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Sample records for emission spectrometry icp-oes

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

    PubMed

    Schenk, Emily R; Almirall, José R

    2012-04-10

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

  4. 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

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

    PubMed

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

    2008-11-01

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

  6. 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.

  7. 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.

  8. 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

  9. 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.

  10. 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.

  11. 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

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

    PubMed

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

    2006-03-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2008-11-01

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

  14. 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.

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

    PubMed

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

    2016-12-01

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

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

    PubMed

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

    2013-12-15

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

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

    PubMed

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

    2013-01-01

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

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

    PubMed

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

    2007-02-15

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

  19. 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.

  20. 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.

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

    PubMed

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

    2009-06-01

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

  2. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2017-01-01

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

  5. 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...

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

    NASA Astrophysics Data System (ADS)

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

    2003-01-01

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

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

    PubMed

    Carpenter, R C

    1985-03-01

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

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

    PubMed

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

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

  9. 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.

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

    PubMed Central

    Chojnacka, Katarzyna; Marycz, Krzysztof

    2010-01-01

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

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

    PubMed

    Michalak, Izabela; Chojnacka, Katarzyna; Marycz, Krzysztof

    2011-02-01

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

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

    PubMed

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

    2015-01-01

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

  13. [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

  14. 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.

  15. 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.

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

    PubMed

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

    2007-05-01

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

  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. 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.

  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.

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

    PubMed

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

    2015-01-01

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

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

    PubMed

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

    2012-06-01

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

  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. 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.

  5. 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.

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

    PubMed

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

    2005-12-01

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

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

    PubMed

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

    2009-03-15

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

  8. 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).

  9. 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.

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

    NASA Astrophysics Data System (ADS)

    Asfaw, Alemayehu; Wibetoe, Grethe

    2009-05-01

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

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

    PubMed

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

    2013-01-30

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

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

    PubMed

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

    2015-10-20

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

  13. 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

  14. 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

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

    PubMed

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

    2017-03-01

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

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

    PubMed

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

    2001-12-01

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

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

    PubMed

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

    2016-09-06

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

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

    PubMed

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

    2016-06-05

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

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

    PubMed

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

    2014-01-01

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

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

    PubMed

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

    2007-10-01

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

  1. 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.

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

    PubMed

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

    2012-09-15

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

  3. 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.

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

    PubMed

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

    2015-07-23

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

  5. 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

  6. 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.

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

    PubMed

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

    2005-02-28

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

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

    PubMed

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

    2009-10-15

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

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

    PubMed

    Tsolakidou, Alexandra; Kilikoglou, Vassilis

    2002-10-01

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

  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. 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.

  12. 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).

  13. [Determination of boron content in natural mineral and spring waters by ICP-OES technique].

    PubMed

    Swiecicka, Dorota; Garbos, Sławomir

    2009-01-01

    Maximum admissible level of boron concentration in water intended for human consumption and in natural mineral and spring waters is usually estimated taking into account actual WHO criteria and requirements listed in Directive No 98/83/EC - 1 mg/l. In majority countries of European Union maximum admissible level of boron in water intended for human consumption is 1 mg/l, however in Slovakia and in Netherlands maximum admissible levels of this element are 0.3 mg/l and 0.5 mg/l, respectively. In this work developed and validated method of determination of boron by inductively coupled plasma emission spectrometry technique was applied for determination of this element in 26 natural mineral and spring waters. Concentrations of boron determined in sixteen mineral and spring waters analyzed were in the range from 0.029 mg/l to 0.552 mg/l while in ten waters analyzed the contents of boron were below 0.026 mg/l. The contents of boron in analyzed waters were below maximum admissible level in Poland presented in the Decree of Minister of Health from 29 March 2007 on the quality of water intended for human consumption and were not dangerous for human health.

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

    PubMed

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

    2012-08-15

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

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

    PubMed

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

    2015-07-23

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

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

    NASA Astrophysics Data System (ADS)

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

    2005-03-01

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

  17. 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.

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

    PubMed

    Vijayaraghavan, K; Joshi, U M

    2013-01-01

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

  19. 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.

  20. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2011-09-01

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

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

    PubMed

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

    2014-10-21

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

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

    PubMed

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

    2005-10-15

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

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

    NASA Astrophysics Data System (ADS)

    Holá, Markéta; Otruba, Vítězslav; Kanický, Viktor

    2006-05-01

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

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

    PubMed

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

    2012-01-01

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

  6. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2013-08-01

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

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

    PubMed

    Faraji, Mohammad; Yamini, Yadollah; Shariati, Shahab

    2009-07-30

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

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

    PubMed

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

    2016-01-01

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

  10. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2009-06-01

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

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

    PubMed

    Mohr, Victoria; Miró, Manuel; Limbeck, Andreas

    2017-04-01

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

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

    SciTech Connect

    Msimanga, N.D.G.

    1992-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2009-06-01

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

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

    PubMed

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

    2015-01-01

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

  16. 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.

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

    PubMed

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

    2004-09-01

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

  18. 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.

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

    PubMed

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

    2004-05-01

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

  20. 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.

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

    PubMed

    Sadiq, Nausheen; Beauchemin, Diane

    2014-12-03

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

  2. 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

  3. 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).

  4. 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

  5. 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.

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

    PubMed

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

    2003-08-29

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

  7. 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.

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

    PubMed

    Ilander, Aki; Väisänen, Ari

    2007-10-29

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

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

    PubMed

    Ilander, Aki; Väisänen, Ari

    2009-08-01

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

  10. 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.

  11. 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).

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

    NASA Astrophysics Data System (ADS)

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

    2014-10-01

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

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

    PubMed

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

    1989-03-15

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

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

    PubMed

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

    2010-02-05

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

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

    PubMed

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

    2016-11-01

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

  16. 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.

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

    PubMed

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

    2011-01-01

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

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

    NASA Astrophysics Data System (ADS)

    Scheffler, Guilherme Luiz; Pozebon, Dirce

    2015-11-01

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

  19. 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.

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

    PubMed

    Garboś, Sławomir; Swiecicka, Dorota

    2011-01-01

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

  1. 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.

  2. 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.

  3. 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

  4. 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.

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

    PubMed

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

    2013-01-01

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

  6. 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.

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

    PubMed

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

    2003-10-01

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

  8. 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).

  9. 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.

  10. 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

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

    PubMed

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

    2017-04-01

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

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

    PubMed

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

    2006-02-28

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

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

    PubMed

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

    2017-05-15

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

  14. 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.

  15. 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.

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

    PubMed

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

    2007-01-09

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

  17. 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.

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

    PubMed

    Khalil, Sabry; Kelzieh, Ahmed

    2002-01-01

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

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

    PubMed

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

    2009-11-01

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

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

    PubMed

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

    2017-01-01

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

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

    ERIC Educational Resources Information Center

    Horlick, Gary

    1984-01-01

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

  2. 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

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

    NASA Astrophysics Data System (ADS)

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

    2011-06-01

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

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

    SciTech Connect

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

    1997-01-15

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

  5. 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.

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

    SciTech Connect

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

    2005-09-15

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

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

    DTIC Science & Technology

    1985-11-25

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

  8. 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.

  9. 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.

  10. 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)

  11. 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

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

    NASA Astrophysics Data System (ADS)

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

    2016-11-01

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

  13. 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.

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

    NASA Astrophysics Data System (ADS)

    Montaser, Akbar

    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.

  15. 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.

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

    PubMed

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

    2008-07-09

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

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

    PubMed

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

    2014-06-17

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

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

    PubMed

    Deng, B; Zhang, Z

    1998-10-01

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

  19. 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.

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

    PubMed

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

    2002-10-01

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

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

    PubMed

    Liu, Dong-yan; Zhang, Yuan-li

    2002-02-01

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

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

    PubMed

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

    2010-02-25

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

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

    NASA Astrophysics Data System (ADS)

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

    1997-05-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2000-06-01

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

  5. 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

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

    PubMed

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

    2007-04-15

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

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

    NASA Astrophysics Data System (ADS)

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

    1999-09-01

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

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

    PubMed

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

    2017-04-01

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

  9. 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...

  10. 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 ...

  11. 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…

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

    PubMed

    Flavelle, F; Westland, A D

    1986-05-01

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

  13. 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...

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

    NASA Astrophysics Data System (ADS)

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

    2012-10-01

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

  15. 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.

  16. 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.

  17. 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.

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

    NASA Astrophysics Data System (ADS)

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

    1997-04-01

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

  19. 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.

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

    PubMed Central

    Park, Jonghoo; Blick, Robert H.

    2016-01-01

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

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

    EPA Pesticide Factsheets

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

  2. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2004-12-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-11-01

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

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

    PubMed

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

    2011-08-01

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

  6. 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.

  7. 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.

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

    PubMed

    Purawatt, Sopon; Siripinyanond, Atitaya; Shiowatana, Juwadee

    2007-10-01

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

  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. 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.

  11. 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.

  12. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

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

  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.

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

    PubMed

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

    2017-05-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2000-10-01

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

  17. 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.

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

    ERIC Educational Resources Information Center

    Smith, Gregory D.; And Others

    1995-01-01

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

  19. 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.

  20. 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.

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

    PubMed

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

    2008-07-15

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

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

    NASA Astrophysics Data System (ADS)

    Schaefer, Klaus; Heland, Joerg

    1999-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2011-12-01

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

  5. 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.

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

    NASA Astrophysics Data System (ADS)

    Luc, Paul

    1995-07-01

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

  8. 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.

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

    PubMed

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

    2007-02-15

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

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

    PubMed

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

    2015-01-20

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

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

    NASA Astrophysics Data System (ADS)

    Montaser, A.

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

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

    PubMed

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

    2015-01-01

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

  13. 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.

  14. On-line complexation/cloud point preconcentration for the sensitive determination of dysprosium in urine by flow injection inductively coupled plasma-optical emission spectrometry.

    PubMed

    Ortega, Claudia; Cerutti, Soledad; Olsina, Roberto A; Silva, María F; Martinez, Luis D

    2003-01-01

    An on-line dysprosium preconcentration and determination system based on the hyphenation of cloud point extraction (CPE) to flow injection analysis (FIA) associated with ICP-OES was studied. For the preconcentration of dysprosium, a Dy(III)-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex was formed on-line at pH 9.22 in the presence of nonionic micelles of PONPE-7.5. The micellar system containing the complex was thermostated at 30 degrees C in order to promote phase separation, and the surfactant-rich phase was retained in a microcolumn packed with cotton at pH 9.2. The surfactant-rich phase was eluted with 4 mol L(-1) nitric acid at a flow rate of 1.5 mL min(-1), directly in the nebulizer of the plasma. An enhancement factor of 50 was obtained for the preconcentration of 50 mL of sample solution. The detection limit value for the preconcentration of 50 mL of aqueous solution of Dy was 0.03 microg L(-1). The precision for 10 replicate determinations at the 2.0 microg L(-1)Dy level was 2.2% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for dysprosium was linear with a correlation coefficient of 0.9994 at levels near the detection limits up to at least 100 microg L(-1). The method was successfully applied to the determination of dysprosium in urine.

  15. 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.

  16. 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.

  17. 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)

  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. Atomic Absorption Spectroscopy, Atomic Emission Spectroscopy, and Inductively Coupled Plasma-Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Miller, Dennis D.; Rutzke, Michael A.

    Atomic spectroscopy has played a major role in the development of our current database for mineral nutrients and toxicants in foods. When atomic absorption spectrometers became widely available in the 1960s, the development of atomic absorption spectroscopy (AAS) methods for accurately measuring trace amounts of mineral elements in biological samples paved the way for unprecedented advances in fields as diverse as food analysis, nutrition, biochemistry, and toxicology (1). The application of plasmas as excitation sources for atomic emission spectroscopy (AES) led to the commercial availability of instruments for inductively coupled plasma - atomic emission spectroscopy (ICP-AES) beginning in the late 1970s. This instrument has further enhanced our ability to measure the mineral composition of foods and other materials rapidly, accurately, and precisely. More recently, plasmas have been joined with mass spectrometers (MS) to form inductively coupled plasma-mass spectrometer ICP-MS instruments that are capable of measuring mineral elements with extremely low detection limits. These three instrumental methods have largely replaced traditional wet chemistry methods for mineral analysis of foods, although traditional methods for calcium, chloride, iron, and phosphorus remain in use today (see Chap. 12).

  20. Highly Simple Deep Eutectic Solvent Extraction of Manganese in Vegetable Samples Prior to Its ICP-OES Analysis.

    PubMed

    Bağda, Esra; Altundağ, Hüseyin; Soylak, Mustafa

    2017-02-23

    In the present work, simple and sensitive extraction methods for selective determination of manganese have been successfully developed. The methods were based on solubilization of manganese in deep eutectic solvent medium. Three deep eutectic solvents with choline chloride (vitamin B4) and tartaric/oxalic/citric acids have been prepared. Extraction parameters were optimized with using standard reference material (1573a tomato leaves). The quantitative recovery values were obtained with 1.25 g/L sample to deep eutectic solvent (DES) volume, at 95 °C for 2 h. The limit of detection was found as 0.50, 0.34, and 1.23 μg/L for DES/tartaric, DES/oxalic, and DES/citric acid, respectively. At optimum conditions, the analytical signal was linear for the range of 10-3000 μg/L for all studied DESs with the correlation coefficient >0.99. The extraction methods were applied to different real samples such as basil herb, spinach, dill, and cucumber barks. The known amount of manganese was spiked to samples, and good recovery results were obtained.

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

    PubMed

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

    2014-01-02

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

  2. Microplasma source based on a dielectric barrier discharge for the determination of mercury by atomic emission spectrometry.

    PubMed

    Zhu, Zhenli; Chan, George C-Y; Ray, Steven J; Zhang, Xinrong; Hieftje, Gary M

    2008-11-15

    A low-power, atmospheric-pressure microplasma source based on a dielectric barrier discharge (DBD) has been developed for use in atomic emission spectrometry. The small plasma (0.6 mm x 1 mm x 10 mm) is generated within a glass cell by using electrodes that do not contact the plasma. Powered by an inexpensive ozone generator, the discharge ignites spontaneously, can be easily sustained in Ar or He at gas flow rates ranging from 5 to 200 mL min(-1), and requires less than 1 W of power. The effect of operating parameters such as plasma gas identity, plasma gas flow rate, and residual water vapor on the DBD source performance has been investigated. The plasma can be operated without removal of residual water vapor, permitting it to be directly coupled with cold vapor generation sample introduction. The spectral background of the source is quite clean in the range from 200 to 260 nm with low continuum and structured components. The DBD source has been applied to the determination of Hg by continuous-flow, cold vapor generation and offers detection limits from 14 (He-DBD) to 43 pg mL(-1) (Ar-DBD) without removal of the residual moisture. The use of flow injection with the He-DBD permits measurement of Hg with a 7.2 pg limit of detection, and with repetitive injections having an RSD of <2% for a 10 ng mL(-1) standard.

  3. 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.

  4. In situ determination of uranium in soil by laser ablation-inductively coupled plasma atomic emission spectrometry

    SciTech Connect

    Zamzow, D.S.; Baldwin, D.P.; Weeks, S.J.; Bajic, S.J.; D'Silva, A.P. )

    1994-02-01

    The concentration of uranium in soil has been determined for 80 sites in an area suspected to have uranium contamination by in situ laser ablation - inductively coupled plasma atomic emission spectrometry (LA-ICPAES), utilizing a field-deployable mobile analytical laboratory. For 15 of the 80 sites analyzed, soil samples are collected so that the field LA-ICPAES results could be compared to laboratory-determined values. Uranium concentrations determined in the field by LA-ICPAES for these 15 sites range from <20 parts per million (ppm) by weight to 285 ppm. The uncertainty in the values determined, however, is large relative to the uranium concentrations encountered at this site. The 95% confidence interval (CI) values are approximately 85 ppm. The uranium concentrations determined by laboratory LA-ICPAES analysis range from <20 to 102 ppm (95% CI of approximately 50 ppm); microwave dissolution and subsequent standard addition determination of uranium by solution nebulization ICPAES using an ultrasonic nebulizer yields 19-124 ppm uranium (95% CI of approximately 10 ppm). For 11 of the 15 samples, the field- and laboratory-determined uranium concentrations agree, within the uncertainty of the determined values. 19 refs., 5 figs., 3 tabs.

  5. Determination of metal impurities in advanced lead zirconate titanate ceramics by axial view mode inductively coupled plasma optical emission spectrometry.

    PubMed

    Villanueva Tagle, M E; Larrea Marín, M T; Martin Gavilán, O; Durruthy Rodríguez, M D; Calderón Piñar, F; Pomares Alfonso, M S

    2012-05-30

    An inductively coupled plasma optical emission spectrometry quantification method for the determination of Al, Ca, Cr Cu, Fe, Mn, Mg, Ni, Zn, Ba, K, In and Co in lead zirconate-titanate (PZT) ceramics, modified with strontium and chromium, was developed. Total digestion of ceramics was achieved with a HNO(3), H(2)O(2) and HF (ac) mixture by using a microwave furnace. The sensitivity of the net signal intensity respect to radiofrequency power (P) and nebulizer argon flow (F(N)) variations was strongly dependent of the total excitation energy of line (TEE). For lines with TEE near metastable atoms and ions of argon, an increment of the sensitivities to P and F(N) variation was observed. At robust plasma conditions the matrix effect was reduced for all matrices and analytes considered. The precision of analysis ranged from 3 to 13%, whereas the analytes recoveries in the spiked samples varied, mostly, from 90 to 110%. The detection limits of studied elements were from 0.004 to 10 mg kg(-1).

  6. 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).

  7. 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.

  8. Simultaneous multielemental analysis of some environmental and biological samples by inductively coupled plasma atomic emission spectrometry

    SciTech Connect

    Hee, S.S.Q.; Boyle, J.R.

