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Sample records for emission spectrometry icp-oes

  1. Extraction inductively coupled plasma-optical emission spectrometry (ICP-OES). Determination of traces of phosphorus in tungsten

    International Nuclear Information System (INIS)

    Bauer, G.; Wegscheider, W.; Mueller, K.

    1989-01-01

    A method for the separation and preconcentration of traces of phosphorus from tungsten was developed. Solid phase extraction of the phosphovanadomolybdate complex performed on a micro-column was applied. Phosphorus was determined by optical emission spectroscopy (OES) with inductively coupled plasma (ICP) excitation. A limit of detection of 0,4 μg/g P with respect to the solid phase is obtained. By directly coupling the extraction/elution step to the ICP instrument a detection limit of 0,06 μg/g P in W was achieved. Besides, the complexity of spectral evaluation in ICP-OES determinations of traces in spectralline-rich matrices is discussed. (Authors)

  2. Determination of total strontium in uruguayan rice by inductively coupled plasma optical emission spectrometry (ICP-OES

    Directory of Open Access Journals (Sweden)

    Mario E. Rivero Huguet

    2011-04-01

    Full Text Available Strontium (Sr is found naturally as a non-radioactive element and has 16 known isotopes. Naturally occurring Sr is found as four stable isotopes: Sr-84, -86, -87, and -88. Twelve other isotopes are radioactive. Sr-90 is the most important radioactive isotope in the environment, discovered mostly after the nuclear experiments conducted in the 1950s and 1960s. In the present work, 86 rice samples (Oryza saliva L. and 7 rice husk samples were digested by dry ashing for the purpose of determining the total Sr levels by ICP-OES. The mean concentrations found were: 0.281 µg g-1 for milled, 0.287 µg g-1 for parboiled milled, 0.564 µg g-1 for brown, 0.73 µg g-1 for parboiled brown, and 1.16 µg g-1 for paddy rice, and 3.44 µg g-1 for the rice husks. Validation of the method was conducted with a certified reference material, NIST CAM 8418 Wheat Gluten, and the recovery obtained ranged from 89-98%. As the outer layers (aleurone, pericarp of the grain are removed, the Sr concentration decreases. It can then be assumed that most of the Sr is stored in these layers. Although no extensive data exist for Sr levels in rice, the values obtained are in good agreement with the results reported for Sr in brown rice from Japan (0.25-0.72 µg g-1 and with non-contaminated foodstuffs from other parts of the world. Thus, the Uruguayan rice has Sr levels that match non-contaminated samples and its consumption presents no health threat.Publicado en: Atomic Spectroscopy.-- 2006, 27(3:80-85

  3. Evaluation of analytical procedures for the determination of cadmium, boron and lithium in UALx samples by inductively coupled plasma optical emission spectrometry (ICP OES)

    International Nuclear Information System (INIS)

    Guilhen, Sabine Neusatz; Kakazu, Mauricio H.; Cotrim, Marycel Elena Barboza; Pires, Maria Aparecida Faustino; Souza, Alexandre Luiz de

    2013-01-01

    Used in over 80% of the worldwide diagnostic procedures, Technetium-99m ( 99m Tc), which is obtained from the decay of molybdenum-99 ( 99 Mo), is the most important radioisotope in nuclear medicine. IPEN/CNEN-SP has been developing technologies in order to produce Mo-99 by the irradiation of low-enriched uranium (LEU < 20% of 235U) targets in its research reactor IEA-R1 (IPEN, Sao Paulo/Brazil). These targets consist of low enriched uranium dispersed in a matrix of aluminum (UAlx-Al). Several impurities may be incorporated during the target's production process, such as boron, cadmium and lithium, which have a high capture cross section that may reduce the irradiation's efficiency. This study describes a simple and rapid inductively coupled plasma optical emission spectrometric method for the determination of cadmium, boron and lithium in uranium aluminum (UAlx) dispersion targets. The method involves a previous separation step, in which uranium gets removed from the matrix by chromatographic extraction with the use of a divinylbenzene resin Amberlite XAD - 4 doped with tri-n-butyl phosphate (TBP). TBP selectively separates the uranium, leaving behind the impurities in an aqueous medium for a further quantification by ICP OES. Possible spectroscopic interferences are also discussed in this article, because of the high amount of aluminum in the remaining solution. Experimental and instrumental conditions, such as initial mass, acid solution ratio and amount, resin mass, emission lines and interfering concentrations are carefully established. This method is to be applied for the determination of several others impurities in UAlx in the future, providing means to verify the UAlx targets' compliance to the current established specifications through routine laboratory analysis. (author)

  4. Electrolytic dissolution of aluminium alloys (chip form) and mullet-element determination by inductively coupled plasma optical emission spectrometry (ICP-OES)

    International Nuclear Information System (INIS)

    Grigoletto, Tania

    2001-01-01

    Several aluminum alloys with different chip's size were dissolved using aqua regia (HCl:HN0 3 ,3:1). The residues of the dissolution procedure were either rejected or used in silicon volatilization with hydrofluoric acid before determination of Fe, Cu, Mn, Mg, Cr, Ni, Zn, Pb, Sn, Ti and Zr by ICP-OES. The influence caused by crescent amounts of aluminum in the determination of other elements and the probable spectral interference by Cu in determination of Zn (with or without electrolytic separation of Cu) was evaluated. The electrolytic dissolution of aluminum alloys was performed by pressing chips against a platinum electrode for the electrolysis to occur, so that way the chips behaved as the anode. A tube (body of syringe of 2.5 mL) with perforations around the open base was used to contain the sample and Pt electrode. The alloy was placed on synthetic wool (perlon) in this tube. An acrylic dowel with a platinum wire across its interior was fixed in the superior part a tube with Teflon film, with an orifice through which the electrolytic solution flowed (HNO 3 1 mol L -1 ; 4.5 mL min -1 ). A platinum dish was fixed at the inferior extremity of the platinum wire to press the sample. The solution came out through the inferior orifices of the tube to a flask, from where it was again captured (with a peristaltic pump) to go into the superior part of the tube. In this flask, a Pt wire cathode was also placed. A current of 0.6 A and ten minutes of electrolysis provided good results. Due to the partial dissolution, the knowledge of percentages of previous elements analyzed after total dissolution, or using certified reference material are necessary. The results were normalized by knowledge percentages. The calculations were made by the ratio between the concentration of the element determined, with the determined concentration of aluminum; the ratio between concentration of the element and the sum of the concentrations of the elements determined, including Al; the ratio

  5. Method validation in plasma source optical emission spectroscopy (ICP-OES) - From samples to results

    International Nuclear Information System (INIS)

    Pilon, Fabien; Vielle, Karine; Birolleau, Jean-Claude; Vigneau, Olivier; Labet, Alexandre; Arnal, Nadege; Adam, Christelle; Camilleri, Virginie; Amiel, Jeanine; Granier, Guy; Faure, Joel; Arnaud, Regine; Beres, Andre; Blanchard, Jean-Marc; Boyer-Deslys, Valerie; Broudic, Veronique; Marques, Caroline; Augeray, Celine; Bellefleur, Alexandre; Bienvenu, Philippe; Delteil, Nicole; Boulet, Beatrice; Bourgarit, David; Brennetot, Rene; Fichet, Pascal; Celier, Magali; Chevillotte, Rene; Klelifa, Aline; Fuchs, Gilbert; Le Coq, Gilles; Mermet, Jean-Michel

    2017-01-01

    Even though ICP-OES (Inductively Coupled Plasma - Optical Emission Spectroscopy) is now a routine analysis technique, requirements for measuring processes impose a complete control and mastering of the operating process and of the associated quality management system. The aim of this (collective) book is to guide the analyst during all the measurement validation procedure and to help him to guarantee the mastering of its different steps: administrative and physical management of samples in the laboratory, preparation and treatment of the samples before measuring, qualification and monitoring of the apparatus, instrument setting and calibration strategy, exploitation of results in terms of accuracy, reliability, data covariance (with the practical determination of the accuracy profile). The most recent terminology is used in the book, and numerous examples and illustrations are given in order to a better understanding and to help the elaboration of method validation documents

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

    Science.gov (United States)

    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. Uncertainties combined in algae and water in chemical analysis in determinations with ICP-OES

    International Nuclear Information System (INIS)

    Souza, Poliana Santos de

    2014-01-01

    One way to determine if some trace elements in algae and water is through uncertainty calculations. Spectrometry and inductively coupled plasma optical emission (ICP-OES) is widely used in this procedure, because it allows the analysis in waters and areas of solid samples. Thus, some elements (Fe, Ca and Mg) were used to calculate the uncertainty. (author)

  8. Leaching of heavy metals from contaminated soils using inductively coupled plasma optical emission spectrometer (ICP-OES) and atomic absorption spectrometer (AAS)

    International Nuclear Information System (INIS)

    Hussain, Z.; Islam, M.

    2010-01-01

    The clean-up of soils contaminated with heavy metals is one of the most difficult tasks for environmental engineering. Heavy metals are highly persistent in soil and a number of techniques have been developed that aim to remove heavy metals from contaminated soil. A method has been adopted to evaluate dynamic leaching of metal contaminants from industrial soil samples obtained from textile industrial sites in Lahore, Pakistan. In the extraction procedures employed five different leaching liquors were used: 0.01 M CaCl/sub 2/, 1 M HNO/sub 3/, a 1:1 mixture of 0.1M HCl and 0.1M NaCl, 0.01 M EDTA and pH controlled 0.5 M acetic acid. The qualitative and quantitative analyses were carried out by Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Plasma-Optical Emission Spectrometer (ICP-OES). The results indicate that Cu, Zn, Cd, Ni, Pb, Fe and As were extracted in the soil samples in varying concentration when using the different leach liquors. The predominant metals which were leached were As 78.7 ng/ml in 0.01 M EDTA; Zn 1.81 mu g/ml and Fe 898.96 macro g/ml in HNO/sub 3/. (author)

  9. Development of ICP-MS and ICP-OES methods for determination of gadolinium in samples related to hospital waste water treatment

    Czech Academy of Sciences Publication Activity Database

    Bendakovská, L.; Krejčovská, A.; Černohorský, T.; Zelenková, Jana

    2016-01-01

    Roč. 70, č. 9 (2016), s. 1155-1165 ISSN 0366-6352 Institutional support: RVO:67985874 Keywords : gadolinium * rare-earth elements * bioaccumulation * gadolinium anomaly * inductively coupled plasma mass spectrometry (ICP-MS) * inductively coupled plasma optical emission spectrometry (ICP-OES) Subject RIV: BK - Fluid Dynamics Impact factor: 1.258, year: 2016

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

    Science.gov (United States)

    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. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

  11. ICP OES Determination of Contaminant Elements Leached from Food Packaging Films

    Directory of Open Access Journals (Sweden)

    Éder José dos Santos

    2017-08-01

    Full Text Available ABSTRACT Determination of potential contaminants elements in food packing films arising from contact with acidic aqueous foods was undertaken by inductively coupled plasma optical emission spectrometry (ICP OES in accordance with DIN EN 1186-1. Test sections from plastic films were totally immersed in 3% w/v CH3COOH used as the food simulant. Testing was conducted under three conditions: (1 10 days at 40 ºC; (2 30 min at 70 ºC and 10 days at 40 ºC; and (3 30 min at 100 ºC and 10 days at 40 ºC. These time and temperature conditions were considered to be the most severe situations likely to be encountered in practice. Several different containers were investigated, including a borosilicate glass beaker, a glass bottle used for food canning, as well as one of polystyrene. The glass bottle was selected for testing treatments according to procedure (3 and a polystyrene one was chosen for use with procedures (1 and (2. Limits of quantitation were adequate for the determination of Ag, B, Ba, Cd, Cr, Cu, Pb, Sb, Sn and Zn by solution nebulization ICP OES and As by chemical vapor generation (CVG-ICP OES. Results for the analysis of AccuStandard certified reference materials as well as spike recoveries show good agreement with expected concentrations, demonstrating the accuracy and precision of the determinations. Eleven samples of food packing material were analyzed. The lead was present in the range 4.8 - 85.3 µg L-1 in 10 of 11 evaluated packing material, showing the importance of quality control measures.

  12. Determination of trace amounts of cerium in paint by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Wong, K.L.

    1981-01-01

    The determination of Ce in paint by inductively coupled plasma atomic emission spectrometry (ICP-OES) is described, and the detection limit of ICP-OES of 0.0004 ppM is compared with that of other methods. The effects of the major elemental components of paint, Si, Pb, Cr, and Na on the ICP-OES determination of Ce were studied. The interference of 400 ppM of the other ions on the determination of 10 ppM Ce was small (0 to 3% error). The method is applicable to the range of 0.2 to 700 ppM Ce

  13. Evaluation of metal ions in rice samples: extraction and direct determination by ICP OES

    International Nuclear Information System (INIS)

    Oliveira, Andrea; Cadore, Solange; Baccan, Nivaldo

    2012-01-01

    A method for extraction of metal ions present in rice samples using ammoniacal EDTA solution, pH = 10, as extractor agent is proposed under the following optimized conditions: 0.20 g of rice sample and 5.00 mL of ammoniacal EDTA (ethylenediaminetetraacetic acid) solution, with 5 min of ultrasound exposure time. Using robust ICP OES (inductively coupled plasma atomic emission spectrometry) conditions, direct analysis of the extraction solution was allowed, and the recovery values obtained were above 90% for most of the studied elements (P, K, Mg, Ca, Zn, Mn, Cu and Mo) with RSD -1 (Mn) - 48.68 mg kg -1 (K), showing adequate detectability for the determination of the analytes. The analysis of different samples indicated that Brazilian 'integral' rice contains higher contents of the constituents studied, followed by 'parboiled' rice, and the 'agulhinha' rice a long and thin grain type. (author)

  14. Utilization of ICP/OES for the determination of trace metal binding to different humic fractions.

    Science.gov (United States)

    de la Rosa, G; Peralta-Videa, J R; Gardea-Torresdey, J L

    2003-02-28

    In this study, the use of inductively coupled plasma/optical emission spectrometry (ICP/OES) to determine multi-metal binding to three biomasses, Sphagnum peat moss, humin and humic acids is reported. All the investigations were performed under part per billion (ppb) concentrations. Batch pH profile experiments were performed using multi-metal solutions of Cd(II), Cu(II), Pb(II), Ni(II), Cr(III) and Cr(VI). The results showed that at pH 2 and 3, the metal affinity of the three biomasses exposed to the multi-metal solution that included Cr(III) presented the following order: Cu(II), Pb(II)>Ni(II)>Cr(III)>Cd(II). On the other hand, when Cr(VI) was in the heavy metal mixture, Sphagnum peat moss and humin showed the following affinity: Cu(II), Pb(II)>Ni(II)>Cr(VI)>Cd(II); however, the affinity of the humic acids was: Cu(II)>Pb(II), Cr(VI)>Ni(II)>Cd(II). The results demonstrated that pH values of 4 and 5 were the most favorable for the heavy metal binding process. At pH 5, all the metals, except for Cr(VI), were bound between 90 and 100% to the three biomasses. However, the binding capacity of humic acids decreased at pH 6 in the presence of Cr(VI). The results showed that the ICP/OES permits the determination of heavy metal binding to organic matter at ppb concentration. These results will be very useful in understanding the role of humic substances in the fate and transport of heavy metals, and thus could provide information to develop new methodologies for the removal of low concentrations of toxic heavy metals from contaminated waters.

  15. Determination of trace elements in plant samples using XRF, PIXE and ICP-OES techniques

    International Nuclear Information System (INIS)

    Ahmed, Hassan Elzain Hassan

    2014-07-01

    The purpose of this study is to determine trace element concentration (Ca, Cu, Cr, K,Fe, Mn,Sr, and Za) in some sudanese wild plants namely, Ziziphus Abyssinica and Grewia Tenax. X-ray fluorescence ( X RF), particle-induced x-ray emission ( PIXE) and inductively coupled plasma-optical emission spectroscopy (ICP-OES) techniques were used for element determination. A series of plants standard references materials were used to check the reliability of the different employed techniques as well as to estimate possible factors for correcting the concentration of some elements that deviated significantly from their actual concentration. The results showed that, X RF, PIXE and ICP-OES are equally competitive methods for measuring Ca,K, Fe, Sr and Zn elements. Unlikely to ICP-OES seems to be superior techniques tend to be appropriate methods for Cu determination in plant samples however, for Mn element PIXE and ICP-OES are advisable techniques for measuring this element rather than X RF method. On the other hand, ICP-OES seems to be the superior techniques over PIXE and X RF methods for Cr and Ni determination in plant samples. The effect of geographical location on trace elements concentration in plants has been examined through determination of element in different species of Grewia Tenax than collected from different location. Most of measured elements showed similarity indicating there is no significant impact of locations on the difference of element contents. In addition, two plants with different genetic families namely, Ziziphus Spina Christi and Ziziphus Abyssinica were collected from the same location and screened for their trace element content. It was found that there were no difference between the two plants for Ca, K, Cu, Fe, and Sr element. However, significant variations were observed for Mn and Zn concentrations implying the possibility of using of those two elements for plant taxonomy purposes.(Author)

  16. Indigenous development of a glove box for ICP-OES

    International Nuclear Information System (INIS)

    Khan, A.M.; Anwar, M.K.; Bangash, M.A.

    2011-01-01

    Chemical analysis involving nuclear materials are bound to be carried out in safety enclosures like glove box, fume hood etc. whereas chemical analysis which produce mist or vapors of these materials like Atomic absorption Spectrometry, Flame photometry and ICP-AE spectrometry etc. must be performed in a glove box with HEPA filters on exhaust. These instruments with glove box adaptation are rare and impossible to import for our country. An ICP-OES, model Integra-XL of GBC-Australia was purchased in 2008 for chemical analysis of similar materials. As usual it was manufactured to operate in open atmosphere. The required analytical work could not be done in open atmosphere due to active nature of the samples. Therefore modification and glove box (GB) adaptation was required. Although large in size yet difficult to adapt for GB, the instrument had to be modified to a large extent as only sample handling part of the instrument had to placed inside GB, leaving rest of the instrument available for later repair/maintenance work. Different options were considered for modification keeping in mind the isolation and negative pressure inside the GB and maintaining the integrity of the instrument. One of such option was finalized which involved shifting the optic tank etc. A no of isolation gadgets were designed and fabricated locally. This indigenization has saved some handsome amount of foreign exchange. (Author)

  17. Impurities determination on nuclear fuel element components for the IEA-R1 research reactor by analytical methods based on ED-XRF and ICP-OES

    International Nuclear Information System (INIS)

    Reis, Edson Luis Tocaia dos; Scapin, Marcos; Cotrim, Marycel Elena Barboza; Salvador, Vera Lucia; Pires, Maria Aparecida Faustino

    2009-01-01

    The production of nuclear fuel used in the research reactor at Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP) requires a series of chemical and metallurgical processes. The quality of the end product depends on the control over all the stages of the manufacturing process and over the quality of raw materials employed. In fact, spectrometric methods are increasingly used as quantitative analytical techniques applicable to uranium compounds because of simultaneous determination of several elements with minimum amounts of sample. However, the main obstacle of uranium compounds analysis by spectrometric techniques such as optical emission spectrometry with inductively coupled plasma (ICP-OES) is the complex emission spectrum of uranium. The ICP-OES is not appropriately capable of determining the major elements of interest without initial chemical separation of uranium. In this sense, the use of X-ray fluorescence spectrometry (XRF) has been considered for quantitative determination of main elements with the advantage of not being destructive and not requiring a prior preparation of samples for analysis. Due to the simplicity of this technique, its applicability includes research and quality control in universities, research institutions, petrochemical industries, metallurgy, mining, etc. In this work, some components considered impurities in nuclear fuel element samples used in the IEA-R1 research reactor of IPEN/CNEN-SP were chemically characterized by ICP-OES analysis after chromatography extraction separation by using TBP/XAD-14 system and compared to results obtained by energy dispersive X-ray fluorescence spectrometry (EDXRF) and wavelength dispersive X-ray fluorescence (WDXRF). (author)

  18. Multielemental determination of trace elements in radiopharmaceuticals produced at the radiopharmacy center using ICP-OES technique

    International Nuclear Information System (INIS)

    Tavares, Angelica T.; Martins, Patricia de A.; Fukumori, Neuza T.O.; Mengatti, Jair; Matsuda, Margareth M.N.

    2013-01-01

    The control of chemical impurities in radiopharmaceuticals is critical to their safety and efficacy. According to the U.S. Pharmacopeia (USP), the elemental impurities with potential toxicity must be quantified. A proposed revision of USP 35 introduces the technique of atomic emission spectrometry for the analysis of elements. The aim of this work was to study the concentration of chemicals elements in FDG-Fluor-18, IPEN-TEC Generator and MIBI-TEC using an ICP-OES technique. One analytical curve composed by 27 elements (Ag, A1, B, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, K, Li, Mg, Mn, Mo, Na, Ni, Pb, Pd, Se, Sr, Te, T1, Zn) was constructed in two analytical ranges. The analyses were carried out simultaneously in an ICP-OES Vista MPX (Agilent). Some parameters for analysis and method validation were evaluated. The cleaning and maintenance of equipment influenced the emission intensity of the elements. 1.2 power and 10s sample uptake resulted in a consumption of 1.6 mL of sample and Mg II/Mg I ratio relation equal to 9.40. Linearity, LOD and LOQ were determined. The analysis were performed using 1:40 dilution with purified water. The main elements studied in this work were A1, Cu and Zn. The % recovery was determined with final concentrations of 0.3, 0.5 and 0.8 μg mL -1 . The analyses were performed in triplicate with three different batches. The % recovery was between 96.65 and 117.61% and the values for precision (CV) were less than 5% indicating good accuracy of the method. (author)

  19. DETERMINAÇÃO SIMULTÂNEA DE METAIS E ENXOFRE POR ICP-OES EM RESÍDUOS DE DESTILAÇÃO DE PETRÓLEO

    Directory of Open Access Journals (Sweden)

    Gabriel T. Druzian

    Full Text Available A method for digestion of crude oil distillation residues (atmospheric residue, AR and vacuum residue, VR using microwave-induced combustion (MIC was developed for simultaneous determination of metals (Ba, Co, Fe, Mg, Mn, Ni and V and sulfur by inductively coupled plasma optical emission spectrometry (ICP-OES. Samples were wrapped in polyethylene films and combusted using 20 bar of oxygen. Nitric acid solutions were evaluated using 5 min of reflux after combustion. Accuracy was evaluated using certified reference material and comparison with the results obtained by microwave-assisted wet digestion (MAWD. No statistical difference was observed between the certified values and those obtained using MIC as well as between the values obtained using MAWD or MIC. In spite of both methods have been apparently suitable for crude oil digestion, MIC was preferable in view of the possibility of using 3 mol L-1 HNO3 as absorbing solution. Furthermore, it is important to notice that using MIC, C content in digests was lower than 10 mg L-1, preventing interferences in ICP-OES. In addition, the simultaneous digestion of eight samples was possible in less than 30 min and without using concentrated acids and/or longer heating times, making the proposed method well-suited for routine analysis.

  20. On-line solid phase extraction using ion-pair microparticles combined with ICP-OES for the simultaneous preconcentration and determination of uranium and thorium

    Energy Technology Data Exchange (ETDEWEB)

    Yousefi, Seyed Reza; Zolfonoun, Ehsan [Nuclear Science and Technology Research Institute, Tehran (Iran, Islamic Republic of). NFCRS

    2016-07-01

    In this work, after on-line and in-situ solid phase extraction technique was used for the extraction and preconcentration of uranium and thorium from aqueous samples prior to inductively coupled plasma optical emission spectrometry (ICP-OES) determination. In this method, sodium hexafluorophosphate (as an ion-pairing agent) was added to the sample solution containing the cationic surfactant (dodecyltrimethylammonium bromide) and the complexing agent (dibenzoylmethane). A cloudy solution was formed as a result of formation of an ion pair between surfactant and hexafluorophosphate. The solid microparticles were passed through a microcolumn filter and the adsorbed microparticles were subsequently eluted with acid, which was directly introduced into the ICP-OES nebulizer. The main variables affecting the pre-concentration and determination steps of uranium and thorium were studied and optimized. Under the optimum conditions, the enhancement factors of 97 and 95 and the detection limits of 0.52 and 0.21 μg L{sup -1} were obtained for uranium and thorium, respectively.

  1. Multi-element determinations of N,N-dimethylformamide (DMF) coal slurries using ICP-OES

    Energy Technology Data Exchange (ETDEWEB)

    M. Mujuru; R.I. McCrindle; B.M. Botha; P.P. Ndibewu [Tshwane University of Technology, Pretoria (South Africa). Department of Chemistry

    2009-04-15

    A slurry nebulisation technique was applied for elemental analysis of bituminous coals SARM 18, SARM 19 and four coals from three different seams in Witbank, South Africa, by inductively coupled plasma optical emission spectroscopy (ICP-OES). Major elements (Al, Ca, Fe, Mg, S, Si and Ti) and trace elements (Ba, Cr, Mn, Ni, Sr, V, Zn and Zr) in coal were determined. Various slurry preparations were evaluated using two dispersants (glycerol and Triton X-100) and by varying the concentration of dispersants, between 0.1% and 1.0% (v/v). The effect of initially solubilising the ground coal in N,N-dimethylformamide (DMF) was investigated by varying the volume of DMF added. The effect of wet grinding with DMF was investigated. Wet grinding with DMF was shown to drastically reduce particle sizes (50.0% < 0.28 m and 90.0% < 6.17 {mu}m) as compared to dry grinding (50.0% < 5.25 {mu}m and 90.0% < 11.1 {mu}m). The reduced particle sizes and increased transport efficiency of the coal slurries led to improved analytical recoveries of elements in the reference coal, SARM 18. The best analytical recoveries for all elements were achieved using 0.1% Triton X-100 with 10.0% DMF. Results obtained by ICP-OES after wet grinding of the coal with DMF, using 0.1% Triton X-100, also gave excellent recoveries (Al, 100%; Ca, 103%; Cr, 106%; Fe, 102%; Mg, 100%; Mn, 104%; Ni, 109%; Si, 102%; Ti, 95.0%; and V, 108%). The results obtained with 10.0% DMF and 0.1% Triton X-100 were in agreement with certified values for all selected elements according to paired t-test at the 95.0% confidence level. Selected elements (Al, Ca, Fe, Mg, Mn, Si, Ti and V) were also analysed with X-ray fluorescence for comparison with results obtained from ICP-OES. Analysis by ICP-OES of microwave digested coal was also carried out. It is suggested that the DMF slurry technique could be used for routine analysis of bituminous coals. 27 refs., 4 figs., 4 tabs.

  2. An easy and fast procedure for the determination of Ca, Cu, Fe, Mn, Mg, Na, K and Si in biodiesel by ICP OES using emulsification as sample preparation strategy

    OpenAIRE

    Lisboa, Meibel T.; Clasen, Caroline D.; Vellar, Daiane C. de Sousa; Oreste, Eliézer Q.; Saint'Pierre, Tatiana D.; Ribeiro, Anderson S.; Vieira, Mariana A.

    2014-01-01

    It is presented an alternative procedure for preparation of biodiesel samples for elemental determination by inductively coupled plasma optical emission spectrometry (ICP OES), based on the sample (10% m/v) emulsion formation with formic acid (15% v/v) and Triton X-100 (0.1% m/v). These concentrations were optimized and the stability of emulsified aqueous standards and samples was found to be of at least 3 h. Experimental conditions (1500 W of RF power and 0.5 L min-1 of Ar nebulizer flow rat...

  3. Analysis of soil and sewage sludge by ICP-OES and the German standard DIN 38414 sample preparation technique (P3)

    International Nuclear Information System (INIS)

    Edlund, M.; Heitland, P.; Visser, H.

    2002-01-01

    Full text: The elemental analyses of soil and sewage sludge has developed to become one of the main applications for ICP optical emission spectrometry (ICP-OES) and is described in many official procedures. These methods include different acid mixtures and digestion techniques. Even though the German standard DIN 38414 part 7 and the Dutch NEN 6465 do not guarantee complete recoveries for all elements, they are widely accepted in Europe. This paper describes sample preparation, line selection and investigates precision, accuracy and Limits of detection. The SPECTRO CIROSCCD EOP with axial plasma observation and the SPECTRO CIROSCCD SOP with radial observation were compared and evaluated for the analyses of soil and sewage sludge. Accuracy was investigated using the certified reference materials CRM-141 R, CRM-143 R and GSD 11. Both instruments show excellent performance in terms of speed, precision, accuracy and detection limits for the determination of trace metals in soil and sewage sludge. (author)

  4. Determination of various elements in the Malva Sylvestris L. from Manisa region in Turkey by using ICP-OES

    International Nuclear Information System (INIS)

    Hicsoenmez, Ue.; Erees, F. S.; Cam, S.; Ozdemir, C.; Oezdemir, A.

    2006-01-01

    Various elements are transmitted into living metabolism through food intake. Although some of these elements are beneficial for living body, some of them may be toxic or radioactive. 4 0K, 2 38U, 2 35U or the radioactive daughters in the U and Th natural decay chains may be taken via consumption of these elements. In particular, since these radioactive elements have very long half-life and emit alpha particles, they may cause internal radiation risk. Manisa region located in the Western part of the Turkey has very productive agricultural soil. The Malva sylvestris L. is a herbaceous being consumed by human and animals in the region. In this work, Malva sylvestris samples were collected from different points in Muradiye areas of Manisa. Then, they were classified according to leaf size. These leaves were dissolved by wet digestion method using a mixture of mineral acid. Concentrations of Co, Na, Ca, Mg, Al, B, Ba, Cu, Mn, Ni, Zn, Cr, Cd, Ag, Sn, K, Ti, Fe, Sr, Sb, Si, Pb, Bi, U, La and Zr in prepared solutions and region soil were determined by using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), which is very sensitive and accurate detecting low level elements in sample, eg. in rocks, plants, animal tissue etc. Obtained values were compared with the internationally allowed values. The results of element were analyzed statistically. For different leaf sizes, concentration factors were calculated

  5. Quantification of Selected Trace and Mineral Elements in Royal Jelly from Bulgaria by Icp-Oes and Etaas

    Directory of Open Access Journals (Sweden)

    Balkanska Ralitsa

    2017-12-01

    Full Text Available The objective of the present study was to investigate selected trace and mineral elements in Royal Jelly (RJ from Bulgaria. A total of 30 RJ samples were included in the study. The analytical procedure consisted of the microwave digestion of the RJ samples with nitric acid followed by instrumental measurement. Concentrations of Al, Ba, Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P, Sr and Zn were determined using inductively coupled plasma optical emission spectroscopy (ICP-OES, while As, Cd, Co, Ni and Pb were determined by electrothermal atomic absorption spectrometry (ETAAS. Our results showed that elements K, Mg, Ca represented 96% from the total mineral content of the RJ samples from Bulgaria, while the most abundant trace element was Na, followed by Zn. The elements Ba, Cr, Cu, Fe, Mn and Sr were found in trace concentration levels and elements As, Pb, Cd, Co and Ni in microconcentration levels. Selected mineral and trace elements were found in relatively constant concentration levels in all of the analyzed RJ samples. It was concluded that chemical element content did not depend on geographical origin and was under homeostatic adjustment in RJs.

  6. Multielement trace analyses of SINQ materials by ICP-OES

    Energy Technology Data Exchange (ETDEWEB)

    Keil, R.; Schwikowski, M. [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-09-01

    Inductively Coupled Plasma Optical Emission Spectrometry was used to analyse 70 elements in various materials used for construction of the SINQ. Detection limits for individual elements depend strongly on the matrix and had to be determined separately. (author) 1 tab.

  7. Determinação seletiva de tributilestanho na presença de Sn(IV em amostras ambientais usando HG-ICP OES e Saccharomyces cerevisiae como material sorvente Selective determination of tributyltin in the presence of Sn(IV in environmental samples using HG-ICP OES and Saccharomyces cerevisiae as sorbing material

    Directory of Open Access Journals (Sweden)

    Monizze Vannuci e Silva

    2010-01-01

    Full Text Available A method for selective determination of tributyltin in the presence of Sn(IV by combining hydride generation inductively coupled plasma optical emission spectrometry (HG-ICP OES and solid phase extraction (SPE using baker's yeast is proposed. The procedure is based on selective retention of TBT by the yeast at pH = 6. Detection limit of 1.9 µg L-1 and quantification limit of 6.3 µg L-1 were obtained. TBT and San(IV were determined in the range of 0-25 µg L-1 and the proposed approach was applied to analyze river water, sea water and biological extracts, with recoveries of 114, 101 and 86%, respectively.

  8. DETERMINATION OF REFRACTORY ELEMENTS IN USED LUBRICATING OIL AND IN FUEL OIL BY ICP OES WITH EMULSIFIED SAMPLES

    OpenAIRE

    ROSELI MARTINS DE SOUZA

    2003-01-01

    O conhecimento da concentração dos elementos traço em óleo lubrificante usado é útil para a avaliação de desgastes de componentes específicos de motores.Em óleo combustível, este monitoramento permite avaliar a qualidade do combustível e prever o potencial das emissões de metais no meio ambiente. Neste trabalho, utilizou-se a espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES) para a determinação de elementos refratários em amostras de ól...

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

    Science.gov (United States)

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

    2014-01-01

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

  10. Comparison between INAA and ICP-OES: analysis of Sudanese medicinal plants

    International Nuclear Information System (INIS)

    Sheikhaldin, Elsadig Abdelmoniem

    2014-07-01

    The aim of this study was to provide elemental concentrations in medicinal plants and mainly to compare the two different determination methods (INAA and ICP-OES after wet digestion) elemental analysis of 14 Sudanese medicinal plants was carried out using INAA and ICP-OES techniques. The selection of reported elements was done according to intersection of elements determined by both techniques. This intersecting element list contained Ca, K, Fe, Mn, Mg, Sr, Zn, Cu, Co, and Cr. INAA correlated well with ICP-OES measurements of the same plants as long as concentrations were sufficiently above LoQ. Correlation coefficients (R 2 ) in this case is close to 1. Generally, INAA results tended to be higher compared to ICP-OES. The performance and possible source of errors of both techniques was discussed also with respect to measurements of certified reference materials. INAA provided the advantage of having both, faster and non destructive sample preparation than ICP-OES. Therefore, INAA may be technique of choice for Ca, K, Zn, and Mg elements specifically when samples are needed for further investigations. Regarding the low concentrations e.g for Cr, Ni or Cu, ICP-OES is the superior technique over INAA due to the sufficiently low limits of determination and thus gaining more detectable results at low concentrations. (author)

  11. Determination of 18 kinds of trace impurities in the vanadium battery grade vanadyl sulfate by ICP-OES

    Science.gov (United States)

    Yong, Cheng

    2018-03-01

    The method that direct determination of 18 kinds of trace impurities in the vanadium battery grade vanadyl sulfate by inductively coupled plasma atomic emission spectrometry (ICP-OES) was established, and the detection range includes 0.001% ∼ 0.100% of Fe, Cr, Ni, Cu, Mn, Mo, Pb, As, Co, P, Ti, Zn and 0.005% ∼ 0.100% of K, Na, Ca, Mg, Si, Al. That the influence of the matrix effects, spectral interferences and background continuum superposition in the high concentrations of vanadium ions and sulfate coexistence system had been studied, and then the following conclusions were obtained: the sulfate at this concentration had no effect on the determination, but the matrix effects or continuous background superposition which were generated by high concentration of vanadium ions had negative interference on the determination of potassium and sodium, and it produced a positive interference on the determination of the iron and other impurity elements, so that the impacts of high vanadium matrix were eliminated by the matrix matching and combining synchronous background correction measures. Through the spectral interference test, the paper classification summarized the spectral interferences of vanadium matrix and between the impurity elements, and the analytical lines, the background correction regions and working parameters of the spectrometer were all optimized. The technical performance index of the analysis method is that the background equivalent concentration -0.0003%(Na)~0.0004%(Cu), the detection limit of the element is 0.0001%∼ 0.0003%, RSD<10% when the element content is in the range from 0.001% to 0.007%, RSD< 20% even if the element content is in the range from 0.0001% to 0.001% that is beyond the scope of the method of detection, recoveries is 91.0% ∼ 110.0%.

