using different instrumental techniques

    NASA Astrophysics Data System (ADS)

    Marrero, Julieta; Polla, Griselda; Jiménez Rebagliati, Raúl; Plá, Rita; Gómez, Darío; Smichowski, Patricia

    2007-02-01

    Different techniques were selected for comprehensive characterization of seven samples of fly ashes collected from the electrostatic precipitator of the San Nicolás thermal power plant (Buenos Aires, Argentina). Particle size was measured using laser based particle size analyzer. X-ray diffraction powder (XRD) analysis and scanning electron microscopy (SEM) were used to characterize the mineral phase present in the matrix consisting basically of aluminosilicates and large amounts of amorphous material. The predominant crystalline phases were mullite and quartz. Major and minors elements (Al, Ca, Cl, Fe, K, Mg, Na, S, Si and Ti) were detected by energy dispersive X-ray analysis (EDAX). Trace elements (As, Cd, Co, Cr, Cu, Mn, Ni, Pb, Se, V and Zn) content was quantified by inductively coupled plasma optical emission spectrometry (ICP OES). Different acid mixtures and digestion procedures were compared for subsequent ICP OES measurements of the dissolved samples. The digestion procedures used were: i) a mixture of FH + HNO 3 + HClO 4 (open system digestion); ii) a mixture of FH + HNO 3 (MW-assisted digestion); iii) a mixture of HF and aqua regia (MW-assisted digestion). Instrumental neutron activation analysis (INAA) was employed for the determination of As, Ba, Co, Cr, Ce, Cs, Eu, Fe, Gd, Hf, La, Lu, Rb, Sb, Sc, Sm, Ta, Tb, Th, U and Yb. The validation of the procedure was performed by the analysis of two certified materials namely, i) NIST 1633b, coal fly ash and ii) GBW07105, rock. Mean elements content spanned from 41870 μg g - 1 for Fe to 1.14 μg g - 1 for Lu. The study showed that Fe (41870 μg g - 1 ) ≫ V (1137 μg g - 1 ) > Ni (269 μg g - 1 ) > Mn (169 μg g - 1 ) are the main components. An enrichment, with respect to crustal average, in many elements was observed especially for As, V and Sb that deserve particular interest from the environmental and human health point of view.

  19. Predictive complexation models of the impact of natural organic matter and cations on scaling in cooling water pipes: A case study of power generation plants in South Africa

    NASA Astrophysics Data System (ADS)

    Bosire, G. O.; Ngila, J. C.; Mbugua, J. M.

    This work discusses simulative models of Ca and Mg complexation with natural organic matter (NOM), in order to control the incidence of scaling in pipes carrying cooling water at the Eskom power generating stations in South Africa. In particular, the paper reports how parameters such as pH and trace element levels influence the distribution of scaling species and their interactions, over and above mineral phase saturation indices. In order to generate modelling inputs, two experimental scenarios were created in the model solutions: Firstly, the trace metals Cu, Pb and Zn were used as markers for Ca and Mg complexation to humic acid and secondly the effect of natural organic matter in cooling water was determined by spiking model solutions. Labile metal ions and total elements in model solutions and water samples were analysed by square wave anodic stripping voltammetry and inductively coupled plasma optical emission spectrometry (ICP-OES), respectively. ICP-OES results revealed high levels of K, Na, S, Mg and Ca and low levels of trace elements (Cd, Se, Pb, Cu, Mn, Mo, Ni, Al and Zn) in the cooling water samples. Using the Tipping and Hurley's database WHAM in PHREEQC format (T_H.DAT), the total elemental concentrations were run as inputs on a PHREEQC code, at pH 6.8 and defined charge as alkalinity (as HCO3-) For model solutions, PHREEQC inputs were based on (i) free metal differences attributed to competitive effect of Ca and the effect of Ca + Mg, respectively; (ii) total Ca and Mg used in the model solutions and (iii) alkalinity described as hydrogen carbonate. Anodic stripping peak heights were used to calculate the concentration of the free/uncomplexed/labile metal ions (used as tracers) in the model solutions. The objective of modelling was to describe scaling in terms of saturation indices of mineral phases. Accordingly, the minerals most likely to generate scale were further simulated (over a range of pH (3-10) to yield results that mimicked changing p

  20. Nickel-based xerogel catalysts: Synthesis via fast sol-gel method and application in catalytic hydrogenation of p-nitrophenol to p-aminophenol

    NASA Astrophysics Data System (ADS)

    Feng, Jin; Wang, Qiang; Fan, Dongliang; Ma, Lirong; Jiang, Deli; Xie, Jimin; Zhu, Jianjun

    2016-09-01

    In order to investigate the roles of three-dimensional network structure and calcium on Ni catalysts, the Ni, Ni-Al2O3, Ni-Ca-Al2O3 xerogel catalysts were successfully synthesized via the fast sol-gel process and chemical reduction method. The crystal structure of three different catalysts was observed with X-ray powder diffraction (XRD). Transmission electron microscopy (TEM), scanning electron microscopy (SEM) and nitrogen adsorption-desorption were employed to investigate the role of network structure of xerogel catalysts and the size distribution of Ni nanoparticles. The catalyst composition was determined by inductively coupled plasma-optical emission spectrometry (ICP-OES) measurement and energy-dispersive X-ray spectroscopy (EDS). Temperature-programmed reduction (TPR) experiments were carried out to investigate the reducibility of nickel species and the interaction between nickel species and alumina. The catalytic hydrogenation of p-nitrophenol to p-aminophenol was investigated over the prepared nickel-based xerogel catalysts. The conversion of p-nitrophenol was monitored by UV spectrophotometry and high performance liquid chromatography (HPLC). The results show that the catalysts are highly selective for the conversion of p-nitrophenol to p-aminophenol and the order of catalytic activities of the catalysts is Ni < Ni-Al2O3 < Ni-Ca-Al2O3. The catalysts were recycled and were used to evaluate the reutilization.

  1. Determination of total chromium in tanned leather samples used in car industry.

    PubMed

    Zeiner, Michaela; Rezić, Iva; Ujević, Darko; Steffan, Ilse

    2011-03-01

    Despite the high competition of synthetic fibers leather is nowadays still widely used for many applications. In order to ensure a sufficient stability of the skin matrix against many factors, such as microbial degradation, heat and sweat, a tanning process is indispensable. Using chromium (III) for this purpose offers a multitude of advantages, thus this way of tanning is widely applied. During the use of chromium tanned leather as clothing material as well as for decoration/covering purposes, chromium is extracted from the leather and may then cause nocuous effects to human skin, e.g. allergic reactions. Thus the knowledge of the total chromium content of leather samples expected to come into prolonged touch with human skin is very important. In car industry leather is used as cover for seats, steering wheel and gearshift lever The chromium contents often chromium tanned leather samples used in car industry were determined. First all samples were dried at 65 degrees C overnight and then cut in small pieces using a ceramic knife, weighed and analyzed by inductively coupled plasma--optical emission spectrometry (ICP-OES) after acidic microwave assisted digestion. The total chromium amounts found were in the range from 19 mg/g up to 32 mg/g. The extraction yield of chromium from leather samples in sweat is approximately 2-7%. Thus especially during long journeys in summer chromium can be extracted in amounts which may cause nocuous effects for example on the palm of the hands or on the back.

  2. Heavy metals contamination in lipsticks and their associated health risks to lipstick consumers.

    PubMed

    Zakaria, Airin; Ho, Yu Bin

    2015-10-01

    This study aimed to determine the heavy metals (lead, cadmium, and chromium) concentration in lipsticks of different price categories sold in the Malaysian market and evaluate the potential health risks due to daily ingestion of heavy metals in lipsticks. A total of 374 questionnaires were distributed to the female staff in a public university in Malaysia in order to obtain information such as brand and price of the lipsticks, body weight, and frequency and duration of wearing lipstick. This information was important for the calculation of hazard quotient (HQ) in health risk assessment. The samples were extracted using a microwave digester and analyzed using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The concentrations of lead, cadmium, and chromium in lipsticks ranged from 0.77 to 15.44 mg kg(-1), 0.06-0.33 mg kg(-1), and 0.48-2.50 mg kg(-1), respectively. There was a significant difference of lead content in the lipsticks of different price categories. There was no significant non-carcinogenic health risk due to the exposure of these heavy metals through lipstick consumption for the prolonged exposure of 35 years (HQ < 1).

  3. Processing and characterization of diatom nanoparticles and microparticles as potential source of silicon for bone tissue engineering.