    1988-05-15

    The Parr bomb technique is found to be the preferred acid digestion method for multielemental analysis by simultaneous inductively coupled plasma atomic emission spectroscopy (ICP-AES) when compared with microwave and hot plate methods for many environmental and biological specimens, but especially for the latter. One digestion alone often did not produce quantitative results compared with a sequential digestion scheme. The digestions were then refined to be as similar as possible for the various substrates studied. The interference of carbon on As and Se had to be corrected at less than or equal to 3000 ..mu..g of C/mL in the analysis solution, and thus the C content had to be monitored to assess the efficiency of the digestions and to determine if interelemental correction for C presence was required. The C correction was adequate in the range 3000-10,000 ..mu..g of C/ml. The use of modified k values was demonstrated to provide accuracy and had to be used for ICP-AES spectrometers where background corrections were performed first for fixed channels. The results on Cincinnati soils and feces of Cincinnati children showed that Si and Ti were possible tracer elements for soil ingestion by the children.

  9. 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.

  10. A Multi-Pumping Flow System for In Situ Measurements of Dissolved Manganese in Aquatic Systems

    PubMed Central

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

    2016-01-01

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

  11. A Multi-Pumping Flow System for In Situ Measurements of Dissolved Manganese in Aquatic Systems.

    PubMed

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

    2016-11-30

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

  12. 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.

  13. 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.

  14. A photon counting dynamic digital lock-in amplifier for background suppression in glow discharge atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Gökmen, Ali; Ulgen, Ahmet; Yalçin, Şerife

    1996-01-01

    A photon counting dynamic digital lock-in amplifier, (PC-DDLIA), has been developed for the suppression of Ar lines in glow discharge lamp atomic emission spectrometry, (GDL-AES). The experimental set-up consists of a Grimm-type GDL, a prism-type scanning monochromator, photon counting electronics, an Apple Ile computer with an interface card and a computer controllable high voltage power supply. The photon counting electronics are designed to convert the photon pulses to logic pulses. A discriminator is used to reject pulses below a threshold level. The high voltage power supply is modulated with a square waveform generated from DAC and photon pulses are counted synchronously by the timer/counter chip, versatile interface adaptor (VIA-6522) on the interface card of computer. The data are analyzed in two steps. In the "learn mode", the GDL is modulated with a square waveform between 370 and 670 V and two spectra consisting of only Ar lines are obtained in a spectral window between 287.1 and 290.0 nm. A new modulation waveform is computed from these spectra which yields two overlapped spectra when the PC-DDLIA is scanned over the same spectral window. In the "analysis mode" of data acquisition, a target material with the analyte element(s) in it is used and the spectrometer is scanned with a dynamically varying rectangular waveform over the same spectral window. The net spectrum consists of pure atomic lines free from any Ar lines. The detection limit for the determination of Si (288.2 nm) in the presence of interfering Ar lines (288.1 and 288.4 nm) is found to be 0.083%, whereas suppression of Ar lines over the same spectral window lowers the detection limit to 0.013%.

  15. [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

  16. A novel approach for reducing toxic emissions during high temperature processing of electronic waste.

    PubMed

    Saini, R; Khanna, R; Dutta, R K; Cayumil, R; Ikram-Ul-Haq, M; Agarwala, V; Ellamparuthy, G; Jayasankar, K; Mukherjee, P S; Sahajwalla, V

    2017-03-09

    A novel approach is presented to capture some of the potentially toxic elements (PTEs), other particulates and emissions during the heat treatment of e-waste using alumina adsorbents. Waste PCBs from mobile phones were mechanically crushed to sizes less than 1mm; their thermal degradation was investigated using thermo-gravimetric analysis. Observed weight loss was attributed to the degradation of polymers and the vaporization of organic constituents and volatile metals. The sample assembly containing PCB powder and adsorbent was heat treated at 600°C for times ranging between 10 and 30min with air, nitrogen and argon as carrier gases. Weight gains up to ∼17% were recorded in the adsorbent thereby indicating the capture of significant amounts of particulates. The highest level of adsorption was observed in N2 atmosphere for small particle sizes of alumina. SEM/EDS results on the adsorbent indicated the presence of Cu, Pb, Si, Mg and C. These studies were supplemented with ICP-OES analysis to determine the extent of various species captured as a function of operating parameters. This innovative, low-cost approach has the potential for utilization in the informal sector and/or developing countries, and could play a significant role in reducing toxic emissions from e-waste processing towards environmentally safe limits.

  17. Energy-dispersive X-ray spectrometry combined with directly suspended droplet microextraction for determination of dissolved silicate in surface water via silicomolybdenum blue complex.

    PubMed

    Pytlakowska, Katarzyna

    2014-10-01

    Energy-dispersive X-ray fluorescence spectrometry (EDXRF) is a well-established analytical technique successfully applied with good precision and accuracy to determination of many elements. However, in the case of elements of low atomic number, such as silicon, direct determination is hampered due to low fluorescence yield and relatively low energy easily absorbed by sample matrix. An indirect method for determining surface water silicate is thus proposed. The method is based on silicate determination via molybdenum present in silicomolybdenum blue complex. Determination follows directly suspended droplet microextraction. Optimum conditions for both microextraction and EDXRF measurement were studied. A good ratio of silicon to molybdenum (1-41) and a sensitive Kα line of molybdenum make it possible to determine low concentrations of silicate. Under optimized conditions, good linearity, up to 3 μg mL(-1) (r=0.9990), and good detection limit (6 ng mL(-1)) were achieved. The total RSD for the EDXRF determination of silicate following DSDME was 6.7%. Taking into account all steps preceding the determination and the uncertainty of XRF measurements, the proposed method can be recognized as precise. The enrichment factor was 140. The developed method was used to determine dissolved silicate content in surface water samples. The accuracy and repeatability of the proposed procedure were checked by standard addition method and compared to the results obtained using ICP-OES technique. The recovery (92.2-96%) was satisfactory and indicates usefulness of the developed procedure.

  18. Investigations on the conditional kinetic and thermodynamic stability of aquatic humic substance-metal complexes by means of EDTA exchange, ultrafiltration and atomic spectrometry.

    PubMed

    Van den Bergh, J; Jakubowski, B; Burba, P

    2001-09-13

    The conditional metal availability and the kinetic stability of humic substance-metal species in humic-rich waters (e.g. bog water) was characterized by means of EDTA exchange. For this purpose a combined procedure consisting of time-controlled ligand exchange by EDTA, species differentiation by a fast single-stage tangential-flow ultrafiltration (TF-UF) technique (cut-off 1 kDa) and sensitive atomic spectrometry methods (e.g. AAS, ICP-OES, TXRF) was developed. The kinetics and the yield of the EDTA exchange served as operational parameters for assessing the kinetic stability and EDTA availability of HS-metal species, respectively. Considerable fractions of natural HS-metal species studied were shown to be EDTA-inert (e.g. 31% of the total Fe, 44% of the total Al) even after long reaction times (48 h), in contrast to artificial ones formed in solutions of isolated HS. Moreover, the conditional thermodynamic stability of HS-metal complexes formed by successive loading of an aquatic reference HS (HO14) with a number of heavy metal ions (e.g. Cr(III), Cu(II), Fe(III), Mn(II), Zn(II)) was also evaluated discriminating the free metal concentrations by means of TF-UF. In addition, from the loading isotherms obtained conditional complexation capacities could be derived for the studied HS exhibiting the order Fe(III)>Cu(II)>Cr(III)>Co(II)>Mn(II).

  19. 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

  20. 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.

  1. Emission mechanism of polyatomic ions Cs2Cl+ and Cs2BO2(+) in thermal ionization mass spectrometry with various carbon materials.

    PubMed

    Wei, Hai-Zhen; Jiang, Shao-Yong; Hemming, Gary N; Yang, Jing-Hong; Xiao, Ying-Kai; Yang, Tao; Yan, Xiong; Yan, Yan

    2011-12-29

    The emission behavior of polyatomic ions Cs(2)Cl(+) and Cs(2)BO(2)(+) in the presence of various carbon materials (Graphite, Carbon, SWNTs, and Fullerenes) in the ionization source of thermal ionization mass spectrometry (TIMS) has been investigated. The emission capacity of various carbon materials are remarkably different as evidenced by the obvious discrepancy in signal intensity of polyatomic ions and accuracy/precision of boron and chlorine isotopic composition determined using Cs(2)Cl(+)-graphite-PTIMS/Cs(2)BO(2)(+)-graphite-PTIMS methods. Combined with morphology and microstructure properties of four selected carbon materials, it could be concluded that the emission behavior of the polyatomic ions strongly depends on the microstructure of the carbon materials used. A surface-induced collision mechanism for formation of such kinds of polyatomic ions in the ionization source of TIMS has been proposed based on the optimized configuration of Cs(2)BO(2)(+) and Cs(2)Cl(+) ions in the gas phase using a molecular dynamics method. The combination of the geometry of the selected carbon materials with the configuration of two polyatomic ions explains the structure effect of carbon materials on the emission behavior of polyatomic ions, where graphite samples with perfect parallels and equidistant layers ensure the capacity of emission to the maximum extent, and fullerenes worsen the emission of polyatomic ions by blocking their pathway.

  2. Simultaneous determination of trace heavy metals in ambient aerosols by inductively coupled plasma atomic emission spectrometry after pre-concentration with sodium diethyldithiocarbamate.

    PubMed

    Talebi, S M; Malekiha, M

    2008-07-01

    The simultaneous determination of heavy metals associated with airborne particulate matter in the atmosphere of the city Isfahan (Iran) was performed by inductively coupled plasma atomic emission spectrometry (ICP-AES) after pre-concentration with sodium diethyldithiocarbamate. The preconcentration procedure developed found instrumental to determine the trace heavy metals associated with ambient aerosols collected at a short sampling period or collected from rural areas where the concentrations of these metals are much less than those in urban areas. Several samples were analyzed by both flame atomic absorption spectrometry (FAAS) as a conventional method and the proposed method. The results obtained by the two methods were found in good agreement. The method was applied to the determination of atmospheric level of heavy metals in rural area and also for study of variation in levels of heavy metals in urban atmosphere during the days and nights.

  3. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2001-09-01

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

  5. On-line monitoring of pine needles combustion emissions in the presence of fire retardant using a "thermogravimetry (TG)-bridge/mass spectrometry method".

    PubMed

    Tzamtzis, N; Karma, S; Pappa, A; Statheropoulos, M

    2006-07-28

    In this work a new method called TG-bridge/mass spectrometry is presented, for the on-line monitoring of the pine needles combustion emissions in a common lab furnace. The TG-bridge (thermogravimetry-bridge) system has been developed in-house as a TG-MS (thermogravimetry-mass spectrometry) interface, for TG-MS analysis. In this work, TG-bridge was used for directly sampling of the combustion emissions from the inside of the furnace and transferring them into the mass spectrometer (MS), without disturbing the sub-pressure conditions inside the MS ion source. The effect of Fire-Trol 931 (a long-term fire retardant) on the emissions, produced during the combustion of pine needles, is tested in the lab for future application in the field. It was shown that in treated samples, increased evolution of ammonia and aromatic compounds took place, compared to untreated samples. Maximum concentrations of specific compounds, such as benzene and toluene, evolved during the combustion experiments in the furnace, were determined.

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

    PubMed

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

    1992-07-01

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

  7. Development and fundamental investigation of Laser Ablation Glow Discharge Time-Of-Flight Mass Spectrometry (LA-GD-TOFMS)

    NASA Astrophysics Data System (ADS)

    Tarik, Mohamed; Lotito, Giovanni; Whitby, James A.; Koch, Joachim; Fuhrer, Katrin; Gonin, Marc; Michler, Johann; Bolli, Jean-Luc; Günther, Detlef

    2009-03-01

    Glow Discharge (GD) spectroscopy is a well known and accepted technique for the bulk and surface composition analysis, while laser ablation (LA) provides analysis with high spatial-resolution analysis in LIBS (laser-induced breakdown spectroscopy) or when coupled to inductively coupled plasma spectrometry (ICP-OES or ICP-MS). This work concerns the construction of a Laser Ablation Glow Discharge Time-Of-Flight Mass Spectrometry (LA-GD-TOFMS) instrument to study the analytical capabilities resulting from the interaction of a laser-generated sample plume with a pulsed glow discharge. Two ablation configurations were studied in detail. In a first approach, the laser-generated plume was introduced directly into the GD, while the second approach generated the plume inside the GD. The ablated material was introduced at different times with respect to the discharge pulse in order to exploit the efficient ionization in the GD plasma. For both LA-GD configurations, direct ablation into the afterglow of the pulsed glow discharge leads to an ion signal enhancement of up to a factor of 7, as compared to the ablation process alone under the same experimental conditions. The LA-GD enhancement was found to occur exclusively in the GD afterglow, with a maximum ablation S/N occurring in a few hundred microseconds after the termination of the glow discharge. The duration of the enhanced signal is about two milliseconds. Both the laser pulse energy and the position of the ablation plume (with respect to the sampling orifice) were found to affect the amount of mass entering the afterglow region and consequently, the enhancement factor of ionization.

  8. 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

  9. 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%.

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

    PubMed

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

    2016-02-02

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

  11. 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.

  12. Lanthanoides in Glass and Glass Ceramics

    NASA Astrophysics Data System (ADS)

    Meinhardt, Jürgen; Kilo, Martin; Somorowsky, Ferdinand; Hopp, Werner

    2017-03-01

    Many types of glass contain lanthanoides; among them, special glass for optical applications is the one with the highest content of lanthanoides. The precise determination of the lanthanoides' concentration is performed by inductively coupled plasma-optical emission spectrometry (ICP-OES). However, up to now, there are no established standard processes guaranteeing a uniform approach to the lanthanoide analysis. The knowledge of the lanthanoides' concentrations is necessary on the microscale in some cases, especially if a suitable separation and recycling procedure is to be applied. Here, the analysis is performed by energy-dispersive X-ray (EDX) or wavelength-dispersive X-ray (WDX) analytics in the scanning electron microscope.

  13. 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.

  14. 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…

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

    NASA Astrophysics Data System (ADS)

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

    2017-01-01

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

  16. Use of gradient dilution to flag and overcome matrix interferences in axial-viewing inductively coupled plasma-atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Cheung, Yan; Schwartz, Andrew J.; Hieftje, Gary M.

    2014-10-01

    Despite the undisputed power of inductively coupled plasma-atomic emission spectrometry (ICP-AES), its users still face serious challenges in obtaining accurate analytical results. Matrix interference is perhaps the most important challenge. Dilution of a matrix-containing sample is a common practice to reduce matrix interference. However, determining the optimal dilution factor requires tedious and time-consuming offline sample preparation, since emission lines and the effect of matrix interferences are affected differently by the dilution. The current study exploits this difference by employing a high-performance liquid chromatography gradient pump prior to the nebulizer to perform on-line mixing of a sample solution and diluent. Linear gradient dilution is performed on both the calibration standard and the matrix-containing sample. By ratioing the signals from two emission lines (from the same or different elements) as a function of dilution factor, the analyst can not only identify the presence of a matrix interference, but also determine the optimal dilution factor needed to overcome the interference. A ratio that does not change with dilution signals the absence of a matrix interference, whereas a changing ratio indicates the presence of an interference. The point on the dilution profile where the ratio stabilizes indicates the optimal dilution factor to correct the interference. The current study was performed on axial-viewing ICP-AES with o-xylene as the solvent.

  17. 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

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

    PubMed

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

    2001-12-01

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

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

    PubMed

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

    1976-12-01

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

  20. Direct determination of trace elements in niobium, tantalum and their oxides by inductively coupled plasma atomic emission spectrometry after microwave dissolution

    NASA Astrophysics Data System (ADS)

    Grebneva, O. N.; Kubrakova, I. V.; Kudinova, T. F.; Kuz'min, N. M.

    1997-07-01

    Analytical schemes for the determination of trace elements in high-purity niobium, tantalum and their oxides are proposed. The schemes are based on microwave dissolution of the metals and oxides followed by inductively coupled plasma atomic emission spectrometry (ICP-AES) determination of impurities in the solutions. The possibilities of interelement and off-peak background corrections in ICP-AES analysis are discussed. The accuracy of the results obtained is confirmed by the determination of trace elements after a matrix sorption separation procedure. For a number of elements, a comparison of the results obtained by ICP-AES without and with the matrix separation procedure and by electrothermal atomic absorption spectrometry (ETAAS) shows good agreement. The limits of detection for direct ICP-AES determination are in the range 0.4*1.0 μg g -1 for Ba, Ca, Fe, Mg, Mn, Y and La; between 2.0 and 10.0 μ g -1 for B, Cd, Co, Cr, Cu, Hf, Mo, Na, Nb, Ni, Pb, Sr, Ti, Zr and Ta; and for K, Sb and W a detection limit of 20 μ g -1 is achieved. The schemes proposed are intended for rapid routine analysis.

  1. Development and Characterization of a 9-mm Inductively Coupled Argon Plasma (ICP) Source for Atomic Emission Spectrometry.

    DTIC Science & Technology

    1980-09-30

    plus inter- fereni (S.,0:l ol; raio Pal :Ca). Rcati\\,e :;talcs X , 10" V. I0(’ V - ,. ’::ire tO. lffect of P0,, on Ca 11 (393.4 tin) emission profiles...mL- I of Ca while 10 curve B is from tile same solution but with phosphate added at a molar ratio of 50 to 1 (P0 4 : Ca). Profile X was obtained at...emission profiles with changing rf power levels klramne X , 500 W; Y, 750 W). Curve A represcnts amalytc (50 jig mLŕ Ca) signal and curve B awi ]ytc

  2. Evolution of In-Cylinder Diesel Engine Soot and Emission Characteristics Investigated with Online Aerosol Mass Spectrometry.

    PubMed

    Malmborg, V B; Eriksson, A C; Shen, M; Nilsson, P; Gallo, Y; Waldheim, B; Martinsson, J; Andersson, Ö; Pagels, J

    2017-02-07

    To design diesel engines with low environmental impact, it is important to link health and climate-relevant soot (black carbon) emission characteristics to specific combustion conditions. The in-cylinder evolution of soot properties over the combustion cycle and as a function of exhaust gas recirculation (EGR) was investigated in a modern heavy-duty diesel engine. A novel combination of a fast gas-sampling valve and a soot particle aerosol mass spectrometer (SP-AMS) enabled online measurements of the in-cylinder soot chemistry. The results show that EGR reduced the soot formation rate. However, the late cycle soot oxidation rate (soot removal) was reduced even more, and the net effect was increased soot emissions. EGR resulted in an accumulation of polycyclic aromatic hydrocarbons (PAHs) during combustion, and led to increased PAH emissions. We show that mass spectral and optical signatures of the in-cylinder soot and associated low volatility organics change dramatically from the soot formation dominated phase to the soot oxidation dominated phase. These signatures include a class of fullerene carbon clusters that we hypothesize represent less graphitized, C5-containing fullerenic (high tortuosity or curved) soot nanostructures arising from decreased combustion temperatures and increased premixing of air and fuel with EGR. Altered soot properties are of key importance when designing emission control strategies such as diesel particulate filters and when introducing novel biofuels.