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

    Science.gov (United States)

    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).

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

    International Nuclear Information System (INIS)

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

    2012-01-01

    Highlights: ► Simultaneous measurements of 23 elements in process gases of a waste wood combustor. ► Mobile ICP spectrometer allows measurements of high quality at industrial plants. ► Continuous online measurements with high temporal resolution. ► Linear correlations among element concentrations in the raw flue gas were detected. ► 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.

  14. Uranium and thorium determination in Santa Quiteria liquor by ICP-OES analysis

    International Nuclear Information System (INIS)

    Pedro Junior, A.; Rezende, Paulo R.; Carvalho, Leonel M.; Ferreira, Elizabeth de Massena

    2009-01-01

    The mineral source of Itataia located in Santa Quiteria (Ceara/Brazil) is a phosphorus uraniferous one, where uranium occurs in collophanite (fluoroapatite) form. Phosphate minerals of the apatite family make possible the uses of uranium as a byproduct. The sulfuric leaching of the phosphate rock in order to obtain phosphoric acid also permits uranium recovery. Thus, the liquor coming from the leaching contains high levels of phosphoric acid as well as elements like Mg, Fe, U, Zr, Th and some rare earths in significant concentrations. The direct determination of U and Th content of this liquor is essential to a rapid response in the uranium separation and purification together process by solvent extraction, aiming its use for commercial purposes, as nuclear industry fuel. In this study U and Th were determined by Inductively Coupled Plasma Spectrometry (ICP-OES) in several samples of liquor, in high concentrations of H 3 PO 4 in environment. Several ratios of U/Th and H 3 PO 4 concentrations were studied, in order to find the optimal conditions for the direct determination of U and Th, without need to prior separation. (author)

  15. LIBS coupled with ICP/OES for the spectral analysis of betel leaves

    Science.gov (United States)

    Rehan, I.; Rehan, K.; Sultana, S.; Khan, M. Z.; Muhammad, R.

    2018-05-01

    Laser-induced breakdown spectroscopy (LIBS) system was optimized and was applied for the elemental analysis and exposure of the heavy metals in betel leaves in air. Pulsed Nd:YAG (1064 nm) in conjunction with a suitable detector (LIBS 2000+, Ocean Optics, Inc) having the optical resolution of 0.06 nm was used to record the emission spectra from 200 to 720 nm. Elements like Al, Ba, Ca, Cr, Cu, P, Fe, K, Mg, Mn, Na, P, S, Sr, and Zn were found to be present in the samples. The abundances of observed elements were calculated through normalized calibration curve method, integrated intensity ratio method, and calibration free-LIBS approach. Quantitative analyses were accomplished under the assumption of local thermodynamic equilibrium (LTE) and optically thin plasma. LIBS findings were validated by comparing its results with the results obtained using a typical analytical technique of inductively coupled plasma-optical emission spectroscopy (ICP/OES). Limit of detection (LOD) of the LIBS system was also estimated for heavy metals.

  16. Characterization of bottom sediment of Adam bridge for its mineral content by spectrochemical and ICP-OES techniques

    International Nuclear Information System (INIS)

    Sharma, P.K.; Bassan, M.K.T.; Avhad, D.K.; Singhal, R.K.; UrsaI, G.R.

    2012-01-01

    Adam's Bridge also known as Rama's Bridge or Rama Setu is a chain of limestone shoals, between Rameswaram Island, off the southeastern coast of Tamil Nadu, India, and Mannar Island, off the northwestern coast of Sri Lanka. Geological evidence suggests that this bridge is a former land connection between India and Sri Lanka. During this work mineral content in the sand sample collected from four different locations were evaluated by using spectrochemical techniques such as FAAS (Flame atomic absorption spectroscopy), FES(Florescence Emission Spectroscopy), ICP-OES (Inductive coupled plasma optical emission spectroscopy) and UV - Visible Spectrophotometry. Various major elements like SiO 2 , Al 2 O 3 , Fe 2 O 3 , MgO, CaO , Na 2 O , K 2 O, minor elements like MnO, TiO 2 , P 2 O 5 and trace elements like Zr O2 ; V 2 O 5 , PbO and U etc. Validation of analytical methodology and reliability of analytical results were carried out by the analysis of the standard reference material. Trace elements were estimated after the selective removal of silica using AAS and ICP-OES technique. (author)

  17. Determination of Heavy Metals in Almonds and Mistletoe as a Parasite Growing on the Almond Tree Using ICP-OES or ICP-MS.

    Science.gov (United States)

    Kamar, Veysi; Dağalp, Rukiye; Taştekin, Mustafa

    2017-12-28

    In this study, the elements of Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Ni, Sr, Pb, Ti, and Zn were determined in the leaves, fruits, and branches of mistletoe, (Viscum albüm L.), used as a medicinal plant, and in the leaves, branches and barks of almond tree which mistletoe grows on. The aim of the study is to investigate whether the mistletoe are more absorbent than the almond tree in terms of the heavy metal contents and the determination of the amount of the elements penetrated into the mistletoe from the almond tree. ICP-MS (inductively coupled plasma-mass spectrometry) was used for the analysis of As, Cd, Mo, and Pb, whereas ICP-OES (inductively coupled plasma optical emission spectrometry) was used for the other elements. The results obtained were statistically evaluated at 95% confidence level. Within the results obtained in this study, it was determined whether there is a significant difference between metal elements in almond tree and mistletoe, or not. As a result, it was observed that there were higher contents of B, Ba, K, Mg, and Zn in the mistletoe than in the almond tree. K was found much higher than other elements in the mistletoe. On the other hand, Al, As, Ca, Cd, Cr, Cu, Fe, Mo, Ni, Sr, Pb, and Ti contents were determined to be more in almond tree than mistletoe.

  18. 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.

    Science.gov (United States)

    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

  19. ICP Mass and Optical Emission Spectrometry of Ore Samples Containing Rare Earth Elements

    International Nuclear Information System (INIS)

    Mohammed, A.E.W.M.

    2013-01-01

    Inductively Coupled Plasma Optical Emission and Mass Spectrometry (ICP-OES and ICPMS) are widely accepted as a rapid and sensitive techniques for Rare Earth Elements (REEs) analysis of geological samples. However, the achievable accuracy of these techniques are seriously limited by the problem of matrix interferences. In this study, matrix effects in ICP-AES were addressed using two approaches. In the first approach, the mechanisms of matrix interferences and analyte excitation were elucidated fundamentally. First, matrix effects from a comprehensive list of thirty-nine elements were investigated. It was confirmed that matrix elements with low second (instead of the widely reported first) ionization potentials (IP) produce a stronger matrix effect in all cases. Another critical parameter defining the severity of the matrix effect was found to be the availability of low-lying energy levels in the doubly charged matrix ion. Penning ionization followed by ion electron recombination through successive cycles is proposed as the mechanism for the more severe matrix effects caused by low second-IP matrices. In the second approach ICP-OES and ICP-MS are applied in this study for the analysis of Rare Earth Elements of two selected standard reference samples namely AGV-2 and BCR-2 beside a fluorspar geological sample (G-9 sample). Effective procedures are developed to avoid the spectral interference from matrix elements by using ion exchange resin Amberlite IR-120 before determination of REEs using ICP-OES and ICPMS. The potential of the method is evaluated by analysis of Certified Reference Materials (AGV-2 and BCR-2). Results obtained by ICP-MS show that experimental data are in agreement with the certified values and their values could be used as a quantitative data. The results obtained using ICP-OES were compared and discussed.

  20. Metal and trace element concentration evaluation in sediment profiles of the TietÊ River, State Of SÃO Paulo, by INAA and ICP OES techniques

    Energy Technology Data Exchange (ETDEWEB)

    Soares, Josiane S., E-mail: josi.s@usp.br [Instituto de Pesquisas Tecnológicas do Estado de São Paulo (LAQ- CQuiM/IPT), São Paulo, SP (Brazil). Lab. de Análises Químicas; Rocha, Flavio R.; Fávaro, Déborah I. T., E-mail: defavaro@ipen.br [Instituto de Pesquisas Energéticas e Nucleares (LAN/IPEN/CNEN-SP), São Paulo, SP (Brazil). Lab. de Análise por Ativação Neutrônica

    2017-07-01

    The present study presents concentration results for heavy metals, major and trace elements, in two sediment cores collected along the Tietê River: Salto de Itu to Porto Feliz ( Core 4 at point T-5) and Laras to Anhembi (Core 6 at point T18). As, Ba, Br, Co, Cr, Cs, Hf, Rb, Sb, Sc, Ta, Th, U and Zn concentrations by Instrumental Neutron Activation Analysis (INAA) and Al, Ba, Cd, Co, Cr, Cu, Mn, Ni, Pb, Ti, V and Zn concentrations by Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) were determined. The enrichment factor (EF), to assess the presence of anthropogenic pollution sources, was calculated and showed FE > 1.5 values for As, Br, Cs, Hf, Rb, Ta, Th, U and Zn, confirming the anthropogenic contribution for these elements, in all fractions from both cores. As, Cd, Cr, Cu, Ni, Pb and Zn concentrations were compared to guideline values (TEL and PEL) from the Canadian Council of Ministers of the Environment (CCME) and adopted by the São Paulo State Environmental Company (CETESB) and concentration values between TEL and PEL were found, for all fractions from both cores, presenting good and or regular sediment quality classification, the worst being Core 6. (author)

  1. Metal and trace element concentration evaluation in sediment profiles of the TietÊ River, State Of SÃO Paulo, by INAA and ICP OES techniques

    International Nuclear Information System (INIS)

    Soares, Josiane S.; Rocha, Flavio R.; Fávaro, Déborah I. T.

    2017-01-01

    The present study presents concentration results for heavy metals, major and trace elements, in two sediment cores collected along the Tietê River: Salto de Itu to Porto Feliz ( Core 4 at point T-5) and Laras to Anhembi (Core 6 at point T18). As, Ba, Br, Co, Cr, Cs, Hf, Rb, Sb, Sc, Ta, Th, U and Zn concentrations by Instrumental Neutron Activation Analysis (INAA) and Al, Ba, Cd, Co, Cr, Cu, Mn, Ni, Pb, Ti, V and Zn concentrations by Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) were determined. The enrichment factor (EF), to assess the presence of anthropogenic pollution sources, was calculated and showed FE > 1.5 values for As, Br, Cs, Hf, Rb, Ta, Th, U and Zn, confirming the anthropogenic contribution for these elements, in all fractions from both cores. As, Cd, Cr, Cu, Ni, Pb and Zn concentrations were compared to guideline values (TEL and PEL) from the Canadian Council of Ministers of the Environment (CCME) and adopted by the São Paulo State Environmental Company (CETESB) and concentration values between TEL and PEL were found, for all fractions from both cores, presenting good and or regular sediment quality classification, the worst being Core 6. (author)

  2. Surfactant assisted chemical vapour generation of silver for AAS and ICP-OES: a mechanistic study

    Czech Academy of Sciences Publication Activity Database

    Matoušek, Tomáš; Sturgeon, R. E.

    2003-01-01

    Roč. 18, č. 5 (2003), s. 487-494 ISSN 0267-9477 Institutional research plan: CEZ:AV0Z4031919 Keywords : vapour generation * ICP-OES * silver Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.200, year: 2003

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

    Directory of Open Access Journals (Sweden)

    J. Dilip Kumar

    2007-01-01

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

  4. A simple, rapid and eco friendly method for determination of uranium in geological samples of low silicate matrix by ICP-OES

    International Nuclear Information System (INIS)

    Hanuman, V.V.; Chakrapani, G.; Singh, A.K.

    2013-01-01

    A simple, rapid, cost effective and eco friendly decomposition and dissolution method is developed for the determination of uranium (U 3 O 8 ) by Inductively Coupled Plasma - Optical Emission Spectrometer (ICP-OES) in low silicate geological samples. The salts of Sodium di-hydrogen phosphate monohydrate and Sodium pyrophosphate deca hydrate are used in the ratio of 1:1 (phosphate flux) for the decomposition of low silicate matrix geological samples. Samples are decomposed by fusion with the phosphate flux after ignition and the dissolution is carried out using distilled water. If the samples contain >10% silica, they have been treated with little amount of (HF+HNO 3 ) prior to fusion with phosphate flux. These samples, are analysed by ICP-OES directly without any separation from the matrix. The spectral interferences of major matrix elements (Al, Ti, Fe, Mn, etc present in the sample) on uranium are studied and it is observed that their interferences are negligible, as dilution is required to bring uranium concentration into calibration range of instrument. This is the first time, the phosphate flux is used for decomposition of low silicate geological samples for uranium determination by ICP-OES

  5. Multi-proxy Reconstructions of the Eastern Equatorial Pacific: Measuring Sr/Ca, Ba/Ca, and Li/Mg in Modern Corals Using ICP-OES

    Science.gov (United States)

    Cheung, A. H.; Cole, J. E.; Vetter, L.; Jimenez, G.; Thompson, D. M.; Tudhope, A. W.

    2017-12-01

    Sea surface temperature (SST) in the Eastern Equatorial Pacific (EEP) exhibits large variability on multiple timescales. These variations are often related to modes of climate variability that exert significant influence on global climate, such as the El Niño Southern Oscillation. However, the short length and sparsity of instrumental data in the EEP limits our ability to discern changes in this region. Geochemical signals in corals can help extend instrumental data further back in time. While δ18O and Sr/Ca are the most commonly analyzed geochemical tracers of SST in corals, they often have site-specific complications. Several alternatives (e.g., Li/Mg) have been proposed to overcome these challenges, but have yet to be applied to long climate records, in part due to the cost and time required to measure these elements. Here, we develop a new method that uses Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) to analyze Li/Mg, Sr/Ca, and Ba/Ca ratios in coral aragonite. We apply this method to two Porites spp. corals collected from the northern Galapagos archipelago (Wolf and Darwin Islands). We specifically assess the fidelity of Li/Mg and Sr/Ca to reconstruct SST, and Ba/Ca to reconstruct upwelling conditions. Our results confirm that both Li/Mg and Sr/Ca track SST. We show that despite analytical noise, downcore reconstructions of Li/Mg have the potential to provide additional information about SST that is not present in reconstructions generated from Sr/Ca alone. Skeletal Ba/Ca shows little relationship with upwelling, perhaps because of the distance of our sites from the center of upwelling in the southern Galapagos. These results demonstrate the potential for analyzing Sr, Li, Ba, Mg simultaneously in corals with a cost- and time- efficient method, which may be applied to coral paleoclimate sites worldwide.

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

    Science.gov (United States)

    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

  7. Determination of heavy metal content of processed fruit products from Tehran's market using ICP- OES: A risk assessment study.

    Science.gov (United States)

    Fathabad, Ayub Ebadi; Shariatifar, Nabi; Moazzen, Mojtaba; Nazmara, Shahrokh; Fakhri, Yadolah; Alimohammadi, Mahmood; Azari, Ali; Mousavi Khaneghah, Amin

    2018-05-01

    In this study, the levels of Cd, Hg, Sn, Al, Pb and As of 72 samples (36 samples for fruits juices and 36 samples for fruits canned) of three different brands including of Peach, Orange, Cherry, and Pineapple (18 samples of each fruits) marketed in Tehran, Iran (2015) were evaluated using Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) technique. Also, Probabilistic risk assessment (non-carcinogenic and carcinogenic risks) was estimated by models include target hazard quotient (THQ) and cancer risk (CR) in the Monte Carlo Simulation (MCS) model. However, all samples were contaminated with the heavy metals investigated, most of them not surpassed established standards. The range of concentration for Al, Sn, As, Cd, Hg, and Pb as average in fruit juices were reported as 340.62 (65.17-1039.2), 72.33 (49.76-119.4), 3.76 (1.137-18.36), 2.12 (0.89-3.44), 0.351 and 40.86 (27.87-66.1) μg/kg, respectively. The level of heavy metals measured in different kinds of fruit juices was ranked as Al > Sn > Pb > As > Cd > Hg, and for fruits canned this rank was Pb > Al > Sn > As > Cd > Hg. The range of concentration for Al, Sn, As, Cd, Hg, and Pb in fruits canned were reported as 361.23 (43.15-1121.2), 101.42 (71.45-141.61), 3.92 (1.279-19.50), 2.78 (1.09-5.56), 0.35 and 690.54 (470.56-910.14) μg/kg, respectively. The lead (Pb) concentration in 97.22% (35 out of 36 samples) of fruit juices samples surpassed Codex limit (0.05 mg/kg) and in all samples of FC was lower than the legal limit of Codex limit (1 mg/kg). All of the samples had Tin (Sn) lower than the legal limit of Codex (fruit juices 100 mg/kg and FC 250 mg/kg). The MCS indicated that the rank order of heavy metals in both adults and children based on THQ was Al > Sn > As > Pb > Cd > Hg. The THQ of Al and Sn in the FJ and FC, for both adults, and children, was considerably higher than 1 value. Also, CR of As in both adults and children

  8. Improved documentation of spectral lines for inductively coupled plasma emission spectrometry

    Science.gov (United States)

    Doidge, Peter S.

    2018-05-01

    An approach to improving the documentation of weak spectral lines falling near the prominent analytical lines used in inductively coupled plasma optical emission spectrometry (ICP-OES) is described. Measurements of ICP emission spectra in the regions around several hundred prominent lines, using concentrated solutions (up to 1% w/v) of some 70 elements, and comparison of the observed spectra with both recent published work and with the output of a computer program that allows calculation of transitions between the known energy levels, show that major improvements can be made in the coverage of spectral atlases for ICP-OES, with respect to "classical" line tables. It is argued that the atomic spectral data (wavelengths, energy levels) required for the reliable identification and documentation of a large majority of the weak interfering lines of the elements detectable by ICP-OES now exist, except for most of the observed lines of the lanthanide elements. In support of this argument, examples are provided from a detailed analysis of a spectral window centered on the prominent Pb II 220.353 nm line, and from a selected line-rich spectrum (W). Shortcomings in existing analyses are illustrated with reference to selected spectral interferences due to Zr. This approach has been used to expand the spectral-line library used in commercial ICP-ES instruments (Agilent 700-ES/5100-ES). The precision of wavelength measurements is evaluated in terms of the shot-noise limit, while the absolute accuracy of wavelength measurement is characterised through comparison with a small set of precise Ritz wavelengths for Sb I, and illustrated through the identification of Zr III lines; it is further shown that fractional-pixel absolute wavelength accuracies can be achieved. Finally, problems with the wavelengths and classifications of certain Au I lines are discussed.

  9. The synergistic effect in coal/biomass blend briquettes combustion on elements behavior in bottom ash using ICP-OES

    Energy Technology Data Exchange (ETDEWEB)

    Lazaroiu, G.; Frentiu, T.; Maescu, L.; Mihaltan, A.; Ponta, M.; Frentiu, M.; Cordos, E. [Universitatea Politehnica din Bucuresti, Bucharest (Romania)

    2009-05-15

    This paper focuses on the study of the synergistic effect in coal/biomass blend briquettes combustion on behavior of Al, As, Ba, Cd, Co. Cr, Cu, Fe, Ga, K, Mn, Mo, Ni, P, Pb, Si, V, W, Zn, Zr and characterization of raw materials and bottom ashes. The manufacturing of coal/biomass briquettes although not commonly used is an attractive approach, as briquettes combustion is more technologically advantageous than the fluidized bed combustion. In the same time this technology is a way to render valuable materials of low calorific power and results in diminishing polluting emission. Raw materials and briquettes from different blends of pitcoal/sawdust were subjected to combustion in a 55 kW-boiler. The total content of elements after digestion in the HNO{sub 3} - HF mixture and the content in water leachate at a solid/liquid ratio of 1:2 were determined both in raw materials and bottom ash by ICP-OES. The total content of elements was higher in pitcoal than in sawdust. The synergistic effect depends both on coal/biomass ratio in blend and element nature. The water leachable fraction of elements from ash decreased along with the increase of sawdust weight excepting macronutrients (K, P) and Si.

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

    CSIR Research Space (South Africa)

    Archer, M

    2003-12-01

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

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

    Science.gov (United States)

    Zhang, Gai; Tian, Min

    2015-04-01

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

  12. Direct rare earth determination by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Marin, Sergio; Cornejo, Silvia; Rojas, Jacqueline

    2003-01-01

    In the present work, the use of the inductively coupled plasma optical emission spectrometry (ICP-OES), for the sequential determination of Rare Earth elements in the metallurgical process samples is described. In the first place, the optimum parameters for the determination of the elements in study are established, like instrumental calibration, wavelengths spectral selection and interference of matrix. Next, the methodology for the digestion of solid samples (system of digestion with pressure) and the recovery of the interest elements are presented. Two material rocks as of reference Syenite SY3 are used. In order to assure the validity of the obtained data, the reference materials SY2 and SY3 were analyzed by means of two different techniques, ICP-OES and ICP-Mass, this last one was made by an international laboratory and a fusion with lithium metaborate was used with digestion method. Finally, the obtained results demonstrate that the reproducibility in the recovery of rare earth analyzed by both techniques is comparable, and that the methodology of digestion used for these elements is statistically valid (author)

  13. Major constituent quantitative determination in uranium alloys by coupled plasma atomic emission spectrometry and X ray fluorescence wavelength dispersive spectrometry

    International Nuclear Information System (INIS)

    Oliveira, Luis Claudio de; Silva, Adriana Mascarenhas Martins da; Gomide, Ricardo Goncalves; Silva, Ieda de Souza

    2013-01-01

    A wavelength-dispersive X-ray fluorescence (WD-XRF) spectrometric method for determination of major constituents elements (Zr, Nb, Mo) in Uranium/Zirconium/Niobium and Uranium/Molybdenum alloy samples were developed. The methods use samples taken in the form of chips that were dissolved in hot nitric acid and precipitate particles melted with lithium tetraborate and dissolved in hot nitric acid and finally analyzed as a solution. Studies on the determination by inductively coupled plasma optic emission spectrometry (ICP OES) using matched matrix in calibration curve were developed. The same samples solution were analyzed in both methods. The limits of detection (LOD), linearity of the calibrations curves, recovery study, accuracy and precision of the both techniques were carried out. The results were compared. (author)

  14. Major and trace elements assessment in sediment from Ituparanga reservoir, by activation analysis and ICP OES

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Sharlleny A., E-mail: sharllenya@cetesbnet.sp.gov.br [Companhia de Tecnologia de Saneamento Ambiental (CETESB), Sao Paulo, SP (Brazil). Lab. de Quimica Inorganica; Bevilacqua, Jose Eduardo [Companhia de Tecnologia de Saneamento Ambiental (CETESB), Sao Paulo, SP (Brazil). Diretoria de Tecnologia, Qualidade e Avaliacao Ambiental; Favaro, Deborah I.T., E-mail: defavaro@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Lab. de Analise por Ativacao Neutronica

    2011-07-01

    The Ituparanga reservoir was built to generate electric power by the LIGHT Company and started its operation in 1912. It is fed by the Una, Sorocamirim and Sorocabucu rivers. This reservoir supplies water to a population of 600.000. This water system is affected by irregular soil occupation and urban development which has caught CETESB's (Environmental Company of Sao Paulo State) attention. In this study four geo-referenced sampling points were used and bottom sediment samples were collected. The sediment samples were dried at 400 deg C, ground in an agate mortar, sieved (200 mesh) and again homogenized. The instrumental neutron activation analysis was applied to the sediment samples in order to determine some major elements (Fe, K and Na), trace (As, Ba, Br, Co, Cr, Cs, Hf, Rb, Sb, Sc, Ta, Tb, Th, U and Zn) and rare earth (Ce, Eu, La, Lu, Nd, Sm, Tb and Yb) elements. By using ICP OES metals determination for Cd, Cr, Cu, Pb and Ni was undertaken after digestion procedure according to the 3051 method from US EPA. The methodology validation for precision and accuracy was carried out by reference material analyses. For metals Cd, Cr, Cu, Pb and Ni the concentration values were compared to the oriented values from Environmental Canada (TEL and PEL). The Enrichment Factor (EF) was calculated for sediment contamination assessment. (author)

  15. Determination of Th and REE in columbite - tantalite samples by ICP-OES

    International Nuclear Information System (INIS)

    Hanuman, V.V.; Khorge, C.R.; Radhamai, R.; Nair, Sajitha; Srivastava, P.K.

    2007-01-01

    A simple method of decomposition and separation of Th and REE in columbite- tantalite is developed for determination by ICP- OES. The sample is decomposed with hydrofluoric and hydrochloric acid in presence of little sulphuric acid to avoid drying on water bath. Th and rare earths are separated as fluoride together with undecomposed sample. The residue is fused with a 1: 1 mixture of sodium di hydrogen orthophosphate and sodium pyrophosphate. The melt is dissolved in water for measurement. Nitric acid is found unsuitable due to loss in Ce in some of the samples. Matrix elements (more than 97.5) are removed in single step by both the treatments. The free cassiterite present in samples is not attacked during acid digestion. However, the same is easily decomposed in fusion. U (IV) is also precipitated along with Th and REE when hydrochloric acid is used. As expected uranium is lost when nitric acid is used. The results are compared with existing well-established procedure involving peroxide fusion for decomposition; hydroxide and fluoride precipitation separation. Both the methods yielded comparable result. The method is simple, comparatively rapid and suitable for routine application for determination of REE , Th and U(IV) content. The RSD of the method was found to be in the range of 1- 1.5% for various elements. (author)

  16. Major and trace elements assessment in sediment from Ituparanga reservoir, by activation analysis and ICP OES

    International Nuclear Information System (INIS)

    Silva, Sharlleny A.; Bevilacqua, Jose Eduardo; Favaro, Deborah I.T.

    2011-01-01

    The Ituparanga reservoir was built to generate electric power by the LIGHT Company and started its operation in 1912. It is fed by the Una, Sorocamirim and Sorocabucu rivers. This reservoir supplies water to a population of 600.000. This water system is affected by irregular soil occupation and urban development which has caught CETESB's (Environmental Company of Sao Paulo State) attention. In this study four geo-referenced sampling points were used and bottom sediment samples were collected. The sediment samples were dried at 400 deg C, ground in an agate mortar, sieved (200 mesh) and again homogenized. The instrumental neutron activation analysis was applied to the sediment samples in order to determine some major elements (Fe, K and Na), trace (As, Ba, Br, Co, Cr, Cs, Hf, Rb, Sb, Sc, Ta, Tb, Th, U and Zn) and rare earth (Ce, Eu, La, Lu, Nd, Sm, Tb and Yb) elements. By using ICP OES metals determination for Cd, Cr, Cu, Pb and Ni was undertaken after digestion procedure according to the 3051 method from US EPA. The methodology validation for precision and accuracy was carried out by reference material analyses. For metals Cd, Cr, Cu, Pb and Ni the concentration values were compared to the oriented values from Environmental Canada (TEL and PEL). The Enrichment Factor (EF) was calculated for sediment contamination assessment. (author)

  17. Characterization of arsenic-contaminated aquifer sediments from eastern Croatia by ion microbeam, PIXE and ICP-OES techniques

    International Nuclear Information System (INIS)

    Ujević Bošnjak, M.; Fazinić, S.; Duić, Ž.

    2013-01-01

    Highlights: •ICP-OES and PIXE used in the characterization of As-contaminated sediments. •Observed high correlations between the results obtained by those techniques. •Discrepancies observed for Mn, and for the highest As concentrations. •Microbeam analyses showed As association with sulphides and iron. -- Abstract: Groundwater arsenic contamination has been evidenced in eastern Croatia and hydrochemical results suggest that the occurrence of arsenic in the groundwater depends on the local geology, hydrogeology, and geochemical characteristics of the aquifer. In order to perform the sediment characterization and to investigate arsenic association with the other elements in the sediments, 10 samples from two boreholes (PVc-3 and Gundinci 1) in eastern Croatia were analyzed using two techniques: PIXE (without sample pre-treatment) and ICP-OES (after digestion), as well by ion microbeam analyses. The results of the PIXE and ICP-OES techniques showed quite good agreement; however, greater discrepancies were observed at the higher arsenic and manganese mass ratios. According to both techniques, higher As mass ratios were observed in the sediments from the PVc-3 core (up to 651 mg/kg and 491 mg/kg using PIXE and ICP-OES analyses respectively) than from the Gundinci 1 core (up to 60 mg/kg using both techniques). Although arsenic association with Fe is expected, no correlation was observed. The microbeam analyses demonstrated that arsenic is associated with sulphides and iron in the most As-contaminated sample from the PVc-3 core, while this relationship was not evident in the most As-contaminated sample from the Gundinci 1 borehole

  18. Characterization of arsenic-contaminated aquifer sediments from eastern Croatia by ion microbeam, PIXE and ICP-OES techniques

    Energy Technology Data Exchange (ETDEWEB)

    Ujević Bošnjak, M., E-mail: magdalena.ujevic@hzjz.hr [Croatian National Institute of Public Health, Rockefelerova 7, 10000 Zagreb (Croatia); Fazinić, S. [Institute Ruđer Bošković, Bijenička cesta, 10000 Zagreb (Croatia); Duić, Ž. [University of Zagreb, Faculty of Mining, Geology and Petroleum Engineering, Pierottijeva 6, Zagreb (Croatia)

    2013-10-01

    Highlights: •ICP-OES and PIXE used in the characterization of As-contaminated sediments. •Observed high correlations between the results obtained by those techniques. •Discrepancies observed for Mn, and for the highest As concentrations. •Microbeam analyses showed As association with sulphides and iron. -- Abstract: Groundwater arsenic contamination has been evidenced in eastern Croatia and hydrochemical results suggest that the occurrence of arsenic in the groundwater depends on the local geology, hydrogeology, and geochemical characteristics of the aquifer. In order to perform the sediment characterization and to investigate arsenic association with the other elements in the sediments, 10 samples from two boreholes (PVc-3 and Gundinci 1) in eastern Croatia were analyzed using two techniques: PIXE (without sample pre-treatment) and ICP-OES (after digestion), as well by ion microbeam analyses. The results of the PIXE and ICP-OES techniques showed quite good agreement; however, greater discrepancies were observed at the higher arsenic and manganese mass ratios. According to both techniques, higher As mass ratios were observed in the sediments from the PVc-3 core (up to 651 mg/kg and 491 mg/kg using PIXE and ICP-OES analyses respectively) than from the Gundinci 1 core (up to 60 mg/kg using both techniques). Although arsenic association with Fe is expected, no correlation was observed. The microbeam analyses demonstrated that arsenic is associated with sulphides and iron in the most As-contaminated sample from the PVc-3 core, while this relationship was not evident in the most As-contaminated sample from the Gundinci 1 borehole.

  19. Avaliação de ICP OES com configuração axial ou radial para determinação de iodo em sal de cozinha

    Directory of Open Access Journals (Sweden)

    Adriana A. Oliveira

    2012-01-01

    Full Text Available The performance of inductively-coupled plasma optical emission spectrometers with axial and radial views for determination of iodine in table salt was evaluated. Interference and memory effects in nitric acid and water-soluble tertiary amines (CFA-C media were studied. Based on a factorial experiment, one optimum instrument operational condition for axial configuration, and two optima conditions for radial configuration was established. The ICP OES with axial view was 5-fold more sensitive than the radial view. Both matrix matching and standard addition methods were used for iodine quantification and for most samples, both strategies of calibration led to similar results. Recoveries ranged from 104 to 114%.

  20. On-line preconcentration and determination of chromium in parenteral solutions by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Gil, R.A.; Cerutti, S.; Gasquez, J.A.; Olsina, R.A.; Martinez, L.D.

    2005-01-01

    A method for the preconcentration and speciation of chromium was developed. On-line preconcentration and determination were obtained using inductively coupled plasma optical emission spectrometry (ICP-OES) coupled with flow injection. To determinate the chromium (III) present in parenteral solutions, chromium was retained on activated carbon at pH 5.0. On the other hand, a step of reduction was necessary in order to determine total chromium content. The Cr(VI) concentration was then determined by difference between the total chromium concentration and that of Cr(III). A sensitivity enrichment factor of 70-fold was obtained with respect to the chromium determination by ICP-OES without preconcentration. The detection limit for the preconcentration of 25 ml of sample was 29 ng l -1 . The precision for the 10 replicate determinations at the 5 μg l -1 Cr level was 2.3% relative standard deviation, calculated with the peak heights. The calibration graph using the preconcentration method for chromium species was linear with a correlation coefficient of 0.9995 at levels near the detection limits up to at least 60 μg l -1 . The method can be applied to the determination and speciation of chromium in parenteral solutions

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

    Directory of Open Access Journals (Sweden)

    Nikolaya Velitchkova

    2013-01-01

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

  2. 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.

    Science.gov (United States)

    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.

  3. Use of fractional factorial design for optimization of digestion procedures followed by multi-element determination of essential and non-essential elements in nuts using ICP-OES technique.

    Science.gov (United States)

    Momen, Awad A; Zachariadis, George A; Anthemidis, Aristidis N; Stratis, John A

    2007-01-15

    Two digestion procedures have been tested on nut samples for application in the determination of essential (Cr, Cu, Fe, Mg, Mn, Zn) and non-essential (Al, Ba, Cd, Pb) elements by inductively coupled plasma-optical emission spectrometry (ICP-OES). These included wet digestions with HNO(3)/H(2)SO(4) and HNO(3)/H(2)SO(4)/H(2)O(2). The later one is recommended for better analytes recoveries (relative errortime, pre-digestion time, temperature of the hot plate and sample weight) were used for optimization of sample digestion procedures. For this purpose Plackett-Burman fractional factorial design, which involve eight experiments was adopted. The factors HNO(3) and H(2)O(2) volume, and the digestion time were found to be the most important parameters. The instrumental conditions were also optimized (using peanut matrix rather than aqueous standard solutions) considering radio-frequency (rf) incident power, nebulizer argon gas flow rate and sample uptake flow rate. The analytical performance, such as limits of detection (LOD<0.74mugg(-1)), precision of the overall procedures (relative standard deviation between 2.0 and 8.2%) and accuracy (relative errors between 0.4 and 11%) were assessed statistically to evaluate the developed analytical procedures. The good agreement between measured and certified values for all analytes (relative error <11%) with respect to IAEA-331 (spinach leaves) and IAEA-359 (cabbage) indicates that the developed analytical method is well suited for further studies on the fate of major elements in nuts and possibly similar matrices.