    PubMed

    Le, Thi Duy Hanh; Bonani, Walter; Speranza, Giorgio; Sglavo, Vincenzo; Ceccato, Riccardo; Maniglio, Devid; Motta, Antonella; Migliaresi, Claudio

    2016-02-01

    Silicon plays an important role in bone formation and maintenance, improving osteoblast cell function and inducing mineralization. Often, bone deformation and long bone abnormalities have been associated with silica/silicon deficiency. Diatomite, a natural deposit of diatom skeleton, is a cheap and abundant source of biogenic silica. The aim of the present study is to validate the potential of diatom particles derived from diatom skeletons as silicon-donor materials for bone tissue engineering applications. Raw diatomite (RD) and calcined diatomite (CD) powders were purified by acid treatments, and diatom microparticles (MPs) and nanoparticles (NPs) were produced by fragmentation of purified diatoms under alkaline conditions. The influence of processing on the surface chemical composition of purified diatomites was evaluated by X-ray photoelectron spectroscopy (XPS). Diatoms NPs were also characterized in terms of morphology and size distribution by transmission electron microscopy (TEM) and Dynamic light scattering (DLS), while diatom MPs morphology was analyzed by scanning electron microscopy (SEM). Surface area and microporosity of the diatom particles were evaluated by nitrogen physisorption methods. Release of silicon ions from diatom-derived particles was demonstrated using inductively coupled plasma optical emission spectrometry (ICP/OES); furthermore, silicon release kinetic was found to be influenced by diatomite purification method and particle size. Diatom-derived microparticles (MPs) and nanoparticles (NPs) showed limited or no cytotoxic effect in vitro depending on the administration conditions.

  4. Multielemental analysis of 20 mushroom species growing near a heavily trafficked road in Poland.

    PubMed

    Mleczek, M; Niedzielski, P; Kalač, P; Budka, A; Siwulski, M; Gąsecka, M; Rzymski, P; Magdziak, Z; Sobieralski, K

    2016-08-01

    The aim of this work was to compare 10 mostly edible aboveground and 10 wood-growing mushroom species collected near a heavily trafficked road (approximately 28,000 vehicles per 24 h) in Poland with regard to their capacity to accumulate 26 trace elements (Ag, Al, As, Au, B, Ba, Bi, Cd, Co, Cr, Cu, Fe, Ga, Ge, In, Li, Mn, Ni, Pb, Re, Sb, Se, Sr, Te, Tl, and Zn) in their fruit bodies in order to illustrate mushroom diversity in element accumulation. All analyses were performed using an inductively coupled plasma optical emission spectrometry (ICP-OES) spectrometer in synchronous dual view mode. The aboveground species had significantly higher levels of 12 elements, including Ag, As, Pb, and Se, compared to the wood-growing species. An opposite relationship was observed only for Au, Ba, and Sr. The results of principal component analysis (PCA) and hierarchical cluster analysis (HCA) implied some new relationships among the analyzed species and elements. Of the analyzed mushroom species, lead content in Macrolepiota procera would seem to pose a health risk; however, at present knowledge regarding lead bioaccessibility from mushrooms is quite limited. PMID:27155831

  5. Assessment and distribution of antimony in soils around three coal mines, Anhui, China

    USGS Publications Warehouse

    Qi, C.; Liu, Gaisheng; Kang, Y.; Lam, P.K.S.; Chou, C.

    2011-01-01

    Thirty-three soil samples were collected from the Luling, Liuer, and Zhangji coal mines in the Huaibei and Huainan areas of Anhui Province, China. The samples were analyzed for antimony (Sb) by inductively coupled plasmaoptical emission spectrometry (ICP-OES) method. The average Sb content in the 33 samples was 4 mg kg-1, which is lower than in coals from this region (6.2 mg kg-1). More than 75% of the soils sampled showed a significant degree of Sb pollution (enrichment factors [EFs] 5-20). The soils collected near the gob pile and coal preparation plant were higher in Sb content than those collected from residential areas near the mines. The gob pile and tailings from the preparation plant were high in mineral matter content and high in Sb. They are the sources of Sb pollution in surface soils in the vicinity of coal mines. The spatial dispersion of Sb in surface soil in the mine region shows that Sb pollution could reach out as far as 350 m into the local environment conditions. Crops in rice paddies may adsorb some Sb and reduce the Sb content in soils from paddyfields. Vertical distribution of Sb in two soil profiles indicates that Sb is normally relatively immobile in soils. ?? 2011 Air & Waste Management Association.

  6. Annual trends in occurrence of submicron particles in ambient air and health risk posed by particle bound metals.

    PubMed

    Izhar, Saifi; Goel, Anubha; Chakraborty, Abhishek; Gupta, Tarun

    2016-03-01

    Risk analysis is highly important in toxicology and public health studies. Health risk related to exposure to toxic metals of PM1 was assessed. Concentrations of 13 heavy metals, adsorbed to submicron particulate matter PM1 were experimentally examined but only 12 metals were found at detectable levels inside IIT Kanpur campus in 2008-2009 for all months excluding June and October. A total of 90 samples collected for 8 h sampling time by a single stage round nozzle, grease impaction substrate based impactor type PM1 sampler were analysed by ICP-OES (Inductively Coupled Plasma Optical Emission Spectrometry). Results showed daily average PM1 concentration is 102.46 ± 35.9 μg/m(3) and metal concentration followed the trend: Ca > Fe > Mg > Zn > Pb > Cu > Cr > Ni > Se > Cd > V > As. Contamination level assessment using geo-accumulation index showed Ca, Fe and Mg exhibited non contamination whereas metals like Cr, Zn, As, Cd, Pb, Se, Ni and Cu exhibited ranges from moderate to extreme contamination. Ingestion is found to be the major exposure pathway for heavy metals. Non-carcinogenic health risk assessment for Pb, Cd and Cr (HI > 1) signified strong chances of adverse impact on children whereas adults are well under safe limit. Cancer Risk for adults and children followed the same decreasing order, Cr(VI)>Cd > Ni > As > Pb. It was found to be higher than permissible limits (10(-6)) for adults and children both.

  7. Development and certification of the new SRM 695 trace elements in multi-nutrient fertilizer

    USGS Publications Warehouse

    MacKey, E.A.; Cronise, M.P.; Fales, C.N.; Greenberg, R.R.; Leigh, S.D.; Long, S.E.; Marlow, A.F.; Murphy, K.E.; Oflaz, R.; Sieber, J.R.; Rearick, M.S.; Wood, L.J.; Yu, L.L.; Wilson, S.A.; Briggs, P.H.; Brown, Z.A.; Budahn, J.; Kane, P.F.; Hall, W.L.

    2007-01-01

    During the past seven years, several states within the US have enacted regulations that limit the amounts of selected non-nutritive elements in fertilizers. Internationally, several countries, including Japan, China, and Australia, and the European Union also limit the amount of selected elements in fertilizers. The elements of interest include As, Cd, Co, Cr, Cu, Hg, Mo, Ni, Pb, Se, and Zn. Fertilizer manufacturers and state regulatory authorities, faced with meeting and verifying these limits, need to develop analytical methods for determination of the elements of concern and to validate results obtained using these methods. Until now, there were no certified reference materials available with certified mass fraction values for all elements of interest in a blended, multi-nutrient fertilizer matrix. A new standard reference material (SRM) 695 trace elements in multi-nutrient fertilizer, has been developed to help meet these needs. SRM 695 has recently been issued with certified mass fraction values for seventeen elements, reference values for an additional five elements, and information values for two elements. The certificate of analysis includes an addendum listing percentage recovery for eight of these elements, determined using an acid-extraction inductively-coupled plasma optical-emission spectrometry (ICP-OES) method recently developed and tested by members of the Association of American Plant Food Control Officials. ?? Springer-Verlag 2007.

  8. Mineral composition, nutritional properties, total phenolics and flavonoids compounds of the atemoya fruit (Annona squamosa L. x Annona cherimola Mill.) and evaluation using multivariate analysis techniques.