  3. 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

  4. 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.

  5. 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

  6. 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.

  7. 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.

  8. Surface modification of hexatriacontane by CF_4 plasmas studied by optical emission and threshold ionization mass spectrometries

    NASA Astrophysics Data System (ADS)

    Poncin-Epaillard, F.; Wang, W.; Ausserré, D.; Scharzenbach, W.; Derouard, J.; Sadeghi, N.

    1998-11-01

    The behavior of tetrafluoromethane microwave plasma (2% argon included) has been studied by emission spectroscopy during the treatment of hexatriacontane, a model for high density polyethylene. The evolution of the densities of F* atoms, and CF, CF^*2, radicals has been followed by using the actinometric technique with 2% argon added to the gas. The surface properties, such as surface energy and surface roughness were correlated to the emission intensity of reactives species in the plasma gas phase. We found that the evolution of the fluorinated species emissions in the plasma gas phase can be a direct indication of the surface modifications by the plasma. A mild exposure to the plasma can result in a great decrease of surface energy corresponding to the fluorination. The surface roughness only changes under drastic plasma conditions. Threshold ionization mass spectroscopy is applied to detect the fluorine atoms and CFx radicals. Time resolved measurements in pulsed plasma, give access to the decay rate of F atoms concentration in the afterglow, and to their sticking coefficient on different surfaces. The influences of the discharge parameters and of the surfaces (metal, silicon or hexatriacontane) in contact with the plasma are investigated. The results show that the plasma generated ions and/or UV radiations highly enhance the reactivity of the F atoms on polymer surface.

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

    SciTech Connect

    Luan, Shen

    1995-10-06

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

  10. Signal enhancement in solution-cathode glow discharge — optical emission spectrometry via low molecular weight organic compounds

    NASA Astrophysics Data System (ADS)

    Doroski, Todd A.; Webb, Michael R.

    2013-10-01

    HCOOH, CH3COOH, and CH3CH2OH were used as chemical modifiers in a solution-cathode glow discharge. Emission was measured directly from the discharge, without a gas-liquid separator or a secondary excitation source. Emission from Ag, Se, Pb, and Hg was strongly enhanced, and the detection limits (DL) for these elements were improved by up to an order of magnitude using a combination of HCOOH and HNO3 compared to using HNO3 alone. The DL was measured for Mg (1 μg/L), Fe (10 μg/L), Ni (6 μg/L), Cu (6 μg/L), Pb (1 μg/L), Ag (0.1 μg/L), Se (300 μg/L), and Hg (2 μg/L). Coefficients of determination (R2) were between 0.9986 and 0.9999. A voltage of 1 kV was used, which produced a current of approximately 70 mA.

  11. A Comparative Analysis of Caries Inhibitory Effect of Remineralizing Agents on Human Enamel Treated With Er:YAG Laser: An In-vitro Atomic Emission Spectrometry Analysis

    PubMed Central

    Nair, Aswin Saseendran; Kumar, R Krishna; Ahameed, Syed Shaheed; Punnathara, Sairaj; Peter, Joby

    2016-01-01

    Introduction The tug of war to maintain tooth integrity is dependent on a ratio between demineralization and remineralization. Hence, demineralization should be retarded and remineralization should be enhanced to maintain a natural equilibrium in the oral cavity. Aim To compare in-vitro acid resistance of human enamel when using Casein Phosphopeptides Amorphous Calcium Phosphate (CPP-ACP) [GC Tooth mousse] cream, Casein Phosphopeptide Amorphous Calcium Fluoride Phosphate (CPP-ACFP) [GC Tooth mousse plus] cream, Er:YAG laser alone, combination of CPP-ACP with Er:YAG laser, CPP-ACFP with Er:YAG laser. Materials and Methods An in-vitro study was done on 100 specimens which were prepared from 50 human premolars to investigate the caries inhibitory effect of remineralizing agents and laser on enamel using an atomic emission spectrometry analysis. The enamel specimens were randomly allocated into 6 groups: Untreated (control); CPP-ACP (GC Tooth mousse); CPP-ACFP (GC Tooth mousse plus); Er:YAG laser treatment alone; CPP-ACP with Er:YAG laser; CPP-ACFP with Er: YAG laser. Then specimens were immersed individually in 5ml of acetate buffer solution (0.1mol/L, pH 4.5) and incubated at 37°C for 24 hours, to determine the acid resistance by analyzing the calcium release using atomic emission spectrometry. An ANOVA model was constructed (p-value 0.05), followed by post-hoc Tukey’s test for multiple pair wise comparisons of mean values. Results There was a significant difference among the various groups with respect to amount of calcium released (p<0.001). The lowest mean score of calcium release was observed for CPP-ACFP with Er:YAG laser followed by CPP-ACFP but the differences between these groups were statistically not significant (p>0.05). Similarly the differences between CPP-ACP with Er:YAG laser and CPP-ACP also were not significant (p>0.05). The highest mean score of calcium release was for Er:YAG laser and no significant statistical difference was noticed in

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

    NASA Astrophysics Data System (ADS)

    Matusiewicz, Henryk; Barnes, Ramon M.

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

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

    PubMed

    Roelandts, I; Robaye, G; Delbrouck-Habaru, J M; Weber, G

    1996-03-01

    The direct non-destructive proton-induced gamma-ray emission (PIGE) technique with a germanium detector was applied to the determination of total fluorine concentration in five coal reference materials (BCR 40, NIST 1632b, NIST 1635, SARM 20 and USGS CLB-1). Duplicate analyses were made from five randomly selected bottles of each coal. Individual data are presented and some problems (calibration, proton stopping power, effects of sample heating by the proton beam, background estimation) which were encountered during this study are discussed. Sensitivity and reproducibility of the determinations, and homogeneity of the coal samples with respect to fluorine contents by analysis of variance were investigated. The present data are also compared with the few published values for these reference samples, including other PIGE data. The use of synthetic standards and spiked samples in the present study suggested that the PIGE method was more accurate than other techniques.

  14. [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.

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

    NASA Astrophysics Data System (ADS)

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

    2006-09-01

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

  16. Beryllium Limits of Detection and Spectral Interferences in 2 Per Cent Nitric Acid, Digested Air Filter Paper, and GHOSTWIPETM Matrices by Inductively Coupled Plasma Emission Spectrometry

    SciTech Connect

    Jurgensen, A.R.

    2004-02-13

    The Analytical Development Section (ADS) of the Savannah River Technology Center (SRTC) has been requested to perform beryllium (Be) analysis on digested Air Filter Paper and GHOSTWIPE (Trade Mark) samples by Inductively Coupled Plasma Emission Spectrometry (ICP-ES). One of the important figures of merit for this analysis is the detection limit (LOD), the smallest concentration of an element that can be detected with a defined certainty. To meet the site Industrial Hygiene (IH) requirements, an instrument LOD of 0.03 mg per Air Filter Paper (1 hr sample) and 0.2 mg per GHOSTWIPE (Trade Mark) must be demonstrated. Another important analytical parameter is the effect on the Be quantization from potential spectral interfering matrix elements. Any existing spectral overlaps could give false positives or increase the measured Be concentrations in these matrices. The purpose of this study was to document the Analytical Development Sections' s contained ICP-ES performance in these two areas. In addition, other Quality Control recommendations will be discussed.

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

    NASA Astrophysics Data System (ADS)

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

    2010-02-01

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

  18. 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.

  19. 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.

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

    PubMed

    Li, Qing; Zhang, Zhen; Wang, Zheng

    2014-10-03

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

  1. 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.

  2. Multi-element analysis using inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectroscopy for provenancing of animals at the continental scale.

    PubMed

    Kreitals, Natasha M; Watling, R John

    2014-11-01

    Chemical signatures within the environment vary between regions as a result of climatological, geochemical and anthropogenic influences. These variations are incorporated into the region's geology, soils, water and vegetation; ultimately making their way through the food chain to higher level organisms. Because the variation in chemical signatures between areas is significant, a specific knowledge of differences in elemental distribution patterns between, and within populations, could prove beneficial for provenancing animals or animal related products when applied to indigenous and feral faunal populations. The domestic pig (Sus scrofa domestica) was used as an investigative model to determine the feasibility of using a chemical traceability method for the provenance determination of animal tissue. Samples of pig muscle, tongue, stomach, heart, liver and kidney were collected from known farming areas around Australia. Samples were digested in 1:3 H2O2:HNO3 and their elemental composition determined using solution based Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Pigs from different growing regions in Australia could be distinguished based on the chemical signature of each individual tissue type. Discrimination was possible at a region, state and population level. This investigation demonstrates the potential for multi-element analysis of low genetic variation native and feral species of forensic relevance.

  3. 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.

  4. 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.

  5. 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.

  6. Comparative determination of Ba, Cu, Fe, Pb and Zn in tea leaves by slurry sampling electrothermal atomic absorption and liquid sampling inductively coupled plasma atomic emission spectrometry.

    PubMed

    Mierzwa, J; Sun, Y C; Chung, Y T; Yang, M H

    1998-12-01

    The comparative determination of barium, copper, iron, lead and zinc in tea leaf samples by two atomic spectrometric techniques is reported. At first, slurry sampling electrothermal atomization atomic absorption spectrometry (ETAAS) was applied. The results of Ba and Pb determination were calculated using the method of standard additions, and results of Cu, Fe and Zn from the calibration graphs based on aqueous standards. These results were compared with the results obtained after microwave-assisted wet (nitric+hydrochloric+hydrofluoric acids) digestion in closed vessels followed by inductively coupled plasma-atomic emission spectrometric (ICP-AES) determination with the calibration by means of aqueous standards. The exception was lead determined after a wet digestion procedure by ETAAS. The accuracy of the studied methods was checked by the use of the certified reference material Tea GBW-07605. The recoveries of the analytes varied in the range from 91 to 99% for slurry sampling ETAAS, and from 92.5 to 102% for liquid sampling ICP-AES. The advantages of slurry sampling ETAAS method are simplicity of sample preparation and very good sensitivity. Slurry sampling ETAAS method is relatively fast but if several elements must be determined in one sample, the time of the whole microwave-assisted digestion procedure and ICP-AES determination will be shorter. However, worse detection limits of ICP-AES must also be taken into the consideration in a case of some analytes.

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

    PubMed

    Kane, Peter F; Hall, William L

    2006-01-01

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

  8. Determination of rare earth elements in geological samples by inductively coupled plasma atomic emission spectrometry with flow injection liquid-liquid extraction.

    PubMed

    Xu, Zhifang; Liu, Congqiang; Zhang, Hongxiang; Ma, Yingjun; Lin, Soulin

    2003-12-01

    A direct sampling with organic solvent extracts for simultaneous multi-element determination implemented with inductively coupled plasma atomic emission spectrometry (ICP-AES) associated with a flow injection liquid-liquid extraction (FI-LLE) sample preconcentration method was studied. The "robustness" of the plasma discharge with tributyl phosphate (TBP) loading was diagnosed by using the Mg II 279.55 nm and Mg I 285.21 nm lines intensity ratio. A FI-LLE preconcentration system for rare earth elements (REEs)-nitrate-TBP was established by using a laboratory-designed phase separator. For these elements, an average sensitivity enhancement factor of 64 was obtained with respect to ICP-AES sampling with aqueous solutions. The precision of the method was characterized by a relative standard deviation (%RSD) of 1.8 - 5.2%. A throughput of 27 samples per hour can be achieved with an organic solvent consumption of less than 200 microl per determination. Good results were obtained for the analysis of standard reference materials.

  9. [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.

  10. 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.

  11. 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.

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

    PubMed

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

    2005-12-01

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

  13. A comparison of benthic foraminiferal Mn / Ca and sedimentary Mn / Al as proxies of relative bottom-water oxygenation in the low-latitude NE Atlantic upwelling system

    NASA Astrophysics Data System (ADS)

    McKay, C. L.; Groeneveld, J.; Filipsson, H. L.; Gallego-Torres, D.; Whitehouse, M. J.; Toyofuku, T.; Romero, O. E.

    2015-09-01

    Trace element incorporation into foraminiferal shells (tests) is governed by physical and chemical conditions of the surrounding marine environment, and therefore foraminiferal geochemistry provides a means of palaeo-oceanographic reconstructions. With the availability of high-spatial-resolution instrumentation with high precision, foraminiferal geochemistry has become a major research topic over recent years. However, reconstructions of past bottom-water oxygenation using foraminiferal tests remain in their infancy. In this study we explore the potential of using Mn / Ca determined by secondary ion mass spectrometry (SIMS) as well as by flow-through inductively coupled plasma optical emission spectroscopy (FT-ICP-OES) in the benthic foraminiferal species Eubuliminella exilis as a proxy for recording changes in bottom-water oxygen conditions in the low-latitude NE Atlantic upwelling system. Furthermore, we compare the SIMS and FT-ICP-OES results with published Mn sediment bulk measurements from the same sediment core. This is the first time that benthic foraminiferal Mn / Ca is directly compared with Mn bulk measurements, which largely agree on the former oxygen conditions. Samples were selected to include different productivity regimes related to Marine Isotope Stage 3 (35-28 ka), the Last Glacial Maximum (28-19 ka), Heinrich Event 1 (18-15.5 ka), Bølling Allerød (15.5-13.5 ka) and the Younger Dryas (13.5-11.5 ka). Foraminiferal Mn / Ca determined by SIMS and FT-ICP-OES is comparable. Mn / Ca was higher during periods with high primary productivity, such as during the Younger Dryas, which indicates low-oxygen conditions. This is further supported by the benthic foraminiferal faunal composition. Our results highlight the proxy potential of Mn / Ca in benthic foraminifera from upwelling systems for reconstructing past variations in oxygen conditions of the sea floor environment as well as the need to use it in combination with other proxy records such as faunal

  14. Determination of lithium and transition metals in Li1 Ni1/3 Co1/3 Mn1/3 O2 (NCM) cathode material for lithium-ion batteries by capillary electrophoresis.

    PubMed

    Vortmann-Westhoven, Britta; Lürenbaum, Constantin; Winter, Martin; Nowak, Sascha

    2017-02-01

    In this work, we present a novel electrophoretic method that was developed for the determination of lithium and transition metals in LiNi1/3 Co1/3 Mn1/3 O2 cathode material after microwave digestion. The cations in the digested LiNi1/3 Co1/3 Mn1/3 O2 material were separated by CE and the element content was determined by UV/Vis detection. To characterize the precision of the measurements, the RSDs and concentrations were calculated and compared to those obtained with ICP-optical emission spectrometry (ICP-OES). Furthermore, a certified reference material (BCR 176R-fly ash) was investigated for all techniques. For active material components, the LOD and LOQ were determined. The LODs and LOQs for the metals determined by CE were as follows: lithium (LOD/LOQ): 17.41/62.70 μg/L, cobalt (LOD/LOQ): 348.4/1283 μg/L, manganese (LOD/LOQ): 540.2/2095 μg/L, and nickel (LOD/LOQ): 838.0/2982 μg/L. Recovery rates for lithium were in the range of 95-103%. It could be proven that with the new technique, the results for the determination of the lithium content of active material were comparable with those obtained by ICP-OES and ion chromatography. Furthermore, the recovery rates of the transition metals were determined to be between 96 and 110% by CE and ICP-OES.

  15. 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.

  16. 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

  17. Determination of mercury, cadmium, lead, zinc, selenium and iron by ICP-OES in mushroom samples from around thermal power plant in Muğla, Turkey.

    PubMed

    Kula, Ibrahim; Solak, M Halil; Uğurlu, Mehmet; Işıloğlu, Mustafa; Arslan, Yasin

    2011-09-01

    Scleroderma verrucosum, Stropharia coronilla, Lactarius deterrimus, Chroogomphus rutilus, Russula delica, Laccaria laccata, Clitocybe odora var. alba, Lyophyllum decastes, Coprinus comatus, Helvella leucomelaena, Melanoleuca cognata, Melanoleuca cognata, Paxina acetabulum, Clitocybe vermicularis, Sarcosphaera crassa, Rhizopogon roseolu and Thelephora caryophyllea were collected from different localities in Muğla-Yatağan region of Turkey. Their trace metals concentrations were determined by ICPOES after microwave digestion. The results were 0.37 ± 0.01-5.28 ± 0.21 for cadmium, 467 ± 19-3,280 ± 131 for iron, 0.69 ± 0.03-9.15 ± 0.37 for lead, 18.70 ± 0.75-67.10 ± 2.68 for selenium, 75 ± 3-213 ± 8 for zinc and 0.15 ± 0.01-0.55 ± 0.01 for mercury (as μg/g). The detection limits for ICPOES were found as 0.25 for Cadmium, 0.2 for iron, 0.1 for lead, 0.5 for selenium, 0.2 for zinc and 0.03 for mercury (as mg L(-1)). The Relatively Standard Deviations (R.S.D.) were found below 4.0%. The accuracy of procedure was confirmed by certified reference material.

  18. 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.

  19. 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

  20. The Levels of Trace Elements in Honey and Molasses Samples That Were Determined by ICP-OES After Microwave Digestion Method.