  4. A single stage simultaneous separation and pre concentration of rare earth elements on activated carbon for its determination by ICP-OES after wet ashing - application to soil samples

    International Nuclear Information System (INIS)

    Chakrapani, G.; Mahanta, P.L.; Hanuman, V.V.; Srivastava, P.K.

    2007-01-01

    A simple, rapid, cost effective simultaneous separation and pre concentration method is developed for determination of Rare earth elements in soil samples at sub ppm levels by inductively coupled plasma-optical emission spectrometry (ICP-OES). The method is based on sorption of REEs on powered activated carbon (AC) in 2 - 3 M HF medium. The soil samples are decomposed by HF-HCl treatment followed by fusion of residue with Na 2 CO 3 . Keeping in view its application to soil samples, experimental parameters such as effect of HF, amount of AC, contact time, sample weight were optimized for quantitative sorption. The unique feature of the method is, REEs are desorbed quantitatively from activated carbon, by completely oxidizing and solubilizing AC by wet digestion (HNO 3 - HClO 4 treatment). Thus the time consuming and tedious method of ignition of charcoal to ashes is avoided, to increase the sample throughput in geochemical exploration studies. The precision of the method is ± 7 % at 1 ppm level. The accuracy of the method is evaluated by analyzing soil standard reference materials i.e. by using CANMET (Canada Center for Mineral and Energy Technology) standards, such as SO-2, SO-3 and SO-4. The composition of these soil standards closely match with the composition of soil samples under investigation. The method is being applied on numerous soil samples collected during geochemical exploration of uranium. The REEs in soil samples are determined down to ppm and sub ppm levels, based on separation of REEs from two gram soil sample, making up to final volume of 25 ml . The method could be adopted by any laboratory as the input involved is inexpensive activated carbon associated with minimal skill unlike the reported methods of ion exchange and solvent extraction. (author)

  5. Determination of lead content in drilling fueled soil using laser induced spectral analysis and its cross validation using ICP/OES method.

    Science.gov (United States)

    Rehan, I; Gondal, M A; Rehan, K

    2018-05-15

    A detection system based on Laser Induced Breakdown Spectroscopy (LIBS) was designed, optimized, and successfully employed for the estimation of lead (Pb) content in drilling fueled soil (DFS) collected from oil field drilling areas in Pakistan. The concentration of Pb was evaluated by the standard calibration curve method as well as by using an approach based on the integrated intensity of strongest emission of an element of interest. Remarkably, our investigation clearly demonstrated that the concentration of Pb in drilling fueled soil collected at the exact drilling site was greater than the safe permissible limits. Furthermore, the Pb concentration was observed to decline with increasing distance away from the specific drilling point. Analytical determinations were carried out under the assumptions that laser generated plasma was optically thin and in local thermodynamic equilibrium (LTE). In order to improve the sensitivity of our LIBS detection system, various parametric dependence studies were performed. To further validate the precision of our LIBS results, the concentration of Pb present in the acquired samples were also quantified via a standard analytical tool like inductively coupled plasma/optical emission spectroscopy (ICP/OES). Both results were in excellent agreement, implying remarkable reliability for the LIBS data. Furthermore, the Limit of detection (LOD) of our LIBS system for Pb was estimated to be 125.14 mg L -1 . Copyright © 2018 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Science.gov (United States)

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

    2015-07-23

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-23

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

  9. Rapid method of element determination in rye crispbread by ICP OES

    Directory of Open Access Journals (Sweden)

    Anna Szymczycha-Madeja

    2017-05-01

    Full Text Available In this work, various sample preparation procedures, i.e., microwave-assisted acid digestion in a mixture of HNO3 and H2O2 solutions, solubilisation in aqua regia or tetramethyl ammonium hydroxide and extraction in diluted HNO3 or in HCl, for the determination of the total content of Ba, Ca, Cd, Cr, Cu, Fe, Mg, Mn, Ni, P, Pb, Sr and Zn in rye crispbread using inductively coupled plasma optical emission spectrometry were compared. Analytical characteristic was evaluated by comparing the accuracy and precision of the results and limits of detection of elements. Among these five procedures solubilisation in aqua regia provides the best results, i.e., limits of detection of elements within 0.12–31.4 ng mL−1, precision of 0.4–5% and accuracy better than 5%. Additionally, a good agreement between the measured and certified values of the NIST 1567a was found for all elements. The proposed procedure is simple, reduces sample handling and minimises time and reagent consumption. Thus, it can be alternatively used instead of microwave-assisted acid digestion for routine analysis. Six different rye crispbreads were analysed with this procedure.

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

    Science.gov (United States)

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

    2015-07-23

    Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review, Electrothermal Vaporization and Laser Ablation will also be shortly described. The second issue is devoted to the analytical strategies for elemental quantification in such matrices, with particular insight into the isotope dilution technique, particularly used in speciation analysis by ICP-coupled separation techniques. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Determination of five kinds of impurity elements such as titanium in uranium titanium alloy by ICP-OES

    International Nuclear Information System (INIS)

    Jiao Yan; Hu Haihong

    2010-01-01

    New description is given of an ICP-OES method in which 5 impurities, Ti, Fe, Ni, Cu, and Al in U-Ti alloy can be determined simultaneously. Studying the dissolution of the sample preparation, separation condition of impurity elements; determining analysis of instrument line, detection limit and detection lower limit; eliminating the matrix effect of Ti and TiO 2 on the measurement of precipitation; standard addition method verify the method accuracy and precision. The results show: taking Uranium titanium alloys containing 0.1000 g sample, 5 kinds of elements Ti detection lower limits is 0.2-0.7 μg·g -1 , recovery were in the range of 98.8%-102.1%, and RSD'S found were less than 8%. The method of measurement proved is accurate and reliable. (authors)

  12. Dispersive liquid-liquid microextraction for simultaneous determination of cadmium, cobalt, lead and nickel in water samples by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Dos Santos Silva, E.; Correia, L.O.; Dos Santos, L.O.; Dos Santos Vieira, E.V.; Lemos, V.A.

    2012-01-01

    We report on a new method for the dispersive liquid-liquid microextraction of Cd(II), Co(II), Pb(II) and Ni (II) from water samples prior to their simultaneous determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on the injection of a ternary solvent system composed of appropriate quantities of extraction solvent (trichloroethylene), dispersive solvent (ethanol), and the chelating reagent 2-(2'-benzothiazolylazo)-p-cresol into the sample solution. The solution turns turbid immediately after injection, and the analytes are extracted into the droplets of the organic phase which was dried and dissolved in a mixture of Triton X-114, nitric acid, and ethanol. The metal ions in this mixture were quantified by ICP-OES. The detection limits under optimized conditions are 0.2, 0.3, 0.2 and 0.7 μg L -1 for Cd(II), Co(II), Pb(II) and Ni(II), respectively. The enrichment factors were also calculated for Cd (13), Co (11), Pb (11) and Ni (8). The procedure was applied to the determination of cadmium, cobalt, lead and nickel in certified reference material (waterway sediment) and water samples. (author)

  13. Comparative study of injection into a pneumatic nebuliser and tungsten coil electrothermal vaporisation for the determination of rare earth elements by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Dittrich, K.

    1988-01-01

    Injection into a pneumatic nebuliser and vaporisation using a tungsten coil electrothermal vaporisation system, with a 3-kW argon-nitrogen inductively coupled plasma (ICP), are compared for the determination of the rare earth elements. The sampling efficiency and thus also the absolute power of detection of the tungsten coil ICP optical emission spectrometric (ICP-OES) technique are better by two orders of magnitude, than the injection technique. The absolute detection limits for the rare earth elements are at the pg level; for the refractory rare earth elements (Er, La, Lu and Y), they are lower than those obtained by graphite furnace atomic absorption spectrometry, whereas for the other rare earth elements (Eu, Sc, Tm and Yb), the detection limits are comparable. With injection of samples into a pneumatic nebuliser and ICP-OES, matrix effects are low and absolute amounts of the order of mg of the rare earth matrix can be tolerated, giving relative detection limits down to 1 μg g -1 . The amount of rare earth matrix that can be tolerated with the tungsten-coil atomiser is two orders of magnitude lower. Thus the relatively detection limits of the two methods are of the same order, although the matrix effects are considerably higher with the tungsten coil. (author)

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

    International Nuclear Information System (INIS)

    Oliveira Souza, Sidnei de; Silvério Lopes da Costa, Silvânio; Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges

    2014-01-01

    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). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO 3 and H 2 O 2 ) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The ICP OES technique can be

  15. In-situ optical emission spectrometry during galvanostatic aluminum anodising

    International Nuclear Information System (INIS)

    Mercier, D.; Van Overmeere, Q.; Santoro, R.; Proost, J.

    2011-01-01

    In this study, we report on the use of optical emission spectrometry (OES) for the online detection of changes in the Al concentration ejected in a 1.0 mol dm -3 sulphuric acid electrolyte during galvanostatic anodising of Al thin film substrates. The technique relies on the coupling of an Inductively Coupled Plasma (ICP) spectrometer to a specially designed electrochemical flow cell. This has allowed to correlate, for the first time, the kinetics of Al dissolution to well-established morphological changes related to porous anodic oxide formation and growth. A deconvolution algorithm was first developed in order to decompose the experimental ICP/OES signal into elementary distributions, each one characteristic for a specific kinetic regime. The highest dissolution rate systematically occurred during the first step, associated with barrier oxide formation. This is followed by a systematic decrease in the rate of Al dissolution during pore formation. During steady-state porous oxide growth, the Al dissolution rate increases again, but still remains below the level established during barrier oxide growth. In each of these three kinetic regimes, a linear variation of the Al dissolution rate with current density was observed in the range 0.5-5.0 mA cm -2 , with slope values of, respectively, 35 ± 2, 24 ± 2 and 28 ± 1 μg C -1 . Regarding the temporal transitions between the different regimes, a desynchronisation was observed between the kinetic (dissolution) and morphological transitions, the time offset going in opposite directions for barrier and steady-state porous oxide growth. Finally, using the measured Al dissolution rates, the current density dependence of the film formation efficiency for both porous and barrier oxide growth has been established.

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

    Science.gov (United States)

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

    2014-05-21

    The present study has attempt to analyze the changes in the biochemical and mineral contents of aluminum intoxicated bone and determine the protective action of desferrioxamine (DFO) and deferiprone (DFP) by using Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), inductively coupled plasma optical emission spectroscopy (ICP-OES), and scanning electron microscopy (SEM) techniques for four groups of animals such as control (Group I), aluminum intoxicated (Group II), Al+DFP (Group III) and Al+DFO+DFP (Group IV) treated groups respectively. The FTIR spectra of the aluminum intoxicated bone showed significant alteration in the biochemical constituents. The bands ratio at I1400/I877 significantly decreased from control to aluminum, but enhanced it by Al+DFP to Al+DFO+DFP treated bone tissue for treatments of 16 weeks. This result suggests that DFO and DFP are the carbonate inhibitor, recovered from chronic growth of bone diseases and pathologies. The alteration of proteins profile indicated by Amide I and Amide II, where peak area values decreased from control to aluminum respectively, but enhanced by treated with DFP (p.o.) and DFO+DFP (i.p.) respectively. The XRD analysis showed a decrease in crystallinity due to aluminum toxicity. Further, the Ca, Mg, and P contents of the aluminum exposed bone were less than those of the control group, and enhanced by treatments with DFO and DFP. The concentrations of trace elements were found by ICP-OES. Therefore, present study suggests that due to aluminum toxicity severe loss of bone minerals, decrease in the biochemical constituents and changes in the surface morphology. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. 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

    International Nuclear Information System (INIS)

    Hola, Marketa; Otruba, Vitezslav; Kanicky, Viktor

    2006-01-01

    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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-05-15

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

  19. Determination of the impurities Al, Mn, Fe, Ni, Cu and Zn in nuclear grade uranium by ICP-OES

    Energy Technology Data Exchange (ETDEWEB)

    Kakazu, Mauricio H.; Cotrim, Marycel E.B.; Silva, Douglas B. da; Pires, Maria Aparecida F., E-mail: mhkakazu@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2011-07-01

    Uranium compounds are specially produced for use in nuclear reactors and must meet strict physical and chemicals specifications. The current study discusses the separation of Al, Mn, Fe, Ni, Cu and Zn from uranium compounds and their quantitative determination using inductively coupled plasma optical emission spectrometry. To avoid interference effect caused by uranium in the spectroscopic emission lines of elements of interest, the chromatographic behavior of TBP impregnated macroporous Amberlite XAD-4 column was investigated. The break through curves of uranium obtained showed maximum retention of up to 11 grams of uranium and the elution curves for the elements showed reproducible recovery rate of 90% on 50 mL elution. Synthetic samples of nuclear grade uranium prepared with the addition of 250 {mu}g/g of U of the above individual elements were used to verify the performance of the method. The method showed a recovery rate of 80 to 90% for the elements under study. (author)

  20. Determination of the impurities Al, Mn, Fe, Ni, Cu and Zn in nuclear grade uranium by ICP-OES

    International Nuclear Information System (INIS)

    Kakazu, Mauricio H.; Cotrim, Marycel E.B.; Silva, Douglas B. da; Pires, Maria Aparecida F.

    2011-01-01

    Uranium compounds are specially produced for use in nuclear reactors and must meet strict physical and chemicals specifications. The current study discusses the separation of Al, Mn, Fe, Ni, Cu and Zn from uranium compounds and their quantitative determination using inductively coupled plasma optical emission spectrometry. To avoid interference effect caused by uranium in the spectroscopic emission lines of elements of interest, the chromatographic behavior of TBP impregnated macroporous Amberlite XAD-4 column was investigated. The break through curves of uranium obtained showed maximum retention of up to 11 grams of uranium and the elution curves for the elements showed reproducible recovery rate of 90% on 50 mL elution. Synthetic samples of nuclear grade uranium prepared with the addition of 250 μg/g of U of the above individual elements were used to verify the performance of the method. The method showed a recovery rate of 80 to 90% for the elements under study. (author)

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-23

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

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

    Directory of Open Access Journals (Sweden)

    Sanda Rončević

    2012-01-01

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

  4. 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.

    Science.gov (United States)

    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%).

  5. IBA and ICP-OES determination of trace elements in indigenous medicinal herbs and their extracts on the infertility in the human male reproductive system

    Energy Technology Data Exchange (ETDEWEB)

    Mars, J.A.; Fisher, D.; Henkel, R. [Department of Medical Bioscience, Universily of the Weslern Cape, Bellville (South Africa); Weilz, F. [Department of Biodiversily and Conservation Biology, University of the Weslern Cape, Bellville (South Africa)

    2013-07-01

    Full text: The abnormality of infertility in humans is biologically defined (Mader, 2004; Wood, 1994; Ellison, 2001) as the inability of a species to reproduce its own kind after period of 12 month of unprotected sexual intercourse/copulation. It is however difficult when one wishes to quantify the occurrence of infertility, since it is seldom expressed explicitly, but mostly in conjunction with population growth dynamics which include socio-economic factors. Various plants (herbs) have been used as treatment for infertility. These plants however have not yet been scientifically analysed. In this paper we determined the major and trace element composition of Typha capensis (rhizome and leaves) Cissampe/os capensis (Ieaves) and Hermannia cilliata, which were sourced from the Cape Flats Nature Reserve, Bellville, Western Cape Province, South Africa. The trace element concentration determination are at time cumbersome, especially when destructive analytical methods such as ICP-OES are used. For our determination, the various samples were freeze-dried. Part of the freeze-dried sample was used for ICP-OES and the other for PIXE analysis. For PIXE the dried sample was pressed into a pellet, then coated with a layer of carbon and irradiated with a 3 MeV proton beam. We report on the trace element content of the various parts of the plant and comment on the applicability of the part in male infertility. (author)

  6. IBA and ICP-OES determination of trace elements in indigenous medicinal herbs and their extracts on the infertility in the human male reproductive system

    International Nuclear Information System (INIS)

    Mars, J.A.; Fisher, D.; Henkel, R.; Weilz, F.

    2013-01-01

    Full text: The abnormality of infertility in humans is biologically defined (Mader, 2004; Wood, 1994; Ellison, 2001) as the inability of a species to reproduce its own kind after period of 12 month of unprotected sexual intercourse/copulation. It is however difficult when one wishes to quantify the occurrence of infertility, since it is seldom expressed explicitly, but mostly in conjunction with population growth dynamics which include socio-economic factors. Various plants (herbs) have been used as treatment for infertility. These plants however have not yet been scientifically analysed. In this paper we determined the major and trace element composition of Typha capensis (rhizome and leaves) Cissampe/os capensis (Ieaves) and Hermannia cilliata, which were sourced from the Cape Flats Nature Reserve, Bellville, Western Cape Province, South Africa. The trace element concentration determination are at time cumbersome, especially when destructive analytical methods such as ICP-OES are used. For our determination, the various samples were freeze-dried. Part of the freeze-dried sample was used for ICP-OES and the other for PIXE analysis. For PIXE the dried sample was pressed into a pellet, then coated with a layer of carbon and irradiated with a 3 MeV proton beam. We report on the trace element content of the various parts of the plant and comment on the applicability of the part in male infertility. (author)

  7. Determination of Cr, Cu, Fe, Ni, Pb and Zn by ICP-OES in mushroom samples from Sakarya, Turkey

    Directory of Open Access Journals (Sweden)

    Esra Altıntığ

    2017-06-01

    Full Text Available Russula cyanoxantha, Russula delica, Lactarius salmonicolor, Lactarius deliciosus, Pleurotus eryngii, Pleurotus ostreatus, Agaricus bisporus, Suillus luteus, Pleurotus spp and Boletus edulis were collected from Sakarya-Turkey respectively. Also canned food in the form of the Pleurotus eryngii, Pleurotus ostreatus, and Lactarius salmonicolor mushrooms were used for the examination. Trace metal concentrations found in these mushrooms were determined inductively using coupled plasma optic emission spectrometry microwave processes. The results were obtained for (Cr 0.3-26.65, (Cu 17.38-132.75, (Fe 26.3-225.40, (Ni 2.57-39.28, (Pb 11.52-185.20, and (Zn 22.86-126.84 mg/kg. The accuracy of the method was checked by the standard reference material; tea leaves (INCY-TL-1 and tomato leaves (1573a.

  8. Development of Exact Matrix-Matching Inductively Coupled Plasma-Optical Emission Spectroscopy for the Analysis of Cu and K in Infant Formula

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Ye-Ji; Yim, Yong-Hyeon [University of Science and Technology, Daejeon (Korea, Republic of); Heo, Sung Woo; Han, Myung-Sub; Lim, Youngran [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

    2016-08-15

    In the present study, we have developed an exact matrix-matching inductively coupled plasma-optical emission spectroscopy (ICP-OES) as a low-cost alternative to the isotope dilution inductively coupled plasma mass spectrometry (ICP-MS) method for accurate and precise measurements of nutrient elements K and Cu in infant formula. In spite of its high precision and accuracy, ICP-OES analysis of complex samples was not reliable due to biases originating from various matrix effects. The elaborated exact matrix-matching approach tested here demonstrated its potential to minimize biases due to matrix mismatch. The exact matrix-matching ICP-OES method was successfully validated by comparing the results with those from an isotope dilution ICP-M S method. Because the model provides reliable results without significant loss of precision, it will be an excellent choice for major element analysis in a complex sample, especially when isotope dilution is not applicable due to the l ck of alternative isotopes or the high cost of enriched isotopes.

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

    International Nuclear Information System (INIS)

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

    2009-01-01

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-06-01

    An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg{sup −1} for Mn to 77.3 mg kg{sup −1} for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO{sub 3} and H{sub 2}O{sub 2}) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The

  11. Method development and validation for simultaneous determination of IEA-R1 reactor’s pool water uranium and silicon content by ICP OES

    Science.gov (United States)

    Ulrich, J. C.; Guilhen, S. N.; Cotrim, M. E. B.; Pires, M. A. F.

    2018-03-01

    IPEN’s research reactor, IEA-R1, an open pool type research reactor moderated and cooled by light water. High quality water is a key factor in preventing the corrosion of the spent fuel stored in the pool. Leaching of radionuclides from the corroded fuel cladding may be prevented by an efficient water treatment and purification system. However, as a safety management policy, IPEN has adopted a water chemistry control which periodically monitors the levels of uranium (U) and silicon (Si) in the pool’s reactor, since IEA-R1 employs U3Si2-Al dispersion fuel. An analytical method was developed and validated for the determination of uranium and silicon by ICP OES. This work describes the validation process, in a context of quality assurance, including the parameters selectivity, linearity, quantification limit, precision and recovery.

  12. Carbon-based magnetic nanocomposites in solid phase dispersion for the preconcentration some of lanthanides, followed by their quantitation via ICP-OES

    International Nuclear Information System (INIS)

    Tajabadi, F.; Sovizi, M.R.; Yamini, Y.

    2013-01-01

    We report on a method for the extraction of the lanthanide ions La(III), Sm(III), Nd(III) and Pr(III) using a carbon-ferrite magnetic nanocomposite as a new adsorbent, and their determination via flow injection ICP-OES. The lanthanide ions were converted into their complexes with 4-(2-pyridylazo)resorcinol, and these were adsorbed onto the nanocomposite. Fractional factorial design and central composite design were applied to optimize the extraction efficiencies to result in preconcentration factors in the range of 141-246. Linear calibration plots were obtained, the limits of detection (at S/N = 3) are between 0. 5 and 10 μg L -1 , and the intra-day precisions (n = 3) range from 3.1 to 12.8 %. The method was successfully applied to a certified reference material. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-10-15

    A novel nonchromatographic speciation technique for the speciation of mercury by sequential cloud point extraction (CPE) combined with inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. The method based on Hg{sup 2+} was complexed with I{sup -} to form HgI{sub 4}{sup 2-}, and the HgI{sub 4}{sup 2-} reacted with the methyl green (MG) cation to form hydrophobic ion-associated complex, and the ion-associated complex was then extracted into the surfactant-rich phase of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114), which are subsequently separated from methylmercury (MeHg{sup +}) in the initial solution by centrifugation. The surfactant-rich phase containing Hg(II) was diluted with 0.5 mol L{sup -1} HNO{sub 3} for ICP-OES determination. The supernatant is also subjected to the similar CPE procedure for the preconcentration of MeHg{sup +} by the addition of a chelating agent, ammonium pyrrolidine dithiocarbamate (APDC), in order to form water-insolvable complex with MeHg{sup +}. The MeHg{sup +} in the micelles was directly analyzed after disposal as describe above. Under the optimized conditions, the extraction efficiency was 93.5% for Hg(II) and 51.5% for MeHg{sup +} with the enrichment factor of 18.7 for Hg(II) and 10.3 for MeHg{sup +}, respectively. The limits of detection (LODs) were 56.3 ng L{sup -1} for Hg(II) and 94.6 ng L{sup -1} for MeHg{sup +} (as Hg) with the relative standard deviations (RSDs) of 3.6% for Hg(II) and 4.5% for MeHg{sup +} (C = 10 {mu}g L{sup -1}, n = 7), respectively. The developed technique was applied to the speciation of mercury in real seafood samples and the recoveries for spiked samples were found to be in the range of 93.2-108.7%. For validation, a certified reference material of DORM-2 (dogfish muscle) was analyzed and the determined values are in good agreement with the certified values.

  14. Determination of Pt, Pd and Rh in Brassica Napus using solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nischkauer, Winfried [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria); Herincs, Esther [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria); University of Natural Resources and Life Sciences, Department of Forest and Soil Sciences, Institute of Soil Research, Konrad Lorenz Straße 24, A-3430 Tulln (Austria); Puschenreiter, Markus; Wenzel, Walter [University of Natural Resources and Life Sciences, Department of Forest and Soil Sciences, Institute of Soil Research, Konrad Lorenz Straße 24, A-3430 Tulln (Austria); Limbeck, Andreas, E-mail: A.Limbeck@tuwien.ac.at [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria)

    2013-11-01

    Conventional approaches for the analysis of platinum group elements (PGEs) in plant material suffer from sample digestion which results in sample dilution and therefore requires high sample intakes to maintain the sensitivity. The presented solid-sampling method avoids sample digestion while improving sensitivity when compared to digestion-based inductively coupled plasma optical emission spectrometry (ICP-OES) methods and allows the analysis of sample masses of 5 mg or less. Detection limits of 0.38 μg g{sup −1}, 0.14 μg g{sup −1} and 0.13 μg g{sup −1} were obtained for Pt, Pd and Rh, respectively using a sample intake of 5 mg. The reproducibility of the procedure ranged between 4.7% (Pd) relative standard deviation (RSD, n = 7) and 7.1% (Rh) RSD for 25 ng analytes. For quantification, aqueous standards were applied on paper filter strips and dried. Only the dried filters were introduced into the electrothermal vaporization unit. This approach successfully removed memory-effects observed during analysis of platinum which occurred only if liquid standards came into contact with the graphite material of the furnace. The presented method for overcoming the Pt-memory-effects may be of further interest for the analysis of other carbide-forming analytes as it does not require any technical modification of the graphite furnace (e.g., metal inlays, pyrolytic coating). Owing to lack of suitable certified reference materials, the proposed method was compared with conventional ICP-OES analysis of digested samples and a good agreement was obtained. As a result of the low sample consumption, it was possible to determine the spatial distribution of PGEs within a single plant. Significant differences in PGE concentrations were observed between the shoots (stem, leaves) and the roots. Pd was mainly found in the roots, whereas Pt and Rh were also found in higher concentrations in the shoots. - Highlights: • The uptake of Pt, Pd and Rh by hydroponically grown plants was

  15. Determination of Pt, Pd and Rh in Brassica Napus using solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Nischkauer, Winfried; Herincs, Esther; Puschenreiter, Markus; Wenzel, Walter; Limbeck, Andreas

    2013-01-01

    Conventional approaches for the analysis of platinum group elements (PGEs) in plant material suffer from sample digestion which results in sample dilution and therefore requires high sample intakes to maintain the sensitivity. The presented solid-sampling method avoids sample digestion while improving sensitivity when compared to digestion-based inductively coupled plasma optical emission spectrometry (ICP-OES) methods and allows the analysis of sample masses of 5 mg or less. Detection limits of 0.38 μg g −1 , 0.14 μg g −1 and 0.13 μg g −1 were obtained for Pt, Pd and Rh, respectively using a sample intake of 5 mg. The reproducibility of the procedure ranged between 4.7% (Pd) relative standard deviation (RSD, n = 7) and 7.1% (Rh) RSD for 25 ng analytes. For quantification, aqueous standards were applied on paper filter strips and dried. Only the dried filters were introduced into the electrothermal vaporization unit. This approach successfully removed memory-effects observed during analysis of platinum which occurred only if liquid standards came into contact with the graphite material of the furnace. The presented method for overcoming the Pt-memory-effects may be of further interest for the analysis of other carbide-forming analytes as it does not require any technical modification of the graphite furnace (e.g., metal inlays, pyrolytic coating). Owing to lack of suitable certified reference materials, the proposed method was compared with conventional ICP-OES analysis of digested samples and a good agreement was obtained. As a result of the low sample consumption, it was possible to determine the spatial distribution of PGEs within a single plant. Significant differences in PGE concentrations were observed between the shoots (stem, leaves) and the roots. Pd was mainly found in the roots, whereas Pt and Rh were also found in higher concentrations in the shoots. - Highlights: • The uptake of Pt, Pd and Rh by hydroponically grown plants was investigated

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

    International Nuclear Information System (INIS)

    Li Yingjie; Hu Bin

    2007-01-01

    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 4 2- , and the HgI 4 2- reacted with the methyl green (MG) cation to form hydrophobic ion-associated complex, and the ion-associated complex was then extracted into the surfactant-rich phase of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114), which are subsequently separated from methylmercury (MeHg + ) 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. Determination of cadmium(II), cobalt(II), nickel(II), lead(II), zinc(II), and copper(II) in water samples using dual-cloud point extraction and inductively coupled plasma emission spectrometry

    International Nuclear Information System (INIS)

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

    2012-01-01

    Highlights: ► A dual-cloud point extraction (d-CPE) procedure was firstly developed for simultaneous pre-concentration and separation of trace metal ions combining with ICP-OES. ► The developed d-CPE can significantly eliminate the surfactant of Triton X-114 and successfully extend to the determination of water samples with good performance. ► The designed method is simple, high efficient, low cost, and in accordance with the green chemistry concept. - Abstract: A dual-cloud point extraction (d-CPE) procedure has been developed for simultaneous pre-concentration and separation of heavy metal ions (Cd 2+ , Co 2+ , Ni 2+ , Pb 2+ , Zn 2+ , and Cu 2+ ion) in water samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on forming complexes of metal ion with 8-hydroxyquinoline (8-HQ) into the as-formed Triton X-114 surfactant rich phase. Instead of direct injection or analysis, the surfactant rich phase containing the complexes was treated by nitric acid, and the detected ions were back extracted again into aqueous phase at the second cloud point extraction stage, and finally determined by ICP-OES. Under the optimum conditions (pH = 7.0, Triton X-114 = 0.05% (w/v), 8-HQ = 2.0 × 10 −4 mol L −1 , HNO 3 = 0.8 mol L −1 ), the detection limits for Cd 2+ , Co 2+ , Ni 2+ , Pb 2+ , Zn 2+ , and Cu 2+ ions were 0.01, 0.04, 0.01, 0.34, 0.05, and 0.04 μg L −1 , respectively. Relative standard deviation (RSD) values for 10 replicates at 100 μg L −1 were lower than 6.0%. The proposed method could be successfully applied to the determination of Cd 2+ , Co 2+ , Ni 2+ , Pb 2+ , Zn 2+ , and Cu 2+ ion in water samples.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-11-15

    Highlights: Black-Right-Pointing-Pointer A dual-cloud point extraction (d-CPE) procedure was firstly developed for simultaneous pre-concentration and separation of trace metal ions combining with ICP-OES. Black-Right-Pointing-Pointer The developed d-CPE can significantly eliminate the surfactant of Triton X-114 and successfully extend to the determination of water samples with good performance. Black-Right-Pointing-Pointer The designed method is simple, high efficient, low cost, and in accordance with the green chemistry concept. - Abstract: A dual-cloud point extraction (d-CPE) procedure has been developed for simultaneous pre-concentration and separation of heavy metal ions (Cd{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Pb{sup 2+}, Zn{sup 2+}, and Cu{sup 2+} ion) in water samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on forming complexes of metal ion with 8-hydroxyquinoline (8-HQ) into the as-formed Triton X-114 surfactant rich phase. Instead of direct injection or analysis, the surfactant rich phase containing the complexes was treated by nitric acid, and the detected ions were back extracted again into aqueous phase at the second cloud point extraction stage, and finally determined by ICP-OES. Under the optimum conditions (pH = 7.0, Triton X-114 = 0.05% (w/v), 8-HQ = 2.0 Multiplication-Sign 10{sup -4} mol L{sup -1}, HNO{sub 3} = 0.8 mol L{sup -1}), the detection limits for Cd{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Pb{sup 2+}, Zn{sup 2+}, and Cu{sup 2+} ions were 0.01, 0.04, 0.01, 0.34, 0.05, and 0.04 {mu}g L{sup -1}, respectively. Relative standard deviation (RSD) values for 10 replicates at 100 {mu}g L{sup -1} were lower than 6.0%. The proposed method could be successfully applied to the determination of Cd{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Pb{sup 2+}, Zn{sup 2+}, and Cu{sup 2+} ion in water samples.

  19. Preconcentration of heavy metals on activated carbon and their determination in fruits by inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Feist, Barbara; Mikula, Barbara

    2014-03-15

    A method of separation and preconcentration of cadmium, cobalt, copper, nickel, lead, and zinc at trace level using activated carbon is proposed. Activated carbon with the adsorbed trace metals was mineralised using a high-pressure microwave mineraliser. The heavy metals were determined after preconcentration by inductively coupled plasma optical emission spectrometry (ICP-OES). The influence of several parameters, such as pH, sorbent mass, shaking time was examined. Moreover, effects of inorganic matrix on recovery of the determined elements were studied. The experiment shows that foreign ions did not influence recovery of the determined elements. The detection limits (DL) of Cd, Co, Cu, Ni, Pb, and Zn were 0.17, 0.19, 1.60, 2.60, 0.92 and 1.50 μg L(-)(1), respectively. The recovery of the method for the determined elements was better than 95% with relative standard deviation from 1.3% to 3.7%. The preconcentration factor was 80. The proposed method was applied for determination of Cd, Co, Cu, Ni, Pb, and Zn in fruits materials. Accuracy of the proposed method was verified using certified reference material (NCS ZC85006 Tomato). Copyright © 2013 Elsevier Ltd. All rights reserved.

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

    International Nuclear Information System (INIS)

    Bezerra, Marcos A.; Santos, Walter N.L. dos; Lemos, Valfredo A.; Korn, Maria das Gracas A.; Ferreira, Sergio L.C.

    2007-01-01

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

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

    Science.gov (United States)

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

    2012-11-15

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

  2. Trends in preconcentration procedures for metal determination using atomic spectrometry techniques

    International Nuclear Information System (INIS)

    Godoi Pereira, M. de; Arruda, M.A.Z.

    2003-01-01

    Methods for metal preconcentration are often described in the literature. However, purposes are often different, depending on whether the methods are applied in environmental, clinical or technological fields. The respective method needs to be efficient, give high sensitivity, and ideally also is selective which is useful when used in combination with atomic spectroscopy. This review presents the actual tendencies in metal preconcentration using techniques such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), hydride generation atomic absorption spectrometry (HGAAS), inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS). Procedures based on related to electrochemical, coprecipitation/precipitation, liquid-liquid and solid-liquid extraction and atom trapping mechanisms are presented. (author)

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

    Science.gov (United States)

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

    2013-04-15

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

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

    Science.gov (United States)

    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. Copyright © 2012 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  6. Determination of Pb in river water samples by inductively coupled plasma optical emission spectrometry after ultrasound-assisted co-precipitation with manganese dioxide

    International Nuclear Information System (INIS)

    Sousa Bispo, Marcia; Santos da Boa Morte, Elane; Korn das Gracas Andrade, Maria; Sena Gomes Teixeira, Leonardo; Korn, Mauro; Costa, Antonio Celso Spinola

    2005-01-01

    A simple and efficient procedure for separation and pre-concentration using ultrasound-assisted co-precipitation with manganese dioxide was developed for Pb determination by inductively coupled plasma optical emission spectrometry (ICP OES). The optimization process was carried out using a two-level factorial design and a Doehlert matrix. Three variables (i.e. concentration of oxidizing solution-KMnO 4 , concentration of MnSO 4 solution and time of ultrasonic irradiation) were used as factors in the optimization. The recoveries, based on the analysis of spiked samples, were between 90% and 105%, and the precision was ≤ 5%. The detection limit and quantification limit for Pb determination were 3.2 and 10.7 μg L -1 , respectively. The proposed method was applied for the determination of Pb in water samples from a river heavily polluted by industrial effluents. The recovery measured by analyte addition technique showed that the proposed pre-concentration method had good accuracy

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

    Science.gov (United States)

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

    2017-12-01

    As a stable isotope, boron plays an important role in hydrogeology, environmental geochemistry, ore deposit geochemistry and marine paleoclimatology. However, there is no report of boron isotopic composition in gypsum. This is mainly confined to complete dissolution of Gypsum by water or acid. In this study, gypsum was converted to calcium carbonate (CaCO 3 ) with ammonium bicarbonate(NH 4 HCO 3 ) by two steps at 50°C. In every step, the mass ratio of NH 4 HCO 3 /CaSO 4 ·2H 2 O was twice, and conversion rate reached more than 98%. Converted CaCO 3 was totally dissolved with hydrochloric acid (the dissolution rate was over 99%). In order to overcome the difficulties of the matrix interference and the detection limit of Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES), we use Amberlite IRA 743 resin to purify and enrichment the boron at first, then eluting boron from the resin with 10mL 0.1mol/L hydrochloric acid at 75°C. The boron isotopic composition of natural gypsum samples was determined using positive thermal ionization mass spectrometry (P-TIMS). The boron isotopic composition of gypsum may be an excellent indicator for the formation environment. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

    Ilander, Aki; Vaeisaenen, Ari

    2007-01-01

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

    Science.gov (United States)

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

    2014-06-01

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

  10. Flame emission, atomic absorption and fluorescence spectrometry

    International Nuclear Information System (INIS)

    Horlick, G.