    PubMed

    Santos, Walter N L Dos; Sauthier, Maria Celeste S; Cavalcante, Dannuza D; Benevides, Clícia M J; Dias, Fábio S; Santos, Daniele C M B

    2016-09-01

    The atemoya is a hybrid fruit obtained by crossing of cherimoya (Annona cherimola Mill.) with sweet sop (Annona squamosa L.). The information about chemical composition of atemoya is scarce. The mineral composition was evaluated employing Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) and the centesimal composition and the physico-chemical parameters were assessed employing procedures described in the AOAC methods. The total phenolic compounds (TPC) and total flavonoids (TF) were determined using spectroanalytical methods. Considering the Reference Daily Intake (RDI), the concentrations of K, Cu and Vitamin C found in atemoya were the highest, representing about 32, 23 and 37% of the RDI, respectively. The total carbohydrates were 32 g 100g-1 and the soluble solids was equivalent to (32.50 ± 0.03) °Brix. The result for TPC was 540.47 ± 2.32 mgGAE 100 g-1 and the TF was 11.56 ± 1.36 mgQE 100 g-1. The exploratory evaluation of 42 atemoya samples was performed through Principal Component Analysis (PCA), which discriminated green and ripe fruits according to their mineral composition. The elements that contributed most for the variability between green and ripe fruits were: Ba, Ca, Cu, K, Mg and P. PMID:27598843

  9. Determination of exposure to lead of subjects from southwestern Poland by human hair analysis.

    PubMed

    Michalak, Izabela; Wołowiec, Paulina; Chojnacka, Katarzyna

    2014-04-01

    The aim of the present work was to investigate the exposure to lead from various sources by investigation of mineral composition of human scalp hair. The research was carried out on hair sampled from 267 young adults living in Wrocław (southwest Poland). The effect of the place of residence, diet, and lifestyle on lead content in hair was examined by inductively coupled plasma optical emission spectrometry (ICP-OES). Lead was determined at the wavelength 220.353 nm. These outcomes were reached by linking the results of lead level in hair with the results of questionnaire survey. The mean lead level in hair of the whole examined population was 2.01 ± 2.10 mg kg(-1). Lead can enter the human body mainly by inhalation and gastrointestinal absorption. It was found that consuming cheese, fish, and lettuce caused increased level of lead in hair. On the other hand, drinking of milk, tea, coffee, or lemon resulted in decreased content of lead in hair. Additional source of exposure to lead could be cigarette smoking, distance to the traffic road, painting the walls, amalgam filling. Based on the results, it can be concluded that exposure to lead can occur mainly from eating habits and environmental exposure. PMID:24346348

  10. Heavy metals contamination in lipsticks and their associated health risks to lipstick consumers.

    PubMed

    Zakaria, Airin; Ho, Yu Bin

    2015-10-01

    This study aimed to determine the heavy metals (lead, cadmium, and chromium) concentration in lipsticks of different price categories sold in the Malaysian market and evaluate the potential health risks due to daily ingestion of heavy metals in lipsticks. A total of 374 questionnaires were distributed to the female staff in a public university in Malaysia in order to obtain information such as brand and price of the lipsticks, body weight, and frequency and duration of wearing lipstick. This information was important for the calculation of hazard quotient (HQ) in health risk assessment. The samples were extracted using a microwave digester and analyzed using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The concentrations of lead, cadmium, and chromium in lipsticks ranged from 0.77 to 15.44 mg kg(-1), 0.06-0.33 mg kg(-1), and 0.48-2.50 mg kg(-1), respectively. There was a significant difference of lead content in the lipsticks of different price categories. There was no significant non-carcinogenic health risk due to the exposure of these heavy metals through lipstick consumption for the prolonged exposure of 35 years (HQ < 1). PMID:26190304

  11. Laser ablation methods for analysis of urinary calculi: Comparison study based on calibration pellets

    NASA Astrophysics Data System (ADS)

    Štěpánková, K.; Novotný, K.; Vašinová Galiová, M.; Kanický, V.; Kaiser, J.; Hahn, D. W.

    2013-03-01

    Methods based on laser ablation, such as Laser-Induced Breakdown Spectroscopy (LIBS) and Laser-Ablation Inductively Coupled Plasma Mass/Optical Emission Spectrometry (LA-ICP-MS/OES) are particularly suitable for urinary calculi bulk and micro analysis. Investigation of spatial distribution of matrix and trace elements can help to explain their emergence and growth. However, quantification is still very problematic and these methods are often used only for qualitative elemental mapping. There are no commercially available standards, which would correspond to the urinary calculi matrix. Internal standardization is also difficult, mainly due to different crystalline phases in one kidney stone. The aim of this study is to demonstrate the calibration capabilities and examine the limitations of laser ablation based techniques. Calibration pellets were prepared from powdered human urinary calculi with phosphate, oxalate and urate matrix. For this comparative study, the most frequently used laser-ablation based analytical techniques were chosen, such as LIBS and LA-ICP-MS. Moreover, some alternative techniques such as simultaneous LIBS-LA-ICP-OES and laser ablation LA-LIBS were also utilized.

  12. Bioaccumulation of heavy metals in fish and Ardeid at Pearl River Estuary, China.

    PubMed

    Kwok, C K; Liang, Y; Wang, H; Dong, Y H; Leung, S Y; Wong, M H

    2014-08-01

    Sediment, fish (tilapia, Oreochromis mossambicus and snakehead, Channa asiatica), eggs and eggshells of Little Egrets (Egretta garzetta) and Chinese Pond Herons (Ardeola bacchus) were collected from Mai Po Ramsar site of Hong Kong, as well as from wetlands in the Gu Cheng County, Shang Hu County and Dafeng Milu National Nature Reserve of Jiangsu Province, China between 2004 and 2007 (n=3-9). Concentrations of six heavy metals were analyzed, based on inductively coupled plasma optical emission spectrometry (ICP-OES). Significant bioaccumulations of Cd (BAF: 165-1271 percent) were observed in the muscle and viscera of large tilapia and snakehead, suggesting potential health risks to the two bird species, as the fishes are the main preys of waterbirds. Significant (p<0.01) linear relationships were obtained between concentrations of Cd, Cr, Cu, Mn, Pb and Zn in the eggs and eggshells of various Ardeid species, and these regression models were used to extrapolate the heavy metal concentrations in the Ardeid eggs of Mai Po. Extrapolated concentrations are consistent with data in the available literature, and advocate the potential use of these models as a non-invasive sampling method for predicting heavy metal contamination in Ardeid eggs.

  13. Occurrence and distribution of selected heavy metals and boron in groundwater of the Gulf of Khambhat region, Gujarat, India.

    PubMed

    Upadhyaya, Devang; Survaiya, Mayur D; Basha, Shaik; Mandal, Subir K; Thorat, R B; Haldar, Soumya; Goel, Sangita; Dave, Himal; Baxi, Krushnakant; Trivedi, Rohit H; Mody, Kalpana H

    2014-03-01

    The concentration of selected heavy metals, like As, Co, Cr, Cu, Fe, Mn, Ni, Pb, and Zn as well as B, was measured by inductively coupled plasma-optical emission spectrometry (ICP-OES) in groundwater samples from various locations in the Gulf of Khambhat (GoK), an inlet of the Arabian Sea in the state of Gujarat, India, during post-monsoon, winter, and pre-monsoon seasons in a year. Most heavy elements are characterized by low mobility under slightly alkaline and reducing conditions; concentrations in confined aquifers are smaller than the maximum permissible values for drinking water. The temporal changes indicate that a majority of metals is entering the aquifer during monsoon. Principle component analysis of the heavy metal data suggests that Co, Cu, Cd, and Zn are interrelated with each other and derived significantly from anthropogenic route, while input of Pb and Cr may be due to atmospheric deposition in the study area. Both weathering of rocks and anthropogenic input were found to be main sources of elements in the groundwater. The heavy metal levels in groundwaters of the GoK region in comparison with some of the European and Asian sites were higher; however, these metal levels were found to be comparable with few urban sites in the world.

  14. Effect of heavy-metal-resistant bacteria on enhanced metal uptake and translocation of the Cu-tolerant plant, Elsholtzia splendens.

    PubMed

    Xu, Chen; Chen, Xincai; Duan, Dechao; Peng, Cheng; Le, Thu; Shi, Jiyan

    2015-04-01

    A hydroponics trial was employed to study the effects of Pseudomonas putida CZ1 (CZ1), a heavy-metal-resistant bacterial strain isolated from the rhizosphere of Elsholtzia splendens (E. splendens), on the uptake and translocation of copper (Cu) in E. splendens. Significant promotion of plant growth coupled with the obvious plant-growth-promoting (PGP) characters of the bacteria suggested that CZ1 would be a plant-growth-promoting rhizobacterium (PGPR) to E. splendens under Cu stress condition. The results of inductively coupled plasma optical emission spectrometry (ICP-OES) showed that CZ1 increased the concentration of Cu in the shoots (up to 211.6% compared to non-inoculation treatment) and translocation factor (TF) (from 0.56 to 1.83%) of those exposed to Cu. The distribution of Cu in root cross section measured by synchrotron-based X-ray fluorescence microscopy (SRXRF) indicated that CZ1 promoted the transport of Cu from cortex to xylem in roots, which contributed to the accumulation of Cu in shoots. Furthermore, CZ1 improved the uptake of nutrient elements by plants to oppose to the toxicity of Cu. In summary, P. putida CZ1 acted as a PGPR in resistance to Cu and promoted the accumulation and translocation of Cu from root to shoot by element redistribution in plant root; hence, CZ1 is a promising assistance to phytoremediation.