    PubMed

    Altundag, Huseyin; Bina, Emel; Altıntıg, Esra

    2016-04-01

    The aim of this study is determining the amount of Al, Cu, Fe, Mn, Ni, Pb and Zn in samples of molasses and honey which were gathered from the Sakarya and Istanbul regions. In this study, trace elements in 8 honey and 20 molasses samples with different botanic features were evaluated. The sample preparation phase was performed via wet decomposition method and microwave digestion system. The accuracy of the method was checked by the standard reference material; tea leaves (INCY-TL-1) and NIST-SRM 1515-apple. The concentrations of essential trace elements (TEs) were observed in the range of 1.61 ± 0.01-287.03 ± 1.07; 0.21 ± 0.01-11.04 ± 0.12; 0.35 ± 0.03-21.71 ± 0.02 and 1.19 ± 0.01-60.90 ± 1.09 μg g(-1) for iron, copper, manganese and zinc ions, respectively, while the toxic element contents were observed in the range of 0.82 ± 0.17-3.06 ± 0.03; 0.04 ± 0.05-1.96 ± 0.03 and 0.62 ± 0.01-120.52 ± 0.10 μg g(-1) for lead, nickel and aluminum ions, respectively. The concentrations of basic TEs iron, copper, manganese and zinc were determined as 3.87 ± 0.04-16.76 ± 0.06; 0.45 ± 0.03-2.15 ± 0.01; 0.13 ± 0.01-15.02 ± 0.14 and 0.80 ± 0.09-12.03 ± 0.19 for honey samples. Also, toxic metal, lead, nickel and aluminum values in the honey samples were determined as 1.21 ± 0.12-2.46 ± 0.21; 0.28 ± 0.14-0.88 ± 0.43 and 2.11 ± 0.02-8.04 ± 0.08. A comparison between gathered data and literature values has performed and it is determined that such findings are suitable with the literature.

  1. 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.

  2. Assessment of the Effects Exerted by Acid and Alkaline Solutions on Bone: Is Chemistry the Answer?

    PubMed

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

    2017-02-01

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

  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. Evaluation and application of argon and helium microstrip plasma for the determination of mercury by the cold vapor technique and optical emission spectrometry.

    PubMed

    Jiménez Zapata, Israel; Pohl, Pawel; Bings, Nicolas H; Broekaert, José A C

    2007-08-01

    The suitability of a 2.45-GHz atmospheric pressure, low-power microwave microstrip plasma (MSP) operated with Ar and He for the determination of Hg by continuous-flow cold vapor (CV) generation, using SnCl2/HCl as the reducing agent, and optical emission spectrometry (OES) using a small CCD spectrometer was studied. The areas of stability for a discharge in the Ar and in the He MSP enclosed in a cylindrical channel in a quartz wafer were investigated. The excitation temperatures as measured for discharge gas atoms (Ar I, He I), and the electron number densities at 35-40 W and 15-400 mL min(-1) were found to be at the order of 3,200-5,500 K and 0.8x10(14)-1.6x10(14) cm(-3), respectively. The relative intensity of the Hg I 253.6-nm line and the signal-to-background ratio as a function of the forward power (35-40 W) as well as of the flow rate of the working gas (15-400 mL min(-1)) were evaluated and discussed. For the selected measurement conditions, the Ar MSP was established to have the lower detection limit for Hg (0.6 ng mL(-1)) compared with the He MSP. The linearity range is up to 300 ng mL(-1) and the precision is on the order of 1-3%. With the optimized CV Ar MSP-OES method a determination of Hg in spiked domestic and natural waters at concentration levels of 20-100 microg L(-1) and an accuracy of 1-4% could be performed. In an NIST domestic sludge standard reference material, Hg (3.64 microg g(-1)) could be determined with a relative standard deviation of 4% and an agreement better than 4%.

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

    NASA Astrophysics Data System (ADS)

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

    2009-06-01

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

  6. Optimized microwave-assisted decomposition method for multi-element analysis of glass standard reference material and ancient glass specimens by inductively coupled plasma atomic emission spectrometry.

    PubMed

    Zachariadis, G; Dimitrakoudi, E; Anthemidis, A; Stratis, J

    2006-02-28

    A novel microwave-assisted wet-acid decomposition method for the multi-element analysis of glass samples using inductively coupled plasma atomic emission spectrometry (ICP-AES) was developed and optimized. The SRM 621 standard reference glass material was used for this purpose, because it has similar composition with either archaeological glass specimens or common modern glasses. For the main constituents of SRM 621 (Ca, Na, Al, Fe, Mg, Ba and Ti), quality control data are given for all the examined procedures. The chemical and instrumental parameters of the method were thoroughly optimized. Thirteen acid mixtures of hydrochloric, nitric, and hydrofluoric acids in relation to two different microwave programs were examined in order to establish the most efficient protocol for the determination of metals in glass matrix. For both microwave programs, an intermediate step was employed with addition of H(3)BO(3) in order to compensate the effect of HF, which was used in all protocols. The suitability of the investigated protocols was evaluated for major (Ca, Na, Al), and minor (Fe, Mg, Ba, Ti, Mn, Cu, Sb, Co, Pb) glass constituents. The analytes were determined using multi-element matrix matched standard solutions. The analytical data matrix was processed chemometrically in order to evaluate the examined protocols in terms of their accuracy, precision and sensitivity, and eventually select the most efficient method for ancient glass. ICP-AES parameters such as spectral line, RF power and sample flow rate were optimized using the proposed protocol. Finally, the optimum method was successfully applied to the analysis of a number of ancient glass fragments.

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

    PubMed

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

    2004-07-01

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

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

    PubMed

    Johnson, K S; Laskin, A; Jimenez, J L; Shutthanandan, V; Molina, L T; Salcedo, D; Dzepina, K; Molina, M J

    2008-09-01

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

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

    PubMed

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

    2011-09-01

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

  10. 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

  11. A combined accelerator mass spectrometry-positron emission tomography human microdose study with 14C- and 11C-labelled verapamil

    PubMed Central

    Wagner, Claudia C; Simpson, Marie; Zeitlinger, Markus; Bauer, Martin; Karch, Rudolf; Abrahim, Aiman; Feurstein, Thomas; Schütz, Matthias; Kletter, Kurt; Müller, Markus; Lappin, Graham; Langer, Oliver

    2013-01-01

    Background and Objective In microdose studies, the pharmacokinetic (PK) profile of a drug in blood after administration of a dose up to 100 μg is measured with sensitive analytical techniques, such as accelerator mass spectrometry (AMS). As most drugs exert their effect in tissue rather than blood, methodology is needed for extending PK analysis to different tissue compartments. In the present study, we combined, for the first time, AMS analysis with positron emission tomography (PET) in order to determine the PK profile of the model drug verapamil in plasma and brain of humans. In order to assess PK dose-linearity of verapamil, data were acquired and compared after administration of an intravenous (iv) microdose and an iv microdose dosed concomitantly with an oral therapeutic dose. Methods Six healthy male volunteers received an iv microdose (0.05 mg) (period 1) and an iv microdose dosed concomitantly with an oral therapeutic dose (80 mg) of verapamil (period 2) in a randomized, cross-over, two-period study design. The iv dose was a mixture of (R/S)-[14C]verapamil and (R)-[11C]verapamil and the oral dose was unlabelled racemic verapamil. Brain distribution of radioactivity was measured with PET whereas plasma PK of (R)- and (S)-verapamil was determined with AMS. PET data were analyzed by kinetic modeling to estimate the rate constants for transfer of radioactivity across the blood-brain barrier. Results Most PK parameters of (R)- and (S)-verapamil as well as parameters describing exchange of radioactivity between plasma and brain (K1=0.030±0.003 and 0.031±0.005 mL·mL−1·min−1 and k2=0.099±0.006 and 0.095±0.008 min−1 for period 1 and 2, respectively) were not statistically different between the two periods although there was a trend for non-linear kinetics for the (R)-enantiomer. On the other hand, all PK parameters (except for t1/2) differed significantly between the (R)- and (S)-enantiomers for both periods. Cmax, AUC(0-24) and AUC(0-inf) were higher

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

    USGS Publications Warehouse

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

    2016-11-23

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

  13. 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.

  14. Fe3O4/salicylic acid nanoparticles versatility in magnetic mediated vascular nanoblockage

    NASA Astrophysics Data System (ADS)

    Mîndrilă, I.; Buteică, S. A.; Mihaiescu, D. E.; Badea, G.; Fudulu, A.; Mărgăritescu, D. N.

    2016-01-01

    An aqueous dispersion of Fe3O4/salicylic acid magnetic nanoparticles (SaMNPs) was synthesized by a modified Massart method, characterized by Inductively Coupled Plasma-Optic Emission Spectrometry (ICP-OES), High-Resolution Transmission Electron Microscopy (HRTEM) and Dynamic Light Scattering (DLS) methods, and tested on the chick chorioallantoic membrane (CAM) model to evaluate biocompatibility, biodistribution, intravascular time persistence, and ability to be magnetically target driven in order to block the blood supply into a tumor xenograft. ICP-OES, DLS, and HRTEM SaMNPs sample analyses showed a 0.356 mg/mL Fe concentration, a good stability in water (average Zeta potential of 39.3 mV), a hydrodynamic diameter around 52 nm and a core diameter in the 7-15 nm range for the Fe3O4 nanoparticles. In vivo CAM assay showed that SaMNPs were biocompatible with the chick embryo, were fixed almost completely by the liver, had no embolic potential, and a threshold-dose-dependent intravascular magnetic targeting time. Study on the CAM tumor model showed that SaMNPs could be used for long-term magnetically mediated nanoblocking of the capillary networks and 70-µm smaller arterioles.

  15. Assessment of the Bioaccessibility of Micronized Copper Wood on Simulated Stomach Fluid

    EPA Pesticide Factsheets

    The widespread use of copper-treated lumber has increased the potential for human exposure. Moreover, there is a lack of information on the fate and behavior of copper-treated wood particles following oral ingestion. In this study, the in vitro bioaccessibility of copper from copper-treated wood dust in simulated stomach fluid and DI water was determined. Three copper-treated wood products, liquid alkali copper quaternary and two micronized copper quarternary from different manufacturers, were incubated in the extraction media then fractionated by centrifugation and filtration through 0.45 ?m and 10 kDa filters. The copper concentrations from isolated fractions were measured using Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). Total amounts of copper from each wood product were also determined using microwave-assisted acid digestion of dried wood samples and quantification using ICP-OES. The percent in vitro bioaccessible copper was between 83 and 90 % for all treated wood types. However, the percent of copper released in DI water was between 14 and 25 % for all wood products. This data suggests that copper is highly bioaccessible at low pH and may pose a potential human exposure risk upon ingestion. This dataset is associated with the following publication:Santiago-Rodrigues, L., J.L. Griggs, K. Bradham , C. Nelson , T. Luxton , W. Platten , and K. Rogers. Assessment of the bioaccessibility of micronized copper wood in synthetic stomach flu

  16. Quantitative analysis of oxide materials by laser-induced breakdown spectroscopy with argon as an internal standard

    NASA Astrophysics Data System (ADS)

    Lasheras, R. J.; Bello-Gálvez, C.; Anzano, J. M.

    2013-04-01

    Laser-induced breakdown spectroscopy (LIBS) is demonstrated as a quantitative technique for geochemical analysis. This study demonstrates the applicability of LIBS to multielemental analysis of minerals using argon as an internal standard. Laser-induced breakdown spectroscopy has been applied to measure elements in oxide form. In the present study, the contents of several oxides, such as Fe2O3, CaO and MgO, in geological samples from the Tierga Mine (Zaragoza, Spain) were analyzed by LIBS. An argon environment was used to eliminate interference from air at atmospheric pressure. Furthermore, argon was used as an internal standard. The result was enhanced signal and enhanced linearity of the calibration curves. The Fe2O3, CaO and MgO concentrations determined by LIBS were compared with the results obtained using another analytical technique, inductively coupled plasma optical emission spectrometry (ICP-OES). The concentrations found using LIBS were in good agreement with the values obtained by ICP-OES.

  17. 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.

  18. 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...

  19. 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 ...

  20. In vitro study of thimerosal reactions in human whole blood and plasma surrogate samples.

    PubMed

    Trümpler, Stefan; Meermann, Björn; Nowak, Sascha; Buscher, Wolfgang; Karst, Uwe; Sperling, Michael

    2014-04-01

    Because of its bactericidal and fungicidal properties, thimerosal is used as a preservative in drugs and vaccines and is thus deliberately injected into the human body. In aqueous environment, it decomposes into thiosalicylic acid and the ethylmercury cation. This organomercury fragment is a potent neurotoxin and is suspected to have similar toxicity and bioavailability like the methylmercury cation. In this work, human whole blood and physiological simulation solutions were incubated with thimerosal to investigate its behaviour and binding partners in the blood stream. Inductively coupled plasma with optical emission spectrometry (ICP-OES) was used for total mercury determination in different blood fractions, while liquid chromatography (LC) coupled to electrospray ionisation time-of-flight (ESI-TOF) and inductively coupled plasma-mass spectrometry (ICP-MS) provided information on the individual mercury species in plasma surrogate samples. Analogous behaviour of methylmercury and ethylmercury species in human blood was shown and an ethylmercury-glutathione adduct was identified.

  1. Multielemental fingerprinting as a tool for authentication of organic wheat, barley, faba bean, and potato.

    PubMed

    Laursen, Kristian H; Schjoerring, Jan K; Olesen, Jørgen E; Askegaard, Margrethe; Halekoh, Ulrich; Husted, Søren

    2011-05-11

    The multielemental composition of organic and conventional winter wheat, spring barley, faba bean, and potato was analyzed with inductively coupled plasma-optical emission spectrometry (ICP-OES) and -mass spectrometry (ICP-MS). The crops were cultivated in two years at three geographically different field locations, each accommodating one conventional and two organic cropping systems. The conventional system produced the highest harvest yields for all crops except the nitrogen-fixing faba bean, whereas the dry matter content of each crop was similar across systems. No systematic differences between organic and conventional crops were found in the content of essential plant nutrients when statistically analyzed individually. However, chemometric analysis of multielemental fingerprints comprising up to 14 elements allowed discrimination. The discrimination power was further enhanced by analysis of up to 25 elements derived from semiquantitative ICP-MS. It is concluded that multielemental fingerprinting with semiquantitative ICP-MS and chemometrics has the potential to enable authentication of organic crops.

  2. Standardisation of elemental analytical techniques applied to provenance studies of archaeological ceramics: an inter laboratory calibration study.

    PubMed

    Hein, A; Tsolakidou, A; Iliopoulos, I; Mommsen, H; Buxeda i Garrigós, J; Montana, G; Kilikoglou, V

    2002-04-01

    Chemical analysis is a well-established procedure for the provenancing of archaeological ceramics. Various analytical techniques are routinely used and large amounts of data have been accumulated so far in data banks. However, in order to exchange results obtained by different laboratories, the respective analytical procedures need to be tested in terms of their inter-comparability. In this study, the schemes of analysis used in four laboratories that are involved in archaeological pottery studies on a routine basis were compared. The techniques investigated were neutron activation analysis (NAA), X-ray fluorescence analysis (XRF), inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). For this comparison series of measurements on different geological standard reference materials (SRM) were carried out and the results were statistically evaluated. An attempt was also made towards the establishment of calibration factors between pairs of analytical setups in order to smooth the systematic differences among the results.

  3. 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.

  4. Raman Spectrometry.

    ERIC Educational Resources Information Center

    Gardiner, Derek J.

    1980-01-01

    Reviews mainly quantitative analytical applications in the field of Raman spectrometry. Includes references to other reviews, new and analytically untested techniques, and novel sampling and instrument designs. Cites 184 references. (CS)

  5. 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.

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

    PubMed Central

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

    2017-01-01

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

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

    PubMed

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

    2017-02-15

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

  8. 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

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

    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.

  10. 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...

  11. 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...

  12. 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.

  13. 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.

  14. 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.

  15. Size-fractionated sampling and chemical analysis by total-reflection X-ray fluorescence spectrometry of PMx in ambient air and emissions

    NASA Astrophysics Data System (ADS)

    John, A. C.; Kuhlbusch, T. A. J.; Fissan, H.; Schmidt, K.-G.

    2001-11-01

    PM 10 and PM 2.5 (PMx) have been recently introduced as new air quality standards in the EU (Council Directive 1999/30/EC) for particulate matter. Different estimates and measurements showed that the limit values for PM 10 will be exceeded at different locations in Europe, and thus measures will have to be taken to reduce PMx mass concentrations. Source apportionment has to be carried out, demanding comparable methods for ambient air and emission sampling and chemical analysis. Therefore, a special ambient-air sampler and a specially designed emission sampler have been developed. Total-reflection X-ray fluorescence analysis (TXRF) was used for multi-element analyses as a fast method with low detection limits. For ambient air measurements, a sampling unit was built, impacting particle size classes 10-2.5 μm and 2.5-1.0 μm directly onto TXRF sample carriers. An electrostatic precipitator (ESP) was used as back-up filter to also collect particles <1 μm directly onto the TXRF sample carriers. Air quality is affected by natural and anthropogenic sources, and the emissions of particles <10 μm and <2.5 μm, respectively, have to be determined to quantify their contributions to the so-called coarse (10-2.5 μm) and fine (<2.5 μm) particle modes in ambient air. For this, an in-stack particle sampling system was developed, according to the new ambient air quality standards and in view of subsequent analysis by TXRF. These newly developed samplers, in combination with TXRF analyses, were employed in field campaigns to prove the feasibility and capabilities of the approach. Ambient air data show the quantification of a wide spectrum of elements. From those concentrations, PMx ratios were calculated as an indicator for different sources of elements. Results useful for source apportionment are also the elemental day/night ratios calculated to determine local contributions to PMx mass concentrations. With regard to the emission measurements, results of mass and elemental

  16. The relationship between epilithic periphyton (biofilm) bound metals and metals bound to sediments in freshwater systems.

    PubMed

    Holding, K L; Gill, R A; Carter, J

    2003-03-01

    Surficial sediments and epilithic periphyton (biofilm) were sampled from six sites on the River Churnet and five sites on the River Manifold in Staffordshire and analysed for cadmium (Cd), copper (Cu), lead (Pb) and zinc (Zn). The sites demonstrated a wide range of sediment trace metal concentrations determined by inductively coupled plasma optical emission spectrometry (ICP-OES) and atomic absorbtion spectroscopy (AAS). Biofilm was removed from the substrate using physical abrasion and 0.005 M ethylenediaminoethanetetra-acetic acid (EDTA) extractant. The European Standards, Measurements and Testing Programmes (BCR) operationally defined geochemical speciation scheme was used to determine the exchangeable, acid soluble fraction of the sediments. Significant positive correlations were determined between the EDTA extractable biofilm and the exchangeable sediment fraction for Cd, Cu and Zn but not for Pb. Natural epilithic periphyton may be a potential metal biomonitor particularly of Cu, Cd and Zn in aquatic systems and provide supporting information in relation to potential sediment toxicity.