    1980-01-01

    Six hundred and thirty references are cited in this review. The information in the review is divided into 12 major areas: books, reviews, and bibliographies; fundamental studies in flames; developments in instrumentation; measurement techniques and procedure; flame emission spectrometry; flame atomic absorption spectrometry; flame molecular absorption spectrometry; electrothermal atomization atomic absorption spectroscopy; hydride generation techniques; graphite furnace atomic emission spectrometry; atomic fluorescence spectrometry; and analytical comparisons

  11. Liquid sample introduction in inductively coupled plasma atomic emission and mass spectrometry — Critical review

    Energy Technology Data Exchange (ETDEWEB)

    Bings, N.H., E-mail: bings@uni-mainz.de; 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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    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

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

    Directory of Open Access Journals (Sweden)

    Petrović Sanja M.

    2016-01-01

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

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

    International Nuclear Information System (INIS)

    Kiera, Arne F.; Schmidt-Lehr, Sebastian; Song, Ming; Bings, Nicolas H.; Broekaert, Jose A.C.

    2008-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-02-15

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

  16. Application of femtosecond laser ablation inductively coupled plasma mass spectrometry for quantitative analysis of thin Cu(In,Ga)Se{sub 2} solar cell films

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Seokhee [School of Mechatronics, Gwangju Institute of Science and Technology, 1 Oryong-dong, Buk-gu, Gwangju 500-712 (Korea, Republic of); Gonzalez, Jhanis J. [Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 94720 (United States); Applied Spectra Inc., 46665 Fremont Boulevard, Fremont, CA 94538 (United States); Yoo, Jong H. [Applied Spectra Inc., 46665 Fremont Boulevard, Fremont, CA 94538 (United States); Chirinos, Jose R. [Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 94720 (United States); Facultad de Ciencias, Universidad Central de Venezuela, Caracas 1041A (Venezuela, Bolivarian Republic of); Russo, Richard E. [Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 94720 (United States); Applied Spectra Inc., 46665 Fremont Boulevard, Fremont, CA 94538 (United States); Jeong, Sungho, E-mail: shjeong@gist.ac.kr [School of Mechatronics, Gwangju Institute of Science and Technology, 1 Oryong-dong, Buk-gu, Gwangju 500-712 (Korea, Republic of)

    2015-02-27

    This work reports that the composition of Cu(In,Ga)Se{sub 2} (CIGS) thin solar cell films can be quantitatively predicted with high accuracy and precision by femtosecond laser ablation-inductively coupled plasma-mass spectrometry (fs-LA-ICP-MS). It is demonstrated that the results are strongly influenced by sampling conditions during fs-laser beam (λ = 1030 nm, τ = 450 fs) scanning on the CIGS surface. The fs-LA-ICP-MS signals measured at optimal sampling conditions generally provide a straight line calibration with respect to the reference concentrations measured by inductively coupled plasma optical emission spectroscopy (ICP-OES). The concentration ratios predicted by fs-LA-ICP-MS showed high accuracy, to 95–97% of the values measured with ICP-OES, for Cu, In, Ga, and Se elements. - Highlights: • Laser ablation inductively coupled plasma mass spectrometry of thin film is reported. • Concentration ratio prediction with a confidence level of 95–97% is achieved. • Quantitative determination of composition is demonstrated.

  17. Construcción y caracterización de un nuevo nebulizador múltiple para técnicas analíticas basadas en plasma (ICP-OES, ICP-MS y MP-AES).

    OpenAIRE

    Lúñez Fernández, Claudia

    2016-01-01

    En la siguiente memoria, se presenta la metodología para la construcción de un nuevo nebulizador múltiple, resultado de una serie de nebulizadores anteriores, los cuales se han ido mejorando para optimizar las características del aerosol generado y con ello los parámetros analíticos de calidad en la espectrometría de emisión atómica con plasma de microondas (MP-AES) y espectrometría de emisión óptica con plasma de acoplamiento inductivo (ICP-OES). Este nuevo nebulizador multiconducto presenta...

  18. 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

    International Nuclear Information System (INIS)

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

    2015-01-01

    Highlights: • Proposed a novel explanation for plumbane generation. • Expounded the role of K 3 Fe(CN) 6 in plumbane generation. • Clarified the controversial aspects in the mechanism of K 3 Fe(CN) 6 enhancement. • Used X-ray diffractometry to analyze the intermediates. • Developed a method to analyze lead in milk using K 3 Fe(CN) 6 and K 4 Fe(CN) 6 as new additives. - Absract: To understand the formation of plumbane in the Pb II -NaBH 4 -K 3 Fe(CN) 6 system, the intermediate products produced in the reaction of lead(II) and NaBH 4 in the presence of K 3 Fe(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 NaBH 4 ; (2) the black Pb is oxidized by K 3 Fe(CN) 6 to form Pb 2 [Fe(CN) 6 ], which further reacts with NaBH 4 to form more plumbane and black Pb; and (3) another round starts in which the produced black Pb from the step 2 is then oxidized continuously by K 3 Fe(CN) 6 to form more Pb 2 [Fe(CN) 6 ] complex, which would produce more plumbane. In short, the black Pb and Pb 2 [Fe(CN) 6 ] complex are the key intermediate products for the formation of plumbane in the Pb II -NaBH 4 -K 3 Fe(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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-04-01

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

  20. Determination of ultratrace elements in natural waters by solid-phase extraction and atomic spectrometry methods.

    Science.gov (United States)

    Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Frache, Roberto

    2003-01-01

    A study was carried out on the preconcentration of ultratrace amounts of cadmium, lead, manganese, copper and iron from high-salinity aqueous samples and determination by atomic spectrometry methods. Sample volume, amount of resin, loading flow rate, and elution volume were optimized in order to obtain the simultaneous preconcentration of all the analytes. Quantitative recoveries were obtained by using 200 mg of iminodiacetic resin with a loading flow rate of 2 mL min(-1), elution volume of 3 mL and sample volume of 50-450 mL. Only copper in seawater samples was not completely retained by the resin (60-70% recovery), due to unfavorable competition of iminodiacetic-active groups with organically bound metal.To quantify the metals in the eluates, two atomic spectrometry techniques were compared: electrothermal atomization atomic absorption spectrometry (ETAAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) with simultaneous CCD detection system. Both techniques are suitable for sample analysis with detection limits of 1.0, 4.7, 3.3, 6.8, and 53 ng L(-1) using ETAAS and 12, 122, 3.4, 17, and 21 ng L(-1) using ICP-OES for Cd, Pb, Mn, Cu, and Fe, respectively. Relative standard deviations of the procedures ranged from 1.7 to 14% at the sub-microg L(-1) concentration level. The accuracy of both methods was verified by analyzing various certified reference materials (river water, estuarine water, coastal and off-shore seawater).

  1. Determination of ultratrace elements in natural waters by solid-phase extraction and atomic spectrometry methods

    Energy Technology Data Exchange (ETDEWEB)

    Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Frache, Roberto [Department of Chemistry and Industrial Chemistry, University of Genoa, Via Dodecaneso, 31-16146, Genoa (Italy)

    2003-01-01

    A study was carried out on the preconcentration of ultratrace amounts of cadmium, lead, manganese, copper and iron from high-salinity aqueous samples and determination by atomic spectrometry methods. Sample volume, amount of resin, loading flow rate, and elution volume were optimized in order to obtain the simultaneous preconcentration of all the analytes. Quantitative recoveries were obtained by using 200 mg of iminodiacetic resin with a loading flow rate of 2 mL min{sup -1}, elution volume of 3 mL and sample volume of 50-450 mL. Only copper in seawater samples was not completely retained by the resin (60-70% recovery), due to unfavorable competition of iminodiacetic-active groups with organically bound metal.To quantify the metals in the eluates, two atomic spectrometry techniques were compared: electrothermal atomization atomic absorption spectrometry (ETAAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) with simultaneous CCD detection system. Both techniques are suitable for sample analysis with detection limits of 1.0, 4.7, 3.3, 6.8, and 53 ng L{sup -1} using ETAAS and 12, 122, 3.4, 17, and 21 ng L{sup -1} using ICP-OES for Cd, Pb, Mn, Cu, and Fe, respectively. Relative standard deviations of the procedures ranged from 1.7 to 14% at the sub-{mu}g L{sup -1} concentration level. The accuracy of both methods was verified by analyzing various certified reference materials (river water, estuarine water, coastal and off-shore seawater). (orig.)

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  3. Evaluation of conductive polymers as an adsorbent for eradication of As (III from aqueous solution using inductively coupled plasma optical emission spectroscopy (ICP-OES

    Directory of Open Access Journals (Sweden)

    Muhammad Imran Din

    2014-04-01

    Full Text Available 1024x768 The main focused of this research work is the preparation of conductive polymers like polypyrrole, polyaniline and polythiophene and their application as adsorbent materials for the removal of hyper toxic metal As (III from aqueous solution. The metal ions get attached on the π-electrons at the back bone of polymer that illustrate excellent affinity for metal ions. The adsorption of As (II ions was carried out on polythiophene due to its redox properties and the stronger interaction between sulfur atoms with arsenic atoms. To attain large surface area and for maximum interaction of As (III ions with polymers, the particle size of polymers was ranged in nano scale. As the surface area increases with decrease in particle size, the active sites for metal ions also increases. These polymers were characterized by FIIR spectroscopy and SEM analysis. Adsorption isothermal data was examined by two parameters (Langmuir, Freundlich, and Dubinin-Radushkevich and three parameters Redlich-Petrson, Sips and Toth models. Experimental results showed that based on standard deviation (SD and Chi square test (χ2 the experimental data was best explained by Freundlich and Toth isotherm. Thermodynamics parameters such as free energy change (ΔG0, enthalpy change (ΔH0 and entropy change (ΔS0 have been calculated respectively, which revealed the spontaneous, endothermic and feasible nature of adsorption process.   Normal 0 false false false EN-US X-NONE X-NONE

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

    Science.gov (United States)

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Lara, R.F. [Inst. de Investigaciones Mineras, Universidad Nacional de San Juan (Argentina); Wuilloud, R.G.; Salonia, J.A. [Dept. of Analytical Chemistry, National University of San Luis (Argentina); Olsina, R.A.; Martinez, L.D. [Dept. of Analytical Chemistry, National University of San Luis (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina)

    2001-12-01

    An on-line cadmium preconcentration and determination system implemented with inductively coupled plasma optical emission spectrometry (ICP-OES) associated to flow injection (FI) with ultrasonic nebulization system (USN) was studied. The cadmium was retained as the cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol, Cd-(5-Br-PADAP), complex, at pH 9.5. The cadmium complex was removed from the knotted reactor (KR) with 3.0 mol/L nitric acid. A total enhancement factor of 216 was obtained with respect to ICP-OES using pneumatic nebulization (12 for USN and 18 for KR) with a preconcentration time of 60 s. The value of the detection limit for the preconcentration of 5 mL of sample solution was 5 ng/L. The precision for 10 replicate determinations at the 5 {mu}g/L Cd level was 2.9% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for cadmium was linear with a correlation coefficient of 0.9998 at levels near the detection limits up to at least 1000 {mu}g/L. The method was successfully applied to the determination of cadmium in wine samples. (orig.)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-05-30

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

  7. Depth-profile analysis of thermoelectric layers on Si wafers by pulsed r.f. glow discharge time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Reinsberg, K.-G.; Schumacher, C.; Tempez, A.; Nielsch, K.; Broekaert, J.A.C.

    2012-01-01

    In this work the depth-profile analysis of thermoelectric layers deposited on Au and Cr covered Si wafers with the aid of pulsed radiofrequency glow discharge time-of-flight mass spectrometry (pulsed RF-GD-TOFMS also called plasma profiling TOFMS (PP-TOFMS™)) is described. For thermoelectric materials the depth resolutions obtained with both PP-TOFMS and secondary ion mass spectrometry (SIMS) are shown to be well comparable and in the order of the roughness of the corresponding layers (between 20 and 3700 nm). With both methods a direct solid analysis without any preparation steps is possible. In addition, the analysis of the samples with PP-TOFMS proved to be faster by a factor of 26 compared to SIMS, as sputtering rates were found to be 80 nm s −1 and 3 nm s −1 , respectively. For the analyzed samples the results of PP-TOFMS and SIMS show that a homogeneous deposition was obtained. Quantitative results for all samples could also be obtained directly by PP-TOFMS when the stoichiometry of one sample was determined beforehand for instance by inductively coupled plasma optical emission spectrometry (ICP-OES) and scanning electron microscopy energy dispersive X-ray fluorescence spectrometry (SEM-EDX). For Bi 2 Te 3 the standard deviation for the main component concentrations within one sample then is found to be between 1.1% and 1.9% and it is 3.6% from sample to sample. For Sb 2 Te 3 the values within one sample are from 1.7% to 4.2% and from sample to sample 5.3%, respectively. - Highlights: ► Depth resolution in sub micrometer size by glow discharge mass spectrometry. ► Bi and Sb telluride layers composition with GD-TOF-MS, ICP-OES and SEM-EDX agree. ► Homogeneities of layers measured with GD-TOF-MS and SIMS agree.

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

    Science.gov (United States)

    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

  9. Determination of barium in natural waters by ICP-OES technique. Part II: Assessment of human exposure to barium in bottled mineral and spring waters produced in Poland.

    Science.gov (United States)

    Garboś, Sławomir; Swiecicka, Dorota

    2013-01-01

    A method of the classification of natural mineral and spring waters and maximum admissible concentration (MAC) levels of metals present in such types of waters are regulated by Commission Directive 2003/40/EC, Directive 2009/54/EC of the European Parliament and of the Council and Ordinance of Minister of Health of 30 March 2011 on the natural mineral waters, spring waters and potable waters. MAC of barium in natural mineral and spring waters was set at 1.0 mg/l, while World Health Organization determined the Ba guideline value in water intended for human consumption at the level of 0.7 mg/l. The aims of the study were: the determination of barium in natural mineral and spring waters (carbonated, non-carbonated and medium-carbonated waters) produced and bottled on the area of Poland, and assessment of human exposure to this metal presents in the above-mentioned types of waters. The study concerning barium determinations in 23 types of bottled natural mineral waters and 15 types of bottled spring waters (bought in Polish retail outlets) was conducted in 2010. The analyses were performed by validated method of determination of barium in water based on inductively coupled plasma optical emission spectrometry, using modern internal quality control scheme. Concentrations of barium determined in natural mineral and spring waters were in the ranges from 0.0136 mg/l to 1.12 mg/l and from 0.0044 mg/l to 0.43 mg/l, respectively. Only in the single case of natural mineral water the concentration of barium (1.12 mg/l), exceeded above-mentioned MAC for this metal, which is obligatory in Poland and the European Union - 1.0 mg/l. The long-term monitoring of barium concentration in another natural mineral water (2006 - 2010), in which incidental exceeding MAC was observed in 2006, was conducted. All measured barium concentrations in this water were lower than 1.0 mg/l and therefore, it is possible to state that the proper method of mixing waters taken from six independent

  10. 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.

    Science.gov (United States)

    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

  11. Effect of organic matrices on the determination of the trace element chemistry (Mg, Sr, Mg/Ca, Sr/Ca) of aragonitic bivalve shells (Arctica islandica). Comparison of ICP-OES and LA-ICP-MS data

    International Nuclear Information System (INIS)

    Schoene, Bernd R.; Zhang, Zengjie; Jacob, Dorrit; Soldate, Analia; Gillikin, David P.; Tuetken, Thomas; Garbe-Shoenberg, Dieter; McConnaughey, Ted

    2010-01-01

    The element chemistry of biogenic carbonates can provide important data on past environments. However, the Sr/Ca and Mg/Ca ratios as well as the Mg and Sr concentrations of biological carbonates, especially aragonitic bivalves often depart from apparent thermodynamic equilibrium. When measured in situ by means of LA-ICP-MS, the Mg concentration is often substantially enriched (two- to threefold) near the organic-rich, annual growth lines. To test the hypothesis that some organic components exert a major influence on the skeletal metal content, the element chemistry of different shell components (insoluble organic matrix, IOM; dissolved CaCO 3 and soluble organics, SOM) of Arctica islandica was measured by means of ICP-OES and LA-ICP-MS. The ICP-OES data indicate that the IOM is strongly enriched in Mg (130 ppm) and depleted in Sr and Ca (10 ppm and 0.22 wt%, respectively) when compared to the whole biomineral (Mg: 68 to 99 ppm, Sr: 860 to 1,060 ppm, Ca: ∼35.72 wt%). Although the average relative abundance of the IOM barely exceeds 0.46 wt%, its chemical composition in combination with its heterogeneous distribution across the shell can significantly increase estimates of the Mg concentration if measured in situ by LA-ICP-MS. Depending on the distribution of the IOM, the Ca concentration may be significantly lower locally than the average Ca concentration of the whole shell (35.72 wt%). If this remains undetected, the Mg concentration of shell portions with higher than average IOM content is overestimated by LA-ICP-MS and, conversely, the Mg concentration is underestimated in shell portions with lower than average IOM content. Removal of the IOM prior to the chemical analysis by LA-ICP-MS or mathematical correction for the IOM-derived magnesium concentrations is therefore strongly advised. The different chemistry of the IOM may also exert a major control on the trace element to calcium ratios. Shell portions enriched in IOM will show up to 200 times higher Mg

  12. Deuterium measurement by emission spectrometry

    International Nuclear Information System (INIS)

    Niemann, E.G.; Heilig, K.; Dumke, I.

    1978-01-01

    The method makes it possible to determine the relative deuterium content of enriched water samples. For this, the relative intensities of the Hα and Dα lines are measured which are emitted by a high-frequency discharge in water vapour. Although the method is not as exact as mass spectrometry, it has the following advantages: - Easy sample preparation (no reduction necessary); - samples of highly different enrichment can be measured one after the other without the danger of memory effects; - much lower apparatus and cost expenditure. The necessary sample size is about the same in both methods. (orig.) [de

  13. Boletus edulis loaded with γ-Fe2O3 nanoparticles as a magnetic sorbent for preconcentration of Co(II) and Sn(II) prior to their determination by ICP-OES.

    Science.gov (United States)

    Ozdemir, Sadin; Serkan Yalcin, M; Kilinc, Ersin; Soylak, Mustafa

    2017-12-20

    The authors show that the fungus Boletus edulis loaded with γ-Fe 2 O 3 nanoparticles is a viable sorbent for magnetic solid phase extraction of trace levels of Co(II) and Sn(II). The surface structure of immobilized magnetized B. edulis was characterized by FT-IR, SEM and EDX. Experimental parameters were optimized. Following elution with 1 M HCl, the ions were quantified by ICP-OES. The limits of detection are 21 pg·mL -1 for Co(II), and 19 pg·mL -1 for Sn(II). The preconcentration factors are 100 for both ions. The sorption capacities of the sorbent are 35.8 mg·g -1 for Co(II) and 29.6 mg·g -1 for Sn(II). The method was applied to the analysis of certificated reference materials and gave ≥95% recoveries with low RSDs. It was also successfully applied to the quantification of Co(II) and Sn(II) in spiked environmental and food samples. Graphical abstract The fungus Boletus edulis loaded with γ-Fe 2 O 3 nanoparticles is a viable biosorbent for magnetic solid phase extraction (MSPE) of trace levels of Co(II) and Sn(II). The surface structure of immobilized magnetized B. edulis was characterized by FT-IR, SEM and EDX. Experimental parameters were optimized.

  14. Application of factorial designs and Doehlert matrix in optimization of experimental variables associated with the preconcentration and determination of vanadium and copper in seawater by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Ferreira, Sergio L.C.; Queiroz, Adriana S.; Fernandes, Marcelo S.; Santos, Hilda C. dos

    2002-01-01

    In the present paper a procedure for preconcentration and determination of vanadium and copper in seawater using inductively coupled plasma optical emission spectrometry (ICP OES) is proposed, which is based on solid-phase extraction of vanadium (IV), vanadium (V) and copper (II) ions as 1-(2-pyridylazo)-2-naphthol (PAN) complexes by active carbon. The optimization process was carried out using two-level full factorials and Doehlert matrix designs. Four variables (PAN mass, pH, active carbon mass and shaking time) were regarded as factors in the optimization. Results of the two-level full factorial design 2 4 with 16 runs for vanadium extraction, based on the variance analysis (ANOVA), demonstrated that the factors pH and active carbon mass, besides the interaction (pHxactive carbon mass), are statistically significant. For copper, the ANOVA revealed that the factors PAN mass, pH and active carbon mass and the interactions (PAN massxpH) and (pHxactive carbon mass) are statistically significant. Doehlert designs were applied in order to determine the optimum conditions for extraction. The procedure proposed allowed the determination of vanadium and copper with detection limits (3σ/S) of 73 and 94 ng l -1 , respectively. The precision, calculated as relative standard deviation (R.S.D.), was 1.22 and 1.37% for 12.50 μg l -1 of vanadium and copper, respectively. The preconcentration factor was 80. The recovery achieved for determination of vanadium and copper in the presence of several cations demonstrated that this procedure improved the selectivity required for seawater analysis. The procedure was applied to the determination of vanadium and copper in seawater samples collected in Salvador City, Brazil. Results showed good agreement with other data reported in the literature

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-05-01

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

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

    Directory of Open Access Journals (Sweden)

    Rahman Mohammed M

    2012-12-01

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

  17. Preliminary studies of laser-induced breakdown spectrometry for the determination of Ba, Cd, Cr and Pb in toys

    International Nuclear Information System (INIS)

    Godoi, Quienly; Santos, Dario; Nunes, Lidiane C.; Leme, Flavio O.; Rufini, Iolanda A.; Agnelli, Jose A.M.; Trevizan, Lilian C.; Krug, Francisco J.

    2009-01-01

    The performance of laser-induced breakdown spectrometry (LIBS) for the determination of Ba, Cd, Cr and Pb in toys has been evaluated by using a Nd:YAG laser operating at 1064 nm and an Echelle spectrometer with intensified charge-coupled device detector. Samples were purchased in different cities of Sao Paulo State market and analyzed directly without sample preparation. Laser-induced breakdown spectrometry experimental conditions (number of pulses, delay time, integration time gate and pulse energy) were optimized by using a Doehlert design. Laser-induced breakdown spectrometry signals correlated reasonably well with inductively coupled plasma optical emission spectrometry (ICP OES) concentrations after microwave-assisted acid digestion of selected samples. Thermal analysis was used for polymer identification and scanning electron microscopy to visualize differences in crater geometry of different polymers employed for toy fabrication. Results indicate that laser-induced breakdown spectrometry can be proposed as a rapid screening method for investigation of potentially toxic elements in toys. The unique application of laser-induced breakdown spectrometry for identification of contaminants in successive layers of ink and polymer is also demonstrated.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-01-01

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

  19. Passive neutralization of acid mine drainage using basic oxygen furnace slag as neutralization material: experimental and modelling

    CSIR Research Space (South Africa)

    Zvimba, JN

    2015-12-01

    Full Text Available emission 147 spectrometry (ICP-OES) (Varian: Vista Pro CCD Simultaneous ICP-OES). The pH, acidity, 148 alkalinity of the AMD were determined using a Mettler Toledo Auto-titrator following 149 filtration. Fe(II) was determined using standard permanganate...

  20. Gas chromatography/plasma spectrometry - an important analytical tool for elemental speciation studies

    International Nuclear Information System (INIS)

    Wuilloud, Jorgelina C.A.; Wuilloud, Rodolfo G.; Vonderheide, Anne P.; Caruso, Joseph A.

    2004-01-01

    In this review, a full discussion and update of the state-of-the-art of gas chromatography (GC) coupled to all known plasma spectrometers is presented. A brief introductive discussion of the advantages and disadvantages of GC-plasma interfaces, as well as types of plasmas and mass spectrometers, is given. The plasma-based techniques covered include inductively coupled plasma mass spectrometry (ICP-MS) microwave-induced plasma optical emission spectrometry (MIP-OES), and inductively coupled plasma optical emission spectrometry (ICP-OES). Also, different variants of plasma sources, such as low power plasmas and glow discharge (GD) sources, are described and compared with respect to their capabilities in elemental speciation. Recent advances and alternative mass analyzers (collision/reaction cell; time-of-flight; double-focusing sector field) are also mentioned. Different aspects of the GC-plasma coupling are discussed with particular attention to the applications of these hyphenated techniques to the analysis of elemental species. Additionally, classical and modern sample preparation methods, including extraction and/or preconcentration and derivatization reactions, are presented and evaluated

  1. New developments in glow discharge optical emission and mass spectrometry

    International Nuclear Information System (INIS)

    Hoffmann, Volker; Dorka, Roland; Wilken, Ludger; Wetzig, Klaus

    2000-01-01

    This paper describes new developments in flow discharge optical emission (GD-OES) and mass spectrometry (GD-MS) at IFW and presents corresponding new applications (analysis of microelectronic multi-layer system by radio frequency glow discharge optical emission spectrometry (RF-GD-OES) and analysis of pure iron by a new Grimm-type GD-MS source)

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

    Energy Technology Data Exchange (ETDEWEB)

    Bentlin, Fabrina R.S. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil); Pozebon, Dirce [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil)], E-mail: dircepoz@iq.ufrgs.br; Mello, Paola A.; Flores, Erico M.M. [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900 Santa Maria, RS (Brazil)

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO{sub 3}){sub 2} was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 {mu}g g{sup -1} of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

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

    International Nuclear Information System (INIS)

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

    2007-01-01

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO 3 ) 2 was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 μg g -1 of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

  4. Depth-profile analysis of thermoelectric layers on Si wafers by pulsed r.f. glow discharge time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Reinsberg, K.-G. [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Schumacher, C. [Institute for Applied Physics, University of Hamburg, Jungiusstrasse 11, D-20355 Hamburg (Germany); Tempez, A. [HORIBA Jobin Yvon, 16-18 rue du Canal, F-91160 Longjumeau (France); Nielsch, K. [Institute for Applied Physics, University of Hamburg, Jungiusstrasse 11, D-20355 Hamburg (Germany); Broekaert, J.A.C., E-mail: jose.broekaert@chemie.uni-hamburg.de [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)

    2012-10-15

    In this work the depth-profile analysis of thermoelectric layers deposited on Au and Cr covered Si wafers with the aid of pulsed radiofrequency glow discharge time-of-flight mass spectrometry (pulsed RF-GD-TOFMS also called plasma profiling TOFMS (PP-TOFMS Trade-Mark-Sign )) is described. For thermoelectric materials the depth resolutions obtained with both PP-TOFMS and secondary ion mass spectrometry (SIMS) are shown to be well comparable and in the order of the roughness of the corresponding layers (between 20 and 3700 nm). With both methods a direct solid analysis without any preparation steps is possible. In addition, the analysis of the samples with PP-TOFMS proved to be faster by a factor of 26 compared to SIMS, as sputtering rates were found to be 80 nm s{sup -1} and 3 nm s{sup -1}, respectively. For the analyzed samples the results of PP-TOFMS and SIMS show that a homogeneous deposition was obtained. Quantitative results for all samples could also be obtained directly by PP-TOFMS when the stoichiometry of one sample was determined beforehand for instance by inductively coupled plasma optical emission spectrometry (ICP-OES) and scanning electron microscopy energy dispersive X-ray fluorescence spectrometry (SEM-EDX). For Bi{sub 2}Te{sub 3} the standard deviation for the main component concentrations within one sample then is found to be between 1.1% and 1.9% and it is 3.6% from sample to sample. For Sb{sub 2}Te{sub 3} the values within one sample are from 1.7% to 4.2% and from sample to sample 5.3%, respectively. - Highlights: Black-Right-Pointing-Pointer Depth resolution in sub micrometer size by glow discharge mass spectrometry. Black-Right-Pointing-Pointer Bi and Sb telluride layers composition with GD-TOF-MS, ICP-OES and SEM-EDX agree. Black-Right-Pointing-Pointer Homogeneities of layers measured with GD-TOF-MS and SIMS agree.

  5. Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young

    2005-01-01

    A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties

  6. Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

    2005-03-15

    A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

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

    International Nuclear Information System (INIS)

    Amberger, Martin A.; Hoeltig, Michael; Broekaert, Jose A.C.

    2010-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-02-15

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

  9. Study of uranium in soil employing Inductively Coupled Plasma Optical Emission Spectrometry

    International Nuclear Information System (INIS)

    Srivastava, A.; Sharma, P.K.; Bassan, M.K.T.; Avhad, D.K.; Singhal, R.K.; Reddy, A.V.R.

    2015-01-01

    Soil samples were collected from different locations in Punjab and Jharkhand States of India. Their Uranium content was measured using ICP-OES with and without chemical separation. It was observed that 98 percent of the uranium could be adsorbed using chitosan based micro-extractant at pH 5. The concentration of uranium in the studied soil samples was found to be higher than its normal natural abundance. (author)

  10. speciation of heavy metals in street dust samples from sakarya

    African Journals Online (AJOL)

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    techniques [26], such as flame atomic absorption spectroscopy (FAAS) [27, 28], inductively coupled plasma-optical emission (ICP-OES) [29] and mass spectrometry ... Analytical validation was conducted through the analysis of certified ...

  11. Determination of inorganic beryllium species in the particulate matter of emissions and working areas

    Energy Technology Data Exchange (ETDEWEB)

    Profumo, A.; Spini, G.; Cucca, L.; Pesavento, M. [Dipartimento di Chimica Gen., Pavia (Italy)

    2002-07-01

    A sequential extraction procedure for separating and determining Be(0), soluble Be(II) inorganic compounds, BeO and beryllium silicates in samples, such as particulate matter of emissions and working areas, has been developed. The proposed procedure has been tested on synthetic samples prepared with the inorganic beryllium compounds, in the presence of atmospherical particulate matter sampled in a laboratory, previously checked for the absence of beryllium. The speciation was then repeated on a sample of fly ash deriving from a solid waste incinerator and on a reference material (Coal Fly ash SRM 1633a, by NIST), followed by an evaluation of matrix spiking and recovery analyses. Performing multiple analyses of the spiked samples assessed the repeatability of the procedure. Quantitative determinations have been made by inductively coupled plasma optical emission spectrometry (ICP-OES) and electrothermal atomic absorption spectrometry (ETAAS). The possible interferences of the most common ions have been investigated. The selective sequential extractions allow one to separate and to determine different inorganic beryllium species, to which a different toxicity and therefore, a different risk are related: it is the case for example of metallic beryllium and beryllium oxide.

  12. Chemical analysis of steel by optical emission spectrometry

    International Nuclear Information System (INIS)

    Hayakawa, M.O.; Kajita, T.; Jeszensky, G.

    1981-01-01

    The development of the chemical analysis for special steels by optical emission spectrometry direct reading method with computer, at the Siderurgica N.S. Aparecida S.A. is presented. Results are presented for the low alloy steels and high speed steel. Also, the contribution of this method to the special steel preparation is commented. (Author) [pt

  13. Determination of lithium and potassium in uranium oxide powders and pellets by Flame Atomic Emission Spectrometric method

    International Nuclear Information System (INIS)

    Jat, J.R.; Balaji Rao, Y.; Prasada Rao, G.; Prahlad, B.

    2012-01-01

    The present paper describes a method developed at Control Laboratory, NFC which includes prior separation of lithium and potassium from uranium matrix before their measurements. Solvent extraction, using Tri-n-Butyl Phosphate (TBP) in CCI 4 followed by Tri-n-Octyl Phosphine Oxide (TOPO) in CCI 4 , is employed for prior separation of Li and K. The resultant aqueous solution was analyzed by Flame-Atomic Emission Spectrometric (AES) method. Solvent extraction conditions are optimized for measurement of Li and K in the same aliquot. Experimental conditions such as instrument calibration, flame condition, fuel flow, sample flow rate through nebulizer, burner height etc. are also optimized. Under the optimal condition the detection limits achieved for lithium is 0.02 ppm and 0.2 ppm for potassium. A RSD of ± 3 % for Li at 0.05 ppm and ± 4% for K at 1 ppm level has been achieved in this method. The results of lithium in the sample are compared with the values obtained by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). Similarly, values of potassium are compared with Flame-Atomic Absorption Spectrometry (Flame-AAS) technique. The comparisons are in good agreement. The above method is simple, sensitive, reproducible and can be used for measurement of lithium and potassium in UO 2 powder and pellets on regular basis

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

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

    2007-01-01

    A robust microwave-assisted acid digestion procedure followed by inductively coupled plasma-mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM 2.5 ). High temperature (200 deg. 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

  16. Lithium determination in whole blood by flame atomic emission spectrometry

    International Nuclear Information System (INIS)

    Rahman, S.; Khalid, N.; Nasimullah; Iqbal, M.Z.

    2003-01-01

    A simple and rapid method for the determination of lithium in whole blood using Flame atomic emission spectrometry is described. No sample preparation was required apart from dilution with 0.02 N HNO/sub 3/. The reliability of the method was determined by analyzing Standard Reference Material (SRM) under identical experimental conditions and comparing the determined lithium concentration with the reported value. These were in good agreement with each other. The determined range of lithium in the whole blood of fifty-six healthy adult volunteers (28 males and 28 females) were 13.1 - 47.8 mg L-1. The determined average concentration of lithium in whole blood was compared with the reported values of other countries. The data was statistically analyzed with respect to sex and different age groups. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

    Smith, D.H. (ed.)

    1978-11-01

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

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

    International Nuclear Information System (INIS)

    Smith, D.H.

    1978-11-01

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

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

    Science.gov (United States)

    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)…

  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.