  15. Use of magnetic folate-dextran-retinoic acid micelles for dual targeting of doxorubicin in breast cancer.

    PubMed

    Varshosaz, J; Sadeghi-aliabadi, H; Ghasemi, S; Behdadfar, B

    2013-01-01

    Amphiphilic copolymer of folate-conjugated dextran/retinoic acid (FA/DEX-RA) was self-assembled into micelles by direct dissolution method. Magnetic iron oxide nanoparticles (MNPs) coated with oleic acid (OA) were prepared by hydrothermal method and encapsulated within the micelles. Doxorubicin HCl was loaded in the magnetic micelles. The characteristics of the magnetic micelles were determined by Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA), transmission electron microscopy (TEM), and vibrating sample magnetometer (VSM). The crystalline state of OA-coated MNPs and their heat capacity were analyzed by X-ray diffraction (XRD) and differential scanning calorimetry (DSC) methods, respectively. The iron content of magnetic micelles was determined using inductively coupled plasma optical emission spectrometry (ICP-OES). Bovine serum albumin (BSA) was used to test the protein binding of magnetic micelles. The cytotoxicity of doxorubicin loaded magnetic micelles was studied on MCF-7 and MDA-MB-468 cells using MTT assay and their quantitative cellular uptake by fluorimetry method. TEM results showed the MNPs in the hydrophobic core of the micelles. TGA results confirmed the presence of OA and FA/DEX-RA copolymer on the surface of MNPs and micelles, respectively. The magnetic micelles showed no significant protein bonding and reduced the IC₅₀ of the drug to about 10 times lower than the free drug. PMID:24381941

  16. Migration of 18 trace elements from ceramic food contact material: influence of pigment, pH, nature of acid and temperature.

    PubMed

    Demont, M; Boutakhrit, K; Fekete, V; Bolle, F; Van Loco, J

    2012-03-01

    The effect of pH, nature of acid and temperature on trace element migration from ceramic ware treated with 18 commercially available glazes was studied. Besides of the well-studied lead and cadmium, migration of other toxic and non toxic elements such as aluminum, boron, barium, cobalt, chrome, copper, iron, lithium, magnesium, manganese, nickel, antimony, tin, strontium, titanium, vanadium, zinc and zirconium was investigated in order to evaluate their potential health hazards. Trace element concentrations were determined with Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). This study suggests that there is indeed a health risk concerning the possible migration of other elements than lead and cadmium. At low pH (2

  17. Homogeneity study of a corn flour laboratory reference material candidate for inorganic analysis.

    PubMed

    Dos Santos, Ana Maria Pinto; Dos Santos, Liz Oliveira; Brandao, Geovani Cardoso; Leao, Danilo Junqueira; Bernedo, Alfredo Victor Bellido; Lopes, Ricardo Tadeu; Lemos, Valfredo Azevedo

    2015-07-01

    In this work, a homogeneity study of a corn flour reference material candidate for inorganic analysis is presented. Seven kilograms of corn flour were used to prepare the material, which was distributed among 100 bottles. The elements Ca, K, Mg, P, Zn, Cu, Fe, Mn and Mo were quantified by inductively coupled plasma optical emission spectrometry (ICP OES) after acid digestion procedure. The method accuracy was confirmed by analyzing the rice flour certified reference material, NIST 1568a. All results were evaluated by analysis of variance (ANOVA) and principal component analysis (PCA). In the study, a sample mass of 400mg was established as the minimum mass required for analysis, according to the PCA. The between-bottle test was performed by analyzing 9 bottles of the material. Subsamples of a single bottle were analyzed for the within-bottle test. No significant differences were observed for the results obtained through the application of both statistical methods. This fact demonstrates that the material is homogeneous for use as a laboratory reference material.

  18. Profile of Trace Elements in Selected Medicinal Plants Used for the Treatment of Diabetes in Eritrea

    PubMed Central

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

    2016-01-01

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

  19. The bioaccumulation of lead in the organs of roe deer (Capreolus capreolus L.), red deer (Cervus elaphus L.), and wild boar (Sus scrofa L.) from Poland.

    PubMed

    Bąkowska, Małgorzata; Pilarczyk, Bogumiła; Tomza-Marciniak, Agnieszka; Udała, Jan; Pilarczyk, Renata

    2016-07-01

    The aim of this study was to evaluate the level of lead (Pb) in the livers and kidneys of free-living animals from Poland, with regard to the differences in tissue Pb content between the species. The research material consisted of liver and kidney samples collected from roe deer (Capreolus capreolus), red deer (Cervus elaphus), and wild boar (Sus scrofa) that had been hunted in 16 voivodeships of Poland. The concentration of lead had been measured using inductively coupled plasma optical emission spectrometry (ICP-OES) method. The results show that differences in lead concentration in the organs depended on the geographic location. In roe deer and red deer, the highest mean lead concentrations in the livers and kidneys, observed in the central region of Poland, were twice as high as the lowest concentration of Pb in these animals from the northeastern region of the country. In wild boar, the highest mean concentration of Pb was noted in the livers of animals from the central region of Poland and in the kidneys of animals from the northwestern region, while the lowest lead concentrations in both organs were typical for wild boar from the southeast part of the country. Our results show that areas located in the center and in the north of Poland carry most of the burden of lead bioaccumulation. PMID:27068893

  20. Heavy metal concentrations in two populations of Mopane worms (Imbrasia belina) in the Kruger National Park pose a potential human health risk.

    PubMed

    Greenfield, R; Akala, N; van der Bank, F H

    2014-09-01

    Metal concentrations in Mopane worms from Phalaborwa and Shangoni sites in the Kruger National Park were determined. Metal concentrations were evaluated by inductively coupled plasma optical emission spectroscopy (ICP-OES) and ICP-MS spectrometry after microwave digestion. The results indicate a substantial bioaccumulation of metals in Mopane worms. In Phalaborwa Cd concentrations were 15 times and Cu two times higher than the EU and UK recommended legal limits for human consumption, Zn levels were tolerable. Likewise, Cd, Cu and Zn concentrations at the Shangoni site were 26, 2.5 and 0.4 times over the EU and UK approved limits. Manganese concentrations were 20 and 67 times higher than FDA standards respectively. During the study the condition factor of the worms was determined. No significant difference between the condition factors indicated the worms at both sites are in similar condition. Potential sources of metals in the worms are either from the food they eat or pollution settling on the leaves.

  1. Antioxidant value and element content in some tinctures used in medication.

    PubMed

    Szentmihályi, Klára; Varga, Ilona Szöllősi; Gergely, Anita; Rábai, Mária; Then, Mária

    2015-09-01

    Tinctures are almost the oldest medicines and their use is substantial in the medication nowadays as well. The antioxidant values by ferric reducing/antioxidant power (FRAP) method and element content by inductively coupled plasma optical emission spectrometry (ICP-OES) were investigated in some tinctures official in the VII. and VIII. Pharmacopoeia Hungarica. The highest FRAP values were found for volatile oil containing Tinctura Aurantii amari epicarpii et mesocarpii, Tinctura Amara and Tinctura Valerianae (764.54 ± 19.90; 757.37 ± 14.46; 826.40 ± 5.89 µmol l⁻¹, respectively). The correlations between the FRAP values and dilution with different alcohol content in Tinctura Chinae, Tinctura Ipecacuanhae normata and Tinctura Strychni were also investigated. Remarkable differences were found between the element concentrations in the different tinctures. The element contents in tinctures are not so high in absolute values nevertheless the presence of essential selenium, zinc, manganese and copper is important since they have key role in the antioxidant system. The common feature of the tinctures seems to be the lithium content. The Ca to Mg concentration ratio was found to be shifted towards magnesium in some of the tinctures that can show a higher Mg absorption which could affect against the proinflammatoric processes in the cases of gastrointestinal diseases. PMID:26344025

  2. Synthesis and characterization of biomatrixed-gold nanoparticles by the mushroom Flammulina velutipes and its heterogeneous catalytic potential.