  17. 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.

  18. Assessment of health risk related to the ingestion of trace metals through fish consumption in Todos os Santos Bay.

    PubMed

    de Santana, Carolina Oliveira; de Jesus, Taíse Bomfim; de Aguiar, Willian Moura; de Jesus Sant'anna Franca-Rocha, Washington; Soares, Carlos Alberto Caroso

    2017-05-01

    This study was carried out to evaluate the concentration of trace elements (As, Cd, Cu, Pb, and Zn) in the muscle of carnivorous fish species from three different areas of Todos os Santos Bay (BTS), Bahia State, Brazil. Trace elements were analyzed using inductively coupled plasma-optical emission spectrometry (ICP-OES), and consumption rates advisory for minimizing chronic systemic effects in children and adults were estimated. As concentrations in fish samples from Jiribatuba were higher than legal limits set by FAO, and Cd concentrations in fish from Iguape Bay were high in comparison with FAO and EC. This study provides information about the fish consumption limits, considering the elements concentrations observed in the analyses, in particular As and Cd, necessary for minimizing potential health risks.

  19. 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.

  20. 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.

  1. Essential and toxic heavy metals in cereals and agricultural products marketed in Kermanshah, Iran, and human health risk assessment.

    PubMed

    Pirsaheb, Meghdad; Fattahi, Nazir; Sharafi, Kiomars; Khamotian, Razieh; Atafar, Zahra

    2016-01-01

    Levels of some essential and toxic heavy metals such as lead, cadmium, chromium, nickel, zinc and copper in cereals and agricultural products obtained from the markets in Kermanshah city, west Iran, were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES). The average concentrations for lead and cadmium in some cereals were higher than the maximum levels set by the Codex Alimentarius. A potential human health risk assessment was conducted by calculating estimated weekly intake (EWI) of the metals from eating cereals and comparison of these values with provisional tolerable weekly intake (PTWI) values. In combination with recent cereal consumption data, the EWIs of heavy metals were calculated for the Kermanshah population. EWI data for the studied metals through cereal consumption were lower than the PTWI values. Cr, Ni, Zn and Cu levels in all samples analysed were within the ranges reported for similar cereals from various parts of the world.

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

    PubMed

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

    2015-06-07

    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.

  3. Monitoring the growth of polyoxomolybdate nanoparticles in suspension by flow field-flow fractionation.

    PubMed

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

    2005-03-30

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

  4. Fluorous oxime palladacycle: a precatalyst for carbon-carbon coupling reactions in aqueous and organic medium.

    PubMed

    Susanto, Woen; Chu, Chi-Yuan; Ang, Wei Jie; Chou, Tzyy-Chao; Lo, Lee-Chiang; Lam, Yulin

    2012-03-16

    To facilitate precatalyst recovery and reuse, we have developed a fluorous, oxime-based palladacycle 1 and demonstrated that it is a very efficient and versatile precatalyst for a wide range of carbon-carbon bond formation reactions (Suzuki-Miyaura, Sonogashira, Stille, Heck, Glaser-type, and Kumada) in either aqueous or organic medium under microwave irradiation. Palladacycle 1 could be recovered through F-SPE in various coupling reactions with recovery ranging from 84 to 95% for the first cycle. Inductively coupled plasma optical emission spectrometry (ICP-OES) analyses of the Pd content in the crude product from each class of transformation indicated extremely low levels of leaching and the palladacycle could be reused four to five times without significant loss of activity.

  5. Cadmium in liver and kidneys of domestic Balkan and Alpine dairy goat breeds from Montenegro and Serbia.

    PubMed

    Tomović, Vladimir; Jokanović, Marija; Tomović, Mila; Lazović, Milana; Šojić, Branislav; Škaljac, Snežana; Ivić, Maja; Kocić-Tanackov, Sunčica; Tomašević, Igor; Martinović, Aleksandra

    2017-06-01

    Concentrations of cadmium (Cd) were determined in the samples of 144 animals around 1 and of 144 animals around 4 years old. Cd was analysed by inductively coupled plasma-optical emission spectrometry (ICP-OES), after microwave digestion. Cd concentrations were higher (p < 0.05) in kidney than in liver and higher (p < 0.05) in older animals than in young ones. In domestic Balkan goat which was raised in a free-ranged system Cd accumulation was lower (p < 0.05) than in Alpine goat raised in an intensive production system. Geographic region did influence Cd accumulation only in older animals. Higher Cd levels (p < 0.05) were determined in goats from Serbia. The highest obtained Cd concentrations in both tissues were lower than maximum levels set by European and national legislation for ruminants (cattle and sheep).

  6. 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.

  7. Plasma concentration of calcium, magnesium and phosphorus in chinchilla with and without tooth overgrowth.

    PubMed

    Muszczyński, Zbigniew; Sulik, Małgorzata; Ogoński, Tadeusz; Antoszek, Jolanta

    2010-01-01

    The aim of the study was to identify the causes underlying overgrowth of incisors in chinchillas through an analysis of selected plasma electrolyte concentrations, with particular consideration of minerals involved in the formation of osseous tissue, i.e., Ca, Mg, and P. The analysis involved 40 female standard chinchillas managed in a commercial farm system, aged 2 to 4 years, divided into two groups of 20 individuals each: D--chinchillas with incisor overgrowth and C--controls with normal dentition. Concentrations of Ca, Mg, and P were measured in blood plasma. The analysis was carried out using ICP OES (inductively coupled plasma optical emission spectrometry) by means of the Optima 2000 DV instrument (Perkin Elmer). The resulting data were analysed statistically using one-way ANOVA with Duncan's range test. The results show that abnormal metabolism of dental tissue minerals, especially Ca and P, cannot be excluded as the cause of tooth overgrowth in chinchilla.

  8. 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.

  9. 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)

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

    PubMed

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

    1998-10-01

    A compact device based on purge-and-trap multicapillary gas chromatography was developed for sensitive species-selective analysis of methylmercury and Hg2+ by atomic spectrometry. The operating mode includes in situ conversion of the analyte species to MeEtHg and HgEt2 and cryotrapping of the derivatives formed in a 0.53-mm-i.d. capillary, followed by their flash (< 30 s) isothermal low-temperature separation on a minimulticapillary (22 cm) column. The very low detection limits obtained (0.01 pg mL-1 of Hg for methylmercury) are due to the narrow injection band and reduced peak broadening in a bundle of 0.038-mm capillaries at high flow rates (> 60 mL min-1) compatible with an MIP AES detector (no dilution with a makeup gas is required). Developments regarding each of the steps of the analytical procedure and effects of operational variables (sample volume, purge flow, trap temperature, separation conditions) are discussed. The device allows speciation of MeHg+ and Hg2+ down to 5 pg g-1 in urine and, after a rapid microwave-assisted hydrolysis, down to 0.1 ng g-1 in solid biological samples with a throughput of 6 samples/h. The analytical protocols developed were validated by the analysis of DORM-1 (dogfish muscle), TORT-1 (lobster hepatopancreas), and Seronorm urine certified reference materials.

  11. 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.

  12. 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.

  13. 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.

  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. Determination of trace impurities in high-purity zirconium dioxide by inductively coupled plasma atomic emission spectrometry using microwave-assisted digestion and wavelet transform-based correction procedure.

    PubMed

    Ma, Xiaoguo; Li, Yibing

    2006-10-02

    This paper describes a rapid, accurate and precise method for the determination of trace Fe, Hf, Mn, Na, Si and Ti in high-purity zirconium dioxide (ZrO2) powders by inductively coupled plasma atomic emission spectrometry (ICP-AES). The samples were dissolved by a microwave-assisted digestion system. Four different digestion programs with various reagents were tested. It was found that using a mixture of sulfuric acid (H2SO4) and ammonium sulfate ((NH4)2SO4), the total sample dissolution time was 30 min, much shorter than that required for conventional digestion in an opening system. The determination of almost all of the target analytes suffered from spectral interferences, since Zr shows a line-rich atomic emission spectrometry. The wavelet transform (WT), a recently developed mathematical technique was applied to the correction of spectral interference, and more accurate and precise results were obtained, compared with traditional off-peak background correction procedure. Experimental work revealed that a high Zr concentration would result in a significant decrease in peak height of the analyte lines, which was corrected by standard addition method. The performance of the developed method was evaluated by using synthetic samples. The recoveries were in the range of 87-112% and relative standard deviation was within 1.1-3.4%. The detection limits (3sigma) for Fe, Hf, Mn, Na, Si and Ti were found to be 1.2, 13.3, 1.0, 4.5, 5.8 and 2.0 microg g(-1), respectively. The results showed that with the microwave-assisted digestion and the WT correction, the detection limits have improved by a factor of about 5 for Fe, 4 for Mn and Ti, 3 for Si, and 2 for Hf and Na, respectively, in comparison with conventional open-system digestion and off-peak correction. The proposed technique was applied to the analysis of trace elements above-mentioned in three types of ZrO2 powders.

  16. 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

  17. Kinetics and isotope patterns of ethanol and acetaldehyde emissions from yeast fermentations of glucose and glucose-6,6-d2 using selected ion flow tube mass spectrometry: a case study.

    PubMed

    Smith, David; Wang, Tianshu; Spanel, Patrik

    2002-01-01

    As a prelude to investigations of the emission of metabolites from human cell lines in vitro, we have conducted a study using selected ion flow tube mass spectrometry (SIFT-MS) of the acetaldehyde and ethanol that appear in the headspace above a fermenting yeast/glucose/water mixture in sealed glass bottles at a temperature of 30 degrees C. A fixed quantity of yeast (10 mg) and varying amounts (2, 4, 8 and 16 mg) of both non-deuterated glucose and glucose-6,6-d2 in 5 mL of water were used and the emission of the acetaldehyde and the ethanol were observed as a function of time. The ethanol and acetaldehyde concentrations in the headspace were obtained from the magnitudes of their characteristic ions on the accumulated SIFT mass spectra and, when the deuterated glucose was used, characteristic singly and doubly deuterated ions were obvious. This study indicates, as expected, that ethanol is the major species generated and that acetaldehyde is a relatively minor component of the headspace and a very minor component of the liquid phase. We estimate that about 10(8) ethanol molecules are produced per minute per cell in this yeast fermentation process. The distribution of the non-deuterated and partially deuterated ethanol under these fermentation conditions is observed to be C2H5OH (66 +/- 4)%, C2H4DOH(6 +/- 1)%, C2H3D2OH(28 +/- 4)%, and the analogous distribution for the acetaldehyde is the same, within error. These results indicate that the D atoms in the glucose-6,6-d2 are mostly retained by the 6-C atom, but the appearance of the singly deuterated ethanol and acetaldehyde indicates that some D/H mixing must be occurring in the enzymatic reactions. The results of this study illustrate the potential and power of on-line SIFT-MS analysis in this area of research.

  18. 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.

  19. 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.

  20. 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%).

  1. Determination of methylmercury in fish tissue by gas chromatography with microwave-induced plasma atomic emission spectrometry after derivatization with sodium tetraphenylborate.

    PubMed

    Palmieri, H E; Leonel, L V

    2000-03-01

    The detection of methylmercury species (MeHg) in fish tissue was investigated. Samples were digested with KOH-methanol and acidified prior to extraction with methylene chloride. MeHg was back-extracted from the organic phase into water. An aliquot of this aqueous solution (buffered to pH 5) was subjected to derivatization with sodium tetraphenylborate (NaBPh4) and then extracted with toluene. The organic phase containing MePhHg was injected into a gas chromatograph (GC) which is on-line with a microwave-induced plasma atomic emission spectrometer (MIP-AED). The quantification limit was about 0.6 microg/g and 0.1 microg/g of MeHg (as Hg) for 0.08 g of freeze-dried fish powder and 0.5 g of fresh samples, respectively. Two certified reference materials, CRM 464 (tuna fish) from Community Bureau of Reference-BCR and DORM-2 (dogfish muscle) from National Research Council Canada-NRC were selected for checking the accuracy of the method. This methodology was applied to the determination of MeHg in some kinds of fish from the Carmo river with alluvial gold recovery activities ("garimpos") in Mariana, Minas Gerais, Brazil.

  2. 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.

  3. Measuring evaporation rates of metal compounds from solid samples.

    PubMed

    Ludwig, Christian; Wochele, Jörg; Jörimann, Urs

    2007-04-01

    A thermogravimeter (TGA, Mettler-Toledo TGA/SDTA851e) was connected to an inductively coupled plasma optical emission spectrometer (ICP-OES, Varian Liberty 110) using a condensation interface (CI), which transforms gaseous high-boiling-temperature substances into solid (or liquid) aerosols. Argon was used as the carrier gas to transfer the aerosols into the ICP-OES for on-line elemental analysis. This new analytical TGA-CI-ICP-OES device, called TGA-ICP, is the first of its kind and allows one to study the thermochemically induced evaporation behavior of high-boiling-temperature substances, such as heavy metal compounds, under different thermochemical conditions. It allows the investigation of the behavior of large solid or liquid samples (100-500 mg), which is important for applying the results to industrial processes. So far, the CI principle has allowed only semiquantitative elemental analyses of hot gases when connected to an ICP-OES. In this work, we show that a direct calibration of the CI-ICP-OES device is possible in combination with a TGA. The intensities determined by ICP-OES could be directly related to gravimetrically determined evaporation rates of volatile model compounds. The results show model evaporation experiments with native CdCl2 and CdCl2 resulting from the reaction of CaCl2 with CdO. Cadmium was studied because it is a volatile toxic heavy metal and its thermal behavior is relevant in various waste-treatment and recycling processes.

  4. 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

  5. Mass spectrometry

    SciTech Connect

    Burlingame, A.L.; Baillie, T.A.; Derrick, P.J.

    1986-04-01

    It is the intention of the review to bring together in one source the direction of major developments in mass spectrometry and to illustrate these by citing key contributions from both fundamental and applied research. The Review is intended to provide the reader with a sense of the main currents, their breadth and depth, and probable future directions. It is also intended to provide the reader with a glimpse of the diverse discoveries and results that underpin the eventual development of new methods and instruments - the keys to obtaining new insights in all the physical, chemical, and biological sciences which depend on mass spectrometry at various levels of sophistication. Focal points for future interdisciplinary synergism might be selective quantitative derivatization of large peptides, which would convey properties that direct fragmentation providing specific sequence information, or optimization of LCMS for biooligomer sequencing and mixture analysis, or the perfect way to control or enhance the internal energy of ions of any size, or many others. 1669 references.

  6. 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

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

    PubMed

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

    2009-05-15

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

  8. 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

    2014-09-09

    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.

  9. 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.

  10. Midwave Infrared Imaging Fourier Transform Spectrometry of Combustion Plumes

    DTIC Science & Technology

    2009-09-01

    resolution at a range of 600 meters featured strong emission from NO, CO, CO2, SO2, and HCl in the spectral region 1800-3000 cm−1. A simplified radiative...4 2.1 Remote Spectrometry of Engine Emissions . . . . . . . . . . . . . . . . . . . . . . . . . . 4 2.2...image scene following background-subtraction to remove instrument self- emission

  11. 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

  12. Calcium extraction from brine water and seawater using oxalic acid

    NASA Astrophysics Data System (ADS)

    Natasha, Nadia Chrisayu; Lalasari, Latifa Hanum

    2017-01-01

    Calcium can be extracted not only from rocks but also from natural liquor such as seawater and brine water. In order to extract the calcium from seawater and brine water, oxalic acid was used in this research. Effect of variations of the volume of the oxalic acid at a constant concentration in seawater and brine water to produce calcium was investigated. The concentration of oxalic acid was 100 g/l and the variations of its volume were 2 ml, 4 ml, 6 ml, 8 ml, 10 ml, 20 ml, 30 ml, 40 ml, and 50 ml. The used seawater and brine water were firstly evaporated from 100 ml into 50 ml and then the oxalic acid was added into them with mixing to produce the calcium precipitates. The precipitates were analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM) and the filtrates were analyzed by inductively coupled plasma-optical emission spectrometry (ICP-OES). The SEM analysis showed that the precipitates from brine water were consisted of only calcium compound while from seawater sodium one was also found along with calcium compound. The XRD analysis showed that the calcium was present in the form of calcium oxalate for both seawater and brine water. The ICP-OES analysis of the filtrate from seawater precipitation showed that the its calcium content was decreased from 826.20 ppm to 0.04 ppm while from brine water, it decreased from 170.06 ppm to 1.96 ppm. These results showed that both seawater and brine water have the potential to be a raw material for calcium production.

  13. 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.

  14. Comments on "Determination of mercury, cadmium, lead, zinc, selenium and iron by ICP-OES in mushroom samples from around thermal power plant in Muğla, Turkey". doi:10.1007/s00128-011-0357-1.

    PubMed

    Falandysz, Jerzy

    2012-05-01

    In several articles on trace elements in mushrooms erroneous data were published on minerals sequestered in fruiting bodies. The biased analytical data published gave a false picture on the composition and nutritional value of mushrooms with respect to minerals. Wild mushrooms are relatively rich in trace elements and some species can hyperaccumulate certain metals. Selenium as reported in the referenced article is discussed in light of typical Se concentrations determined using validated methods as reported by other authors.