    Science.gov (United States)

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

    2017-01-01

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

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

    Science.gov (United States)

    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

  2. Mineral distribution in rice: Measurement by Microwave Plasma Atomic Emission Spectroscopy (MP-AES)

    International Nuclear Information System (INIS)

    Ramos, Nerissa C.; Ramos, R.G.A.; Quirit, L.L.; Arcilla, C.A.

    2015-01-01

    Microwave Plasma Atomic Emission Spectroscopy (MP-AES) is a new technology with comparable performance and sensitivity to Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). Both instrument use plasma as the energy source that produces atomic and ionic emission lines. However, MP-AES uses nitrogen as the plasma gas instead of argon which is an additional expense for ICP-OES. Thus, MP-AES is more economical. This study quantified six essential minerals (Se, Zn, Fe, Cu, Mn and K) in rice using MP-AES. Hot plate digestion was used for sample extraction and the detection limit for each instrument was compared with respect to the requirement for routine analysis in rice. Black, red and non-pigmented rice samples were polished in various intervals to determine the concentration loss of minerals. The polishing time corresponds to the structure of the rice grains such as outer bran layer (0 to 15), inner bran layer (15 to 30), outer endosperm layer (30 to 45), and middle endosperm layer (45 to 60). Results of MP-AES analysis showed that black rice had all essential materials (except K) in high concentration at the outer bran layer. The red and non-pigmented rice samples on the other hand, contained high levels of Se, Zn, Fe, and Mn in the whole bran portion. After 25 seconds, the mineral concentrations remained constant. The concentration of Cu however, gave consistent value in all polishing intervals, hence Cu might be located in the inner endosperm layer. Results also showed that K was uniformly distributed in all samples where 5% loss was consistently observed for every polishing interval. Therefore, the concentration of K was also affected by polishing time. Thus, the new MP-AES technology with comparable performance to ICP-OES is a promising tool for routine analysis in rice. (author)

  3. Determination of trace elements in soy milk using ICP atomic emission spectrometry

    International Nuclear Information System (INIS)

    Tanaka, Satoko; Chayama, Kenji

    2009-01-01

    The present study investigated the optimal method for the multi-element quantification of 9 elements in soy milk: calcium, copper, iron, potassium, magnesium, manganese, sodium, phosphorus, and zinc. Results obtained using ICP atomic emission spectrometry were compared with those obtained by atomic absorption spectrometry, which is the standard method. The same sample was measured using both ICP atomic emission spectrometry and atomic absorption spectrometry. The percentage of minerals recovered by ICP atomic emission spectrometry ranged from 99.3% to 102%, which was equivalent to that by atomic absorption spectrometry. Therefore, a good result with standard deviation was obtained. The mineral contents of 16 samples of commercially-available soy milk products were measured. The Cu content was significantly proportional to the amount of soybean solids (P < 0.001). Moreover, although relation-ships did not attain statistical significance, the consents of Fe, Zn, K, Mg and P were proportional to the amount of soybean solids, and were highest in soy milk, followed by prepared soy milk and so milk beverage. The Ca content of modified soy milk was significantly higher than that of soy milk and soy milk-based beverages (P < 0.001). Furthermore, the Na content in soy milk was significantly lower. (author)

  4. Determination of Trace Iron in Red Wine by Isotope Dilution Mass Spectrometry Using Multiple-Collector Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Zhou Tao; Wang Jun; Lu Hai; Zhou Yuanjing; Li Haifeng

    2009-01-01

    This paper introduces determination of trace iron in red wine certified reference material by isotope dilution mass spectrometry (IDMS) method using a multiplecollector inductively coupled plasma mass spectrometry, equipped with a hexapole collision cell. The measurement procedure of iron isotopic abundance ratios was deeply researched. Reduced polyatomic ion interferences to iron isotopes ion by collision reaction using Ar and H 2 gas, high precise isotopic abundance ratios were achieved. Two relative measurement methods (ICP-MS and ICP-OES) were used to analyze trace iron in red wine. The results are compared with IDMS results, which indicate that they are accordant. The uncertainty analyses include each uncertainty factor in whole experiment and the uncertainty of used certified reference material and it shows that the procedure blank is not neglectable to detect limit and precision of the method. The establishment of IDMS method for analysis of trace iron in red wine supports the certification of certified reference materials. (authors)

  5. The Determination of Composite Elements in Zircaloy-2 by X-Ray Fluorescence and Emission Spectrometry Method

    International Nuclear Information System (INIS)

    Dian Anggraini; Rosika Kriswarini; Yusuf N

    2007-01-01

    Analysis of composing elements in zircaloy-2 has been done by Emission Spectrometry method and X-Ray Fluorescence (XRF). The aim of the analysis is to verify conformity between composing elements in zircaloy-2 and the material certificate. Spectrometry Emission method has higher sensitivity in element determination of a material than that of XRF method, so can be estimated that emission spectrometry method has higher accuracy than that of XRF method. The result of qualitative analysis by Emission Spectrometry indicate that the composing elements in zircaloy-2 were Sn, Cr and Ni. However, the qualitative analysis result by XRF method indicated that the composing elements in zircaloy 2 were Sn, Cr, Ni and Fe. Fe element can not be analysed by Emission Spectrometry method because Emission Spectrometer did not equipped with Fe detector. The quantitative analysis result of the composing elements in the material with both methods showed that Sn, Cr and Ni concentration of zircaloy 2 existed in concentration ranges of the material certificate. Result of statistical test (F and t-test) of analysis result of both methods can be used for analyzing composing elements in zircaloy 2. Emission Spectrometry method was more sensitive and accurate for determining Cr and Ni element in zircaloy 2 than that of emission Spectrometry method but both methods had same accuracy. The precision of measurement of Sn, Cr and Ni element using XRF method was better than that of Emission spectrometry method. (author)

  6. Comparison of 15N analysis by optical emission spectrometry and mass spectrometry for clinical studies during total parenteral nutrition

    International Nuclear Information System (INIS)

    Ragon, A.; Reynier, J.P.; Guiraud, G.

    1985-01-01

    During total and stable parenteral nutrition, a branched chain amino acid enriched solution containing [ 15 N]leucine was infused into a patient to determine the fate of the nitrogen administered through this formulation. Measurements of 15 N isotopic enrichments were performed on the same biological samples (urinary urea, total plasma proteins and albumin) by optical emission spectrometry (OES) and mass spectrometry (MS) to determine if OES with its specific advantages (cost, handling maintenance) constituted even with low enrichments a useful alternative technique to MS considered as the reference method. The results show that OES constituted a very useful analytical technique to obtain reliable information in clinical metabolic studies when low 15 N enrichments must be determined. (Auth.)

  7. Pulsed, atmospheric pressure plasma source for emission spectrometry

    Science.gov (United States)

    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.

  8. Copper Determination in Gunshot Residue by Cyclic Voltammetric and Inductive Coupled Plasma-Optical Emission Spectroscopy

    Directory of Open Access Journals (Sweden)

    Mohd Hashim Nurul’Afiqah Hashimah

    2016-01-01

    Full Text Available Analysis of gunshot residue (GSR is a crucial evidences for a forensic analyst in the fastest way. GSR analysis insists a suitable method provides a relatively simple, rapid and precise information on the spot at the crime scene. Therefore, the analysis of Cu(II in GSR using cyclic voltammetry (CV on screen printed carbon electrode (SPCE is a better choice compared to previous alternative methods such as Inductive Coupled Plasma-Optical Emission Spectroscopy (ICP-OES those required a long time for analysis. SPCE is specially designed to handle with microvolumes of sample such as GSR sample. It gives advantages for identification of copper in GSR on-site preliminary test to prevent the sample loss on the process to be analyzed in the laboratory. SPCE was swabbed directly on the shooter’s arm immediately after firing and acetate buffer was dropped on SPCE before CV analysis. For ICP-OES analysis, cotton that had been soaked in 0.5 M nitric acid was swabbed on the shooter’s arm immediately after firing and kept in a tightly closed sampling tube. Gold coated SPCE that had been through nanoparticles modification exhibits excellent performance on voltammograms. The calibration was linear from 1 to 50 ppm of copper, the limit of detection for copper was 0.3 ppm and a relative standard deviation was 6.1 %. The method was successfully applied to the determination of copper in GSR. The Cu determination on SPCE was compared and validated by ICP-OES method with 94 % accuracy.

  9. Apparatus and method for transient thermal infrared emission spectrometry

    Science.gov (United States)

    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. 134Cs emission probabilities determination by gamma spectrometry

    Science.gov (United States)

    de Almeida, M. C. M.; Poledna, R.; Delgado, J. U.; Silva, R. L.; Araujo, M. T. F.; da Silva, C. J.

    2018-03-01

    The National Laboratory for Ionizing Radiation Metrology (LNMRI/IRD/CNEN) of Rio de Janeiro performed primary and secondary standardization of different radionuclides reaching satisfactory uncertainties. A solution of 134Cs radionuclide was purchased from commercial supplier to emission probabilities determination of some of its energies. 134Cs is a beta gamma emitter with 754 days of half-life. This radionuclide is used as standard in environmental, water and food control. It is also important to germanium detector calibration. The gamma emission probabilities (Pγ) were determined mainly for some energies of the 134Cs by efficiency curve method and the Pγ absolute uncertainties obtained were below 1% (k=1).

  11. 934 -IJBCS-Article-Dr Emmanuel A Oluyemi

    African Journals Online (AJOL)

    DR GATSING

    coupled plasma-optical emission spectrometer. (ICP-OES) was ... Table 2: Hair standard (NCS DC 73347) analysis with ICP-OES. Elements ..... electrons from the lipids in cell membranes. The HO. ... cereals, vegetable and milk (Goyer and.

  12. {sup 134}Cs emission probabilities determination by gamma spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, M.C.M. de, E-mail: candida@cnen.gov.br [Comissão Nacional de Energia Nuclear (DINOR/CNEN), Riode Janeiro, RJ (Brazil); Poledna, R.; Delgado, J.U.; Silva, R.L.; Araujo, M.T.; Silva, C.J. da [Instituto de Radioproteção e Dosimetria (LNMRI/IRD/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

    2017-07-01

    The National Laboratory for Ionizing Radiation Metrology (LNMRI/IRD/CNEN) of Rio de Janeiro performed primary and secondary standardization of different radionuclides reaching satisfactory uncertainties. A solution of {sup 134}Cs radionuclide was purchased from commercial supplier to emission probabilities determination of some of its energies. {sup 134}Cs is a beta gamma emitter with 754 days of half-life. This radionuclide is used as standard in environmental, water and food control. It is also important to germanium detector calibration.The gamma emission probabilities (Pγ) were determined mainly for some energies of the {sup 134}Cs by efficiency curve method and the Pγ absolute uncertainties obtained were below 1% (k=1). (author)

  13. Analysis of iron-base alloys by low-wattage glow discharge emission spectrometry

    International Nuclear Information System (INIS)

    Wagatsuma, K.; Hirokawa, K.

    1984-01-01

    Several iron-base alloys were investigated by low-wattage glow discharge emission spectrometry. The emission intensity principally depended on the sputtering parameters of constituent elements in the alloy. However, in the case of chromium, stable and firm oxides formed on the surface influencing the yield of ejected atoms. This paper discusses the relation between the sputtering parameters in Fe-Ni, Fe-Cr, and Fe-Co alloys and their relative emission intensities. Additionally, quantitative analysis was performed for some ternary iron-base alloys and commercial stainless steels with the calibration factors of binary alloy systems

  14. Analysis of zirconium alloys using inductively-coupled plasma emission spectrometry

    International Nuclear Information System (INIS)

    White, G.F.; Pickford, C.J.

    1982-06-01

    As part of an interlaboratory collaborative exercise, certain trace and minor elements have been determined in a proposed zircaloy reference material using inductively-coupled plasma emission spectrometry. A dissolution procedure involving hydrochloric and hydrofluoric acids was used for determination of Hf, Cr, Fe and Sn. Data have also been obtained for Ni, Cu and Mn. Use of a high resolution monochromator in a scanning mode was found necessary for measurement of the emission intensities in order to resolve the spectral lines of interest from the intense and complex emission from the zirconium matrix. (author)

  15. Determination of aluminium, scandium and rare earth elements by emission flame spectrometry

    International Nuclear Information System (INIS)

    Otruba, V.; Sommer, L.

    1989-01-01

    Emission spectrometry in nitrous oxide-acetylene flames in combination with a highly resolving double monochromator and sensitive detecting system enables simple, sensitive and selective determinations of aluminium, scandium and all rare earth elements with exception of cerium in complicated matrices. Calibration plots are linear for a large concentration interval (≤ 100 μgxml -1 ), detection limits are in ngxml -1 level and RSD does not exceed 3% on the optimal concentration level of the particular element. The determination of Al, Sc, Eu and Yb showed particular advantages as to methods using ICP-spectrometry. (orig.)

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

    Science.gov (United States)

    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

  17. Levels of Major and Minor Elements in Some Commercial Fruit ...

    African Journals Online (AJOL)

    Purpose: To evaluate the macro- and micro-nutrient elements of some commercially available fruit juices in Serbia. Methods: Inductively coupled plasma optical emission spectrometry (ICP-OES) technique was employed for determination of the major and minor elements in samples of two different types of fruit juices - clear ...

  18. Analytical chemistry of actinides

    International Nuclear Information System (INIS)

    Chollet, H.; Marty, P.

    2001-01-01

    Different characterization methods specifically applied to the actinides are presented in this review such as ICP/OES (inductively coupled plasma-optical emission spectrometry), ICP/MS (inductively coupled plasma spectroscopy-mass spectrometry), TIMS (thermal ionization-mass spectrometry) and GD/OES (flow discharge optical emission). Molecular absorption spectrometry and capillary electrophoresis are also available to complete the excellent range of analytical tools at our disposal. (authors)

  19. Direct isotope ratio measurement of uranium metal by emission spectrometry on a laser-produced plasma

    International Nuclear Information System (INIS)

    Pietsch, W.; Petit, A.; Briand, A.

    1995-01-01

    The method of Optical Emission Spectrometry on a Laser-Produced Plasma (OES/LPP) at reduced pressure has been studied for the determination of the uranium isotope ratio ( 235 U/ 238 U). Spectral profiles of the investigated transition U-II 424.437 nm show the possibility to obtain an isotopic spectral resolution in a laser-produced plasma under exactly defined experimental conditions. Spectroscopic data and results are presented. (author)

  20. Environmental samples analysis by Atomic Absorption Spectrophotometry and Inductively Coupled Plasma-Optical Emission Spectroscopy

    International Nuclear Information System (INIS)

    Popescu, I.V.; Iordan, M.; Stihi, C.; Bancuta, A.; Busuioc, G.; Dima, G.; Ciupina, V.; Belc, M.; Vlaicu, Gh.; Marian, R.

    2002-01-01

    Biological samples are interesting from many aspects of environmental monitoring. By analyzing tree leaves conclusions can be drown regarding the metal loading in the growth medium. So that, starting from assumption that the pollution factors from environmental medium can modify the normal concentration of elements, we decided to control the presence of toxic elements and the deviation from normal state of elements in leaves of different trees from areas situated at different distances of pollution source. The aim of this work is to determine the elemental composition of tree leaves using Atomic Absorption Spectrophotometry (AAS) method and Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) method. Using AAS spectrophotometer SHIMADZU we identified and determined the concentration of: Cd, Co, Cu, Zn, Mn, Cr, Fe, Se, Pb with an instrumental error less than 1% for most of the elements analyzed. The same samples were analyzed by ICP-OES spectrometer, BAIRD ICP2070-Sequential Plasma spectrometer. We identified and determined in leaves of different trees the concentration of Mg, Ca, and Sr with a precision less than 6%. (authors)

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

    International Nuclear Information System (INIS)

    Montaser, A.

    1993-01-01

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

  2. Study of mineral and essential trace elements in milk and dairy products by inductively coupled plasma atomic emission spectrometry and neutron activation analysis

    International Nuclear Information System (INIS)

    Kira, Carmen Silvia

    2002-01-01

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

  3. Experimental evidence of state-selective charge transfer in inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

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

    2004-01-01

    State-selective charge-transfer behavior was observed for Fe, Cr, Mn and Cu in inductively coupled plasma (ICP)-atomic emission spectrometry. Charge transfer from Ar + to Fe, Cr and Mn is state-selective because of inefficient collisional mixing of the quasiresonant charge-transfer energy levels with nearby levels. This low efficiency is the consequence of differences in electronic configuration of the core electrons. The reason for state-selective charge-transfer behavior to Cu is not clear, although a tentative explanation based on efficiency of intramultiplet and intermultiplet mixing for this special case is offered

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

    Institute of Scientific and Technical Information of China (English)

    LI Jianqiang; LU Yiqiang; JIANG Wei

    2005-01-01

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

  5. X-ray fluorescence analysis and optical emission spectrometry of an roman mirror from Tomis, Romania

    International Nuclear Information System (INIS)

    Belc, M.; Bogoi, M.; Ionescu, D.; Guita, D.; Caiteanu, S.; Caiteanu, D.

    2000-01-01

    The miscellaneous population of Roman Empire, their diverse cultural tradition, their ability to assimilate the roman civilization spirits, had determined a permanent reassessment superimposed upon the roman contribution. Analysis was undertaken using optical emission spectrometry and non-destructive X-ray fluorescence. X-ray fluorescence analysis is a well-established method and is often used in archaeometry and other work dealing with valuable objects pertaining to the history of art and civilization. Roman mirror analysed has been found not to be made of speculum (a high tin bronze). (authors)

  6. Simple, sensitive nitrogen analyzer based on pulsed miniplasma source emission spectrometry

    International Nuclear Information System (INIS)

    Jin Zhe; Duan Yixiang

    2003-01-01

    The development of pulsed miniplasma source emission spectrometry for trace nitrogen determination in inert gases is described in this article. The instrument consists of a pulsed miniplasma source generated by an in-house fabricated portable high-voltage supply, an optical beam collection system, an integrated small spectrometer with a charge-coupled-device detector, an interface card, and a notebook computer for controlling spectrometer parameters and signal processing. Trace nitrogen in the inert gases, such as helium and argon, was determined by monitoring the emission intensities from nitrogen molecules at 357 and 337 nm. The analytical performance was examined under various experimental conditions. The system has a detection limit of about 15 ppb (v/v) for nitrogen in helium with a relative standard deviation of 1.5%. The newly developed instrument offers a simple, low-cost, and sensitive method for continuously monitoring trace nitrogen in high-purity inert gases

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

    Science.gov (United States)

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

    2014-05-01

    High-resolution alpha-particle spectrometry was performed with an ion-implanted silicon detector in vacuum on a homogeneously electrodeposited (236)U source. The source was measured at different solid angles subtended by the detector, varying between 0.8% and 2.4% of 4π sr, to assess the influence of coincidental detection of alpha-particles and conversion electrons on the measured alpha-particle emission probabilities. Additional measurements were performed using a bending magnet to eliminate conversion electrons, the results of which coincide with normal measurements extrapolated to an infinitely small solid angle. The measured alpha emission probabilities for the three main peaks - 74.20 (5)%, 25.68 (5)% and 0.123 (5)%, respectively - are consistent with literature data, but their precision has been improved by at least one order of magnitude in this work. © 2013 Published by Elsevier Ltd.

  8. Cold excitation and determination of hydrogen sulfide by dielectric barrier discharge molecular emission spectrometry.

    Science.gov (United States)

    Wu, Zhongchen; Jiang, Jie; Li, Na

    2015-11-01

    A low-temperature microplasma generated in a dielectric barrier discharge (DBD) was used as a radiation source for the excitation of hydrogen sulfide and its determination by molecular emission spectrometry (MES). The excitation/emission chamber was enclosed to eliminate spectral interference from ambient air. The spectral emission lines of hydrogen sulfide were clearly discriminated from the background spectrum, and the emission line at 365.06 nm was selected for parameter optimization and quantitative analysis. The S(2-) ions in aqueous samples were reacted with acid to generate hydrogen sulfide and then determined. The experimental parameters affecting the determination of hydrogen sulfide and S(2-) were optimized. The limits of detection were 1.4 mg m(-3) for H2S and 11.2 mg L(-1) for S(2-). The repeatability of the method was satisfactory, as the RSD values were 2.3% for H2S and 1.8% for S(2-). The enclosed DBD-MES system was demonstrated to be a useful tool for the determination of hydrogen sulfide in gas samples and S(2-) in aqueous samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Qualitative and quantitative chemical investigation of orthopedic alloys by combining wet digestion, spectro analytical methods and direct solid analysis

    Energy Technology Data Exchange (ETDEWEB)

    Figueiredo, Caio M.; Castro, Jeyne P.; Sperança, Marco A.; Fialho, Lucimar L.; Nóbrega, Joaquim A.; Pereira-Filho, Edenir R., E-mail: erpf@ufscar.br [Universidade Federal de São Carlos (GAIA/UFSCar), SP (Brazil). Grupo de Análise Instrumental Aplicada

    2018-05-01

    In this study, two laser-based techniques, laser-induced breakdown spectroscopy (LIBS) and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) were used for analytical signal evaluation of Ti, Al, and V and investigation of possible harmful elements eventually present as minor elements in Ti alloys. Due to the lack of certified reference materials, samples were also analyzed by wavelength dispersive X-ray fluorescence (WDXRF) and inductively coupled plasma optical emission spectrometry (ICP OES) after microwave-assisted digestion. To maximize the efficiency of LIBS and LA-ICP-MS, operational conditions were adjusted aiming to find optimal analytical performance. LIBS showed several Ti emission lines and few signals for Al and V. LA-ICP-MS was able to detect all three major constituents. For quantitative analysis, the correlation of intensity signals from LIBS analysis with reference values obtained by ICP OES was not successful, showing that there are still difficulties for quantification using solid samples. Measurements using ICP OES showed that additionally to major constituents, only Fe was present in concentrations around 0.2%. Analysis by WDXRF confirmed the presence of Fe. Results using both methods, i.e., ICP OES and WDXRF, were in good agreement. (author)

  10. Spectroscopic analysis of high protein nigella seeds (Kalonji) using laser-induced breakdown spectroscopy and inductively coupled plasma/optical emission spectroscopy

    Science.gov (United States)

    Rehan, Imran; Khan, M. Zubair; Ali, Irfan; Rehan, Kamran; Sultana, Sabiha; Shah, Sher

    2018-03-01

    The spectroscopic analysis of high protein nigella seeds (also called Kalonji) was performed using pulsed nanosecond laser-induced breakdown spectroscopy (LIBS) at 532 nm. The emission spectrum of Kalonji recorded with an LIBS spectrometer exposed the presence of various elements like Al, B, Ba, Ca, Cr, K, P, Mg, Mn, Na, Ni, S, Si, Cu, Fe, Ti, Sn, Sr, and Zn. The plasma parameters (electron temperature and electron density) were estimated using Ca-I spectral lines and their behavior were studied against laser irradiance. The electron temperature and electron density was observed to show an increasing trend in the range of 5802-7849 K, and (1.2-3.9) × 1017 cm- 3, respectively, in the studied irradiance range of (1.2-12.6) × 109 W/cm2. Furthermore, the effect of varying laser energy on the integrated signal intensities was also studied. The quantitative analysis of the detected elements was performed via the calibration curves drawn for all the observed elements through typical samples made in the known concentration in the Kalonji matrix, and by setting the concentration of P as the calibration. The validity of our LIBS findings was verified via comparison of the results with the concentration of every element find in Kalonji using the standard analytical tool like ICP/OES. The results acquired using LIBS and ICP/OES were found in fine harmony. Moreover, limit of detection was measured for toxic metals only.

  11. Urinary nickel: measurement of exposure by inductively coupled plasma argon emission spectrometry.

    Science.gov (United States)

    Koizumi, Chisato; Usuda, Kan; Hayashi, Satsuki; Dote, Tomotaro; Kono, Koichi

    2004-09-01

    Nickel is a rare earth metal and is widely used in modern industry. Its overexposure in human beings can provoke significant effects including lung, cardiovascular and kidney diseases. As an index of occupational exposure, urine is widely used for the monitoring of nickel concentration because it is a minimally invasive method. Recent studies have used atomic absorption spectrometry to measure nickel concentration. In this study, we introduced novel inductively coupled plasma argon emission spectrometry (ICPAES) which enables us to measure multiple elements simultaneously with smaller volume and with lower detection limits compared to conventional atomic absorption emission spectrometry, and we established the new measuring method by determining the appropriate wavelengths for nickel concentration. Furthermore, using the established new measuring method, we investigated the correlation between a single oral administration of nickel and urine elimination in rats. As a result, different concentrations of nickel standard solutions were measured by ICPAES, and among five specific wavelengths of nickel, 221.647 and 231.604 nm were chosen because they had the highest inclines of both signal to background ratio and emission intensity in simple linear regression analysis. Next, by using healthy human urine samples that had not been exposed to nickel, 231.604 nm was determined to be the most appropriate wavelength because it did not present abnormal intensity due to obstacle wavelength. Male Wistar rats received an oral administration of nickel ranging from 0.025 to 250 mg/kg, which is equivalent to 0.0015 - 15% of LD50, and during the following 24 h, urine samples were collected and the nickel concentration was measured by ICPAES. With a single oral administration of nickel, there was an increase in urine nickel concentration in a dose-dependent manner and the appropriate equation was developed. Acute renal failure was not observed in this dosage of oral nickel

  12. Assessment of high precision, high accuracy Inductively Coupled Plasma-Optical Emission Spectroscopy to obtain concentration uncertainties less than 0.2% with variable matrix concentrations

    International Nuclear Information System (INIS)

    Rabb, Savelas A.; Olesik, John W.

    2008-01-01

    The ability to obtain high precision, high accuracy measurements in samples with complex matrices using High Performance Inductively Coupled Plasma-Optical Emission Spectroscopy (HP-ICP-OES) was investigated. The Common Analyte Internal Standard (CAIS) procedure was incorporated into the High Performance Inductively Coupled Plasma-Optical Emission Spectroscopy method to correct for matrix-induced changes in emission intensity ratios. Matrix matching and standard addition approaches to minimize matrix-induced errors when using High Performance Inductively Coupled Plasma-Optical Emission Spectroscopy were also assessed. The High Performance Inductively Coupled Plasma-Optical Emission Spectroscopy method was tested with synthetic solutions in a variety of matrices, alloy standard reference materials and geological reference materials

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

    Science.gov (United States)

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

    2016-01-01

    Acetone is a predominant volatile organic compound (VOC) in the exhaled breath and a promising biomarker for diabetes and ketoacidosis. A non-thermal micro-plasma generated in a planar dielectric barrier discharge (DBD) is used as a radiation source for the excitation of gaseous acetone followed by its quantification with optical emission spectrometry (OES). Gaseous acetone can be directly sampled, while liquid acetone is evaporated by heated tungsten coil and then introduced into the DBD micro-plasma by a helium carrier flow for performing optical emission and detection at a 519 nm emission line. In the present study, the exhaled breath is collected and transferred into aqueous medium for sampling. With a sampling volume of 7 μL in a micro-drop, a linear range of 40-1600 mg L(-1) is obtained along with a detection limit of 44 ng and a precision of 5.7% RSD. The present system is successfully applied to the determination of breath acetone for both diabetic patients and healthy volunteers. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Multielement determination of rare earth elements by liquid chromatography/inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Sawatari, Hideyuki; Asano, Takaaki; Hu, Xincheng; Saizuka, Tomoo; Itoh, Akihide; Hirose, Akio; Haraguchi, Hiroki

    1995-01-01

    The rapid determination of rare earth elements (REEs) has been investigated by an on-line system of high performance liquid chromatography/multichannel inductively coupled plasma atomic emission spectrometry. In the present system, all REEs could be detected simultaneously in a single chromatographic measurement without spectral interferences. Utilizing a cation exchange column and 2-hydroxy-2-methylpropanoic acid aqueous solution as the mobile phase, the detection limits of 0.4-30 ng ml -1 for all REEs were obtained. The system was applied to the determination of REEs in geological standard rock samples and rare earth impurities in high purity rare earth oxides. The REEs in standard rocks could be determined by the present HPLC/ICP-AES system without pretreatment after acid digestion, although the detection limits were not sufficient for the analysis of rare earth oxides. (author)

  15. Some metals determination in beers by atomic emission spectrometry of induced argon plasma

    International Nuclear Information System (INIS)

    Matsushige, I.

    1990-01-01

    It was made the identification and determination of metals in brazilian bottled and canned beer, using atomic emission spectrometry with d.c. are and argon coupled plasma excitation sources. The elements Co, Cr, Cu, Fe, Pb and Zn were determined in beer samples, after treatment with HNO sub(3) conc. /H sub(2) O sub(2) (30%). In the determination of Co, Cr, Cu, Pb and Zn and alternative method using HNO sub(3) conc. /O sub(3) was proved be useful. The results obtained for Co, Cr, Cu, Fe, Pb and Zn were below the limits established by brazilian legislation, showing the good quality of the beer concerning the metals. The results of this work were requested by the previous Ministerio do Meio Ambiente e Urbanismo in order to contribute to review the brazilian legislation in foods and beverages about metals contents. (author)

  16. The Diagnosis of Plasma Parameters in Surface Alloying Technique by Optical Emission Spectrometry

    International Nuclear Information System (INIS)

    Fu Yabo; Zhang Yuefei; Chen Qiang; Zhang Guangqiu; Gao Yuan; Wang Jianzhong; Kui Xiaoyun

    2006-01-01

    Electron density (Ne) in a glow discharge plasma for the surface alloying technique is diagnosed by optical emission spectrometry (OES). With CH 4 as the feeding gas, Ne is obtained by comparing the Hβ spectrum according to the Stark broadening effect. It is noticed that Ne varies with the working pressures (30 Pa to 70 Pa) and cathode voltages (500 V to 1000 V), respectively. Due to an abnormal glow discharge, Ne is between 1.71x10 15 /cm 3 to 6.64x10 15 /cm 3 and increases rapidly with working gas pressures and cathode voltages. The results show that OES is a useful method to measure the plasma parameters in a surface alloying glow discharge plasma

  17. Determination of rare earth elements by liquid chromatography/inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Yoshida, K.; Haraguchi, H.

    1984-01-01

    Inductively coupled plasma atomic emission spectrometry (ICP-AES) interfaced with high-performance liquid chromatography (HPLC) has been applied to the determination of rare earth elements. ICP-AES was used as an element-selective detector for HPLC. The separation of rare earth elements with HPLC helped to avoid erroneous analytical results due to spectral interferences. Fifteen rare earth elements (Y and 14 lanthanides) were determined selectively with the HPLC/ICP-AES system using a concentration gradient method. The detection limits with the present HPLC/ICP-AES system were about 0.001-0.3 μg/mL with a 100-μL sample injection. The calibration curves obtained by the peak height measurements showed linear relationships in the concentration range below 500 μg/mL for all rare earth elements. A USGS rock standard sample, rare earth ores, and high-purity lanthanide reagents (>99.9%) were successfully analyzed without spectral interferences

  18. Determination of Cr, Mn, Si, and Ni in carbon steels by optical emission spectrometry with spark source

    International Nuclear Information System (INIS)

    Garcia Gonzalez, M.A.; Pomares Alfonso, M.; Mora Lopez, L.

    1995-01-01

    Elemental composition of steels determines some important of his characteristic moreover it is necessary to obtain their quality certification. Analytical procedure has performed for determination of Cr, Mn, Si and Ni in carbon steels by optical emission spectrometry with spark source. reproducibility of results is 5-11 %. Exactitude has tested with results that have obtained by internationally recognised methods-

  19. Thallium and manganese complexes involved in the luminescence emission of potassium-bearing aluminosilicates

    Energy Technology Data Exchange (ETDEWEB)

    Gomez-Gonzalez, Miguel A., E-mail: miguel.gomez@mncn.csic.es [Museo Nacional de Ciencias Naturales, CSIC, Jose Gutierrez Abascal 2, Madrid E-28006 (Spain); Garcia-Guinea, Javier, E-mail: guinea@mncn.csic.es [Museo Nacional de Ciencias Naturales, CSIC, Jose Gutierrez Abascal 2, Madrid E-28006 (Spain); Garrido, Fernando, E-mail: fernando.garrido@mncn.csic.es [Museo Nacional de Ciencias Naturales, CSIC, Jose Gutierrez Abascal 2, Madrid E-28006 (Spain); Townsend, Peter D., E-mail: pdtownsend@gmail.com [School of Science and Technology, University of Sussex, Brighton BN1 9QH (United Kingdom); Marco, Jose-Francisco, E-mail: jfmarco@iqfr.csic.es [Instituto de Química-Física Rocasolano, CSIC, Calle Serrano 119, Madrid E-28006 (Spain)

    2015-03-15

    The luminescence emission at 285 nm in natural K-feldspar has been studied by Russian groups and associated with thallium ions in structural positions of K{sup +} sites as artificially thallium-doped feldspars display the same emission band. Here attention is focussed on spectra of CL emission bands centered near 285 and 560 nm from paragenetic adularia, moscovite and quartz micro-inclusions. With accesorial thallium they show clear resemblances to each other. Associated sedimentary and hydrothermal aluminosilicate samples collected from Guadalix (Madrid, Spain) were analyzed with a wide range of experimental techniques including Environmental Scanning Electron Microscopy (ESEM) with an attached X-Ray Energy-Dispersive Spectrometer (EDS) and a cathodoluminescence probe (CL) and Electron Probe Microanalysis (EPMA), X-Ray Fluorescence Spectrometry (XRF), Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES), Differential and Thermogravimetric Analyses (DTA-TG), radioluminescence (RL), Mössbauer spectroscopy and X-Ray Photoelectron Spectrometry (XPS). The luminescence emission bands at 285 and 560 nm seem to be associated with hydrous thallium–manganese complexes bonded to potassium-bearing aluminosilicates since various minerals such as K-feldspar, moscovite and quartz micro-inclusions display similar CL spectra, accesorial thallium and hydroxyl groups. The presence of iron introduces a brown color which is attributed to submicroscopic iron oxides detectable in the optical and chemical microanalysis, but this does not contribute to the luminescence emission. The XPS Mn 2p spectrum of the adularia sample at room temperature is composed of a spin–orbit doublet plus clear shake-up satellite structure ∼4 eV above the main photoemision lines and is consistent with Mn{sup 2+} in good agreement with the observed luminescence emission at 560 nm for aluminosilicates produced by a {sup 4}T1({sup 4}G)→{sup 6}A1({sup 6}S) transition in tetrahedrally

  20. An improved microstrip plasma for optical emission spectrometry of gaseous species

    Energy Technology Data Exchange (ETDEWEB)

    Schermer, Susanne; Bings, Nicolas H.; Bilgic, Attila M.; Stonies, Robert; Voges, Edgar; Broekaert, Jose A.C. E-mail: jose.broekaert@chemie.uni-hamburg.de

    2003-09-26

    A modified compact 2.45 GHz microstrip plasma (MSP) operated with Ar as working gas at atmospheric pressure has been characterized and examined for its suitability for the determination of Hg as gaseous species by optical emission spectrometry. As a formerly described MSP the new device is provided on a sapphire substrate. The areas of plasma stability in terms of gas flow rates and microwave power for both MSPs with respect to plasma form and reflected power were investigated. Power levels of 5-40 W and Ar flow rates of 15-60 l/h were used. The modified MSP, which extends out of the channel in the sapphire substrate, was used for the recording of emission spectra for Hg vapor at different working conditions. Using optimized parameters a detection limit for Hg of less than 10 ng Hg/l Ar is obtained. The attainable excitation temperatures in the modified MSP at different microwave power were determined under the use of Fe as thermometric species and introducing ferrocene into the plasma. They were found to be at the order of 6000-7000 K for a power of 10-40 W and a gas flow of 15 l/h. It was shown that the modified MSP source can be combined with both a conventional monochromator with photomultiplier detection and a miniaturized spectrometer with CCD detection, whereby space-angle limitations are not stringent.