    PubMed

    Narayanan, Kannan Badri; Park, Hyun Ho; Han, Sung Soo

    2015-12-01

    Sustainable and greener synthesis of intracellular gold nanoparticles using mushroom Flammulina velutipes is reported. Incubation of a mushroom in chloroaurate solution resulted in the synthesis and immobilization of stable gold nanoparticles inside the mushroom mycelia. Transmission electron microscopic (TEM) analysis revealed the presence of gold nanoparticles (⩽20nm) inside the mycelia, primarily on the inner surface of the cell membrane. Inductively coupled plasma-optical emission spectrometry (ICP-OES) revealed that the accumulated gold concentration ranged from 64.4 to 330.5mgkg(-1) dry weight (DW) in the mushroom mycelia. The reduction of Au(3+) ions to Au(0) and stabilization of gold nanoparticles occurred within 1h, and the formation of fcc crystalline gold nanoparticles was confirmed by X-ray diffraction (XRD) analysis. This facile intracellular synthesis of gold nanoparticles by a mushroom without using any toxic chemicals or technologically expensive processes is used as a heterogeneous catalyst in the reduction of organic pollutants methylene blue (MB) and 4-nitrophenol (4NP). The reduction reaction follows pseudo-first order kinetics with a reaction rate constant of 0.0529min(-1) and 0.1236min(-1) for MB and 4NP, respectively. This biological process of biomatrixing of metal nanoparticles for heterogeneous catalytic reactions is simple, nontoxic, environmentally benign, and economically viable compared to the chemical synthetic routes.

  3. Green direct determination of mineral elements in artichokes by infrared spectroscopy and X-ray fluorescence.

    PubMed

    Mir-Marqués, Alba; Martínez-García, Maria; Garrigues, Salvador; Cervera, M Luisa; de la Guardia, Miguel

    2016-04-01

    Near infrared (NIR) and X-ray fluorescence (XRF) spectroscopy were investigated to predict the concentration of calcium, potassium, iron, magnesium, manganese and zinc in artichoke samples. Sixty artichokes were purchased from different Spanish areas (Benicarló, Valencia and Murcia). NIR and XRF spectra, combined with partial least squares (PLS) data treatment, were used to develop chemometric models for the prediction of mineral concentration. To obtain reference data, samples were mineralised and analysed by inductively coupled plasma optical emission spectrometry (ICP-OES). Coefficients of determination obtained for the regression between predicted values and reference ones for calcium, potassium, magnesium, iron, manganese and zinc were 0.61, 0.79, 0.53, 0.77, 0.54 and 0.60 for NIR and 0.96, 0.93, 0.80, 0.79, 0.76 and 0.90 for XRF, respectively. Both assayed methodologies, offer green alternatives to classical mineral analysis, but XRF provided the best results in order to be used as a quantitative screening method.

  4. Construction of inorganic elemental fingerprint and multivariate statistical analysis of marine traditional Chinese medicine Meretricis concha from Rushan Bay

    NASA Astrophysics Data System (ADS)

    Wu, Xia; Zheng, Kang; Zhao, Fengjia; Zheng, Yongjun; Li, Yantuan

    2014-08-01

    Meretricis concha is a kind of marine traditional Chinese medicine (TCM), and has been commonly used for the treatment of asthma and scald burns. In order to investigate the relationship between the inorganic elemental fingerprint and the geographical origin identification of Meretricis concha, the elemental contents of M. concha from five sampling points in Rushan Bay have been determined by means of inductively coupled plasma optical emission spectrometry (ICP-OES). Based on the contents of 14 inorganic elements (Al, As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Mo, Ni, Pb, Se, and Zn), the inorganic elemental fingerprint which well reflects the elemental characteristics was constructed. All the data from the five sampling points were discriminated with accuracy through hierarchical cluster analysis (HCA) and principle component analysis (PCA), indicating that a four-factor model which could explain approximately 80% of the detection data was established, and the elements Al, As, Cd, Cu, Ni and Pb could be viewed as the characteristic elements. This investigation suggests that the inorganic elemental fingerprint combined with multivariate statistical analysis is a promising method for verifying the geographical origin of M. concha, and this strategy should be valuable for the authenticity discrimination of some marine TCM.

  5. Uptake and translocation of metals and nutrients in tomato grown in soil polluted with metal oxide (CeO₂, Fe₃O₄, SnO₂, TiO₂) or metallic (Ag, Co, Ni) engineered nanoparticles.

    PubMed

    Vittori Antisari, Livia; Carbone, Serena; Gatti, Antonietta; Vianello, Gilmo; Nannipieri, Paolo

    2015-02-01

    The influence of exposure to engineered nanoparticles (NPs) was studied in tomato plants, grown in a soil and peat mixture and irrigated with metal oxides (CeO2, Fe3O4, SnO2, TiO2) and metallic (Ag, Co, Ni) NPs. The morphological parameters of the tomato organs, the amount of component metals taken up by the tomato plants from NPs added to the soil and the nutrient content in different tomato organs were also investigated. The fate, transport and possible toxicity of different NPs and nutrients in tomato tissues from soils were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES). The tomato yield depended on the NPs: Fe3O4-NPs promoted the root growth, while SnO2-NP exposure reduced it (i.e. +152.6 and -63.1 % of dry matter, respectively). The NP component metal mainly accumulated in the tomato roots; however, plants treated with Ag-, Co- and Ni-NPs showed higher concentration of these elements in both above-ground and below-ground organs with respect to the untreated plants, in addition Ag-NPs also contaminated the fruits. Moreover, an imbalance of K translocation was detected in some plants exposed to Ag-, Co- and Fe3O4-NPs. The component metal concentration of soil rhizosphere polluted with NPs significantly increased compared to controls, and NPs were detected in the tissues of the tomato roots using electron microscopy (ESEM-EDS).

  6. Trace metals geochemistry of Bengkulu river and estuary

    NASA Astrophysics Data System (ADS)

    Firdaus, M. Lutfi; Darti, Puspa; Alwi, Wiwit; Swistoro, Eko; Sundaryono, Agus; Ruyani, Aceng

    2015-09-01

    Unique feature of Indonesian archipelago in addition to its location that settled between the Pacific Ocean and the Indian Ocean has made Indonesian seas as important parts of the world ocean system. In contrast, research on Indonesian seas including its marine geochemistry is scarce. Research findings have proven that Indonesian seas and its characteristics, such as Indonesian throughflow, are important in the seawater thermohaline circulation that affect world's global climate. The transports of mass and heat from the Pacific into the Indian Ocean are crucial for the oceanic circulation and sea surface temperatures. It is only until recently known that water masses movement could be traced using chemical elements such as Zr and Hf. In modern ocean, sources of these chemicals are mostly from continents. Chemicals had been brought to the oceans through river, estuary, coastal and eventually open seawater. We have analyzed selected important trace metals of Bengkulu river and estuary starting from upper stream of Bengkulu River to coastal seawater of the Indian Ocean. Concentrations of trace metals in the sample were determined by inductively coupled plasma - optical emission spectrometry (ICP-OES). Dissolved and labile particulate concentrations of Al, Fe, Mn, V, Sr and Zn are reported in this study.

  7. Classification and individualization of used engine oils using elemental composition and discriminant analysis.

    PubMed

    Kim, Yuna; Kim, Nam Yee; Park, Seh Youn; Lee, Dong-Kye; Lee, Jin Hoon

    2013-07-10

    The six most common commercial automotive gasoline and diesel engine oils in the Republic of Korea, ZIC A, ZIC XQ RV/SUV, Kixx G1, Kixx RV, and the brand name products HD Premium gasoline and HD Premium diesel, were randomly used in nineteen different vehicles. Samples of seventy-six used engine oils, which were withdrawn from the sumps of those vehicles at different intervals, were analyzed using inductively coupled plasma-optical emission spectrometry (ICP-OES), and statistically compared. Two data analysis strategies were used to interpret and understand the elemental profiles in the multi-dimensional data. Macro (additive elements of Ca, Zn and P) and trace (wear metal elements of Ag, Al, Ba, Cd, Cr, Cu, Fe, Mg, Mo, Na, Ni, Pb and Sn) elements were used as potential markers to determine the brand of oil used and the engine type in which the oil was used, and to trace the individual vehicle for forensic purposes. The discriminant analysis statistical technique was applied, and its prediction ability was assessed. In this study, 92.1%, 82.9% and 92.1% of the cross-validated grouped cases correctly predicted the brand of oil, the engine type and the vehicle that was the source of the oil, respectively. PMID:23806831

  8. Determination of inorganic contaminants in polyamide textiles used for manufacturing sport T-shirts.

    PubMed

    Matoso, Erika; Cadore, Solange

    2012-01-15

    An acid microwave closed vessel digestion method was used for the determination of inorganic contaminants (Sb, As, Pb, Cd, Cr, Co, Cu, Ni and Hg) in polyamide raw materials (pellets) and textiles by inductively coupled plasma optical emission spectrometry (ICP OES). The initial tests were carried out with samples of polyamide pellets, which is the main raw material used to manufacture sport textiles. The recovery factors obtained were 94.4-105.7% with relative standard deviation (RSD) of 0.5-2.2%. The proposed method was evaluated by addition and recovery tests and also using certified reference materials (ERM-BCR680 and ERM-BCR681) showing good accuracy. The residual acidity was about 4% HNO(3) (w/w) and the quantification limits were from 0.1 to 6.6 mg kg(-1). After the development of these parameters for the raw material, the method was applied to textile samples from different sport fabrics obtained from three different brands. The residual carbon after sample digestion was 0.2% (w/w) and the most significant result was obtained for chromium, 901 mg kg(-1), in black fabric. Lixiviation tests using synthetic sweat and temperature were carried out on two black samples, showing that only 0.3% of the initial concentration migrated to the solution.