  15. Micro- and nano-volume samples by electrothermal, near-torch vaporization sample introduction using removable, interchangeable and portable rhenium coiled-filament assemblies and axially-viewed inductively coupled plasma-atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Badiei, Hamid R.; Lai, Bryant; Karanassios, Vassili

    2012-11-01

    An electrothermal, near-torch vaporization (NTV) sample introduction for micro- or nano-volume samples is described. Samples were pipetted onto coiled-filament assemblies that were purposely developed to be removable and interchangeable and were dried and vaporized into a small-volume vaporization chamber that clips onto any ICP torch with a ball joint. Interchangeable assemblies were also constructed to be small-size (e.g., less than 3 cm long with max diameter of 0.65 cm) and light-weight (1.4 g) so that they can be portable. Interchangeable assemblies with volume-capacities in three ranges (i.e., < 1 μL, 1-10 μL and 10-100 μL) were fabricated and used. The horizontally-operated NTV sample introduction was interfaced to an axially-viewed ICP-AES (inductively coupled plasma-atomic emission spectrometry) system and NTV was optimized using ICP-AES and 8 elements (Pb, Cd, Zn, V, Ba, Mg, Be and Ca). Precision was 1.0-2.3% (peak height) and 1.1-2.4% (peak area). Detection limits (obtained using 5 μL volumes) expressed in absolute-amounts ranged between 4 pg for Pb to 0.3 fg (~ 5 million atoms) for Ca. Detection limits expressed in concentration units (obtained using 100 μL volumes of diluted, single-element standard solutions) were: 50 pg/mL for Pb; 10 pg/mL for Cd; 9 pg/mL for Zn; 1 pg/mL for V; 0.9 pg/mL for Ba; 0.5 pg/mL for Mg; 50 fg/mL for Be; and 3 fg/mL for Ca. Analytical capability and utility was demonstrated using the determination of Pb in pg/mL levels of diluted natural water Certified Reference Material (CRM) and the determination of Zn in 80 nL volumes of the liquid extracted from an individual vesicle. It is shown that portable and interchangeable assemblies with dried sample residues on them can be transported without analyte loss (for the concentrations tested), thus opening up the possibility for "taking part of the lab to the sample" applications, such as testing for Cu concentration-compliance with the lead-copper rule of the Environmental

  16. 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

  17. KEY COMPARISON: Final report on CCQM-K57: Chemical composition of clay

    NASA Astrophysics Data System (ADS)

    Salas, Antonio; Ramírez, Estele

    2009-01-01

    After the successful completion of the pilot study, CCQM-P65 [1], the Inorganic Analysis Working Group of CCQM agreed to conduct key comparison CCQM-K57, Chemical composition of clay, in Paris, April 2006. The natural mass fraction levels of five elements—Si, Ca, Fe, Al and Mg—were measured and reported as oxides in clay. Six national metrology institutes participated in CCQM K57, and CENAM (Querétaro, Mexico) coordinated. The methods employed were isotope dilution mass spectrometry (IDMS), inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-optical emission spectrometry (ICP-OES) using the dehydration method and condensation method, gravimetric analysis, neutron activation analysis (NAA), prompt gamma activation analysis (PGAA) and x-ray fluorescence spectrometry (XRF) with the reconstitution method and external calibration. This final report presents the capability of the participant institutes, based on the KCRV, which was approved at the IAWG spring meeting in 2008, and the equivalence statements regarding the KCRV, approved at its autumn meeting. 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 (MRA).

  18. 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

  19. Characterization of edible seaweed harvested on the Galician coast (northwestern Spain) using pattern recognition techniques and major and trace element data.

    PubMed

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

    2010-02-10

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

  20. Characterization of PCBs from computers and mobile phones, and the proposal of newly developed materials for substitution of gold, lead and arsenic.

    PubMed

    Dervišević, Irma; Minić, Duško; Kamberović, Željko; Ćosović, Vladan; Ristić, Mirjana

    2013-06-01

    In this paper, we have analyzed parts of printed circuit board (PCB) and liquid crystal display (LCD) screens of mobile phones and computers, quantitative and qualitative chemical compositions of individual components, and complete PCBs were determined. Differential thermal analysis (DTA) and differential scanning calorimetry (DSC) methods were used to determine the temperatures of phase transformations, whereas qualitative and quantitative compositions of the samples were determined by X-ray fluorescence spectrometry (XRF), inductively coupled plasma optical emission spectrometry (ICP-OES), and scanning electron microscopy (SEM)-energy dispersive X-ray spectrometry (EDS) analyses. The microstructure of samples was studied by optical microscopy. Based on results of the analysis, a procedure for recycling PCBs is proposed. The emphasis was on the effects that can be achieved in the recycling process by extraction of some parts before the melting process. In addition, newly developed materials can be an adequate substitute for some of the dangerous and harmful materials, such as lead and arsenic are proposed, which is in accordance with the European Union (EU) Restriction of the use of certain hazardous substances (RoHS) directive as well as some alternative materials for use in the electronics industry instead of gold and gold alloys.

  1. 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.

  2. 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.

  3. Laser Ablation Molecular Isotopic Spectrometry

    NASA Astrophysics Data System (ADS)

    Russo, Richard E.; Bol'shakov, Alexander A.; Mao, Xianglei; McKay, Christopher P.; Perry, Dale L.; Sorkhabi, Osman

    2011-02-01

    A new method of performing optical isotopic analysis of condensed samples in ambient air and at ambient pressure has been developed: Laser Ablation Molecular Isotopic Spectrometry (LAMIS). The technique uses radiative transitions from molecular species either directly vaporized from a sample or formed by associative mechanisms of atoms or ions in a laser ablation plume. This method is an advanced modification of a known atomic emission technique called laser-induced breakdown spectroscopy (LIBS). The new method — LAMIS — can determine not only chemical composition but also isotopic ratios of elements in the sample. Isotopic measurements are enabled by significantly larger isotopic shifts found in molecular spectra relative to atomic spectra. Analysis can be performed from a distance and in real time. No sample preparation or pre-treatment is required. Detection of the isotopes of hydrogen, boron, carbon, and oxygen are discussed to illustrate the technique.

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

    NASA Astrophysics Data System (ADS)

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

    2014-08-01

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

  5. Emissions Inventory

    EPA Pesticide Factsheets

    This page describes the role of emission inventories in the air quality management process, a description of how emission inventories are developed, and where U.S. emission inventory information can be found.

  6. 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.

  7. 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

    2015-02-03

    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.

  8. 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.

  9. 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.

  10. Determination of certain micro and macroelements in plant stimulants and their infusions.

    PubMed

    Malik, Jan; Szakova, Jirina; Drabek, Ondrej; Balik, Jiri; Kokoska, Ladislav

    2008-11-15

    The quantitative analysis of Al, B, Cu, Fe, Mn, P and Zn by inductively coupled plasma optical emission spectrometry (ICP-OES) and Ca, K and Mg by atomic absorption spectrometry (AAS) has been carried out in both the raw material and infusions from 31 samples of traditional plant stimulants (tea and coffee) and mate, rooibos, honeybush and chamomile. The results were discussed with respect to differences to the beverage quality and their role in the human diet. The levels of elements not significantly differ between tea types (black, green, oolong, white), and between Arabica and Robusta coffee. In comparison with tea, coffee was found to be a poor source of elements with the exception of Ca and Fe. High levels of B, Ca, Cu, Mn, Mg and Zn were found in mate (mainly green type) and of B, Ca, Cu, Fe and P in chamomile, whereas the amounts of all elements in rooibos and honeybush infusions were low (except of Ca). Apart from tea, other stimulants appeared to not represent important sources of potentially harmful amounts of Al for the human diet.

  11. 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

  12. Report of the CCQM-K123: trace elements in biodiesel fuel

    NASA Astrophysics Data System (ADS)

    Kuroiwa, T.; Zhu, Y.; Inagaki, K.; Long, S. E.; Christopher, S. J.; Puelles, M.; Borinsky, M.; Hatamleh, N.; Murby, J.; Merrick, J.; White, I.; Saxby, D.; Sena, R. C.; Almeida, M. D.; Vogl, J.; Phukphatthanachai, P.; Fung, W. H.; Yau, H. P.; Okumu, T. O.; Kang'iri, J. N.; Télle, J. A. S.; Campos, E. Z.; Gal&vacute; n, E. C.; Kaewkhomdee, N.; Taebunpakul, S.; Thiengmanee, U.; Yafa, C.; Tokman, N.; Tunç, M.; Can, S. Z.

    2017-01-01

    The CCQM-K123 key comparison was organized by the Inorganic Analysis Working Group (IAWG) of CCQM to assess and document the capabilities of the national metrology institutes (NMIs) or the designated institutes (DIs) to measure the mass fractions of sodium, calcium, potassium, magnesium phosphorous and sulfur in biodiesel fuel (BDF). National Metrology Institute of Japan (NMIJ) and National Institute of Standards and Technology (NIST) acted as the coordinating laboratories. Results were submitted by 11 NMIs and DIs. Most of the participants used inductively coupled plasma-mass spectrometry (ICP-MS), isotope dilution technique with ICP-MS and inductively coupled plasma-optical emission spectrometry (ICP-OES) with microwave acid digestion. Accounting for relative expanded uncertainty, comparability of measurement results for each of Na, Ca, K, Mg and P was successfully demonstrated by the participants. Concerning S, the variation in results between participants, particularly those using IDMS methods was observed. According to the additional evaluation and investigation, the revised results were overlapping between IDMS measurements at the k = 2 level. However, this KC does not support S measurements. 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).

  13. Surface modification of Au/TiO2 catalysts by SiO2 via atomic layer deposition

    SciTech Connect

    Ma, Zhen; Brown, Suree; Howe, Jane Y; Overbury, Steven {Steve} H; Dai, Sheng

    2008-01-01

    Atomic layer deposition (ALD) was utilized for the surface engineering of metallic nanoparticles to tame their sintering problems and catalytic activities. We chose the surface modification of gold nanocatalysts as an example to demonstrate the concept of this ALD-based approach. Herein, an active Au/TiO{sub 2} catalyst was modified by amorphous SiO{sub 2} via ALD, and the samples were characterized by inductively coupled plasma-optical emission spectrometry (ICP-OES), scanning (SEM-EDX) and transmission electron microscope-energy-dispersive X-ray spectrometry (TEM-EDX), X-ray diffraction (XRD), and thermogravimetry/differential thermogravimetry (TG/DTG), and the catalytic activities in CO oxidation and H{sub 2} oxidation were tested with respect to the pretreatment temperature and SiO{sub 2} content. A significant sintering resistance and changes in catalytic activities were observed. The difference between the SiO{sub 2}/Au/TiO{sub 2} samples prepared by gas-phase ALD and solution-phase chemical grafting was discussed.

  14. 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).

  15. Evolution of dispersive liquid-liquid microextraction method.

    PubMed

    Rezaee, Mohammad; Yamini, Yadollah; Faraji, Mohammad

    2010-04-16

    Dispersive liquid-liquid microextraction (DLLME) has become a very popular environmentally benign sample-preparation technique, because it is fast, inexpensive, easy to operate with a high enrichment factor and consumes low volume of organic solvent. DLLME is a modified solvent extraction method in which acceptor-to-donor phase ratio is greatly reduced compared with other methods. In this review, in order to encourage further development of DLLME, its combination with different analytical techniques such as gas chromatography (GC), high-performance liquid chromatography (HPLC), inductively coupled plasma-optical emission spectrometry (ICP-OES) and electrothermal atomic absorption spectrometry (ET AAS) will be discussed. Also, its applications in conjunction with different extraction techniques such as solid-phase extraction (SPE), solidification of floating organic drop (SFO) and supercritical fluid extraction (SFE) are summarized. This review focuses on the extra steps in sample preparation for application of DLLME in different matrixes such as food, biological fluids and solid samples. Further, the recent developments in DLLME are presented. DLLME does have some limitations, which will also be discussed in detail. Finally, an outlook on the future of the technique will be given.

  16. 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

    2015-03-03

    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.

  17. Trace anion determination in concentrated hydrofluoric acid solutions by two-dimensional ion chromatography I. Matrix elimination by ion-exclusion chromatography.

    PubMed

    Vermeiren, Koen

    2005-08-26

    Since years, ion exclusion chromatography (ICE) has been the standard method to separate strong acid analyte anions from concentrated weak acid matrices such as hydrofluoric acid (HF). In this work, the commercially available IonPac ICE-AS 1 column was used to separate trace levels of chloride, nitrate, sulfate and phosphate from HF solutions at 20% (w/w). The efficiency of the separation was studied in more detail using techniques such as ion chromatography (IC), inductively coupled plasma optical emission spectrometry (ICP-OES) and ICP-mass spectrometry (ICP-MS). For 20% (w/w) HF solutions and at a water carrier flow-rate of 0.50 ml/min, the cut window was set from 8.5 to 14.5 min. Under these conditions, analyte recoveries of better than 90% were obtained for chloride, nitrate and sulfate, but only about 75% for phosphate. The HF rejection efficiency was better than 99.9%. It was found that the ICP techniques, measuring total element levels and not species, yielded significantly higher recoveries for phosphorus and sulfur compared to IC. Evidence will be given that part of the added phosphorus (approximately 15% for an addition of 10 mg PO4/kg) is present as mono-fluorophosphoric acid (H2FPO3). In the case of sulfate, the difference between IC and ICP-MS could be attributed to an important matrix effect from the residual HF concentration.

  18. 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.

  19. Forensic Mass Spectrometry.

    PubMed

    Hoffmann, William D; Jackson, Glen P

    2015-01-01

    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.

  20. Etalon Array Reconstructive Spectrometry

    NASA Astrophysics Data System (ADS)

    Huang, Eric; Ma, Qian; Liu, Zhaowei

    2017-01-01

    Compact spectrometers are crucial in areas where size and weight may need to be minimized. These types of spectrometers often contain no moving parts, which makes for an instrument that can be highly durable. With the recent proliferation in low-cost and high-resolution cameras, camera-based spectrometry methods have the potential to make portable spectrometers small, ubiquitous, and cheap. Here, we demonstrate a novel method for compact spectrometry that uses an array of etalons to perform spectral encoding, and uses a reconstruction algorithm to recover the incident spectrum. This spectrometer has the unique capability for both high resolution and a large working bandwidth without sacrificing sensitivity, and we anticipate that its simplicity makes it an excellent candidate whenever a compact, robust, and flexible spectrometry solution is needed.

  1. Etalon Array Reconstructive Spectrometry

    PubMed Central

    Huang, Eric; Ma, Qian; Liu, Zhaowei

    2017-01-01

    Compact spectrometers are crucial in areas where size and weight may need to be minimized. These types of spectrometers often contain no moving parts, which makes for an instrument that can be highly durable. With the recent proliferation in low-cost and high-resolution cameras, camera-based spectrometry methods have the potential to make portable spectrometers small, ubiquitous, and cheap. Here, we demonstrate a novel method for compact spectrometry that uses an array of etalons to perform spectral encoding, and uses a reconstruction algorithm to recover the incident spectrum. This spectrometer has the unique capability for both high resolution and a large working bandwidth without sacrificing sensitivity, and we anticipate that its simplicity makes it an excellent candidate whenever a compact, robust, and flexible spectrometry solution is needed. PMID:28074883

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

    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.

  3. Particulate matters collected from ceramic factories in Lampang Province affecting rat lungs*

    PubMed Central

    Fongmoon, Duriya; Pongnikorn, Surathat; Chaisena, Aphiruk; Iamsaard, Sitthichai

    2014-01-01

    Background: Lung cancer ranks as the fifth largest of all cancer cases in Thailand. However, it is the first leading cancer in the northern part of Thailand (data from 2003–2007). There are several predisposing causes that lead to lung cancer and one important inducement is particulate matters (PMs). Lampang Province in Thailand is famous for the ceramic industry, where there are over 200 ceramic industrial factories. PMs are produced during the ceramic manufacturing process and spread throughout all of the working areas. It is very possible that workers could directly inhale PM-contaminated air during working hours. Objective: This study focuses on the toxic effects of PMs collected from ceramic factories on genes and lungs of rats. Methods: PMs collected from six ceramic factories in Lampang Province were extracted using dimethyl sulfoxide (DMSO). The inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES) were used to analyze the chemical elements at lower and higher concentrations, respectively. Then, the toxicity of PMs on the genes was examined by the Ames test, and subsequently, the effect of PMs on DNA was examined by quantifying the amount of 8-hydroxy-2′-deoxyguanosine (8-OHdG). Finally, the toxicity of the PMs on rat’s lungs was examined by histology. Results: As chemical elements of lower concentrations, cadmium, chromium, nickel, copper, and lead were detected by ICP-MS. As chemical elements of higher concentrations, manganese, magnesium, zinc, iron, potassium, calcium, and sodium were detected by ICP-OES. No mutagenicity in Salmonella typhimurium was found in the PM extracts from all six factories by utilizing the Ames test. In the histological study, the reduction in spaces of alveolar ducts and sacs, and terminal bronchioles, the thickening of interstitial connective tissues were noted by PM extracts in high amounts (100 and 350 μg). Female rats were more sensitive to PM

  4. Fate of Thallium(I) in Reverse Osmosis and Chlorinated Water Matrices

    DTIC Science & Technology

    2014-02-01

    THALLIUM(I) IN REVERSE OSMOSIS AND CHLORINATED WATER MATRICES ECBC-TR-1127 Approved for public release; distribution is unlimited...3. DATES COVERED (From - To) Apr 2010 - Dec 2011 4. TITLE AND SUBTITLE Fate of Thallium(I) in Reverse Osmosis and Chlorinated Water Matrices... osmosis (RO) and RO water with added chlorine (RO-Cl) was measured using inductively coupled plasma optical emission spectroscopy (ICP-OES) for a period of

  5. 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.

  6. 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.

  7. 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.

  8. Fourier Transform Mass Spectrometry.

    ERIC Educational Resources Information Center

    Gross, Michael L.; Rempel, Don L.

    1984-01-01

    Discusses the nature of Fourier transform mass spectrometry and its unique combination of high mass resolution, high upper mass limit, and multichannel advantage. Examines its operation, capabilities and limitations, applications (ion storage, ion manipulation, ion chemistry), and future applications and developments. (JN)

  9. 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)

  10. 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)

  11. 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...

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

    PubMed

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

    2017-03-14

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

  13. 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.

  14. 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.

  15. An Analysis of Systematic Elemental Changes in Decomposing Bone.

    PubMed

    Walden, Steven J; Mulville, Jacqui; Rowlands, Jeffrey P; Evans, Sam L

    2017-03-10

    The aim of this pilot study was to investigate compositional changes in bone during decomposition. Elemental concentrations of barium, calcium, iron, potassium, magnesium, zinc and phosphorus in porcine bone (as an experimental analog for human bone) were analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES). The samples were taken from porcine bone subjected to shallow burial and surface depositions at 28-day intervals for a period of 140 days. Results indicated that ICP-OES elemental profiling has potential to be developed as a forensic test for determining whether a bone sample originates from the early stages of soft tissue putrefaction. Significant changes in iron, sodium and potassium concentrations were found over 140 days. These elements are known to be primarily associated with proteins and/or tissue fluids within the bone. Changes in their respective concentrations may therefore be linked to dehydration over time and in turn may be indicative of time since deposition.