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

    Science.gov (United States)

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

    1987-01-01

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

  2. Spectroscopic investigations of ceramic materials using ICP-OES with modern vaporisation systems

    International Nuclear Information System (INIS)

    Reisch, M.U.; Mazurkiewicz, M.; Nickel, H.

    1990-10-01

    The object of this work was to study the evaporation and excitation process in the analysis of ceramic powders by the direct insertion of the samples into an inductively coupled plasma (ICP) as well as by external electrothermal evaporation. The evaporation rates were monitored by using 59 Fe and 115 Cd radiaoactive isotopes. The influence of various parameters such as the geometrical conditions, the carrier gas injection and the flow characteristics have been investigated. These methods have the advantage of easy preparation, no dilution and short experiment durations. The influence of different thermochemical additives as well as third elements, matrix compositions and grain size of the powders was determined. (orig.) [de

  3. Reference measurement procedure for the determination of electrolytes in human blood via ICP-OES measurement

    Science.gov (United States)

    Grote-Koska, D.; Klauke, R.; Brand, K.; Schumann, G.

    2018-04-01

    The determination of electrolytes in human body fluids is one of the most frequently performed analyses in clinical routine laboratories. Metrological traceability of measurement results in patient samples is essential and requires the involvement of higher order reference measurement procedures wherever available. Here, the authors present the evaluation of a higher order reference system for the simultaneous determination of K+, Li+, Na+, Ca2+ and Mg2+ in blood serum and plasma. In the same order, the determined measurement performances were as follows: measurement ranges: 0.75 mmol l-1-75.0 mmol l-1, 0.05 mmol l-1-5.00 mmol l-1, 5 mmol l-1-200 mmol l-1, 0.4 mmol l-1-8.0 mmol l-1 and 0.1 mmol l-1-4.0 mmol l-1. Measurement imprecision: CVs were  ⩽1.1% for intra assay investigations and  ⩽1.8% for long term inter assay investigations for all measurands. Excellent accuracy was found testing certified Standard Reference Materials from NIST: SRM 909 (deviations from 0.0% to 1.1%) and SRM 956 (deviations from 0.0% to 1.5%). Intercomparisons with the German Metrology Institute (PTB) revealed differences from 0.1% to 0.8%. Matrix influences and carry over were not detectable. The expanded combined measurement uncertainties for the determination of the reference method values were estimated as  ⩾1.5% (k  =  2) for each measurand. The reference measurement procedure is accredited by the German accreditation body (DAkkS) in association with the German calibration service (DKD) according to ISO 17025 and ISO 15195. Services comprise the certification of calibrators, control materials and samples used in proficiency testing schemes.

  4. Use of magnesium as a test element for inductively coupled plasma atomic emission spectrometry diagnosis

    International Nuclear Information System (INIS)

    Mermet, J.M.

    1991-01-01

    To optimize atomization and ionization processes in an inductively coupled plasma used as a source in atomic emission spectrometry, the Mg II 280.270-nm/Mg I 285-213-nm line intensity ratio is used. A theoretic ratio is calculated assuming a local thermodynamic equilibrium.A review of previously published experimental values of the ratio is given as a function of the parameters influencing the energy transfer between the plasma and injected species. In particular, the effects of the power, the carrier gas flow-rate, the i.d. of the torch injector, the use of a sheathing gas and the presence of hydrogen are described. Values of the ratio close to the theoretical values are obtained with a high power (>1.4 kW), a lower carrier gas flow-rate ( -1 ) and a large i.d. of the injector (>2 mm). This optimization can also be applied to the minimization of interference effects due to the presence of sodium. (author). 64 refs.; 9 figs.; 1 tab

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

    Energy Technology Data Exchange (ETDEWEB)

    Peterson, Charlie Albert [Iowa State Univ., Ames, IA (United States)

    1977-12-01

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

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

    Science.gov (United States)

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

    2010-08-03

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

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

    Science.gov (United States)

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

    2009-10-01

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

  8. Isotopic Tracing of Fuel Components in Particulate Emissions from Diesel Engines using Accelerator Mass Spectrometry (AMS)

    International Nuclear Information System (INIS)

    Buchholz, B A; Mueller, C J; Garbak, J.

    2001-01-01

    Accelerator mass spectrometry (AMS) is an isotope-ratio measurement technique developed in the late 1970s for tracing long-lived radioisotopes (e.g., 14 C half life = 5760 y). The technique counts individual nuclei rather than waiting for their radioactive decay, allowing measurement of more than 100 low-level 14 C samples per day (Vogel et al, 1995). The LLNL AMS system is shown in Fig.1. The contemporary quantity of 14 C in living things ( 14 C/C = 1.2 x 10 -12 or 110 fmol 14 C/ g C) is highly elevated compared to the quantity of 14 C in petroleum-derived products. This isotopic elevation is sufficient to trace the fate of bio-derived fuel components in the emissions of an engine without the use of radioactive materials. If synthesis of a fuel component from biologically-derived source material is not feasible, another approach is to purchase 14 C-labeled material (e.g., dibutyl maleate (DBM)) and dilute it with petroleum-derived material to yield a contemporary level of 14 C. In each case, the virtual absence of 14 C in petroleum based fuels gives a very low 14 C background that makes this approach to tracing fuel components practical. Regulatory pressure to significantly reduce the particulate emissions from diesel engines is driving research into understanding mechanisms of soot formation. If mechanisms are understood, then combustion modeling can be used to evaluate possible changes in fuel formulation and suggest possible fuel components that can improve combustion and reduce PM emissions. The combustion paradigm assumes that large molecules break down into small components and then build up again during soot formation. AMS allows us to label specific fuel components, including oxygenates, trace the carbon atoms, and test this combustion modeling paradigm. Volatile and non-volatile organic fractions (VOF, NVOF) in the PM can be further separated. The VOF of the PM can be oxidized with catalysts in the exhaust stream to further decrease PM. The effectiveness

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

    International Nuclear Information System (INIS)

    Chung, Yong Sam; Choi, Kwang Soon; Moon, Jong Hwa; Kim, Sun Ha; Lim, Jong Myoung; Kim, Young Jin; Quraishi, Shamshad Begum

    2003-05-01

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

  10. Quantitative determination of total cesium in highly active liquid waste by using liquid electrode plasma optical emission spectrometry.

    Science.gov (United States)

    Do, Van-Khoai; Yamamoto, Masahiko; Taguchi, Shigeo; Takamura, Yuzuru; Surugaya, Naoki; Kuno, Takehiko

    2018-06-01

    A sensitive analytical method for determination of total cesium (Cs) in highly active liquid waste (HALW) by using modified liquid electrode plasma optical emission spectrometry (LEP-OES) is developed in this study. The instrument is modified to measure radioactive samples in a glove box. The effects of important factors, including pulsed voltage sequence and nitric acid concentration, on the emission of Cs are investigated. The limit of detection (LOD) and limit of quantification (LOQ) are 0.005 mg/L and 0.02 mg/L, respectively. The achieved LOD is one order lower than that of recently developed spectroscopic methods using liquid discharge plasma. The developed method is validated by subjecting a simulated HALW sample to inductively coupled plasma mass spectrometry (ICP-MS). The recoveries obtained from a spike-and-recovery test are 96-102%, implying good accuracy. The method is successfully applied to the quantification of Cs in a real HALW sample at the Tokai reprocessing plant in Japan. Apart from dilution and filtration of the HALW sample, no other pre-treatment process is required. The results agree well with the values obtained using gamma spectrometry. The developed method offers a reliable technique for rapid analysis of total Cs in HALW samples. Copyright © 2018 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2004-01-01

    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)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-12-01

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

  13. Matrix digestion of soil and sediment samples for extraction of lead, cadmium and antimony and their direct determination by inductively coupled plasma-mass spectrometry and atomic emission spectrometry

    International Nuclear Information System (INIS)

    Chattopadhyay, P.; Fisher, A.S.; Henon, D.N.; Hill, S.J.

    2004-01-01

    An environmentally friendly and simple method has been developed for complete digestion of lead, cadmium and antimony from soil samples using a magnesium nitrate assisted dry ashing procedure. Statistical data for a series of experiments with standard reference materials are presented, and precision values are found to be comparable for inductively coupled plasma-mass spectrometry and for inductively coupled plasma-atomic emission spectrometry. From a single digest solution all analytes are quantified without involving any preconcentration routes. Inter-method comparison of inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) shows that the probability of the results being different is less than 99 %. (author)

  14. Phonon-assisted field emission in silicon nanomembranes for time-of-flight mass spectrometry of proteins.

    Science.gov (United States)

    Park, Jonghoo; Aksamija, Zlatan; Shin, Hyun-Cheol; Kim, Hyunseok; Blick, Robert H

    2013-06-12

    Time-of-flight (TOF) mass spectrometry has been considered as the method of choice for mass analysis of large intact biomolecules, which are ionized in low charge states by matrix-assisted-laser-desorption/ionization (MALDI). However, it remains predominantly restricted to the mass analysis of biomolecules with a mass below about 50,000 Da. This limitation mainly stems from the fact that the sensitivity of the standard detectors decreases with increasing ion mass. We describe here a new principle for ion detection in TOF mass spectrometry, which is based upon suspended silicon nanomembranes. Impinging ion packets on one side of the suspended silicon nanomembrane generate nonequilibrium phonons, which propagate quasi-diffusively and deliver thermal energy to electrons within the silicon nanomembrane. This enhances electron emission from the nanomembrane surface with an electric field applied to it. The nonequilibrium phonon-assisted field emission in the suspended nanomembrane connected to an effective cooling of the nanomembrane via field emission allows mass analysis of megadalton ions with high mass resolution at room temperature. The high resolution of the detector will give better insight into high mass proteins and their functions.

  15. Efficient high-resolution X-ray emission spectrometry using synchrotron radiation

    International Nuclear Information System (INIS)

    Unterumsberger, Rainer

    2015-01-01

    The aim of the present work is to get access to high-resolution X-Ray Emission Spectrometry (XES) at nanoscaled materials, consisting of light elements and transition metals, by the increase of the sensitivity of a Wavelength-Dispersive Spectrometer (WDS) in the soft X-Ray range. The increase of the sensitivity was achieved by a refocusing of the incident radiation. With the increased sensitivity of the WDS, it was possible to determine the chemical species of different, nominal 100 nm thin titanium oxides. The combination of the refocusing optic and calibrated spectrometer enabled the detection and deconvolution of the L-fluorescence radiation of these nanoscaled titanium oxides. Due to the calibration of the spectrometer, a reliable determination of the transition probabilities of the titanium La- and Ll-fluorescence lines as a function of the chemical state is possible. To the best of my knowledge, the determination of the transition probabilities as a function of the chemical state in the soft X-Ray range has not been investigated yet. The quality of the refocusing was characterized using different diagnostic tools. Vertical full width at half maximum (FWHM) values of the focused beam between 10 μm to 20 μm and horizontal FWHM values between 12 μm and 25 μm could be achieved over an energy range of 180 eV to 1310 eV. Using calibrated photodiodes, it was possible to determine the absolute transmission of the used single bounce monocapillary as well as to monitor the absolute photon flux. By means of the refocusing, it was possible to increase the photon flux by a factor of 4.9 experimentally. The increase of the photon flux enables the analysis of nanoscaled materials with the used spectrometer. This could be shown based on the determination of the lower limit of detection of boron Ka and titanium La. In both cases, the lower limit of detection of 0.4 nm equivalent layer thickness was achieved (about 1.10 -7 g/cm 2 to 2.10 -7 g/cm 2 or 3.10 15 atoms/cm 2 to

  16. Chemical analysis of zinc electroplating solutions by x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Jung, Sung-Mo; Cho, Young-Mo; Na, Han-Gil

    2007-01-01

    A quantitative analysis method used to analyze chlorine, iron and zinc in electroplating solutions, using X-ray spectrometry in atmospheric He mode, is proposed. The present research concerns the replacement of the conventional analyses of electroplating solutions with rapid and reproducible quantification using X-ray fluorescence spectrometer. An in-depth investigation conducted in the present study identifies the species present in the real electroplating solutions. XRD patterns and semi-quantitative results for the electroplating solutions show synthetic standards based on the compositional range of solutions by analyzing the electroplating solutions obtained in real processes. 28 calibration standard solutions are prepared by diluting liquid standard solutions certified by titration and ICP-OES analyses used to construct the XRF calibration curves for Cl, Fe and Zn. The suggested method showed satisfactory precision and accuracy in the analysis of electroplating solutions. The present study provides evidences that the proposed XRF spectrometry could be an alternative analytical method to replace the conventional techniques by comparing the uncertainties estimated for each method. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

    Balbinot, L. [Departamento de Quimica Analitica-Instituto de Quimica-Unicamp, PO Box 6154, CEP: 13083-971, Campinas, SP (Brazil); Smichowski, P. [Comision Nacional de Energia Atomica, Unidad de Actividad Quimica, Centro Atomico Constituyentes, Av. Gral Paz 1499, B1650KNA, San Martin, Provincia de Buenos Aires (Argentina); Farias, S. [Comision Nacional de Energia Atomica, Unidad de Actividad Quimica, Centro Atomico Constituyentes, Av. Gral Paz 1499, B1650KNA, San Martin, Provincia de Buenos Aires (Argentina); Arruda, M.A.Z. [Departamento de Quimica Analitica-Instituto de Quimica-Unicamp, PO Box 6154, CEP: 13083-971, Campinas, SP (Brazil); Vodopivez, C. [Instituto Antartico Argentino, Cerrito 1010, C1248AAZ, Buenos Aires (Argentina); Poppi, R.J. [Departamento de Quimica Analitica-Instituto de Quimica-Unicamp, PO Box 6154, CEP: 13083-971, Campinas, SP (Brazil)]. E-mail: ronei@iqm.unicamp.br

    2005-06-30

    Optical emission spectrometers can generate results, which sometimes are not easy to interpret, mainly when the analyses involve classifications. To make simultaneous data interpretation possible, the Kohonen neural network is used to classify different Antarctic algae according to their taxonomic groups from the determination of 14 analytes. The Kohonen neural network architecture used was 5x5 neurons, thus reducing 14-dimension input data to two-dimensional space. The input data were 14 analytes (As, Co, Cu, Fe, Mn, Sr, Zn, Cd, Cr, Mo, Ni, Pb, Se, V) with their concentrations, determined by inductively coupled plasma optical emission spectrometry in 11 different species of algae. Three taxonomic groups (Rhodophyta, Phaeophyta and Cholorophyta) can be differentiated and classified through only their Cu content.

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

    International Nuclear Information System (INIS)

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

    2005-01-01

    Optical emission spectrometers can generate results, which sometimes are not easy to interpret, mainly when the analyses involve classifications. To make simultaneous data interpretation possible, the Kohonen neural network is used to classify different Antarctic algae according to their taxonomic groups from the determination of 14 analytes. The Kohonen neural network architecture used was 5x5 neurons, thus reducing 14-dimension input data to two-dimensional space. The input data were 14 analytes (As, Co, Cu, Fe, Mn, Sr, Zn, Cd, Cr, Mo, Ni, Pb, Se, V) with their concentrations, determined by inductively coupled plasma optical emission spectrometry in 11 different species of algae. Three taxonomic groups (Rhodophyta, Phaeophyta and Cholorophyta) can be differentiated and classified through only their Cu content

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    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. - Highlights: • Non-spectral matrix interference in ICP-AES is flagged and minimized. • Emission from different locations of the plasma are collected simultaneously. • Spatially dependent determined concentrations indicate the presence of interference. • Gradient dilution is performed on both calibration standards and sample. • Optimal dilution factor to minimize interference is found as dilution increases

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

    Energy Technology Data Exchange (ETDEWEB)

    Cheung, Yan; Schwartz, Andrew J.; Chan, George C.-Y.; Hieftje, Gary M., E-mail: hieftje@indiana.edu

    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. - Highlights: • Non-spectral matrix interference in ICP-AES is flagged and minimized. • Emission from different locations of the plasma are collected simultaneously. • Spatially dependent determined concentrations indicate the presence of interference. • Gradient dilution is performed on both calibration standards and sample. • Optimal dilution factor to minimize interference is found as dilution increases.

  1. Spectrochemical determination of tantalum in plutonium metal using direct current plasma emission spectrometry

    International Nuclear Information System (INIS)

    Fadeff, S.K.; Morris, W.F.

    1983-01-01

    Tantalum is determined by direct current plasma spectrometry after separation of plutonium from solution as PuF 3 . After centrifugation of the PuF 3 precipitate, a low level of plutonium remains in solution in sufficient quantity to cause spectral interferences. It is necessary to determine the plutonium by dc plasma spectrometry and apply a correction to determine low tantalum concentrations with good accuracy and precision. Tantalum can be determined down to 0.4 ppM in solution with a relative standard deviation of 10 percent. Better precision can be achieved at higher concentrations. The procedure is simple and convenient for glovebox work. 5 references, 1 figure, 1 table

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

    Science.gov (United States)

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

    2017-12-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-05-15

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

  4. An isotopic analysis process with optical emission spectrometry on a laser-produced plasma

    International Nuclear Information System (INIS)

    Mauchien, P.; Pietsch, W.; Petit, A.; Briand, A.

    1994-01-01

    The sample that is to be analyzed is irradiated with a laser beam to produce a plasma at the sample surface; the spectrum of the light emitted by the plasma is analyzed and the isotope composition of the sample is derived from the spectrometry. The process is preferentially applied to uranium and plutonium; it is rapid, simpler and cheaper than previous methods, and may be applied to 'in-situ' isotopic analysis in nuclear industry. 2 figs

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-02-01

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

  6. Spectrometry and dosimetric evaluation of the gamma-ray emissions of 241Am

    International Nuclear Information System (INIS)

    Bradley, D.A.; Chong, C.S.

    1991-01-01

    New, detailed measurements have been made of the photon spectrum of the radionuclide 241 Am. Observations, recorded for a 95% confidence level over local background, provide affirmation of a number of lines previously considered to be of equivocal existence. A number of hitherto unreported emissions are similarly observed. Peak areas, expressed as a percentage of that for the 59.54 keV emission, have been ascribed to all lines of the detailed spectrum. This leads to an estimated increase in the value of exposure calculated from the measured fluence spectrum, relative to that from the 59.54 keV line, of (3.1 ± 0.8)%, taking into account all emissions beyond the predominating 59.54 keV gamma-ray emission. (author)

  7. Simultaneous determination of Cr, Ga, In and V in soil and water samples by tungsten coil atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Donati, George L.; Kron, Benjamin E. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Jones, Bradley T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States)], E-mail: jonesbt@wfu.edu

    2009-06-15

    Tungsten coil atomic emission spectrometry is employed for the simultaneous determination of Cr, Ga, In, and V. Both V and In are detected by this technique for the first time. The atomizer is a simple, inexpensive tungsten filament extracted from a mass-produced, commercially-available 150 W, 15 V microscope bulb. A 25 {mu}l sample aliquot is placed directly on the coil and a small constant-current power source is used to carefully dry, ash and atomize the sample. Analytical signals are detected with a Czerny-Turner spectrograph and a charge coupled device detector. Multiple emission lines from all 4 elements are monitored simultaneously in a 54 nm spectral window. Concentration limits of detection are in the {mu}g l{sup - 1} range for all elements, and the absolute limits of detection are 0.2, 2, 0.5, and 10 ng for Cr, Ga, In, and V, respectively. Even lower values may be obtained by combining the signals for the multiple emission lines of a single element. The method precision is typically better than 5.0% relative standard deviation, and sometimes as good as 0.95% (Ga). Standard reference materials of soil and water are used to check the method accuracy. After a simple acid extraction, the values determined by the method presented no significant difference from the reported values at the 95% confidence level.

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

    Science.gov (United States)

    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.

  9. Determination of daily intake of elements from Philippine total diet samples using inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Leon, G.C. de; Shiraishi, K.; Kawamura, H.; Igaraishi, Y.; Palattao, M.V.; Azanon, E.M.

    1990-10-01

    Total diet samples were analyzed for major elements (Na, K, Ca, Mg, P) and some minor trace elements (Fe, Zn, Mn, Al, Sr, Cu, Ba, Yt) using inductively coupled plasma-atomic emission spectrometry (ICP-AES). Samples analyzed were classified into sex and age groups. Results for some elements (Na, K, Mg, Zn, Cu, Mn) were compared with values from Bataan dietary survey calculated using the Philippine composition table. Exceot for Na, analytical results were similar to calculated values. Analytical results for Ca and Fe were also compared with the values from Food and Nutrition Research Institute. In general, values obtained in the study were lower than the FNRI values. Comparison of the analytical and calculated results with the Japanese and ICRP data showed that Philippine values were lower than foreign values. (Auth.). 22 refs., 9 tabs

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  11. Accuracy and Precision in Elemental Analysis of Environmental Samples using Inductively Coupled Plasma-Atomic Emission Spectrometry

    International Nuclear Information System (INIS)

    Quraishi, Shamsad Begum; Chung, Yong-Sam; Choi, Kwang Soon

    2005-01-01

    Inductively Coupled Plasma-Atomic Emission Spectrometry followed by micro-wave digestion have been performed on different environmental Certified Reference Materials (CRMs). Analytical results show that accuracy and precision in ICP-AES analysis were acceptable and satisfactory in case of soil and hair CRM samples. The relative error of most of the elements in these two CRMs is within 10% with few exceptions and coefficient of variation is also less than 10%. Z-score as an analytical performance was also within the acceptable range (±2). ICP-AES was found as an inadequate method for Air Filter CRM due to incomplete dissolution, low concentration of elements and very low mass of the sample. However, real air filter sample could have been analyzed with high accuracy and precision by increasing sample mass during collection. (author)

  12. Inductively coupled plasma optical emission spectrometry analysis of lanthanum, samarium and gadolinium oxides for rare earths impurities

    International Nuclear Information System (INIS)

    Reino, L.C.P.; Lordello, A.R.

    1990-09-01

    An inductively coupled plasma optical emission spectrometry method is described for the determination of Sm, Eu, La, Gd, Dy, Pr, Ho, Nd, Tb and Y in purified oxides of lanthanum, samarium and gadolinium. The method enables a simple, precise and readily available determination. Dissolution of the samples is achieved with diluted hydrochloric acid (1:1). The solutions are diluted to volume for a concentration of 1mg/ml. The lowest determination limit is 0,01% for most elements and 0,05 or 0,1% for a few rare earths in samarium and gadolinium matrices. Lanthanum, Samarium and Gadolinium concentrates with purity grade of 99,9%, 99,6% and 99,8%, respectively, can be analysed by this procedure. (author)

  13. Proton Induced X-Rays Emission (PIXE) and Atomic Absorption Spectrometry (AAS) applied in the environmental sample analysis

    International Nuclear Information System (INIS)

    Popescu, Ion V.; Iordan, M.; Stihi, C.; Bancuta, A.; Dima, G.; Busuioc, G.; Ciupina, V.; Belc, M.; Badica, T.

    2003-01-01

    The aim of this work is to determine the elemental composition of tree leaves using Proton-Induced X-Rays Emission (PIXE) and Atomic Absorption Spectrophotometry (AAS) methods. By PIXE Spectrometry we identified and determined the concentration of S, Cl, K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu Zn, As, Br, Sr and by AAS method the concentration of elements: Cr, Mn, Fe, Co, Cu, Zn, Se, Cd. Pb was identified in only 2 samples from 29. For tree leave samples collected at a large distance to the polluting source the Sr concentration decreased and the Mg, Ca, Se, Zn and Fe concentrations increased. Also, we can observe a small affinity of these leaves for the environmental Pb which was detected for two samples at a small distance to polluting source. (authors)

  14. Semi-automatic determination of tin in marine materials by continuous flow hydride generation inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Feng Yonglai; Narasaki, Hisataki; Chen Hongyuan; Tian Liching

    1997-01-01

    A semi-automated continuous flow hydride generation system with inductively coupled plasma atomic emission spectrometry (ICP-AES) was used for the determination of tin in marine materials. The effects of acids (H 2 SO 4 and HCl) were studied. The analytical parameters were thoroughly investigated. Under optimized conditions, the detection limit is 0.4 ng/ml. Interferences from transition elements were investigated and seven masking reagents were tested. L-cysteine hydrochloride monohydrate (1%) was used to mask the interferences from foreign ions. Finally, the accuracy, checked with a marine standard reference material obtained from the National Research Council (NRC), was within the certified value. (orig.). With 6 figs., 4 tabs

  15. Glow Discharge Emission Spectrometry (GDOES): Theoretical Introduction, General Aspects, and its Applications within the Framework of the Technofusion Programs

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    Science.gov (United States)

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

    2015-01-01

    The article presents the optimisation, validation and application of the microwave induced plasma optical emission spectrometry (MIP-OES) dedicated for a routine determination of Ag, Al, B, Ba, Bi, Ca, Cd, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Ni, Pb, Sr, Tl, Zn, in the geological samples. The three procedures of sample preparation has been proposed: sample digestion with the use of hydrofluoric acid for determination of total concentration of elements, extraction by aqua regia for determination of the quasi-total element concentration and extraction by hydrochloric acid solution to determine contents of the elements in acid leachable fraction. The detection limits were on the level 0.001-0.121 mg L(-1) (from 0.010-0.10 to 1.2-12 mg kg(-1) depend on the samples preparation procedure); the precision: 0.20-1.37%; accuracy 85-115% (for recovery for certified standards materials analysis and parallel analysis by independent analytical techniques: X-ray fluorescence (XRF) and flame absorption spectrometry (FAAS)). The conformity of the results obtained by MIP-OES analytical procedures with the results obtained by XRF and FAAS analysis allows to propose the procedures for studies of elemental composition of the fraction of the geological samples. Additionally, the MIP-OES technique is much less expensive than ICP techniques and much less time-consuming than AAS techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2017-08-15

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

  18. Arsenic speciation in marine organisms: from the analytical methodology to the constitution of reference materials

    Energy Technology Data Exchange (ETDEWEB)

    El Moll, A. [Laboratoire de Chimie Minerale et Analytique, URA 405 du CNRS, E. H. I. C. S., 1 rue Blaise Pascal, F-67008 Strasbourg Cedex (France); Heimburger, R. [Laboratoire de Chimie Minerale et Analytique, URA 405 du CNRS, E. H. I. C. S., 1 rue Blaise Pascal, F-67008 Strasbourg Cedex (France); Lagarde, F. [Laboratoire de Chimie Minerale et Analytique, URA 405 du CNRS, E. H. I. C. S., 1 rue Blaise Pascal, F-67008 Strasbourg Cedex (France); Leroy, M.J.F. [Laboratoire de Chimie Minerale et Analytique, URA 405 du CNRS, E. H. I. C. S., 1 rue Blaise Pascal, F-67008 Strasbourg Cedex (France); Maier, E. [Commission of the European Communities, Measurements and Testing Programme (BCR), 75 rue Montoyer, B-1049 Brussels (Belgium)

    1996-03-01

    An analytical procedure for total arsenic and arsenic species quantification in marine organisms has been developed. Fresh materials are freeze-dried and reduced to powders before analysis. Arsenic is determined either by energy dispersive X-ray fluorescence (EDXRF) directly or by inductively coupled plasma optical emission spectrometry (ICP/OES) after microwave digestion. Arsenic speciation is performed on the extracted sample using liquid chromatography coupled to ICP/OES for arsenobetaine and arsenocholine determination and to the hydride generation-quartz furnace atomic absorption spectrometric technique for arsenite, arsenate, monomethylarsonic and dimethylarsinic acids quantification. Special precautions are taken to avoid losses or contaminations as well as to prevent analytical errors during the quantification stage. Other methods are applied and the corresponding results compared for each step of the procedure. The method is finally validated by means of intercomparison studies within the Measurements and Testing Programme of the European Community (formely BCR). (orig.). With 9 figs., 5 tabs.

  19. Antimony removal from aqueous solutions using Zirconium hydroxide

    International Nuclear Information System (INIS)

    Petrescu, D.; Velciu, L.; Bucur, C.

    2016-01-01

    In this paper it is presented an experimental test for non-radioactive antimony removal from aqueous solutions using zirconium hydroxide powder. Also, it was studied how the temperature and pH influences antimony adsorption onto zirconium hydroxide surface. After the adsorption, solutions were filtered on Cellulose Mixed Ester Membrane with 0.2 μm pore size to remove the zirconium powder and then the aqueous solutions were sent to Inductively Coupled Plasma Optic Emission Spectrometry (ICP-OES) for quantitative analysis of Sb. Zirconium hydroxide powders were examined by optical microscopy. For the solutions that were tested at pH 4.5 and 10.2 the antimony concentration dropped below the detection limit of ICP-OES device, proof of antimony adsorption on zirconium hydroxide. Also, for the other tested solutions which had pH=12 the antimony concentration reduced with 77% and 80%. The temperature had no influence upon adsorption mechanism. (authors)

  20. Determination of rare-earth elements content in granitic rocks by argon plasma emission spectrometry

    International Nuclear Information System (INIS)

    Merodio, J.C.; Martinez, J.M.

    1990-01-01

    A method has been developed that enables the rare-earth elements in granitic rocks to be measured sequentially, using an inductively coupled plasma (ICP) source spectrometer with medium spectral resolution (0,02nm). The rocks were dissolved in an open system with a mixture of nitric-hydrofluoric-perchloric acids. Any residues remaining at this stage were removed by filtration and digested using a mini-fusion method with lithium tetraborate. Prior to the excitation in the spectrometer the rare-earth group was separated from other constituents using cation-exchange chromatography. A detailed study of spectral interferences and the evaluation of the detection limits have been performed. Five geochemical reference sample (granitic rocks) were analyzed and the obtained results agree favourably with recommended values and with reported determinations, using high spectral resolution ICP spectrometry. (Author) [es

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-01-02

    Graphical abstract: -- Highlights: •Direct analysis of biodiesel on a tungsten coil atomizer. •Determination of Na, K, Cr and V by tungsten coil atomic emission spectrometry. •Sample dilution with methanol or ethanol. •Ten-microliter sample aliquots and limits of detection between 20 and 90 μg kg{sup −1}. •Low consumption of reagents, samples and gases in a 140 s per run procedure. -- Abstract: High levels of sodium and potassium can be present in biodiesel fuel and contribute to corrosion, reduced performance and shorter engine lifetime. On the other hand, trace amounts of chromium and vanadium can increase the emission of pollutants during biodiesel combustion. Sample viscosity, immiscibility with aqueous solutions and high carbon content can compromise biodiesel analyzes. In this work, tungsten filaments extracted from microscope light bulbs are used to successively decompose biodiesel's organic matrix, and atomize and excite the analytes to determine sodium, potassium, chromium and vanadium by tungsten coil atomic emission spectrometry (WCAES). No sample preparation other than simple dilution in methanol or ethanol is required. Direct analysis of 10-μL sample aliquots using heating cycles with less than 150 s results in limits of detection (LOD) as low as 20, 70, 70 and 90 μg kg{sup −1} for Na, K, Cr and V, respectively. The procedure's accuracy is checked by determining Na and K in a biodiesel reference sample and carrying out spike experiments for Cr and V. No statistically significant differences were observed between reference and determined values for all analytes at a 95% confidence level. The procedure was applied to three different biodiesel samples and concentrations between 6.08 and 95.6 mg kg{sup −1} for Na and K, and between 0.22 and 0.43 mg kg{sup −1} for V were obtained. The procedure is simple, fast and environmentally friendly. Small volumes of reagents, samples and gases are used and no residues are generated

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    Graphical abstract: -- Highlights: •Direct analysis of biodiesel on a tungsten coil atomizer. •Determination of Na, K, Cr and V by tungsten coil atomic emission spectrometry. •Sample dilution with methanol or ethanol. •Ten-microliter sample aliquots and limits of detection between 20 and 90 μg kg −1 . •Low consumption of reagents, samples and gases in a 140 s per run procedure. -- Abstract: High levels of sodium and potassium can be present in biodiesel fuel and contribute to corrosion, reduced performance and shorter engine lifetime. On the other hand, trace amounts of chromium and vanadium can increase the emission of pollutants during biodiesel combustion. Sample viscosity, immiscibility with aqueous solutions and high carbon content can compromise biodiesel analyzes. In this work, tungsten filaments extracted from microscope light bulbs are used to successively decompose biodiesel's organic matrix, and atomize and excite the analytes to determine sodium, potassium, chromium and vanadium by tungsten coil atomic emission spectrometry (WCAES). No sample preparation other than simple dilution in methanol or ethanol is required. Direct analysis of 10-μL sample aliquots using heating cycles with less than 150 s results in limits of detection (LOD) as low as 20, 70, 70 and 90 μg kg −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

  4. Flame emission spectrometry using atomic absorption apparatus. I. Determination of Sr in sea water

    International Nuclear Information System (INIS)

    Aizawa, S.; Yoshimura, E.; Hamachi, M.; Haraguchi, H.; Dokiya, Y.; Fuwa, K.

    1976-01-01

    Flame emission determination of Sr in seawater was studied using an ordinary atomic absorption apparatus. The analytical line 4607 A was used with a background correction at 4616 A. The ionization was negligible in an air acetylene flame with seawater, and the interference of H 2 SO 4 was eliminated using the higher part of the flame. Sr concentration of seawater of Tokyo Bay and Sagami Bay has been determined

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

    International Nuclear Information System (INIS)

    Ortega, Claudia; Cerutti, Soledad; Silva, Maria F.; Olsina, Roberto A.; 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 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 μg L -1 . The precision for 10 replicate determinations at the 2.0 μg 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 μg L -1 . The method was successfully applied to the determination of dysprosium in urine. (orig.)