  9. Human contribution to trace elements in urban areas as measured in holm oak (Quercus ilex L.) bark.

    PubMed

    Minganti, Vincenzo; Drava, Giuliana; Giordani, Paolo; Malaspina, Paola; Modenesi, Paolo

    2016-06-01

    The effect of human activities on the presence of trace elements in the atmosphere was evaluated by analyzing samples of holm oak bark, collected in Italy in a large city, in a small town, and in a reference area, scarcely inhabited. In all cases, point sources of pollution were excluded (e.g., industries and incinerators). The concentrations of As, Cd, Co, Cu, Fe, Mn, Ni, Pb, V, and Zn were measured using inductively coupled plasma optical emission spectrometry (ICP-OES). The element concentrations in the small town are not different from the reference area, except for Pb and Cu, while the samples collected in the large city show higher concentrations of Co, Cu, Fe, Ni, Pb, V, and Zn with respect to the rural area. In particular, the Pb levels in the large city are approximately 16 times higher than in the reference site, and five times higher than in the small town. Most element concentrations are correlated in the large city, while in the reference site, only a few significant correlations between elements were found. Even in the absence of specific sources of pollution, populations living in big cities are exposed to higher concentrations of trace elements than those living in rural environments or in small urban centers. PMID:27000118

  10. Mineral composition, nutritional properties, total phenolics and flavonoids compounds of the atemoya fruit (Annona squamosa L. x Annona cherimola Mill.) and evaluation using multivariate analysis techniques.

    PubMed

    Santos, Walter N L Dos; Sauthier, Maria Celeste S; Cavalcante, Dannuza D; Benevides, Clícia M J; Dias, Fábio S; Santos, Daniele C M B

    2016-09-01

    The atemoya is a hybrid fruit obtained by crossing of cherimoya (Annona cherimola Mill.) with sweet sop (Annona squamosa L.). The information about chemical composition of atemoya is scarce. The mineral composition was evaluated employing Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) and the centesimal composition and the physico-chemical parameters were assessed employing procedures described in the AOAC methods. The total phenolic compounds (TPC) and total flavonoids (TF) were determined using spectroanalytical methods. Considering the Reference Daily Intake (RDI), the concentrations of K, Cu and Vitamin C found in atemoya were the highest, representing about 32, 23 and 37% of the RDI, respectively. The total carbohydrates were 32 g 100g-1 and the soluble solids was equivalent to (32.50 ± 0.03) °Brix. The result for TPC was 540.47 ± 2.32 mgGAE 100 g-1 and the TF was 11.56 ± 1.36 mgQE 100 g-1. The exploratory evaluation of 42 atemoya samples was performed through Principal Component Analysis (PCA), which discriminated green and ripe fruits according to their mineral composition. The elements that contributed most for the variability between green and ripe fruits were: Ba, Ca, Cu, K, Mg and P.

  11. Use of Magnetic Folate-Dextran-Retinoic Acid Micelles for Dual Targeting of Doxorubicin in Breast Cancer

    PubMed Central

    Varshosaz, J.; Sadeghi-aliabadi, H.; Ghasemi, S.; Behdadfar, B.

    2013-01-01

    Amphiphilic copolymer of folate-conjugated dextran/retinoic acid (FA/DEX-RA) was self-assembled into micelles by direct dissolution method. Magnetic iron oxide nanoparticles (MNPs) coated with oleic acid (OA) were prepared by hydrothermal method and encapsulated within the micelles. Doxorubicin HCl was loaded in the magnetic micelles. The characteristics of the magnetic micelles were determined by Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA), transmission electron microscopy (TEM), and vibrating sample magnetometer (VSM). The crystalline state of OA-coated MNPs and their heat capacity were analyzed by X-ray diffraction (XRD) and differential scanning calorimetry (DSC) methods, respectively. The iron content of magnetic micelles was determined using inductively coupled plasma optical emission spectrometry (ICP-OES). Bovine serum albumin (BSA) was used to test the protein binding of magnetic micelles. The cytotoxicity of doxorubicin loaded magnetic micelles was studied on MCF-7 and MDA-MB-468 cells using MTT assay and their quantitative cellular uptake by fluorimetry method. TEM results showed the MNPs in the hydrophobic core of the micelles. TGA results confirmed the presence of OA and FA/DEX-RA copolymer on the surface of MNPs and micelles, respectively. The magnetic micelles showed no significant protein bonding and reduced the IC50 of the drug to about 10 times lower than the free drug. PMID:24381941

  12. Screening of Trace Elements in Hair of the Female Population with Different Types of Cancers in Wielkopolska Region of Poland

    PubMed Central

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

    2014-01-01

    Background. Cancer constitutes a major health problem worldwide. Thus, search for reliable and practical markers of the disease process remains the key issue of the diagnostic process. Objectives. The study aims at linking the trace element status of an organism, assessed by hair analysis, with the occurrence of cancer diseases. Material and Methods. Hair samples were collected from 299 patients with cancer diseases confirmed by a histopathological test and from 100 controls. Cancer patients were divided into three groups, depending on cancer type: hormone-dependent cancer, cancer of the alimentary tract, and cancer with high glycolytic activity. Mineral element analysis of hair was performed using an atomic emission spectrophotometer with inductively coupled plasma (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). Results. Statistically significantly lower concentrations of selenium, zinc, copper, germanium and boron, iron, and magnesium were observed in the three groups of cancer patients. Disturbance in the axis glucose-insulin and changes in concentrations of heavy metals and toxic elements were also noted. Conclusions. It seems safe to conclude that our results confirmed usefulness of hair element analysis in screening tests for the assessment of the biomarker of various cancer diseases in a female population. PMID:25580464

  13. Selective solid-phase extraction using oxidized activated carbon modified with triethylenetetramine for preconcentration of metal ions

    NASA Astrophysics Data System (ADS)

    Zhang, Li; Chang, Xijun; Li, Zhenhua; He, Qun

    2010-02-01

    A new selective solid-phase extractant using activated carbon as matrix which was purified, oxidized and modified by triethylenetetramine (AC-TETA) was prepared and characterized by FT-IR spectroscopy. At pH 4, quantitative extraction of trace Cr(III), Fe(III) and Pb(II) was obtained and determined by inductively coupled plasma optical emission spectrometry (ICP-OES). Complete elution of the adsorbed metal ions from the sorbent surface was carried out using 0.5 mol L -1 HCl. The maximum static adsorption capacity of sorbent for Cr(III), Fe(III) and Pb(II) was 34.6, 36.5 and 51.9 mg g -1, respectively. The time of quantitative adsorption was less than 2 min. The detection limits of the method was found to be 0.71, 0.35 and 0.45 ng mL -1 for Cr(III), Fe(III) and Pb(II), and the relative standard deviation (RSD) was 3.7%, 2.2% and 2.5%, respectively. Moreover, the method was free from interference with common coexiting ions. The method was also successfully applied to the preconcentration of trace Cr(III), Fe(III) and Pb(II) in synthetic samples and a real sample with satisfactory results.

  14. Pressurized liquid extraction-assisted mussel cytosol preparation for the determination of metals bound to metallothionein-like proteins.