  16. Mapping surface mineralogy using imaging spectrometry

    NASA Astrophysics Data System (ADS)

    Kruse, Fred A.

    2012-01-01

    Imaging spectrometry, simultaneous measurement of spectra and images in up to hundreds of spectral channels or bands, is a proven technology for identifying and mapping minerals based on their reflectance or emissivity signatures. Also known as hyperspectral imaging or "HSI", extraction of key spectral signatures from these data allows direct identification of iron minerals such as hematite, goethite, and jarosite in the visible/near infrared (VNIR); clays, carbonates, micas, sulfates, and other minerals in the short wave infrared (SWIR); and silicates and carbonates in the long wave infrared (LWIR). The unique capability of imaging spectrometry to produce detailed maps of the spatial distribution of specific minerals, mineral assemblages, and mineral variability on the surface of Earth makes it an ideal tool for enhanced geomorphic mapping. Case histories illustrate the use of HSI for characterizing and mapping active and relict geothermal/hydrothermal systems and determining relations between mineralogy and derived landforms. Imaging spectrometry, used in conjunction with complimentary datasets such as InSAR (Interferometric Synthetic Aperture Radar), Light Detection and Ranging (LiDAR), or stereo (photogrammetric-derived) digital elevation models (DEMs), provides a unique means of visualizing the spatial distribution and association of mineralogy with topography, thus contributing to the understanding of the relations between geology and landscape and to improved interpretation of surface geologic processes.

  17. Endocrine disrupting chemical emissions from combustion sources: diesel particulate emissions and domestic waste open burn emissions

    NASA Astrophysics Data System (ADS)

    Sidhu, Sukh; Gullett, Brian; Striebich, Richard; Klosterman, Joy; Contreras, Jesse; DeVito, Michael

    Emissions of endocrine disrupting chemicals (EDCs) from combustion sources are poorly characterized due to the large number of compounds present in the emissions, the complexity of the analytical separations required, and the uncertainty regarding identification of chemicals with endocrine effects. In this work, multidimensional gas chromatographic-mass spectrometry (MDGC-MS) was used to characterize emissions from both controlled (diesel engine) and uncontrolled (open burning of domestic waste) combustion sources. The results of this study suggest that, by using MDGC-MS, one can resolve a much greater percentage of the chromatogram and identify about 84% of these resolved compounds. This increase in resolution helped to identify and quantify various classes of polycyclic aromatic hydrocarbons (PAHs) in the combustion emissions that had not been identified previously. Significant emissions (when compared to industrial sources) of known EDCs, dioctyl phthalate (over ˜2,500,000 kg year -1) and bisphenol A (over ˜75,000 kg year -1) were estimated from uncontrolled domestic waste burning. Emissions of several suspected EDCs (oxygenated PAHs) were observed in both diesel soot and the uncontrolled domestic waste burn samples. The emission rates of known and suspected EDCs estimated in this study suggest that combustion emissions need to be characterized for EDCs to further assess its importance as a source of EDC exposure.

  18. Desorption in Mass Spectrometry.

    PubMed

    Usmanov, Dilshadbek Tursunbayevich; Ninomiya, Satoshi; Chen, Lee Chuin; Saha, Subhrakanti; Mandal, Mridul Kanti; Sakai, Yuji; Takaishi, Rio; Habib, Ahsan; Hiraoka, Kenzo; Yoshimura, Kentaro; Takeda, Sen; Wada, Hiroshi; Nonami, Hiroshi

    2017-01-01

    In mass spectrometry, analytes must be released in the gas phase. There are two representative methods for the gasification of the condensed samples, i.e., ablation and desorption. While ablation is based on the explosion induced by the energy accumulated in the condensed matrix, desorption is a single molecular process taking place on the surface. In this paper, desorption methods for mass spectrometry developed in our laboratory: flash heating/rapid cooling, Leidenfrost phenomenon-assisted thermal desorption (LPTD), solid/solid friction, liquid/solid friction, electrospray droplet impact (EDI) ionization/desorption, and probe electrospray ionization (PESI), will be described. All the methods are concerned with the surface and interface phenomena. The concept of how to desorb less-volatility compounds from the surface will be discussed.

  19. Desorption in Mass Spectrometry

    PubMed Central

    Usmanov, Dilshadbek Tursunbayevich; Ninomiya, Satoshi; Chen, Lee Chuin; Saha, Subhrakanti; Mandal, Mridul Kanti; Sakai, Yuji; Takaishi, Rio; Habib, Ahsan; Hiraoka, Kenzo; Yoshimura, Kentaro; Takeda, Sen; Wada, Hiroshi; Nonami, Hiroshi

    2017-01-01

    In mass spectrometry, analytes must be released in the gas phase. There are two representative methods for the gasification of the condensed samples, i.e., ablation and desorption. While ablation is based on the explosion induced by the energy accumulated in the condensed matrix, desorption is a single molecular process taking place on the surface. In this paper, desorption methods for mass spectrometry developed in our laboratory: flash heating/rapid cooling, Leidenfrost phenomenon-assisted thermal desorption (LPTD), solid/solid friction, liquid/solid friction, electrospray droplet impact (EDI) ionization/desorption, and probe electrospray ionization (PESI), will be described. All the methods are concerned with the surface and interface phenomena. The concept of how to desorb less-volatility compounds from the surface will be discussed. PMID:28337398

  20. 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

  1. 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.

  2. 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

  3. 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

  4. Where is the lithium? Quantitative determination of the lithium distribution in lithium ion battery cells: Investigations on the influence of the temperature, the C-rate and the cell type

    NASA Astrophysics Data System (ADS)

    Vortmann-Westhoven, Britta; Winter, Martin; Nowak, Sascha

    2017-04-01

    With lithium being the capacity determining species in lithium-ion battery (LIB) cells, the local quantification is of enormous importance for understanding of the cell performance. The investigation of the lithium distribution in LIB full cells is performed with two different cell types, T-cells of the Swagelok® type and pouch bag cells with lithium nickel cobalt manganese oxide and mesocarbon microbead graphite as the active materials as well as a lithium hexafluorophosphate based organic carbonate solvent electrolyte. The lithium content of/at the individual components of the cells is analyzed for different states of charge (SOCs) by inductively coupled plasma-optical emission spectrometry (ICP-OES) and the lithium distribution as well as the loss of active lithium within the cells is calculated after cycling. With increasing the SOC, the lithium contents decrease in the cathodes and simultaneously increase in the anodes. The temperature increase shows a clear shift of the lithium content in the direction of the anode for the T-cells. The comparison of the C-rate influence shows that the lower the C-rate, the more the lithium content on the electrodes is shifted into the direction of the anode.

  5. Investigation of ruthenium promoted palladium catalysts for methanol electrooxidation in alkaline media

    NASA Astrophysics Data System (ADS)

    Jurzinsky, Tilman; Kammerer, Patricia; Cremers, Carsten; Pinkwart, Karsten; Tübke, Jens

    2016-01-01

    In this study, the investigation of binary palladium based electrocatalysts for methanol oxidation in alkaline media is reported. For this purpose, electrocatalysts with a loading of 20wt% metal on VulcanXC72-R were synthesized via wet chemical reduction with various compositions of palladium and ruthenium. Physical characterization via transmission electron microscopy (TEM), thermogravimetric analysis (TGA) and inductively coupled plasma optical emission spectroscopy (ICP-OES) was done and verified the synthesis of nanoparticles on carbon support. Electrochemical evaluation of the catalytic behavior of Pd/C, Ru/C and PdXRu/C (X = 1, 3, 5) via cyclic voltammetry and chronoamperometry was conducted in a 3-electrode setup. These measurements suggested that Pd3Ru/C is a promising material for methanol oxidation reaction in alkaline media with an onset potential of 0.465 VRHE and a peak current density of over 1 A mg-1Pd. To further investigate the oxidation of methanol on Pd/C and Ru promoted catalysts, differential electrochemical mass spectrometry (DEMS) measurements were done. From these results a higher CO2 current efficiency (CCE) of 86% for Pd3Ru/C compared to 65% for Pd/C was found. Moreover, fuel cell tests verified the results and showed that Pd3Ru/C has the better performance.

  6. Structural and magnetic properties of calcium doped nickel ferrite nanoparticles by co-precipitation method

    NASA Astrophysics Data System (ADS)

    Vigneswari, T.; Raji, P.

    2017-01-01

    It is a truism that a sequence of calcium doped nickel ferrite (with x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0) nanoparticles are combined by co-precipitation technique. X-Ray Diffraction (XRD) and Fourier Transform Infrared (FTIR) scrutinize the formation of single-phase inverse spinel structure in all the compositions. The lattice framework increases with the increase in calcium concentration and it exhibits the development of unit cell. Crystallite size in the range of 22-34 nm is viewed and also augmented the level of calcium. The elemental composition of pure and calcium doped nickel ferrite has been procured from Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) and Energy Dispersive X-ray analysis (EDX). It is interesting to note that the substitution of calcium increasingly exerts influence on the magnetic characteristics. These observations paved the way for the room temperature of magnetization measurements. The saturation magnetization and the experimental value of magnetic moment are noticed to enlarge initially up to x = 0.2, and then decrease incessantly with increase in the Ca content x. The increase and the decrease of saturation magnetization have widely been expounded by Neel's collinear two-sublattice model and Yafet-Kittel (Y-K) three-sub lattice model.

  7. 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.

  8. 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.

  9. 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

  10. 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.

  11. Comparison of various digestion procedures in chemical analysis of spent hydrodesulfurization catalyst.

    PubMed

    Szymczycha-Madeja, Anna; Mulak, Władysława

    2009-05-30

    Four digestion procedures have been tested to verify their applicability to the determination of major and trace elements (Al, Ba, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Sr, Ti, V, Zn) in a spent catalyst by inductively coupled plasma optical emission spectrometry (ICP-OES). Two digestion procedures have been carried out in a closed microwave system using: (1) HCl+HNO(3)+H(2)O(2); (2) HNO(3)+HF, whereas the remaining two in an open system using: (1) aqua regia+NH(4)F, HNO(3), H(2)SO(4); (2) HF+HClO(4), H(3)BO(3), HCl. Among these four procedures the microwave digestion system (1) gave the best recovery results. The quality of the analytical results has been evaluated by the analysis of the CTA-FFA-1 Fine Fly Ash Certified Reference Material. A good agreement between the measured and reference values was found for almost all elements. The precision was assessed from the replicate analyses of microwave digestion (1) system and was found to be less than 5% of the relative standard deviation (R.S.D.).

  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. Antioxidative effects of N-acetylcysteine, lipoic acid, taurine, and curcumin in the muscle of Cyprinus carpio L. exposed to cadmium.

    PubMed

    Sevgiler, Yusuf; Karaytug, Sahire; Karayakar, Fahri

    2011-03-01

    We investigated the muscle tissue of a teleost Cyprinus carpio L. to find out whether N-acetylcysteine (NAC), alpha-lipoic acid (LA), taurine (TAU), and curcumin (CUR) were able to counteract oxidative stress induced by acute exposure to cadmium (Cd). The muscle tissue was dissected 96 h after a single intraperitoneal injection of Cd (5 mg kg(-1)) and of antioxidant substances (50 mg kg(-1)). Using spectrophotometry, we determined the glutathione redox status, lipid peroxidation levels and the activities of superoxide dismutase (SOD), catalase (CAT), glutathione peroxidase (GPx), and glutathione disulphide reductase (GR). Accumulation of Cd in the muscle was analysed using inductively coupled plasma - optical emission spectrometry (ICP-OES).All substances lowered Cd levels in the following order of efficiency; LA=NAC>TAU=CUR. Cadmium increased SOD activity, but CAT activity declined, regardless of antioxidant treatment. Treatment with CUR induced GPx activity. Treatment with TAU lowered Cd due to higher total glutathione (tGSH). The most effective substances on lipid peroxidation were LA and NAC due to a greater Cd-lowering potential. It seems that the protective role of TAU, LA, and NAC is not necessarily associated with antioxidant enzymes, but rather with their own activity.

  14. 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.

  15. The Role of Ligand in the Mechanical Properties of Self-Assembled Nanoparticle Films

    NASA Astrophysics Data System (ADS)

    Griesemer, Sean; You, Sean; Kanjanaboos, Pongsakorn; Barry, Edward; Bu, Wei; Rice, Stuart; Lin, Binhua

    Self-assembled films of nanoparticles (NP) capped with ligands at the air/water interface exhibit rich mechanical responses to compression including hashing, wrinkling, and folding, which are the combined result of particle- and ligand-based interactions. Previous studies have shown that a high concentration of ligands inhibits wrinkling and folding, but the mechanism remains elusive. By using inductively coupled plasma optical emission spectrometry (ICP-OES) to measure the ligand concentration of our NP solutions and then back-adding excess ligands at controlled amounts, we precisely control ligand-based interactions, enabling an investigation of how these interactions guide self-assembly and correspondingly on mechanical properties. Our experiments reveal that increasing the ligand concentration of the films causes the formation of free-ligand islands in addition to an increase in the interparticle separation. These effects are correlated with the previously observed inhibition of wrinkling and folding, as well a decrease in the dilatational and shear moduli. This work was supported by the University of Chicago Materials Research Science and Engineering Center, NSF-DMR-1420709.

  16. 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

  17. Fully Automatic In-Syringe Magnetic Stirring-Assisted Dispersive Liquid-Liquid Microextraction Hyphenated to High-Temperature Torch Integrated Sample Introduction System-Inductively Coupled Plasma Spectrometer with Direct Injection of the Organic Phase.

    PubMed

    Sánchez, Raquel; Horstkotte, Burkhard; Fikarová, Kateřina; Sklenářová, Hana; Maestre, Salvador; Miró, Manuel; Todolí, Jose-Luis

    2017-03-21

    A proof of concept study involving the online coupling of automatic dispersive liquid-liquid microextraction (DLLME) to inductively coupled plasma optical emission spectrometry (ICP OES) with direct introduction and analysis of the organic extract is herein reported for the first time. The flow-based analyzer features a lab-in-syringe (LIS) setup with an integrated stirring system, a Meinhard nebulizer in combination with a heated single-pass spray chamber, and a rotary injection valve, used as an online interface between the microextraction system and the detection instrument. Air-segmented flow was used for delivery of a fraction of the nonwater miscible extraction phase, 12 μL of xylene, to the nebulizer. All sample preparative steps including magnetic stirring assisted DLLME were carried out inside the syringe void volume as a size-adaptable yet sealed mixing and extraction chamber. Determination of trace level concentrations of cadmium, copper, lead, and silver as model analytes has been demonstrated by microextraction as diethyldithiophosphate (DDTP) complexes. The automatic LIS-DLLME method features quantitative metal extraction, even in troublesome sample matrixes, such as seawater, salt, and fruit juices, with relative recoveries within the range of 94-103%, 93-100%, and 92-99%, respectively. Furthermore, no statistically significant differences at the 0.05 significance level were found between concentration values experimentally obtained and the certified values of two serum standard reference materials.

  18. Major and trace elements in whole blood of phlebotomized patients with porphyria cutanea tarda.

    PubMed

    Dinya, Mariann; Székely, E; Szentmihályi, K; Tasnádi, Gy; Blázovics, A

    2005-01-01

    Porphyria cutanea tarda (PCT) is a disorder of hem biosynthesis resulting from a decreased activity of the uroporphyrinogen decarboxylase enzyme. Hem precursors are accumulated in the blood, liver and skin. Inherited and acquired factors also contribute to the pathogenesis of PCT. Hem precursors and porphyrins are excreted with urine and faeces. Whole blood of 8 PCT patients and 6 volunteers of Caucasian origin were analysed. In addition to routine laboratory measurements, 19 elements (Al, B, Ba, Ca, Cd, Co, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, S, V, Zn) were determined by means of inductively coupled plasma optical emission spectrometry (ICP-OES). Mg, P and S concentrations in whole blood were decreased significantly (p<0.05), whereas Ba was increased in PCT patients compared to controls. Metabolic alterations are reflected in the correlation of parameters. Positive correlations were found between the element pairs of Zn-Al, Zn-Mg, Zn-Mn, B-S, Fe-Mg, K-P, Mg-Mn for PCT patients, whereas in the control group Al-Mn, Ca-Cu, Ca-Na, Cu-Mg, Fe-K, Mg-Na, Zn-P showed positive correlations.

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

    PubMed

    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

    2007-04-01

    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.

  20. 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.

  1. Lead, cadmium and mercury contents and bioaccumulation potential of wild edible saprophytic and ectomycorrhizal mushrooms, Croatia.

    PubMed

    Širić, Ivan; Kasap, Ante; Bedeković, Dalibor; Falandysz, Jerzy

    2017-03-04

    Lead (Pb), cadmium (Cd), and mercury (Hg) contents in ten species of edible mushrooms in Trakošćan, Croatia were determined. In addition, the similarity between the studied species was determined by cluster analysis. The caps and stipes of the fruiting bodies were analysed separately. The analyses were carried out by inductively coupled plasma - optical emission spectrometry (ICP-OES). The greatest mean lead concentrations of 1.91 and 1.60 mg kg (-1) were determined in caps and stipes of Macrolepiota procera. The greatest mean concentrations of cadmium (3.23 and 2.24 mg kg(-1)) were determined in caps and stipes of Agaricus campestris and of mercury (2.56 and 2.35 mg kg(-1)) in Boletus edulis. In terms of the anatomical parts of the fruiting body (cap-stipe), a considerably greater concentration of the analysed elements was found in the cap for all mushroom species. According to calculated bio-concentration factors, all the examined species were found to be bio-accumulators of Cd and Hg. On the basis of the accumulation of the studied metals, great similarity of mushroom species belonging to the same genus and partial similarity of species of the same ecological affiliation was obtained by cluster analysis.

  2. 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.

  3. 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.

  4. 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.

  5. Speciation analysis of Sb(III) and Sb(V) in antileishmaniotic drug using Dowex 1 x 4 resin from hydrochloric acid solution.