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

    Science.gov (United States)

    Wagatsuma, Kazuaki

    2009-04-01

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

  7. Quenching of the OH and nitrogen molecular emission by methane addition in an Ar capacitively coupled plasma to remove spectral interference in lead determination by atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-07-15

    A new method is proposed to remove the spectral interference on elements in atomic fluorescence spectrometry by quenching of the molecular emission of the OH radical (A{sup 2{Sigma}+} {yields} X{sup 2{Pi}}) and N{sub 2} second positive system (C{sup 3{Pi}}{sub u} {yields} B{sup 3{Sigma}}{sub g}) in the background spectrum of medium power Ar plasmas. The experiments were carried out in a radiofrequency capacitively coupled plasma (275 W, 27.12 MHz) by CH{sub 4} addition. The quenching is the result of the high affinity of OH radical for a hydrogen atom from the CH{sub 4} molecule and the collisions of the second kind between nitrogen excited molecules and CH{sub 4}, respectively. The decrease of the emission of N{sub 2} second positive system in the presence of CH{sub 4} is also the result of the deactivation of the metastable argon atoms that could excite the nitrogen molecules. For flow rates of 0.7 l min{sup -1} Ar with addition of 7.5 ml min{sup -1} CH{sub 4}, the molecular emission of OH and N{sub 2} was completely removed from the plasma jet spectrum at viewing heights above 60 mm. The molecular emission associated to CH and CH{sub 2} species was not observed in the emission spectrum of Ar/CH{sub 4} plasma in the ultraviolet range. The method was experimented for the determination of Pb at 283.31 nm by atomic fluorescence spectrometry with electrodeless discharge lamp and a multichannel microspectrometer. The detection limit was 35 ng ml{sup -1}, 2-3 times better than in atomic emission spectrometry using the same plasma source, and similar to that in hollow cathode lamp microwave plasma torch atomic fluorescence spectrometry.

  8. Development of multilayer optics for X-ray broadband spectrometry of plasma emission

    International Nuclear Information System (INIS)

    Emprin, Benoit

    2014-01-01

    Within the framework of the research on inertial confinement fusion, the 'Commissariat a l'energie atomique et aux energies alternatives' has studied and implemented an absolute calibrated time-Resolved broadband soft x-Ray spectrometer, called 'Diagnostic de Mesure du rayonnement X'. This diagnostic, composed of 20 measurement channels, measures the emitted radiant power from a laser created plasma in the range from 50 eV to 20 keV. We have developed additional measurement channels to obtain redundancy and an improvement in measurement accuracy. The principle of these new channels is based on an original concept to obtain spectral bounded flat-Responses. Two channels have been developed for the 2 - 4 keV and 4 - 6 keV spectral ranges, using aperiodic multilayer mirrors made at the 'Laboratoire Charles Fabry' with Cr/Sc and Ni/W/SiC/W layers respectively. These mirrors were characterized at synchrotron radiation facilities and integrated into the spectrometer. The two new channels were used during laser-Plasma experimental campaigns at the OMEGA laser facility in Rochester (USA). This allowed us to determine directly the radiant power with only one measurement within a certain spectral band, and with a better precision when compared with using standard channels. The results, in good agreement with the standard measurement channels, allowed us to validate the use of aperiodic multilayer mirrors for X-Ray broadband spectrometry. (author) [fr

  9. Determination of boron in waters by using methyl borate generation and flame atomic-emission spectrometry

    International Nuclear Information System (INIS)

    Castillo, J.R.; Mir, J.M.; Martinez, C.; Bendicho, C.

    1985-01-01

    An improved method is proposed for the determination of boron in waters. The esterification reaction between boric acid and methanol in a concentrated sulphuric acid medium and the vaporisation of the methyl borate formed (boiling-point, 68 C) are used in the determination by boron by measuring the emission of the BO 2 radical at 548 nm. This reaction is carried out in a simple and inexpensive generator, designed for this purpose, and the heat developed in it causes the rapid volatilisation of the methyl borate. Thus no collection systems or carrier gas are required. The proposed method gives an improved detection limit and it can be applied to the determination of boron in water samples. It is both rapid and highly selective. (author)

  10. Study of uranium matrix interference on ten analytes using inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ghazi, A.A.; Qamar, S.; Atta, M.A. (A.Q. Khan Research Labs., Rawalpindi (Pakistan))

    1993-08-01

    Maximum allowable concentrations of 12 elements in uranium hexafluoride feed for enrichment to reactor grade material (about 3%), vary from 1 to 100 ppm ([mu]g/g). Using an inductively coupled plasma atomic emission spectrometer, 51 lines of tine of these elements (B, Cr, Mo, P, Sb, Si, Ta, Ti, V and W) has been studied with a uranium matrix to investigate the matrix interference on the basis of signal to background (SBR), and background to background ratios (BBR). Detection limits and limits of quantitative determination (LQDs) were calculated for these elements in a uranium matrix using SBR and relative standard deviation of the background signal (RSD[sub B]) approach. In almost all cases, the uranium matrix interference reduces the SBRs to the extent that direct trace analysis is impossible. A uranium sample having known concentrations of impurities (around LQDs) was directly analysed with results that showed reasonable accuracy and precision. (Author).

  11. Determination of the mineral compositions of in six beans by microwave digestion with inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Yan, Q.; Yang, L.; Chen, S.; Liu, X.; Ma, X.

    2012-01-01

    In the study, microwave digestion procedure optimized was applied for digesting beans. Nineteen mineral element concentrations were determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The result indicated detection limits for the 19 elements were less than 0.0998, and relative standard deviations were 1.01% - 5.02% for all the elements, and recoveries were 90.89% - 104.55% by adding standard recovery experiment. The study showed the beans selected were abundant in mineral element contents in human nutrition, determination mineral element contents by ICP-AES with microwave digestion technology were a lot of merits of small environmental pollution, fast and accurate determination result, which could satisfy the examination request of bean samples. The results provided evidence that the six beans were a good source of K, P, Mg and Ca. This study is to give important reference value to people due to individual differences by adjusting the dietary to complement the different mineral elements. (author)

  12. Inductively coupled plasma-atomic emission spectrometry: analytical assessment of the technique at the beginning of the 90's

    International Nuclear Information System (INIS)

    Sanz-Medel, A.

    1991-01-01

    The main application of the inductively coupled plasma (ICP) today is in atomic emission spectroscopy (AES), as an excitation spectrochemical source, although uses of an ICP for fluorescence as just an atomizer, and specially for mass spectrometry, as an ionization source, are rocketing in the last few years. Since its inception, only a quarter of a century ago, ICP-AES has rapidly evolved to one of the preferred routine analytical techniques for convenient determination of many elements with high speed, at low levels and in the most varied samples. Perhaps its comparatively high kinetic temperature (capable of atomizing virtually every compound of any sample), its high excitation and ionization temperatures, and its favourable spatial structure at the core of the ICP success. By now, the ICP-AES can be considered as having achieved maturity in that a huge amount of analytical problems can be tackled with this technique, while no major or fundamental changes have been adopted for several years. Despite this fact, important driving forces are still in operation to further improve the ICP-AES sensitivity, selectivity, precision, sample throughput, etc. Moreover, proposals to extend the scope of the technique to traditionally elusive fields (e.g. non-metals and organic compound analysis) are also appearing in the recent literature. In this paper the 'state of the art', the last developments and the expectations in trying to circumvent the limitations of the ICP-AES (on the light of literature data and personal experience) are reviewed. (author)

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

    International Nuclear Information System (INIS)

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

    2011-01-01

    Highlights: → Use of a miniaturized analytical system with microtorch plasma for Hg determination. → Determination of Hg in non- and biodegradable materials using cold vapor generation. → Figures of merit and advantages of the miniaturized system for Hg determination. - Abstract: A new analytical system consisting of a low power capacitively coupled plasma microtorch (20 W, 13.56 MHz, 150 ml min -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).

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

    Science.gov (United States)

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

    2011-10-15

    A new analytical system consisting of a low power capacitively coupled plasma microtorch (20 W, 13.56 MHz, 150 ml min(-1) Ar) and a microspectrometer was investigated for the Hg determination in non- and biodegradable materials by cold-vapor generation, using SnCl(2) reductant, and atomic emission spectrometry. The investigated miniaturized system was used for Hg determination in recyclable plastics from electronic equipments and biodegradable materials (shopping bags of 98% biodegradable polyethylene and corn starch) with the advantages of easy operation and low analysis costs. Samples were mineralized in HNO(3)-H(2)SO(4) mixture in a high-pressure microwave system. The detection limits of 0.05 ng ml(-1) or 0.08 μg g(-1) in solid sample were compared with those reported for other analytical systems. The method precision was 1.5-9.4% for Hg levels of 1.37-13.9 mg kg(-1), while recovery in two polyethylene certified reference materials in the range 98.7 ± 4.5% (95% confidence level). Copyright © 2011 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-10-15

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

  16. Nanometric resolution in glow discharge optical emission spectroscopy and Rutherford backscattering spectrometry depth profiling of metal (Cr, Al) nitride multilayers

    International Nuclear Information System (INIS)

    Escobar Galindo, R.; Gago, R.; Fornies, E.; Munoz-Martin, A.; Climent Font, A.; Albella, J.M.

    2006-01-01

    In this work, we address the capability of glow discharge optical emission spectroscopy (GDOES) for fast and accurate depth profiling of multilayer nitride coatings down to the nanometer range. This is shown by resolving the particular case of CrN/AlN structures with individual thickness ranging from hundreds to few nanometers. In order to discriminate and identify artefacts in the GDOES depth profile due to the sputtering process, the layered structures were verified by Rutherford backscattering spectrometry (RBS) and scanning electron microscopy (SEM). The interfaces in the GDOES profiles for CrN/AlN structures are sharper than the ones measured for similar metal multilayers due to the lower sputtering rate of the nitrides. However, as a consequence of the crater shape, there is a linear degradation of the depth resolution with depth (approximately 40 nm/μm), saturating at a value of approximately half the thickness of the thinner layer. This limit is imposed by the simultaneous sputtering of consecutive layers. The ultimate GDOES depth resolution at the near surface region was estimated to be of 4-6 nm

  17. Internal standardization in atomic-emission spectrometry using inductively coupled plasma

    International Nuclear Information System (INIS)

    Moore, G.L.

    1985-01-01

    The principle of internal standardization has been used in quantitative analytical emission spectroscopy since 1925 to minimize the errors arising from fluctuations in sample preparation, excitation-source conditions, and detection parameters. Although modern spectroscopic excitation sources are far more stable and electronic detection methods are more precise than before, the system for the introduction of the sample in spectrometric analysis using inductively coupled plasma (ICP) introduces significant errors, and internal standardization can still play a useful role in improving the overall precision of the analytical results. The criteria for the selection of the elements to be used as internal standards in arc and spark spectrographic analysis apply to a much lesser extent in ICP-spectrometric analysis. Internal standardization is recommended for use in routine ICP-simultaneous spectrometric analysis to improve its accuracy and precision and to provide a monitor for the reassurance of the analyst. However, the selection of an unsuitable reference element can result in misuse of the principle of internal standardization and, although internal standardization can be applied when a sequential monochromator is used, the main sources of error will not be minimized

  18. Rapid determination of uranium in natural waters by fthermal emission mass spectrometry

    International Nuclear Information System (INIS)

    Ferguson, J.R.; Caylor, J.D.; Rogers, E.R.; Cole, S.H.

    1977-03-01

    A method has been developed to rapidly analyze natural water samples for part-per-trillion (ng/l) concentrations of uranium using a custom-built thermal-emission mass spectrometer. The filtered water sample is spiked with 233 U as an internal standard and extracted with a 2 percent solution of TOPO (trioctylphosphine oxide) in carbon tetrachloride. An aliquot of the organic phase is evaporated and the uranium in the residue extracted with aqueous ammonium carbonate. A 5j-μl aliquot is taken and dried on a flat uranium concentration of 3 ng/l will yield a count rate greater than three times the standard deviation, plus the mean of the background, and is defined as the lowest determinable concentration. The standard deviation of the method is 3 percent at accuracy of the method has been evaluated by comparing the results with a fluorescence procedure. There is very good agreement for water samples with uranium concentrations from 200 to 1000 ng/l. The mass spectrometer is a 6-in. -radius, 60-degree-sector instrument equipped for ion counting and having a vacuum system allowing rapid sample changing while maintaining a high source vacuum. A multiplexer and high-voltage s witch provide synchronized peak switching and scaler gating for monitoring three isotopes of uranium 238, 235, and 233. With this instrument, an analyst can achieve an analysis rate in excess of 50 samples per eight-hour shift

  19. Spectrometry and emission tomographic image reconstruction stimulated by neutrons via EM algorithm and Monte Carlo Method

    International Nuclear Information System (INIS)

    Viana, Rodrigo Sartorelo Salemi

    2014-01-01

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

  20. Pré-concentração de cádmio com Saccharomyces cerevisiae e determinação em águas fluviais usando espectrometria de emissão óptica com plasma indutivamente acoplado Preconcentration of cadmium with Saccharomyces cerevisiae and determination in river water using inductively coupled plasma optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    Priscila Andreoli Biscaro

    2007-04-01

    Full Text Available A preconcentration method based on the use of Saccharomyces cerevisiae as sorbent material is proposed for the determination of Cd(II in river water. The solid phase extraction was performed in batch mode and the determination of the analyte in the solid phase was easily carried out by introducing a slurry of the yeast (0.0625 g / 2.5 mL directly into the ICP OES. A limit of detection of 0.11 µg L-1 and a sample throughput in the range of 4 - 54 sample h-1 were obtained. Determinations of cadmium in a certified sample and in real river water samples were in excellent agreement with the expected values.

  1. Effects of airflow on odorants' emissions in a model pig house — A laboratory study using Proton-Transfer-Reaction Mass Spectrometry (PTR-MS)

    International Nuclear Information System (INIS)

    Saha, Chayan Kumer; Feilberg, Anders; Zhang, Guoqiang; Adamsen, Anders Peter S.

    2011-01-01

    Identification of different factors that affect emissions of gasses, including volatile organic compounds (VOCs) is necessary to develop emission abatement technology. The objectives of this research were to quantify and study temporal variation of gas emissions from a model pig house under varying ventilation rates. The used model was a 1:12.5 scale of a section of a commercial finishing pig house. The VOC concentrations at inlet, outlet, and slurry pit of the model space were measured using Proton-Transfer-Reaction Mass Spectrometry (PTR-MS). PTR-MS can measure the temporal variations of odor compounds' emission from the slurry pit in real time. The emissions of H 2 S and 14 VOCs were lower compared to real pig buildings except for ammonia, which indicated possible other sources of those compounds than the slurry in the slurry pit. The ventilation rate affected significantly on ammonia and trimethylamine emission (p 2 S) emission was independent of the ventilation rate. VFAs' emission dependency on ventilation rate increased with the increase of carbon chain. Phenols, indoles and ketones showed the positive correlation with ventilation rate to some extent. Generally, compounds with high solubility (low Henry's constant) showed stronger correlation with ventilation rates than the compounds with high Henry's constant.

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

    Science.gov (United States)

    Bağda, Esra; Altundağ, Hüseyin; Soylak, Mustafa

    2017-10-01

    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.

  3. Trace element determination using static high-sensitivity inductively coupled plasma optical emission spectrometry (SHIP-OES).

    Science.gov (United States)

    Engelhard, Carsten; Scheffer, Andy; Nowak, Sascha; Vielhaber, Torsten; Buscher, Wolfgang

    2007-02-05

    A low-flow air-cooled inductively coupled plasma (ICP) design for optical emission spectrometry (OES) with axial plasma viewing is described and an evaluation of its analytical capabilities in trace element determinations is presented. Main advantage is a total argon consumption of 0.6 L min(-1) in contrast to 15 L min(-1) using conventional ICP sources. The torch was evaluated in trace element determinations and studied in direct comparison with a conventional torch under the same conditions with the same OES system, ultrasonic nebulization (USN) and single-element optimization. A variety of parameters (x-y-position of the torch, rf power, external air cooling, gas flow rates and USN operation parameters) was optimized to achieve limits of detection (LOD) which are competitive to those of a conventional plasma source. Ionic to atomic line intensity ratios for magnesium were studied at different radio frequency (rf) power conditions and different sample carrier gas flows to characterize the robustness of the excitation source. A linear dynamic range of three to five orders of magnitude was determined under compromise conditions in multi-element mode. The accuracy of the system was investigated by the determination of Co, Cr, Mn, Zn in two certified reference materials (CRM): CRM 075c (Copper with added impurities), and CRM 281 (Trace elements in rye grass). With standard addition values of 2.44+/-0.04 and 3.19+/-0.21 microg g(-1) for Co and Mn in the CRM 075c and 2.32+/-0.09, 81.8+/-0.4, 32.2+/-3.9 for Cr, Mn and Zn, respectively, were determined in the samples and found to be in good agreement with the reported values; recovery rates in the 98-108% range were obtained. No influence on the analysis by the matrix load in the sample was observed.

  4. Determination of lead in bone tissues by axially viewed inductively coupled plasma multichannel-based emission spectrometry.

    Science.gov (United States)

    Grotti, Marco; Abelmoschi, Maria Luisa; Dalla Riva, Simona; Soggia, Francesco; Frache, Roberto

    2005-04-01

    A new procedure for determining low levels of lead in bone tissues has been developed. After wet acid digestion in a pressurized microwave-heated system, the solution was analyzed by inductively coupled plasma multichannel-based emission spectrometry. Internal standardization using the Co 228.615 nm reference line was chosen as the optimal method to compensate for the matrix effects from the presence of calcium and nitric acid at high concentration levels. The detection limit of the procedure was 0.11 microg Pb g(-1) dry mass. Instrumental precision at the analytical concentration of approximately 10 microg l(-1) ranged from 6.1 to 9.4%. Precision of the sample preparation step was 5.4%. The concentration of lead in SRM 1486 (1.32+/-0.04 microg g(-1)) found using the new procedure was in excellent agreement with the certified level (1.335+/-0.014 microg g(-1)). Finally, the method was applied to determine the lead in various fish bone tissues, and the analytical results were found to be in good agreement with those obtained through differential pulse anodic stripping voltammetry. The method is therefore suitable for the reliable determination of lead at concentration levels of below 1 microg g(-1) in bone samples. Moreover, the multi-element capability of the technique allows us to simultaneously determine other major or trace elements in order to investigate inter-element correlation and to compute enrichment factors, making the proposed procedure particularly useful for investigating lead occurrence and pathways in fish bone tissues in order to find suitable biomarkers for the Antarctic marine environment.

  5. Investigation of spectral interference effects on determination of uranium concentration in phosphate ore by inductively coupled plasma optical emission spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Bachari, Ayoob H.; Jalali, Fatemeh; Alahyarizadeh, Ghasem [Tehran Univ. (Iran, Islamic Republic of). Engineering Dept.

    2017-04-01

    Effects of spectral interferences on determination of the uranium concentration in phosphate ore were investigated by inductively coupled plasma optical emission spectroscopy (ICP-OES). Eleven high intensity emission lines including four lines recommended by ICP-OES apparatus were chosen to determine the uranium concentration. The ore samples were collected from phosphate acid producing industry in the south of Iran. Three different acid combinations [(HNO{sub 3}:HCl:HF-2:6:2), (H{sub 3}PO{sub 4}:H{sub 2}SO{sub 4}:HF-3:3:3), (HNO{sub 3}:H{sub 2}O{sub 2}:HF-4:2:2)] used in microwave digestion method to explore the spectral interference effects in different solvent environments. The results showed that the trusty uranium concentration, obtained in the 367.007 nm, 386.592 nm, 389.036 nm and 409.014 nm by second acid digestion method which were 0.665 ppm, 0.972 ppm, 0.670 ppm and 0.801 ppm, respectively. Although the line of 409.014 nm was reported as the best line for determining of the uranium concentration in several literatures, the results showed that this line has a significant spectral interference with vanadium in some ores which should be considered in determining of the uranium concentration. Spectral interference effects of some elements which have high concentrations in the phosphate ore including Ca, Fe, Mg, Pb, V, Mn, and Ti on the line intensities were also investigated. Results indicated that the chosen elements affect emission intensities of all of 11 lines. They also indicated that the line of 409.014 nm provides a trusty precision in the determination of the uranium concentration in the ore sample with low vanadium concentration (at least, U/V ratio of 1:5). Results show that the line of 409.014 nm provides acceptable precision with some corrections in comparison with other selected lines. For instance in high concentrations of other elements including Fe and Ti in the ore samples, strong influences on the line intensities of the 367.007 nm (by Fe

  6. Atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Haswell, S.J.

    1991-01-01

    Atomic absorption spectroscopy is now well established and widely used technique for the determination of trace and major elements in a wide range analyte types. There have been many advances in the atomic spectroscopy over the last decade and for this reason and to meet the demand, it was felt that there was a need for an updated book. Whilst interest in instrumental design has tended to dominate the minds of the spectrocopist, the analyst concerned with obtaining reliable and representative data, in diverse areas of application, has been diligently modifying and developing sample treatment and instrumental introduction techniques. Such methodology is de fundamental part of analysis and form the basis of the fourteen application chapters of this book. The text focuses in the main on AAS; however, the sample handling techniques described are in many cases equally applicable to ICP-OES and ICP-MS analysis. (author). refs.; figs.; tabs

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

    DEFF Research Database (Denmark)

    Laursen, Kristian Holst; Schjørring, Jan Kofod; Olesen, Jørgen Eivind

    2011-01-01

    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...

  8. [Pretreatment of Aluminum-Lithium Alloy Sample and Determination of Argentum and Lithium by Spectral Analysis].

    Science.gov (United States)

    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

  9. Formation and emission of PM10 in combustion of biofuels. Final report

    International Nuclear Information System (INIS)

    Johansson, Linda; Tullin, Claes; Leckner, Bo

    2004-02-01

    .g. soot). Submicron particles (particles less than 1 μm) dominated the emission, both with respect to mass and number. Analyses with EDX (Electron Dispersive X-ray), ICP-MS (Inductively Coupled Plasma Mass-Spectrometry), and IC (Ion-Chromatography) showed that the main components in the submicron particles were potassium, sulphur, chlorine, and oxygen. TOF-SIMS (Time-of-flight Secondary Ion Mass Spectrometry) analysis showed that potassium-sulphate followed by potassium chloride were the most dominant substances among alkali -sulphates -chlorides, and -carbonates. For morphology, many spherical particles around 0.1 μm were found. In the second part of the project, the formation of particles during bio-fuel combustion is studied by first measurements on metal release during biofuel combustion. Results from the first part of the project have shown that the particle emission is dominated by inorganic particles at favourable combustion conditions, and the second part is therefore focused on inorganic particles, in which metals are a part. The release of metals is studied to investigate the possibilities to influence formation of combustion particles, and consequently the particle emission. To be able to perform as many tests as possible and to include wide variations in combustion conditions, the second part of the project is carried out using a laboratory reactor. To obtain a time-resolved signal of the release of metals, a large number of single pellets were fired in a laboratory reactor and chemically analysed afterwards using ICP-OES (Inductively Coupled Plasma - Optical Emission Spectrometry). The combustion lapse was interrupted after devolatisation, and after 25 %, 50 %, and 75 % of the char burnout. To obtain a time resolved signal of the emission of unburnt particulate matter a photoelectric aerosol sensor was used as a soot indicator. The results of the initial tests show that the main part of the metals was released during char combustion, but a certain metal

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

    Science.gov (United States)

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

    2016-03-01

    The chemical composition of single particles deposited on industrial filters located in three different chimneys of an iron-manganese (Fe-Mn) alloy manufacturing plant have been compared using aerosol time-of-flight mass spectrometry (ATOFMS) and scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX). Very similar types of particles were observed using both analytical techniques. Calcium-containing particles dominated in the firing area of the sintering unit, Mn and/or Al-bearing particles were observed at the cooling area of the sintering unit, while Mn-containing particles were dominant at the smelting unit. SEM-EDX analysis of particles collected downstream of the industrial filters showed that the composition of the particles emitted from the chimneys is very similar to those collected on the filters. ATOFMS analysis of ore samples was also performed to identify particulate emissions that could be generated by wind erosion and manual activities. Specific particle types have been identified for each emission source (chimneys and ore piles) and can be used as tracers for source apportionment of ambient PM measured in the vicinity of the industrial site. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. Determination of Micro minerals in Milk from Farm and Pasture-reared Cow, Goat and Camel; using Inductively Coupled Plasma-Optical Emission Spectrometry

    OpenAIRE

    SirelkhatimBalla Elhardallou; Ashraf Yehia El-naggar

    2016-01-01

    This study covers raw fresh milk of cow, goat and camel (farm and pasture-reared),in addition to two brands of commercial milk samples, liquid milk of powder origin and drinking yoghurt samples. Camel milk showed a relatively lower pH range (6.15 - 6.46) compared cow, goat and commercial milk. The pH of drinking yoghurt was found (4.35 - 4.47).Microwave digestion, was selected followed by mineral analysis using Inductively Coupled Plasma-Optical Emission Spectrometry. Micro minerals; Cd, Cr...

  12. Semi-automated technique for the separation and determination of barium and strontium in surface waters by ion exchange chromatography and atomic emission spectrometry

    International Nuclear Information System (INIS)

    Pierce, F.D.; Brown, H.R.

    1977-01-01

    A semi-automated method for the separation and the analysis of barium and strontium in surface waters by atomic emission spectrometry is described. The method employs a semi-automated separation technique using ion exchange and an automated aspiration-analysis procedure. Forty specimens can be prepared in approximately 90 min and can be analyzed for barium and strontium content in 20 min. The detection limits and sensitivities provided by the described technique are 0.003 mg/l and 0.01 mg/l respectively for barium and 0.00045 mg/l and 0.003 mg/l respectively for strontium

  13. Use of oxidative and reducing vapor generation for reducing the detection limits of iodine in biological samples by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Vtorushina, Eh.A.; Saprykin, A.I.; Knapp, G.

    2009-01-01

    Procedures of microwave combustion in an oxygen flow and microwave acid decomposition of biological samples were optimized for the subsequent determination of iodine. A new method was proposed for the generation of molecular iodine from periodate iona using hydrogen peroxide as a reductant. Procedures were developed for determining iodine in biological samples by inductively coupled plasma atomic emission spectrometry (ICP-AES) using oxidative and reducing vapor generation; these allowed the detection limit for iodine to be lowered by 3-4 orders of magnitude. The developed procedures were used to analyze certified reference materials of milk (Skim Milk Powder BCR 150) and seaweed (Sea Lettuce BCR 279) and a Supradyn vitamin complex

  14. Determination of trace elements and screening of metalloproteins in human blood and tissues

    International Nuclear Information System (INIS)

    Prohaska, K.

    2003-02-01

    Sequential and simultaneous atomic spectrometric detection was applied for the determination of metals in human whole blood, blood fractions and joint tissues. For this purpose ICP-OES (inductively coupled plasma - optical emission spectrometry) and GFAAS (graphite furnace - atomic absorption spectrometry) were optimized. The nebulizing technique of the ICP-OES causes a high consumption of the sample (2.4 mL /min uptake rate). Using the simultaneous modus of measurement it is possible to determine up to 20 elements in the samples of interest. Using GFAAS the elements can be detected sequentially only, the method is more time consuming in comparison. For the direct sample injection into the graphite tube only 20 aeL are needed. Since 1 mL sample has to be filled in the sample vessel of the autosampler, up to six elements can be determined in this volume. The most important advantage of the simultaneous multi-element detection is the low sample consumption, which is essential for analysis of biological samples. Normally only small amounts of human blood or tissues can be collected, and the concentrations of analytes are usually very low. Therefore in many cases a sample preparation is of advantage, which enables a pre-concentration of the analyte. The sample digestion was optimized with respect to the possible pre-concentration of the analytes. Ashing of the freeze-dried blood enabled a six fold higher concentration in the measuring solution compared with wet digestion of blood. For the ICP-OES sample introduction system two different nebulizers were tested in the complex matrix of the digested blood samples. A Meinhard and the microconcentric nebulizer were compared according to their analytical performance. The matrix of the samples caused LODs three to five times higher than in the aqueous standards. The application of the Meinhard nebulizer enabled sufficiently low LODs in the matrix for some elements of interest (Ca, Cu, Fe, Mg, P, S, Zn in freeze-dried blood

  15. Thermoluminescence emission spectrometry of glass display in mobile phones and resulting evaluation of the dosimetric properties of a specific type of display glass

    International Nuclear Information System (INIS)

    Discher, Michael; Woda, Clemens

    2014-01-01

    Glass displays of mobile phones are sensitive to ionizing radiation and can be used for retrospective dosimetry for the purpose of triage after a radiological accident or attack. In this study the two main types of glass display that are used in modern mobile phones were investigated using thermoluminescence (TL) emission spectrometry. A different TL spectrum was observed for the glass display of category A (lime-aluminosilicate glass) and category B (boron-silicate glass). Based on the spectral measurements an optimized detection window was chosen to re-evaluate the dosimetric properties (dose response, optical and long-term stability) of glass display category B. - Highlights: • Two display glass types show similar TL emission peaks but with strongly different relative intensities. • The intrinsic background TL signal peaks at similar wavelengths as the radiation induced signal. • Dosimetric properties of one display glass type were re-evaluated using an optimized detection window

  16. 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

    Science.gov (United States)

    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

  17. Comparison of inductively coupled plasma mass spectrometry with inductively coupled plasma atomic emission spectrometry and instrumental neutron activation analysis for the determination of rare earth elements in Greek bauxites

    International Nuclear Information System (INIS)

    Ochsenkuehn-Petropoulou, Maria; Luck, Joachim

    1991-01-01

    Fore the determination of rare earth elements (REE) in bauxitic materials the techniques of inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and instrumental neutron activation analysis (INAA) were compared. In the NIST (National Institute of Standards and Technology) bauxites SRM 697 Dominican, and SRM 69 b Arkansas, the concentration of some REEs were determined. With the reference bauxite BX-N of the ARNT (Association Nationale de la Recherche Technique) the precision and accuracy of ICP-AES for the determination of REEs in bauxites was tested. Furthermore, Greek bauxites of the Parnassos-Giona area were investigated. In a comparison of the three methods it was possible to calculate from the data series the precision of each method, which showed that the tendency found in the deviations for the different REEs is in accordance with published values. Also the limits of detection for REEs in bauxites were calculated and found to be in the same range as those in the literature. (author)

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    Graphical abstract: -- Highlights: •We worked out ICP-MS method of Hf determination in Zr and Zr compounds. •We used NAA method as reference one. •We obtained pure zirconium matrix by ion exchange (Diphonix ® resin). •These permit to determine ≥1 × 10 −4 % Hf in Zr sample by ICP MS with good precision and accuracy. -- Abstract: Hafnium at the very low level of 1–8 ppm (in relation to zirconium) was determined in zirconium sulfate solutions (originating from investigations of the separation of ca. 44 ppm Hf from zirconium by means of the ion exchange method) by using three independent methods: inductively coupled plasma mass spectrometry (ICP MS), neutron activation analysis (NAA) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The results of NAA and ICP MS determinations were consistent with each other across the entire investigated range (the RSD of both methods did not exceed 38%). The results of ICP-AES determination were more diverse, particularly at less than 5 ppm Hf (RSD was significantly higher: 29–253%). The ion exchange method exploiting Diphonix ® resin proved sufficient efficiency in Zr–Hf separation when the initial concentration ratio of the elements ([Zr] 0 /[Hf] 0 ) ranged from 1200 to ca. 143,000

  19. 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

    International Nuclear Information System (INIS)

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

    2016-01-01

    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. - Highlights: • Similar composition for emitted particles as those collected on the chimney filters. • Emitted particles dominated by Ca-, Mn and/or Al-containing particles. • Identification of specific particle types emitted by the different process units. - The particles emitted by metallurgy activities are fully described by ATOFMS and SEM-EDX, enabling the identification of specific particle types from the different units of the process.

  20. In-situ determination of cross-over point for overcoming plasma-related matrix effects in inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

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

    2008-01-01

    A novel method is described for overcoming plasma-related matrix effects in inductively coupled plasma-atomic emission spectrometry (ICP-AES). The method is based on measurement of the vertically resolved atomic emission of analyte within the plasma and therefore requires the addition of no reagents to the sample solution or to the plasma. Plasma-related matrix effects enhance analyte emission intensity low in the plasma but depress the same emission signal at higher positions. Such bipolar behavior is true for all emission lines and matrices that induce plasma-related interferences. The transition where the enhancement is balanced by the depression (the so-called cross-over point) results in a spatial region with no apparent matrix effects. Although it would be desirable always to perform determinations at this cross-over point, its location varies between analytes and from matrix to matrix, so it would have to be found separately for every analyte and for every sample. Here, a novel approach is developed for the in-situ determination of the location of this cross-over point. It was found that the location of the cross-over point is practically invariant for a particular analyte emission line when the concentration of the matrix was varied. As a result, it is possible to determine in-situ the location of the cross-over point for all analyte emission lines in a sample by means of a simple one-step sample dilution. When the original sample is diluted by a factor of 2 and the diluted sample is analyzed again, the extent of the matrix effect is identical (zero) between the original sample and the diluted sample at one and only one location - the cross-over point. This novel method was verified with several single-element matrices (0.05 M Na, Ca, Ba and La) and some mixed-element matrices (mixtures of Na-Ca, Ca-Ba, and a plant-sample digest). The inaccuracy in emission intensity due to the matrix effect could be as large as - 30% for conventional measurements in the

  1. Study of the removal of cesium from aqueous solutions by graphene oxide; Estudo da remocao de cesio em solucoes aquosas por oxido de grafeno

    Energy Technology Data Exchange (ETDEWEB)

    Bueno, Vanessa N.; Rodrigues, Debora F. [University of Houston (UH), Houston, TX (United States); Vitta, Patricia B. Di [Universidade de Sao Paulo (STRES/USP), Sao Paulo, SP (Brazil). Inst. de Quimica. Setor Tecnico de Residuos Quimicos e Solventes; Oshiro, Mauricio T.; Vicente, Roberto; Hiromoto, Goro; Potiens Junior, Ademar; Sakata, Solange K., E-mail: sksakata@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2013-07-01

    Graphene oxide, used in this work, was synthesized from the oxidation of graphite by Hummer method. The experiments were performed in batch and analyzed for the following parameters: contact time, pH, cesium ion concentration in aqueous solution and removing capacity of the graphene oxide. After the experiments the samples were vacuum filtered and the remaining cesium in solution was quantified by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The equilibrium was reached after 60 minutes of contact in neutral solution. The percentage of removal was around 80%.

  2. Utilization of bromeliad Tillandsia Usneoides L. in biomonitoring of air pollution in the metropolitan region of Sao Paulo - SP, Brazil

    International Nuclear Information System (INIS)

    Albuquerque, Caroline R.; Figueiredo, Ana M.G.; Silva, Barbara C. da; Ticianelli, Regina B.; Figueira, Rubens C.L.; Ribeiro, Andreza P.

    2013-01-01

    In this study, it was determined the metals Cd, Cu, Fe, Mo, Ni, Pb and Sb in plant Tillandsia Usneoides L., an epiphyte species popularly known as old beard and able to absorb water and nutrients directly from air, aiming to estimate the contribution of human activities in atmospheric metal pollution in the metropolitan region of Sao Paulo. The samples were collected at five different points, located near the South West and stretches of highway Mario Covas (SP-21). The Neutron Activation Analysis (NAA) and Optical Emission Spectrometry with Inductively Coupled Plasma (ICP-OES) were the analytical techniques used in the quantification of metals of interest

  3. Digestão de óleo lubrificante encapsulado em forno de microondas com radiação focalizada por adição de amostra ao reagente pré-aquecido

    Directory of Open Access Journals (Sweden)

    Flavia A. Bressani

    2006-12-01

    Full Text Available The applicability of the recently proposed procedure based on gradual sample addition to microwave-assisted pre-heated concentrated acid is limited by the sample viscosity. In this work, lubricating oil samples with high viscosity were encapsulated and manually added to the microwave-assisted pre-heated concentrated digestion mixture. The procedure was applied for determination of Al, Ca, Cr, Cu, Fe, Mg, Ni, P, Pb, Si, Sn, Sr, V, W, and Zn in lubricating oil by inductively coupled plasma optical emission spectrometry (ICP OES. Determined and certified values for Ca, Mg, P, and Zn in lubricating oil were in agreement at a 95% confidence level.