    PubMed

    Santiago-Rivas, Sandra; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Jorge; Alonso-Rodríguez, Elia; Muniategui-Lorenzo, Soledad; López-Mahía, Purificación; Prada-Rodríguez, Darío

    2007-11-01

    The possibilities of pressurized liquid extraction (PLE) have been novelty tested to assist the cytosol preparation from wet mussel soft tissue before the determination of metals bound to metallothionein-like proteins (MLPs). Results obtained after PLE were compared with those obtained after a classical blending procedure for mussel cytosolic preparation. Isoforms MLP-1 (retention time of 4.1 min) and MLP-2 (retention time of 7.4 min) were separated by anion exchange high-performance liquid chromatography (HPLC) and the concentrations of Ba, Cu, Mn, Sr and Zn bound to MLP isoforms were directly measured by inductively coupled plasma-atomic emission spectrometry (ICP-OES) as a multi-element detector. The optimized PLE-assisted mussel cytosol preparation has consisted of one extraction cycle at room temperature and 1500 psi for 2 min. Since separation between the solid mussel residue and the extract (cytosol) is performed by the PLE system, the cytosol preparation method is faster than conventional cytosol preparation methods by cutting/blending using Ultraturrax or Stomacher devices. PMID:17950055

  15. Elemental analysis of Egyptian phosphate fertilizer components.

    PubMed

    El-Bahi, S M; El-Dine, N Walley; El-Shershaby, A; Sroor, A

    2004-03-01

    The accumulation of certain elements in vitally important media such as water, soil, and food is undesirable from the medical point of view. It is clear that the fertilizers vary widely in their heavy metals and uranium content. A shielded high purity germanium HPGe detector has been used to measure the natural concentration of 238U, 232Th, and 40K activities in the phosphate fertilizer and its components collected from Abu-Zaabal fertilizers and chemical industries in Egypt. The concentration ranges were 134.97-681.11 Bq kg(-1), 125.23-239.26 Bq kg(-1), and 446.11-882.45 Bq kg(-1) for 238U, 232Th, and 40K, respectively. The absorbed dose rate and external hazard index were found to be from 177.14 to 445.90 nGy h(-1) and 1.03 to 2.71 nGy y(-1), respectively. The concentrations of 22 elements (Be, Na, Mg, Si, P, S, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Sr, Zr, Mo, Cd, Ba) in the samples under investigation were determined by inductively coupled plasma optical-emission spectrometry (ICP-OES). The results for the input raw materials (rock phosphate, limestone and sulfur) and the output product as final fertilizer are presented and discussed. PMID:14982231

  16. Reductive spectrophotometry of divalent tin sensitization on soda lime glass

    NASA Astrophysics Data System (ADS)

    Bejugam, Vinith; Wei, Xingfei; Roper, D. Keith

    2016-07-01

    Rapid and facile evaluation of tin (II) sensitization could lead to improved understanding of metal deposition in electroless (EL) plating. This report used a balanced redox reaction between 3,3‧,5,5‧-tetramethylbenzidine dihydrochloride (TMB-HCL) and N-bromosuccinimide (NBS) to evaluate effects of sensitization conditions (i.e., sensitization time, analyte concentration, aqueous immersion, and acid content) on the accumulated mass of surface-associated divalent tin ion. The accumulated mass of tin (II) increased as the sensitization time increased up to 30 s in proportion to aqueous tin (II) chloride concentrations between 2.6 and 26 mM at a trifluoroacetic acid (TFA) content of 68 mM. The average mass peaked at 7.3 nanomoles (nmol) per cm2 after a 5 s aqueous immersion post-sensitization, and then decreased with increasing aqueous immersion post-sensitization. The total average tin (II) + tin (IV) accumulated on soda lime glass measured by inductively coupled plasma optical emission spectrometry (ICP-OES) was 17% higher at 30 s sensitization, suggesting a fraction of the tin (II) present may have oxidized to tin (IV). These results indicated that in situ spectrophotometric evaluation of tin (II) could support development of EL plating for electronics, catalysis, and solar cells.

  17. Quantitative analysis of heavy metals in automotive brake linings: a comparison between wet-chemistry based analysis and in-situ screening with a handheld X-ray fluorescence spectrometer.

    PubMed

    Figi, R; Nagel, O; Tuchschmid, M; Lienemann, P; Gfeller, U; Bukowiecki, N

    2010-08-31

    Two extraction procedures for ecologically relevant elements present in automotive brake linings (Sb, Bi, Pb, Cd, Cr (total), Co, Cu, Mo, Ni, Sr, V, Zn, Sn) were developed and validated, applying a high pressure asher (HPA-S) and microwave extraction, respectively. Both of these methods allowed for the quantitative analysis of the extracted elements by inductively coupled plasma optical emission spectrometry (ICP-OES). The results were compared to measurements using a handheld energy-dispersive X-ray fluorescence spectrometer (ED-XRF), being in discussion by regulating agencies as in-situ screening tool for brake pads. The comparison indicates that the handheld ED-XRF analysis is basically an efficient screening tool for a reliable assessment of trace metal contents in automotive brake pads with respect to legal standards. While a quantitative determination of elements like Cd, Co, Cr, Mn, Mo, Ni, Pb and Sb was achievable, other elements (V, Cu, Bi, Zn, Sn and Sr) could only be determined qualitatively due to the special matrix characteristics of brake pads.

  18. Amino-functionalized mesoporous silica modified glassy carbon electrode for ultra-trace copper(II) determination.

    PubMed

    Dai, Xingxin; Qiu, Fagui; Zhou, Xuan; Long, Yumei; Li, Weifeng; Tu, Yifeng

    2014-10-27

    This paper described a facile and direct electrochemical method for the determination of ultra-trace Cu(2+) by employing amino-functionalized mesoporous silica (NH2-MCM-41) as enhanced sensing platform. NH2-MCM-41 was prepared by using a post-grafting process and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and fourier transform infrared (FTIR) spectroscopy. NH2-MCM-41 modified glassy carbon (GC) electrode showed higher sensitivity for anodic stripping voltammetric (ASV) detection of Cu(2+) than that of MCM-41 modified one. The high sensitivity was attributed to synergistic effect between MCM-41 and amino-group, in which the high surface area and special mesoporous morphology of MCM-41 can cause strong physical absorption, and amino-groups are able to chelate copper ions. Some important parameters influencing the sensor response were optimized. Under optimum experimental conditions the sensor linearly responded to Cu(2+) concentration in the range from 5 to 1000 ng L(-1) with a detection limit of 0.9 ng L(-1) (S/N=3). Moreover, the sensor possessed good stability and electrode renewability. In the end, the proposed sensor was applied for determining Cu(2+) in real samples and the accuracy of the results were comparable to those obtained by inductively coupled plasma optical emission spectrometry (ICP-OES) method.

  19. Heavy metals in cigarettes for sale in Spain.

    PubMed

    Rubio Armendáriz, Carmen; Garcia, Tiago; Soler, Alfredo; Gutiérrez Fernández, Ángel José; Glez-Weller, Dailos; Luis González, Gara; de la Torre, Arturo Hardisson; Revert Gironés, Consuelo

    2015-11-01

    The aim of the present study was to determine the concentrations of eight metals (Al, Cd, Co, Cr, Mn, Ni, Pb, Sr) in 33 cigarette brands for sale in Spain. Samples were analysed by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). Mean values obtained were 428 µg Al/g, 0.810 µg Cd/g, 0.558 µg Co/g, 1.442 µg Cr/g, 112.026 µg Mn/g, 2.238 µg Ni/g, 0.602 µg Pb/g and 82.206 µg Sr/g. Statistically significant differences were observed with respect to concentrations of Co (0.004), Cr (0.045), Mn (0.005) and Sr (0.005) between black and blond tobacco and between levels of Mn (0.027) among manufacturers. Considering a Cd inhalation rate of 10% and a Cd absorption rate of 50%, absorption of Cd for smokers of 30 cigarettes/day was estimated at 0.75 µg Cd/day. An inhalation rate of 2-6% and an absorption rate of 86% were considered for Pb, Pb absorption in smokers of 30 cigarettes/day was therefore 0.18-0.54 μg/day. In view of the significant toxic effects of these metals, quantification and control of their concentrations in this drug are of the utmost importance.

  20. Chemical Speciation and Potential Mobility of Heavy Metals in the Soil of Former Tin Mining Catchment

    PubMed Central

    Ashraf, M. A.; Maah, M. J.; Yusoff, I.

    2012-01-01

    This study describes the chemical speciation of Pb, Zn, Cu, Cr, As, and Sn in soil of former tin mining catchment. Total five sites were selected for sampling and subsequent subsamples were collected from each site in order to create a composite sample for analysis. Samples were analysed by the sequential extraction procedure using optical emission spectrometry (ICP OES). Small amounts of Cu, Cr, and As retrieved from the exchangeable phase, the ready available for biogeochemical cycles in the ecosystem. Low quantities of Cu and As could be taken up by plants in these kind of acidic soils. Zn not detected in the bioavailable forms while Pb is only present in negligible amounts in very few samples. The absence of mobile forms of Pb eliminates the toxic risk both in the trophic chain and its migration downwards the soil profile. The results also indicate that most of the metals have high abundance in residual fraction indicating lithogenic origin and low bioavailability of the metals in the studied soil. The average potential mobility for the metals giving the following order: Sn > Cu > Zn > Pb > Cr > As. PMID:22566758

  1. Synthesis and characterization of silver nanoparticles from Alpinia calcarata by Green approach and its applications in bactericidal and nonlinear optics

    NASA Astrophysics Data System (ADS)

    Pugazhendhi, S.; Kirubha, E.; Palanisamy, P. K.; Gopalakrishnan, R.