    PubMed

    Łukaszczyk, L; Zyrnicki, W

    2010-09-05

    A new and simple method for the direct and simultaneous determination of Sb(III) and Sb(V) in meglumine antimoniate, the first-choice drug for leishmaniasis treatment, was developed. Speciation analysis was carried out using the quantitative separation of inorganic trivalent and pentavalent antimony on Dowex 1 x 4 resin from 1.5 mol l(-1) hydrochloric acid solution. The inductively coupled plasma optical emission spectrometry (ICP-OES) was used for determination of antimony. The interfering effects of As, Bi, Cd, Cu, Mn, Pb and Zn were examined and only Bi was found to be a significant interferent. The liberation of Sb(V) and Sb(III) from organoantimonial compounds without changing of oxidation state was carried out by means of 1.5 mol l(-1) hydrochloric acid solution. The spike recovery values obtained for Sb(III) in pharmaceutical sample varied from 92 to 100%. The method was successfully applied for the direct determination of antimony(III) and of antimony(V) in meglumine antimoniate.

  6. A biogeochemical approach to understanding the accumulation patterns of trace elements in three species of dragonfly larvae: evaluation as biomonitors.

    PubMed

    Lavilla, Isela; Rodríguez-Liñares, Genma; Garrido, Josefina; Bendicho, Carlos

    2010-03-01

    The accumulation patterns of different trace elements (As, Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn) were studied in three species of dragonfly larvae (Cordulegaster boltoni, Boyeria irene and Onychogomphus uncatus). Additionally these species were assessed as potential biomonitors in a lotic ecosystem (Louro River, Spain). Element concentrations were determined by inductively coupled plasma optical emission spectrometry (ICP-OES) in both dragonfly larvae and river sediments. The surface of the larvae was observed and analyzed with scanning electron microscopy (SEM). A desorption test was used to establish the percentage of element adsorbed into the exoskeleton. Field biomonitoring studies were made considering the first part of the river as a control area in relation to the second part, which was severely polluted by industrial and domestic activities. Upon application of principal component analysis (PCA), two different element groups were found in relation to element bioaccumulation. Cu, Cd and Zn were mainly associated with the inner part of the larvae. As, Cr, Fe, Mn, Ni and Zn were found on the outer body parts, related with deposition of oxyhydroxides in the hydrocycle. SEM revealed a layer of inorganic particles, similar in composition to fine bed sediments. Significant relations between the element content of this group and that of sediments at the sampling site were found. Differences in bioaccumulation for each of the three species, except for As, were observed. Dragonfly larvae revealed their ability to reflect environmental concentrations of As in freshwater media.

  7. 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.

  8. In Vitro Iron Availability from Insects and Sirloin Beef.

    PubMed

    Latunde-Dada, Gladys O; Yang, Wenge; Vera Aviles, Mayra

    2016-11-09

    Interest in the consumption of insects (entomophagy) as an alternative environmentally sustainable source of protein in the diet of humans has recently witnessed a surge. Knowledge of the nutrient composition and, in particular, the bioavailability of minerals from insects is currently sparse. This study evaluated the availability of Fe, Ca, Cu, Mg, Mn, and Zn from four commonly eaten insects and compared these to sirloin beef. Soluble iron from the samples was measured by inductively coupled plasma optical emission spectrometry (ICP-OES). Iron bioavailability was determined using an in vitro simulated peptic-pancreatic digestion, followed by measurement of ferritin (a surrogate marker for iron absorption) in Caco-2 cells. Cricket and sirloin beef had comparably higher levels of Fe, Ca, and Mn than grasshopper, meal, and buffalo worms. However, iron solubility was significantly higher from the insect samples than from beef. The complementation of whole-wheat flour with insect or beef protein resulted in overall decreases in mineral content and iron solubility in the composite mixtures. Collectively, the data show that grasshopper, cricket, and mealworms contain significantly higher chemically available Ca, Cu, Mg, Mn, and Zn than sirloin. However, buffalo worms and sirloin exhibited higher iron bioavailability comparable to that of FeSO4. Commonly consumed insect species could be excellent sources of bioavailable iron and could provide the platform for an alternative strategy for increased mineral intake in the diets of humans.

  9. 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.

  10. Metals Content in Herbal Supplements.

    PubMed

    Barrella, Michelle Vieira; Heringer, Otavio Arruda; Cardoso, Priscylla Maria Martins; Pimentel, Elisangela Flavia; Scherer, Rodrigo; Lenz, Dominik; Endringer, Denise C

    2017-02-01

    Obesity has become an international epidemic. To evaluate the level of metals in extracts of plants prescribed as weight loss supplements, different brands containing Camellia sinensis (L.) Kuntze, Citrus aurantium L., Cordia ecalyculata Vell, Ilex paraguariensis A. St.-Hil, Cissus quadrangularis L., Senna alexandrina Mill were purchased in local market, hot acid digested, and analyzed while metal content by inductively coupled plasma optical emission spectrometry, ICP-OES. Quality assurance and quality control tests were carried out in order to monitor and control the reliability of the analytical method. For each metal evaluated, a calibration curve was prepared with certified reference material. The recovery test was performed for each batch of samples. Analyses were performed in triplicate. Quantification of aluminum, barium, cadmium, cobalt, chromium, copper, iron, lithium, manganese, molybdenum, nickel, lead, vanadium, and zinc were determined. The metals most frequently detected were manganese (15.3-329,60 mg kg(-1)) aluminum (11.76-342.4 mg kg(-1)), and iron (11.14-73.01 mg kg(-1)) with higher levels in products containing C. sinensis China origin, I. paraguariensis Brazilian origin, C. quadrangularis, and C. aurantium China origin, respectively. To ensure safety consumption, an adequacy of the certification of Brazilian suppliers for herbal weight loss products is indispensable.

  11. Development of a new sample pre-treatment procedure based on pressurized liquid extraction for the determination of metals in edible seaweed.

    PubMed

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

    2007-08-13

    A new, simple, fast and automated method based on acetic acid-pressurized liquid extraction (PLE) has been developed for the simultaneous extraction of major and trace elements (As, Ca, Cd, Co, Cr, K, Mg, Mn, Na, Pb, Sr and Zn) from edible seaweeds. The target elements have been simultaneously determined by inductively coupled plasma-optical emission spectrometry (ICP-OES). The influence of several extraction parameters (e.g. acetic acid concentration, extraction temperature, extraction time, pressure, number of cycles, particle size and diatomaceous earth (DE) mass/sample mass ratio) on the efficiency of metal leaching has been evaluated. The results showed that metal extraction efficiency depends on the mass ratio of the dispersing agent mass and the sample. The optimized procedure consisted of the following conditions: acetic acid (0.75 M) as an extracting solution, 5 min of extraction time, one extraction cycle at room temperature at a pressure of 10.3 MPa and addition of a dispersing agent (at a ratio of 5:1 over the sample mass). The leaching procedure was completed after 7 min (5 min extraction time plus 1 min purge time plus 1 min end relief time). Limits of detection and quantification and repeatability of the over all procedure have been assessed. Method validation was performed analysing two seaweed reference materials (NIES-03 Chlorella Kessleri and NIES-09 Sargasso). The developed extraction method has been applied to red (Dulse and Nori), green (Sea Lettuce) and brown (Kombu, Wakame and Sea Spaghetti) edible seaweeds.

  12. [Study on the chemical form and extraction rate of Cr, Cu, Fe, Mn, Ni and Zn in tea].

    PubMed

    Gao, G; Tao, R

    2000-07-01

    The content of Cr, Cu, Fe, Mn, Ni and Zn in the tea commonly available in China market were measured by inductivity coupled plasma-optical emission spectrometry (ICP-OES). The extraction rates of the six elements in tea leachate were measured. The solubilitied were 39.8% for Cr, 42.5% for Cu, 8.6% for Fe, 45.5% for Mn, 87.1% for Ni and 71.0% for Zn. The process of making tea leachate affects the elements extraction rates. The content of the microelements in tea leave extracts decreases gradually with the processing. About 80% of Cr, Cu, Mn, Ni and Zn and 60% of Fe were in the first infusion of tea. Moreover, the chemical forms of six elements were determined. The ratios of organic to inorganic forms were 0.33 for Cr, 0.022 for Cu, 0.18 for Fe, 0.002 for Mn, 0.01 for Ni and 0.18 for Zn. It is concluded that the six elements from the tea infusion extracted from 5 g tea are too little to meet the recommend dietary allowance (RDA). Therefore, tea is not a rich food source of Cr, Cu, Fe, Mn, Ni and Zn.

  13. Estimation of human daily boron exposure in a boron-rich area.

    PubMed

    Korkmaz, Mehmet; Sayli, Uğur; Sayli, Bekir Sitki; Bakirdere, Sezgin; Titretir, Serap; Yavuz Ataman, Osman; Keskin, Siddik

    2007-09-01

    Although, the safe limits of human daily boron (B) exposure are not absolutely clear, there is a growing interest in B and its effects on human health. The aim of the present study was to estimate daily B exposure in 66 males in Turkey living in a B-rich area using water containing at least 2 mg/l boron, with an average age of 38.55 (se 1.66) years and an average number of years of residence in the B-rich area of 35.89 (se 1.73). Another group of males (n 57), living in the city centres of Balikesir and Ankara, were taken as controls; the average age and number of years of residence for this group were 29.44 (se 1.43) and 10.26 (se 1.83) years, respectively. As it is assumed that the B level in urine reflects daily B exposure, the amount of urinary B of both the study and control groups was analysed by using an inductively coupled plasma optical emission spectrometry (ICP-OES) technique. The average daily B exposure value was calculated as 6.77 (se 0.47) mg in the study group and 1.26 (se 0.1) mg in the controls. The results of this study are expected to contribute to creating a reference value for a safe daily B exposure.

  14. 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.

  15. 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.

  16. 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.

  17. Chemical speciation and potential mobility of heavy metals in the soil of former tin mining catchment.

    PubMed

    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.

  18. Differences in the accumulation and tissue distribution of Pb, Cd, and Cu in Mediterranean mussels (Mytilus galloprovincialis) exposed to single, binary, and ternary metal mixtures.

    PubMed

    García-Navarro, José A; Franco, Lorena; Romero, Diego

    2017-01-12

    Heavy metals often accumulate in complex mixtures in the environment and are currently a source of concern in many marine ecosystems. Pb, Cd, and Cu are regarded as priority hazardous metals due to their great persistence, bioaccumulation, and toxicity. The aim of the present study was to investigate the tissue accumulation and distribution of these heavy metals in Mediterranean mussels (Mytilus galloprovincialis) exposed to binary and ternary mixtures of metals as opposed to only single exposures. Heavy metal concentrations in the digestive gland, gills, and the other soft tissues were determined by inductively coupled plasma optical emission spectrometry (ICP-OES), and the distribution of each metal was analyzed according to compartments. The concentrations of Pb, Cd, and Cu increased significantly in the group exposed to the ternary mixture; however, there was no common response pattern to exposure in single and binary mixtures. Above all, the metals concentrated in the digestive gland, although the percentages of each element varied between compartments and varied between tissues according to the treatment.

  19. Metallic elements (Ca, Hg, Fe, K, Mg, Mn, Na, Zn) in the fruiting bodies of Boletus badius.

    PubMed

    Kojta, Anna K; Falandysz, Jerzy

    2016-06-01

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

  20. Effects of chronic lead exposure on bone mineral properties in femurs of growing rats.

    PubMed

    Álvarez-Lloret, Pedro; Lee, Ching Ming; Conti, María Inés; Terrizzi, Antonela Romina; González-López, Santiago; Martínez, María Pilar

    2017-02-15

    Lead exposure has been associated with several defective skeletal growth processes and bone mineral alterations. The aim of the present study is to make a more detailed description of the toxic effects of lead intoxication on bone intrinsic material properties as mineral composition, morphology and microstructural characteristics. For this purpose, Wistar rats were exposed (n=12) to 1000ppm lead acetate in drinking water for 90days while control group (n=8) were treated with sodium acetate. Femurs were examined using inductively coupled plasma optical emission spectrometry (ICP-OES), Attenuated Total Reflection Fourier transform infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD), and micro-Computed Tomography (μCT). Results showed that femur from the lead-exposed rats had higher carbonate content in bone mineral and (Ca(2+)+Mg(2+)+ Na(+))/P ratio values, although no variations were observed in crystal maturity and crystallite size. From morphological analyses, lead exposure rats showed a decreased in trabecular bone surface and distribution while trabecular thickness and cortical area increased. These overall effects indicate a similar mechanism of bone maturation normally associated to age-related processes. These responses are correlated with the adverse actions induced by lead on the processes regulating bone turnover mechanism. This information may explain the osteoporosis diseases associated to lead intoxication as well as the risk of fracture observed in populations exposed to this toxicant.

  1. Green synthesis of hyaluronan fibers with silver nanoparticles.

    PubMed

    Abdel-Mohsen, A M; Hrdina, Radim; Burgert, Ladislav; Krylová, Gabriela; Abdel-Rahman, Rasha M; Krejčová, Anna; Steinhart, Miloš; Beneš, Ludvík

    2012-06-20

    The application of green chemistry in the nano-science and technology is very important in the area of the preparation of various materials. In this work, an eco-friendly chemical method was successfully used for the preparation of hyaluronan fibers containing silver nanoparticles (AgNPs). Thus, hyaluronic acid (HA) was dissolved in an aqueous solution of sodium hydroxide to prepare a transparent solution, which was used for the preparation of fibers by a wet-spinning technique. Consequently, silver nanoparticles inside the fiber were prepared. Different parameters affecting the preparation of final product, such as concentration of silver nitrate, hyaluronan fiber concentration, time and temperature of the reaction, pH of the reaction mixture, were studied. AgNPs were confirmed by transmission electron microscopy (TEM), X-ray diffraction (XRD), two-dimensional X-ray scattering (2D SWAXS), UV/Vis spectroscopy, inductively coupled plasma optical emission spectrometry (ICP OES) and scan electron microscopy (SEM). Mechanical properties of prepared fibers were also measured.

  2. 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.

  3. 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.

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

    PubMed

    Qi, Cuicui; Liu, Guijian; Kang, Yu; Lam, Paul K S; Chou, Chenlin

    2011-08-01

    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 plasma-optical 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.

  5. 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

  6. 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.

  7. 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).

  8. Characterization of radioactive contaminants and water treatment trials for the Taiwan Research Reactor's spent fuel pool.

    PubMed

    Huang, Chun-Ping; Lin, Tzung-Yi; Chiao, Ling-Huan; Chen, Hong-Bin

    2012-09-30

    There were approximately 926 m(3) of water contaminated by fission products and actinides in the Taiwan Research Reactor's spent fuel pool (TRR SFP). The solid and ionic contaminants were thoroughly characterized using radiochemical analyses, scanning electron microscopy equipped with an energy dispersive spectrometer (SEM-EDS), and inductively coupled plasma optical emission spectrometry (ICP-OES) in this study. The sludge was made up of agglomerates contaminated by spent fuel particles. Suspended solids from spent ion-exchange resins interfered with the clarity of the water. In addition, the ionic radionuclides such as (137)Cs, (90)Sr, U, and α-emitters, present in the water were measured. Various filters and cation-exchange resins were employed for water treatment trials, and the results indicated that the solid and ionic contaminants could be effectively removed through the use of <0.9 μm filters and cation exchange resins, respectively. Interestingly, the removal of U was obviously efficient by cation exchange resin, and the ceramic depth filter composed of diatomite exhibited the properties of both filtration and adsorption. It was found that the ceramic depth filter could adsorb β-emitters, α-emitters, and uranium ions. The diatomite-based ceramic depth filter was able to simultaneously eliminate particles and adsorb ionic radionuclides from water.

  9. 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.

  10. 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.

  11. Advances in the chemistry of nanosized zirconium phosphates: a new mild and quick route to the synthesis of nanocrystals.

    PubMed

    Pica, Monica; Donnadio, Anna; Capitani, Donatella; Vivani, Riccardo; Troni, Elisabetta; Casciola, Mario

    2011-11-21

    Simple addition of zirconyl propionate to phosphoric acid in alcoholic media surprisingly led to the formation, in few minutes, of transparent gels containing solvent intercalated zirconium phosphate (ZrP) nanoparticles with hexagonal shape and a planar size of about 40 nm. With the help of elemental analysis, inductively coupled plasma-optical emission spectrometry (ICP-OES), and (31)P magic angle spinning (MAS) NMR, the nanoparticle composition was formulated as Zr(R)(w)(HPO(4))(x)(H(2)PO(4))(y), in which R can be an hydroxyl or a propionate group. The stoichiometric coefficients for propanol intercalated ZrP are x = 1.43, y = 0.83, and w = 0.32. Solvent elimination at 60 °C gave rise to an increase in the x value and a decrease in the y and w values. X-ray powder diffraction analysis and transmission electron microscopy (TEM) observations showed a concomitant increase in the particle size: planar size and thickness ranged from 90 to 200 nm and from 20 to 85 nm, respectively, depending on the nature of the solvent. A possible mechanism explaining the change in the x, y, and w values, the growth of nanoparticles, and the role of the solvent is proposed. Finally, the possibility of using these gels to disperse the ZrP nanoparticles within the polymer matrix of Nafion117 is shown.

  12. Trace elements in sediments, blue spotted tilapia Oreochromis leucostictus (Trewavas, 1933) and its parasite Contracaecum multipapillatum from Lake Naivasha, Kenya, including a comprehensive health risk analysis.

    PubMed

    Otachi, Elick O; Körner, Wilfried; Avenant-Oldewage, Annemariè; Fellner-Frank, Christine; Jirsa, Franz

    2014-06-01

    This study presents the distribution of 15 major and trace elements in sediments and fish and their pericardial parasites from Lake Naivasha, Kenya. The lake is one of the few freshwater lakes in the Great Rift Valley and is under strong anthropogenic pressure mainly due to agricultural activities. Its fish provide a valuable protein source for approximately 100,000 people in the area. Fish and their parasites have been acknowledged as indicators of environmental quality due to their accumulation potential for both essential and nonessential trace elements. A total of 34 specimens of the blue spotted tilapia Oreochromis leucostictus and pooled samples of their pericardial parasite, the anisakid nematode Contracaecum multipapillatum (larvae 3), were examined. Element concentrations were determined by inductively coupled plasma-optical emission spectroscopy (ICP-OES) and graphite furnace atomic absorpti