    2015-12-01

    Development of green route for the synthesis of nanoparticles with plant extracts plays a very important role in nanotechnology without any toxicity chemicals. Herein we report a new approach to synthesize silver nanoparticles (AgNPs) using aqueous extract of Alpinia calcarata root as a reducing as well as stabilizing agent. The crystal structure and purity of the synthesized AgNPs were studied using Powder X-ray Diffraction analysis. The Surface Plasmon Resonance bands of synthesized silver nanoparticles have been obtained and monitored using UV-Visible spectrum. The morphologies of the AgNPs were analyzed using High resolution transmission electron microscopy (HRTEM). The elements present in the A. calcarata extract were determined by the inductively coupled plasma-optical emission Spectrometry (ICP-OES) and Fourier transform infrared spectroscopy (FTIR). Silver nanoparticles from A. calcarata possess very good antimicrobial activity which was confirmed by resazurin dye reduction assay method and thus it is a potential source of antimicrobial agent. The synthesized Ag nanoparticles exhibit good optical nonlinearity and the nonlinear optical studies have been carried out by Z-scan technique.

  2. Green direct determination of mineral elements in artichokes by infrared spectroscopy and X-ray fluorescence.

    PubMed

    Mir-Marqués, Alba; Martínez-García, Maria; Garrigues, Salvador; Cervera, M Luisa; de la Guardia, Miguel

    2016-04-01

    Near infrared (NIR) and X-ray fluorescence (XRF) spectroscopy were investigated to predict the concentration of calcium, potassium, iron, magnesium, manganese and zinc in artichoke samples. Sixty artichokes were purchased from different Spanish areas (Benicarló, Valencia and Murcia). NIR and XRF spectra, combined with partial least squares (PLS) data treatment, were used to develop chemometric models for the prediction of mineral concentration. To obtain reference data, samples were mineralised and analysed by inductively coupled plasma optical emission spectrometry (ICP-OES). Coefficients of determination obtained for the regression between predicted values and reference ones for calcium, potassium, magnesium, iron, manganese and zinc were 0.61, 0.79, 0.53, 0.77, 0.54 and 0.60 for NIR and 0.96, 0.93, 0.80, 0.79, 0.76 and 0.90 for XRF, respectively. Both assayed methodologies, offer green alternatives to classical mineral analysis, but XRF provided the best results in order to be used as a quantitative screening method. PMID:26593585

  3. Heavy metals in cigarettes for sale in Spain.

    PubMed

    Rubio Armendáriz, Carmen; Garcia, Tiago; Soler, Alfredo; Gutiérrez Fernández, Ángel José; Glez-Weller, Dailos; Luis González, Gara; de la Torre, Arturo Hardisson; Revert Gironés, Consuelo

    2015-11-01

    The aim of the present study was to determine the concentrations of eight metals (Al, Cd, Co, Cr, Mn, Ni, Pb, Sr) in 33 cigarette brands for sale in Spain. Samples were analysed by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). Mean values obtained were 428 µg Al/g, 0.810 µg Cd/g, 0.558 µg Co/g, 1.442 µg Cr/g, 112.026 µg Mn/g, 2.238 µg Ni/g, 0.602 µg Pb/g and 82.206 µg Sr/g. Statistically significant differences were observed with respect to concentrations of Co (0.004), Cr (0.045), Mn (0.005) and Sr (0.005) between black and blond tobacco and between levels of Mn (0.027) among manufacturers. Considering a Cd inhalation rate of 10% and a Cd absorption rate of 50%, absorption of Cd for smokers of 30 cigarettes/day was estimated at 0.75 µg Cd/day. An inhalation rate of 2-6% and an absorption rate of 86% were considered for Pb, Pb absorption in smokers of 30 cigarettes/day was therefore 0.18-0.54 μg/day. In view of the significant toxic effects of these metals, quantification and control of their concentrations in this drug are of the utmost importance. PMID:26492401

  4. Processing and characterization of diatom nanoparticles and microparticles as potential source of silicon for bone tissue engineering.

    PubMed

    Le, Thi Duy Hanh; Bonani, Walter; Speranza, Giorgio; Sglavo, Vincenzo; Ceccato, Riccardo; Maniglio, Devid; Motta, Antonella; Migliaresi, Claudio

    2016-02-01

    Silicon plays an important role in bone formation and maintenance, improving osteoblast cell function and inducing mineralization. Often, bone deformation and long bone abnormalities have been associated with silica/silicon deficiency. Diatomite, a natural deposit of diatom skeleton, is a cheap and abundant source of biogenic silica. The aim of the present study is to validate the potential of diatom particles derived from diatom skeletons as silicon-donor materials for bone tissue engineering applications. Raw diatomite (RD) and calcined diatomite (CD) powders were purified by acid treatments, and diatom microparticles (MPs) and nanoparticles (NPs) were produced by fragmentation of purified diatoms under alkaline conditions. The influence of processing on the surface chemical composition of purified diatomites was evaluated by X-ray photoelectron spectroscopy (XPS). Diatoms NPs were also characterized in terms of morphology and size distribution by transmission electron microscopy (TEM) and Dynamic light scattering (DLS), while diatom MPs morphology was analyzed by scanning electron microscopy (SEM). Surface area and microporosity of the diatom particles were evaluated by nitrogen physisorption methods. Release of silicon ions from diatom-derived particles was demonstrated using inductively coupled plasma optical emission spectrometry (ICP/OES); furthermore, silicon release kinetic was found to be influenced by diatomite purification method and particle size. Diatom-derived microparticles (MPs) and nanoparticles (NPs) showed limited or no cytotoxic effect in vitro depending on the administration conditions. PMID:26652398

  5. Effects of Sulfate during CO2 Attack on Portland Cement and Their Impacts on Mechanical Properties under Geologic CO2 Sequestration Conditions.

    PubMed

    Li, Qingyun; Lim, Yun Mook; Jun, Young-Shin

    2015-06-01

    To investigate the effects of sulfate on CO2 attack on wellbore cement (i.e., chemical and mechanical alterations) during geologic CO2 sequestration (GCS), we reacted cement samples in brine with 0.05 M sulfate and 0.4 M NaCl at 95 °C under 100 bar of either N2 or supercritical CO2. The results were compared to those obtained from systems without additional sulfate at the same temperature, pressure, salinity, and initial brine pHs. After 10 reaction days, chemical analyses using scanning electron microscopy with a backscattered electron detector (SEM-BSE) and inductively coupled plasma optical emission spectrometry (ICP-OES) showed that the CO2 attack in the presence of additional sulfate was much less severe than that in the system without additional sulfate. The results from three-point bending tests also indicated that sulfate significantly mitigated the deterioration of the cement's strength and elastic modulus. In all our systems, typical sulfate attacks on cement via formation of ettringite were not observed. The protective effects of sulfate on cement against CO2 attack resulted from sulfate adsorption, coating of CaSO4 on the CaCO3 grains in the carbonated layer, or both, which inhibited dissolution of CaCO3. Findings from this study provide new, important information for understanding the integrity of wellbores at GCS sites and thus promote safer GCS operations. PMID:25938805

  6. Total suspended dust and heavy metal levels emitted from a workplace compared with nearby residential houses

    NASA Astrophysics Data System (ADS)

    Abdul-Wahab, Sabah A.; Yaghi, Basma

    Total suspended particulate matter (TSP) were collected from the workplace in Sohar Industrial Estate (SIE) in Oman. The samples were taken from 19 different industrial activities that represent major sources of particulate matter in the SIE. The collected samples were analyzed for 9 heavy metals (Cr, Cu, Mn, Ni, Pb, Zn, Cd, V and Mo) by using the inductively coupled plasma optical emission spectrometry analysis (ICP-OES). Furthermore, the indoor TSP and heavy metal concentrations were measured inside 12 houses within Sohar residential area to determine the contributions of various industrial activities on nearby residential houses. The results indicated that the mean concentrations of heavy metals in the TSP were too low to yield any known environmental health effects. In general, the results showed that the concentrations of heavy metals in the workplaces of SIE and its nearby houses were low compared to the guideline values. In addition, the values were low in comparison with other known sites around the world. Moreover, significant contribution from industrial sources at SIE was evidenced at nearby houses.

  7. International Mass Spectrometry Society (IMSS).

    PubMed

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

    2001-02-01

    This paper gives a brief description of the recently formalized International Mass Spectrometry Society (IMSS). It is presented here in order to increase awareness of the opportunities for collaboration in mass spectrometry in an international context. It also describes the recent 15th International Mass Spectrometry Conference, held August/September 2000, in Barcelona. Each of the authors is associated with the IMSS. The 15th Conference, which covers all of mass spectrometry on a triennial basis, was chaired by Professor Emilio Gelpi of the Instituto de Investigaciones Biomedicas, Barcelona. The outg