  4. Visualisation of axolotl blastema cells and pig endothelial progenitor cells using very small super paramagnetic iron oxide particles in MRI: A technique with applications for non invasive visualisation of regenerative processes

    DEFF Research Database (Denmark)

    Lauridsen, Henrik; Kjær, N.B.; Bek, Maria

    oxide particles (VSOP) in animal cells enable non invasive cell tracking using magnetic resonance imaging (MRI) and can prove useful, when visualising regenerative processes. This study examines the possibility of labelling limited numbers of axolotl blastema cells (aBC) and pig endothelial progenitor...... implanted in live axolotl tail and dead porcine heart, respectively. Cellular iron uptake was determined using inductively coupled plasma optical emission spectrometry (ICP-OES). Results: T2*-weighted 2D gradient-echo sequences on samples of 10˄5 cells yielded at significant linear correlations between...

  5. Utilization of bromeliad Tillandsia Usneoides L. in biomonitoring of air pollution in the metropolitan region of Sao Paulo - SP, Brazil; Utilizacao da bromelia Tillandsia Usneoides L. no biomonitoramento da poluicao atmosferica na Regiao metropolitana de Sao Paulo - SP, Brasil

    Energy Technology Data Exchange (ETDEWEB)

    Albuquerque, Caroline R.; Figueiredo, Ana M.G.; Silva, Barbara C. da; Ticianelli, Regina B., E-mail: calbuuquerque@gmail.com, E-mail: anamaria@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Figueira, Rubens C.L., E-mail: aportellar@yahoo.com.br [Universidade de Sao Paulo (USP), Sao Paulo, SP (Brazil). Instituto Oceanografico; Nievola, Catarina C.; Alves, Edenise S.; Domingos, Marisa, E-mail: ccnievola@uol.com.br, E-mail: ealves@ibot.sp.gov.br, E-mail: mmingos@superig.com.br [Instituto de Botanica (IBt-SMA/SP), Sao Paulo, SP (Brazil); Ribeiro, Andreza P., E-mail: andrezp@uninove.br [Universidade Nove de Julho (UNINOVE), Sao Paulo, SP (Brazil)

    2013-07-01

    In this study, it was determined the metals Cd, Cu, Fe, Mo, Ni, Pb and Sb in plant Tillandsia Usneoides L., an epiphyte species popularly known as old beard and able to absorb water and nutrients directly from air, aiming to estimate the contribution of human activities in atmospheric metal pollution in the metropolitan region of Sao Paulo. The samples were collected at five different points, located near the South West and stretches of highway Mario Covas (SP-21). The Neutron Activation Analysis (NAA) and Optical Emission Spectrometry with Inductively Coupled Plasma (ICP-OES) were the analytical techniques used in the quantification of metals of interest.

  6. Surface modification-a novel way of attaching cocatalysts on CdS semiconductors for photocatalytic hydrogen evolution

    KAUST Repository

    Yu, Weili

    2014-08-22

    Noble metals as cocatalysts for hydrogen evolution are widely investigated for semiconductor photocatalytic water splitting. In this paper, we present a novel way to attach not only noble metals, but also transitional metals onto CdS nanocrystals as cocatalysts for hydrogen evolution. The hydrogen evolution performances for each metal were compared and result shows that Pd attached CdS gives the highest hydrogen evolution rate of 250 μmol/h. The amounts of metal ions attached on the surface were measured by inductively coupled plasma optical emission spectrometry (ICP-OES). This work confirms that surface modification is a promising way of attaching cocatalysts onto semiconductor photocatalysts.

  7. Surface modification-a novel way of attaching cocatalysts on CdS semiconductors for photocatalytic hydrogen evolution

    KAUST Repository

    Yu, Weili; Isimjan, Tayirjan; Lin, Bin; Takanabe, Kazuhiro

    2014-01-01

    Noble metals as cocatalysts for hydrogen evolution are widely investigated for semiconductor photocatalytic water splitting. In this paper, we present a novel way to attach not only noble metals, but also transitional metals onto CdS nanocrystals as cocatalysts for hydrogen evolution. The hydrogen evolution performances for each metal were compared and result shows that Pd attached CdS gives the highest hydrogen evolution rate of 250 μmol/h. The amounts of metal ions attached on the surface were measured by inductively coupled plasma optical emission spectrometry (ICP-OES). This work confirms that surface modification is a promising way of attaching cocatalysts onto semiconductor photocatalysts.

  8. Study of the removal of cesium from aqueous solutions by graphene oxide

    International Nuclear Information System (INIS)

    Bueno, Vanessa N.; Rodrigues, Debora F.; Vitta, Patricia B. Di

    2013-01-01

    Graphene oxide, used in this work, was synthesized from the oxidation of graphite by Hummer method. The experiments were performed in batch and analyzed for the following parameters: contact time, pH, cesium ion concentration in aqueous solution and removing capacity of the graphene oxide. After the experiments the samples were vacuum filtered and the remaining cesium in solution was quantified by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The equilibrium was reached after 60 minutes of contact in neutral solution. The percentage of removal was around 80%

  9. Measurement of non-enteric emission fluxes of volatile fatty acids from a California dairy by solid phase micro-extraction with gas chromatography/mass spectrometry

    Science.gov (United States)

    Alanis, Phillip; Sorenson, Mark; Beene, Matt; Krauter, Charles; Shamp, Brian; Hasson, Alam S.

    Dairies are a major source of volatile organic compounds (VOCs) in California's San Joaquin Valley; a region that experiences high ozone levels during summer. Short-chain carboxylic acids, or volatile fatty acids (VFAs), are believed to make up a large fraction of VOC emissions from these facilities, although there are few studies to substantiate this. In this work, a method using a flux chamber coupled to solid phase micro-extraction (SPME) fibers followed by analysis using gas chromatography/mass spectrometry was developed to quantify emissions of six VFAs (acetic acid, propanoic acid, butanoic acid, pentanoic acid, hexanoic acid and 3-methyl butanoic acid) from non-enteric sources. The technique was then used to quantify VFA fluxes from a small dairy located on the campus of California State University Fresno. Both animal feed and animal waste are found to be major sources of VFAs, with acetic acid contributing 70-90% of emissions from the sources tested. Measured total acid fluxes during spring (with an average temperature of 20 °C) were 1.84 ± 0.01, 1.06 ± 0.08, (1.3 ± 0.5) × 10 -2, (1.7 ± 0.2) × 10 -2 and (1.2 ± 0.5) × 10 -2 g m -2 h -1 from silage, total mixed rations, flushing lane, open lot and lagoon sources, respectively. VFA emissions from the sources tested total 390 ± 80 g h -1. The data indicate high fluxes of VFAs from dairy facilities, but differences in the design and operation of dairies in the San Joaquin Valley as well as seasonal variations mean that additional measurements must be made to accurately determine emissions inventories for the region.

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

    Science.gov (United States)

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

    2006-07-01

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    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

  12. Determination of Cu, Zn, Pb and Cd by atomic emission spectrometry with inductively coupled plasma in waters and sediments from San Juan Ecosystem, Santiago de Cuba

    International Nuclear Information System (INIS)

    Argota Perez, George; Argota Coello, Humberto; Fernandez-Heredia, Angel

    2014-01-01

    In this paper the levels of concentration of copper, zinc, lead and cadmium in waters and sediments from the ecosystem San Juan in the Santiago of Cuba province were evaluated. Two sampling of the ecosystem in two stations belonging to the high and middle part of the river, in rainy and little rainy periods were carried out. The conservation and treatment of the samples were developed according to established standards and the determinations of the elements were realized using atomic emission spectrometry with inductively coupled plasma. The concentrations intervals of the studied elements were established so much in the superficial waters like in the sediments and it was demonstrated that exists statistical significant differences for the factors station, period and type of sample, being the middle part of the river, the little rainy period and the sediments, where the grater concentrations of the pollutants appear

  13. Critical comparison of performances of inductively coupled plasma atomic emission spectrometry and neutron activation analysis for the determination of elements in human lungs

    International Nuclear Information System (INIS)

    Alimonti, A.; Coni, E.; Caroli, S.; Sabbioni, E.; Nicolaou, G.E.; Pietra, R.

    1989-01-01

    A study was carried out to assess the performance of inductively coupled plasma atomic emission spectrometry (ICP-AES) and neutron activation analysis (NAA) techniques for determining reference values for Al, Cd, Cr, Cu, Mg, Mn, V and Zn in human lungs of urban non-smoking subjects. Experimental data were subjected to the usual basic statistical tests to evaluate the respective merits of the two basically different analytical techniques. Both approaches, if used under carefully optimised experimental conditions, can yield reliable results affected only minimally by systematic and random errors. On the other hand, on a more routine basis, particular attention should be paid to elements such as Al, Cd and V which may pose some problems with both techniques. (author)

  14. Curve resolution and figures of merit estimation for determination of trace elements in geological materials by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Lorber, A.; Harel, A.; Goldbart, Z.; Brenner, I.B.

    1987-01-01

    In geochemical analysis using inductively coupled plasma atomic emission spectrometry (ICP-AES), spectral interferences and background enhancement in response to sample concomitants are the main cause of deterioration of the limit of detection (LOD) and inaccuracy of the determination at the trace and minor element levels. In this account, the authors describe the chemometric procedure of curve resolution for compensating for these sources of error. A newly developed method for calculating figures of merit is used to evaluate the correction procedure, test the statistical significance of the determined concentration, and determine LODs for each sample. The technique involves scanning the vicinity of the spectral line of the analyte. With prior knowledge of potential spectral interferences, deconvolution of the overlapped response is possible. Analytical data for a wide range of geological standard reference materials demonstrate the effectiveness of the chemometric techniques. Separation of 0.002 nm spectral coincidence, employing a 0.02 nm resolution spectrometer, is demonstrated

  15. Electronic structure and photocatalytic activity of wurtzite Cu–Ga–S nanocrystals and their Zn substitution

    KAUST Repository

    Kandiel, Tarek; Anjum, Dalaver H.; Sautet, Philippe; Le Bahers, Tangui; Takanabe, Kazuhiro

    2015-01-01

    by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), diffuse reflectance spectroscopy (DRS), photoluminescence (PL), and inductively coupled plasma atomic emission spectroscopy (ICP-OES). Electronic

  16. Recent advances in nuclear techniques for environmental radioactivity monitoring

    International Nuclear Information System (INIS)

    Kumar, Ajay; Tripathi, R.M.

    2016-01-01

    The environmental radioactivity monitoring was first started in the late 1950s following the global fallout from testing of nuclear weapons in the atmosphere. Nuclear analytical techniques are generally classified into two categories: destructive and non-destructive. Destructive techniques are carried out through several analytical methods such as α-spectrometry, liquid Scintillation counting system, solid state nuclear track detector, spectrophotometry, fluorimetry, atomic absorption spectrometry (AAS), inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma optical emission spectrometry (ICP-OES), chromatography techniques, electro-analytical techniques etc. However, nondestructive methods include gamma spectrometry, X-Ray fluorescence (XRF) spectrometry, neutron activation analysis (NAA) etc. The development of radiochemical methods and measurement techniques using alpha and gamma spectrometry have been described in brief

  17. An evaluation of inductively coupled plasma optical emission spectrometry using electrothermal atomisation sample introduction and photographic plate detection

    International Nuclear Information System (INIS)

    Khathing, D.T.; Pickford, C.J.

    1984-05-01

    A photographic radiation measurement approach has been used with an inductively coupled plasma source to evaluate and tabulate the more prominent optical emission lines of 66 elements. Compared with the more common sample introduction technique using nebulisation, increased sensitivity for multielement analysis of small samples was achieved by using a simple graphite electrothermal atomisation system. This was constructed to serve as a dual purpose atomiser ie both for Atomic Absorption and for Inductively Coupled Plasma Emission spectroscopy. The system offers the advantage of a wide multi-elemental coverage, but sensitivities achieved with photographic detection are poorer than those obtained photoelectrically. (author)

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

    Science.gov (United States)

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

    2004-12-01

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

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

    Science.gov (United States)

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

    2016-04-01

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

  20. Development of a high energy resolution magnetic bolometer for the determination of photon emission intensities by gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Rodrigues, M.

    2007-12-01

    In this research thesis, a first chapter describes the metrological difficulties for the determination of radionuclide photon emission intensities. Then, it discusses the understanding and the required tools for the computing of a magnetic bolometer signal with respect to the different operation parameters and to the sensor geometry. The author describes the implementation of the experimental device and its validation with a first sensor. The new sensor is then optimised for the measurement of photon emission intensities with a good efficiency and a theoretical energy resolution less than 100 eV up to 200 keV. The sensor's detection efficiency and operation have been characterized with a 133 Ba source. The author finally presents the obtained results

  1. Development of inductively coupled plasma atomic emission spectrometry for palladium and Rhodium determination in platinum-based alloy

    International Nuclear Information System (INIS)

    Kovacevic, R.; Todorovic, M.; Manojlovic, D.; Mutic, J.

    2008-01-01

    Inductively coupled plasma atomic emission spectroscopy with internal standardization was applied for the analysis of an in-house reference platinum alloy containing palladium and rhodium (approximately 5% by weight). In order to compensate for variations in signal recovery due to matrix interferences, and therefore to improve the precision, platinum. the major component, was chosen as an internal standard. Quantitative analysis was based on calibration using a set of matrix-matched calibration standards with and without employing the internal standard. These results were compared with those obtained by X-ray fluorescence spectroscopy. The results for both techniques were in a good agreement, although the precision was slightly better in the inductively coupled plasma atomic emission spectroscopy technique, with or without the internal standard

  2. Analysis of nickel-base alloys by Grimm-type glow discharge emission and x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Ferreira, N.P.; Strauss, J.A.; Van Maarseveen, I.; Ivanfy, A.B.

    1985-01-01

    Nickel-base alloys can be analysed as satisfactorily as steels by XRF as well as by the Grimm-type source, in spite of problems caused by element combinations, spectral line overlap and the influence of the structure and heat conduction properties on sputtering in the glow discharge source. This extended abstract briefly discusses the use of Grimm-type glow discharge emission and XRF as techniques for the analysis of nickel-base alloys

  3. Preconcentration of uranium in water samples using dispersive liquid-liquid micro- extraction coupled with solid-phase extraction and determination with inductively coupled plasma-optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    M. Rezaee,

    2015-10-01

    Full Text Available A new liquid phase microextraction method based on the dispersion of an extraction solvent into aqueous phase coupled with solid-phase extraction was investigated for the extraction, preconcentration and determination of uranium in water samples. 1-(2-Pyridylazo-2-naphthol reagent (PAN at pH 6.0 was used as a chelating agent prior to extraction. After concentration and purification of the samples in SPE C18 sorbent, 1.5 mL elution sample containing 40.0 µL chlorobenzene was injected into the 5.0 mL pure water. After extraction and centrifuging, the sedimented phase was evaporated and the residue was dissolved in nitric acid (0.5 M and was injected by injection valve into the ICP-OES. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition were studied and optimized. Under the optimum conditions, the calibration graph was linear in the range of 0.5-500 µg L-1. The detection limit was 0.1 µg L-1. The relative standard deviation (RSD at 5.0 µg L-1 concentration level was 6.6%. Finally, the developed method was successfully applied to the extraction and determination of uranium in the well, river, mineral, waste and tap water samples and satisfactory results were obtained.DOI: http://dx.doi.org/10.4314/bcse.v29i3.4

  4. Plasma-related matrix effects in inductively coupled plasma--atomic emission spectrometry by group I and group II matrix-elements

    International Nuclear Information System (INIS)

    Chan, George C.-Y.; Chan, W.-T.

    2003-01-01

    The effects of Na, K, Ca and Ba matrices on the plasma excitation conditions in inductively coupled plasma-atomic emission spectrometry (ICP-AES) were studied. Normalized relative intensity was used to indicate the extent of the plasma-related matrix effects. The group I matrices have no effects on the plasma excitation conditions. In contrast, the group II matrices depress the normalized relative intensities of some spectral lines. Specifically, the Group II matrices have no effects on the normalized relative intensity of atomic lines of low upper energy level (soft lines), but reduce the normalized relative intensity of some ionic lines and atomic lines of high energy level (hard lines). The Group II matrices seem to shift the Saha balance of the analytes only; no shift in the Boltzmann balance was observed experimentally. Moreover, for some ionic lines with sum of ionization and excitation potentials close to the ionization potential of argon (15.75 eV), the matrix effect is smaller than other ionic lines of the same element. The reduced matrix effects may be attributed qualitatively to charge transfer excitation mechanism of these ionic lines. Charge transfer reaction renders ionic emission lines from the quasi-resonant levels similar in characteristics of atomic lines. The contribution of charge transfer relative to excitation by other non-specific excitation mechanisms (via Saha balance and Boltzmann balance) determines the degree of atomic behavior of a quasi-resonant level. A significant conclusion of this study is that plasma-related matrix effect depends strongly on the excitation mechanism of a spectral line. Since, in general, more than one excitation mechanism may contribute to the overall excitation of an emission line, the observed matrix effects reflect the sum of the effects due to individual excitation mechanisms. Excitation mechanisms, in addition to the often-used total excitation energy, should be considered in matrix effect studies

  5. Reliability of graphite furnace atomic absorption spectrometry as ...

    African Journals Online (AJOL)

    spectrometry as alternative method for trace analysis of ... Purpose: To evaluate the comparative efficiency of graphite furnace atomic absorption spectrometry .... Methods comparison and validation .... plasma-optical emission spectrometry.

  6. Examining Heavy Metals in Acid Mine Drainage Wetlands in Western Pennsylvania through the use of Inductively Coupled Plasma Optical Emission Spectroscopy and Drone Aerial Photography.

    Science.gov (United States)

    Santoro, N.; Mount, G.

    2017-12-01

    Acid mine drainage (AMD) emanating from three abandoned mines feed an estimated 126 pounds of iron per day into the Tanoma remediation wetlands located in Tanoma, Pennsylvania. Along with the iron released into the system, 1500-2800 gallons of AMD per minute is seasonally discharged into the passive system. This high rate of discharge produces areas of high velocity flow that scour the wetland bottom moving precipitants and destroying vegetation roots. Although the discharge into Tanoma is known to be damaging, other discharges to surface waters have shown iron and heavy metal concentrations several times higher, and are left untreated to enter reservoir systems. This draws attention to these remediation sites, the processes used to treat them, and the effectiveness of each site. With most of the research that's been conducted in the AMD remediation field relating to in-lab experiments on iron concentrations, there is very little information in the literature about the effects of these large influxes of heavy metals and the effects it has on the biodiversity and methane production within a AMD remediation site. This research investigates the presence and concentration of heavy metals with the treatment wetland and other surface water sources using inductively coupled plasma optical emission spectroscopy (ICP-OES) and drone based aerial photography. Furthermore, our ICP data is compared with biodiversity patterns and methane levels within the Tanoma AMD site to identify relationships and the potential effect they have on the productivity and effectiveness of the remediation site through time.

  7. Determination of As, Cd, Hg and Pb in continuous use drugs and excipients by plasma-based techniques in compliance with the United States Pharmacopeia requirements

    Science.gov (United States)

    da Silva, Caroline Santos; Pinheiro, Fernanda Costa; do Amaral, Clarice Dias Britto; Nóbrega, Joaquim Araújo

    2017-12-01

    Some inorganic impurities are toxic to human health even when present at low concentrations and therefore must be carefully monitored in products as continuous use drugs. This work aimed the development of a simple microwave-assisted digestion procedure for different types of drugs and excipients and the analytical determination of elemental impurities according to the new regulations of the United States Pharmacopeia (USP) 232 and 233 using inductively coupled plasma optical emission spectrometry (ICP-OES) or inductively coupled plasma mass spectrometry (ICP-MS). Eight drugs samples and two excipients of different brands were microwave-assisted digested with inverse aqua regia. Addition and recovery experiments were performed according to J values, once permissible daily exposure value is specific for each element and estimated according to the maximum daily dose of drug indicated by the label. Samples were spiked with values of 1.5J in order to check accuracies for As, Cd, Hg, and Pb. Recoveries obtained by ICP-OES ranged from 75 to 148% and for ICP-MS ranged from 74 to 120%. The limits of detection for ICP-OES ranged from 0.4 to 17 mg kg- 1 and for ICP-MS from 7.4 to 41.6 μg kg- 1. Both analytical methods were adequate in terms of accuracies and sensitivities. Considering the maximum daily dose, all drugs samples and excipients contained As, Cd, Hg and Pb below the maximum limits stipulated by USP since all of them presented contents below respective limits of detection.

  8. Nature of unresolved complex mixture in size-distributed emissions from residential wood combustion as measured by thermal desorption-gas chromatography-mass spectrometry

    Science.gov (United States)

    Hays, Michael D.; Smith, N. Dean; Dong, Yuanji

    2004-08-01

    Unresolved complex mixture (UCM) is an analytical artifact of gas chromatographs of combustion source-related fine aerosol extracts. In this study the UCM is examined in size-resolved fine aerosol emissions from residential wood combustion. The aerosols are sorted by size in an electrical low-pressure impactor (ELPI) and subsequently analyzed by thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS). A semiquantitative system for predicting the branched alkane, cycloalkane, alkylbenzene, C3-, C4-, C5-alkylbenzene, methylnaphthalene, C3-, C4-, C5-alkylnaphthalene, methylphenanthrene C2-, C3-alkylphenanthrene, and dibenzothiophene concentrations in the UCM is introduced. Analysis by TD/GS/MS detects UCM on each ELPI stage for all six combustion tests. The UCM baseline among the different fuel types is variable. In particular, the UCM of Pseudotsuga sp. is enriched in later-eluting compounds of lower volatility. A high level of reproducibility is achieved in determining UCM areas. UCM fractions (UCM ion area/total extracted ion chromatograph area) by individual ELPI stage return a mean relative standard deviation of 19.1% over the entire combustion test set, indicating a highly consistent UCM fraction across the ELPI size boundaries. Among the molecular ions investigated, branched alkane (m/z 57) and dibenzothiophene (m/z 212 and 226) constituents are most abundant in UCM emissions from RWC, collectively accounting for 64-95% of the targeted chemical species. The total UCM emissions span 446-756 mg/kg of dry biomass burned and correspond to an upper limit of 7.1% of the PM2.5 mass. The UCM emissions are primarily accumulation mode (0.1 μm ≤ aerodynamic diameter (da) ≤ 1 μm), with a geometric mean diameter (dg) range of 120.3-518.4 nm. UCM in PM2.5 is chemically asymmetric (shifted to finer da), typically clustering at da ≤ 1 μm. Measurable shifts in dg and changes in distribution widths (σg) on an intratest basis suggest that the particle density

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-03-01

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

  10. Evaluation of slurry preparation procedures for the determination of mercury by axial view inductively coupled plasma optical emission spectrometry using on-line cold vapor generation

    International Nuclear Information System (INIS)

    Santos, Eder Jose dos; Herrmann, Amanda Beatriz; Antunes Vieira, Mariana; Azzolin Frescura, Vera Lucia; Curtius, Adilson Jose

    2005-01-01

    Five different slurry preparation procedures were tested, after grinding the solid samples to a particle size ≤53 μm: (1) using aqua regia plus HF, 30 min of sonication, standing time of 24 h followed by another 30 min of sonication; (2) same as the previous one, except that the standing time and the second ultrasound treatment were omitted; (3) same as the previous one, except that HF was not used; (4) same as the previous one, except that the aqua regia was replaced by nitric acid; (5) same as the previous one, except that the acid nitric was replaced by tetramethylammonium hydroxide (TMAH). The Hg vapor was generated on-line, and the emission signal intensity measured at 253.652 nm by axial view inductively coupled plasma optical emission spectrometry. Initially, four experimental conditions were optimized using a multivariate factorial analysis: the concentrations of HCl and of the reducing agent, NaBH 4 , used in the cold vapor generation, and two instrumental parameters, the plasma radiofrequency power and the carrier gas flow rate. The radiofrequency power was statistically significant, but limited to 1.2 kW for practical reasons. The procedures were applied to 11 biological and environmental materials. Both, the slurries and the filtrates were analyzed, using calibration solutions in the same medium as in the slurries. The first three procedures produced results in agreement with the certified values. The two last procedures, using nitric acid or TMHA could not be used for quantitative analysis. For practical reasons, Procedure 3, with a detection limit (3s, n=10) of 0.06 μg g -1 for a sample mass of 20 mg in a final volume of 15 mL is recommended. The relative standard deviations for mercury in the investigated materials, using the recommended procedure, were lower than 12.5%, indicating a good precision for slurry sampling. The recommended procedure is simple, rapid and robust

  11. On-line digestion in a focused microwave-assisted oven for elements determination in orange juice by inductively coupled plasma optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    Fili Sabrina P.

    2003-01-01

    Full Text Available A flow injection system coupled to focused microwave-assisted oven was used for on-line orange juice sample digestion for determination of Ca, Cu, Fe, K, Mg, Mn, Na, P, and Zn by inductively coupled plasma optical emission spectrometry. The reactor coil was a PTFE tube (4.0 m long and 1.6 mm i.d. positioned into the commercial glass tube of the focused microwave oven. Aliquots of 500 muL of sample and 1000 muL of reagent (80% v/v HNO3 were mixed in a confluence and carried out to the reactor coil by air carrier. The relative standard deviation for five replicates of sample was lower than 5.0%. Good recoveries varying from 91 to 111% were obtained for added concentrations of the interest elements. The results obtained using the proposed digestion system are in agreement with those obtained for total digestion at the 95% confidence level. With this on-line digestion system was possible to carry out 12 samples h-1, minimizing contamination, saving consumption of samples and reagent and low residue generation.

  12. Preconcentration of uranium, thorium, zirconium, titanium, molybdenum and vanadium with oxine supported on microcrystalline naphthalene and their determinations by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Naveen Kumar, P.; Sanjay Kumar; Vijay Kumar; Nandakishore, S.S.; Bangroo, P.N.

    2013-01-01

    A sensitive and rapid method for the determination of uranium, thorium, zirconium, titanium, molybdenum and vanadium by inductively coupled plasma atomic emission spectrometry (ICP-AES) after solid-liquid extraction with microcrystalline naphthalene is developed. Analytes were quantitatively adsorbed as their oxinate complexes on naphthalene and determined by ICP-AES after stripping with 2 M HCl. The effect of various experimental parameters such as pH, reagent amounts, naphthalene amount and stripping conditions on the determination of these elements was investigated in detail. Under the optimized experimental conditions, the detection limits of this method for U (VI), Th (IV), Zr (IV), Ti (IV), Mo (VI) and V (V) were 20.0 ng mL -1 and the relative standard deviations obtained for three replicate determinations at a concentration of 1.0 µg mL -1 were 1.5-3.0%. The proposed method has been applied in the analysis of SY-2, SY-3 and pre-analysed samples for U, Th, Zr, Ti, Mo and V the analytical results are in good agreement with recommended values. (author)

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

    International Nuclear Information System (INIS)

    Matusiewicz, Henryk; Golik, Bartosz

    2004-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Matusiewicz, Henryk E-mail: Henryk.Matusiewicz@put.poznan.pl; Golik, Bartosz

    2004-05-21

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-12-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-01-16

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

  17. Simultaneous Pre-Concentration of Cadmium and Lead in Environmental Water Samples with Dispersive Liquid-Liquid Microextraction and Determination by Inductively Coupled Plasma-Atomic Emission Spectrometry

    Directory of Open Access Journals (Sweden)

    M. Salahinejad

    2013-06-01

    Full Text Available The dispersive liquid–liquid microextraction (DLLME method for determination of Pb+2 and Cd+2 ions in the environmental water samples was combined with inductively coupled plasma-atomic emission spectrometry (ICP-AES. Ammonium pyrrolidine dithiocarbamate (APDC, chloroform and ethanol were used as chelating agent, extraction solvent and disperser solvent, respectively. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters included extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH, sample volume and amount of the chelating agent.   Under the optimum conditions, the enrichment factor of 75 and 105 for Cd+2 and Pb+2 ions respectively was obtained from only 5.00mL of water sample. The detection limit (S/N=3 was 12 and 0.8ngmL−1 for Pb and Cd respectively. The relative standard deviation (RSDs for five replicate measurements of 0.50 mgL−1 of lead and cadmium was 6.5 and 4.4 % respectively. Mineral, tap, river, sea, dam and spiked water samples were analyzed for Cd and Pb amount.

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

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-06-01

    A novel method was developed for the determination of calcium, magnesium, potassium, iron, copper, zinc, and manganese and phosphorous in various kinds of breads samples sold in Turkey by microwave plasma-atomic emission spectrometry (MIP-AES). Breads were dried at 100 °C for one day, ground thoroughly and then digested using nitric acid/hydrogen per oxide (3:1). The analytes in certified reference wheat flour and maize flour samples were determined in the uncertainty limits of the certified values as well as the analytes added to the mixture of ground bread and acid mixture prior to digestion were recovered quantitatively (>90%). Therefore, all determinations were made by linear calibration technique using aqueous standards. The LOD values for Ca, Cu, Fe, K, Mg, Mn, P and Zn were 13.1, 0.28, 4.47, 118, 1.10, 0.41, 7550 and 3.00 ng mL(-1), respectively. No spectral interference was detected at the working wavelengths of the analytes. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Application of particle-induced X-ray emission, backscattering spectrometry and scanning electron microscopy in the evaluation of orthodontic materials

    International Nuclear Information System (INIS)

    Gihwala, D.; Mars, J.A.; Pineda-Vargas, C.

    2013-01-01

    The focus of this investigation was on orthodontic materials used in the manufacture of dental brackets. The properties of these dental materials are subjected to various physical parameters such as elongation, yield strength and elasticity that justify their application. In turn, these parameters depend on the quantitative elemental concentration distribution (QECD) in the materials used in the manufacture. For compositional analysis, proton-induced X-ray emission (PIXE), backscatter spectrometry (BS) and scanning electron microscopy (SEM) were applied. QECD analysis was performed to correlate the physical parameters with the composition and to quantify imperfections in the materials. PIXE and BS analyses were performed simultaneously with a 3 MeV proton beam while electrons accelerated at 25 keV were used for the SEM analysis. From the QECDs it was observed that: (1) the major elements Cr, Fe and Ni were homogeneously distributed in the orthodontic plate; (2) the distribution of Mo and O correlated with one another; (3) there was a spread of Cr around regions of high C concentration; and, (4) areas of high concentrations of Mo and O corresponded to a decrease in C concentrations. Elemental concentration correlations are shown to indicate the similarities and differences in the ease of formation of phases, based on the tangent of linearity. (author)

  20. Investigation into spatial distribution of macroelements in dried drops of albumins and proteins by the methods of atomic-emission multichannel spectrometry

    International Nuclear Information System (INIS)

    Chin', N.Kh.; Zazhogin, A.P.; Bulojchik, Zh.I.; Tanin, A.L.; Pashkovskaya, I.D.; Nechipurenko, N.I.

    2011-01-01

    Based on local analysis of the line intensities of Al, Ca, Mg, and Zn in spectra for the samples of dried drops of egg albumin, the possibility for estimation of the spatial elemental distribution by the drop diameter was demonstrated using the atomic-emission multichannel spectrometry method. It was found that with an increase in the concentration of the elements with a high diffusion coefficient (Ca) diffusion counteracts their carry-over to the boundary of evaporating drops, simultaneously displacing the salts of other elements (Al, Fe, Zn) to the drop periphery. This work shows that excitation of the analyzed surface of a dried protein drop by double laser pulses enables a semi-quantitative estimation of the distribution of essential elements by the drop radius. Such investigations look very promising in search for markers of various diseases and in the development of methods revealing the pathological processes at the preclinical stage, making it possible to look for the causes of the elemental unbalance, to realize a targeted selection of preparations and active additives, to correct the treatment course. (authors)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-02-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-03-03

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

  3. Fully automated dissolution and separation methods for inductively coupled plasma atomic emission spectrometry rock analysis. Application to the determination of rare earth elements

    International Nuclear Information System (INIS)

    Govindaraju, K.; Mevelle, G.

    1987-01-01

    In rock analysis laboratories, sample preparation is a serious problem, or even an enormous bottleneck. Because this laboratory is production-oriented, this problem was attacked by automating progressively, different steps in rock analysis for major, minor and trace elements. This effort has been considerably eased by the fact that all sample preparation schemes in this laboratory for the past three decades have been based on an initial lithium borate fusion of rock samples and all analytical methods based on multi-element atomic emission spectrometry, with switch-over from solid analysis by arc/spark excitation to solution analysis by plasma excitation in 1974. The sample preparation steps which have been automated are: weighing of samples and fluxes, lithium borate fusion, dissolution and dilution of fusion products and ion-exchange separation of difficult trace elements such as rare earth elements (REE). During 1985 and 1986, these different unit operations have been assembled together as peripheral units in the form of a workstation, called LabRobStation. A travelling robot is the master of LabRobStation, with all peripheral units at its reach in 10 m 2 workspace. As an example of real application, the automated determination of REE, based on more than 8000 samples analysed during 1982 and 1986, is presented. (author)

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

    Science.gov (United States)

    Li, Qing; Zhang, Zhen; Wang, Zheng

    2014-10-03

    A simple and sensitive method to determine Hg(2+) was developed by combining solution-cathode glow discharge atomic emission spectrometry (SCGD-AES) with flow injection (FI) based on on-line solid-phase extraction (SPE). We synthesized l-cysteine-modified mesoporous silica and packed it in an SPE microcolumn, which was experimentally determined to possess a good mercury adsorption capacity. An enrichment factor of 42 was achieved under optimized Hg(2+) elution conditions, namely, an FI flow rate of 2.0 mL min(-1) and an eluent comprised of 10% thiourea in 0.2 mol L(-1) HNO3. The detection limit of FI-SCGD-AES was determined to be 0.75 μg L(-1), and the precision of the 11 replicate Hg(2+) measurements was 0.86% at a concentration of 100 μg L(-1). The proposed method was validated by determining Hg(2+) in certified reference materials such as human hair (GBW09101b) and stream sediment (GBW07310). Copyright © 2014. Published by Elsevier B.V.

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

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

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

  6. Organic salt NEDC (N-naphthylethylenediamine dihydrochloride) assisted laser desorption ionization mass spectrometry for identification of metal ions in real samples.

    Science.gov (United States)

    Hou, Jian; Chen, Suming; Zhang, Ning; Liu, Huihui; Wang, Jianing; He, Qing; Wang, Jiyun; Xiong, Shaoxiang; Nie, Zongxiu

    2014-07-07

    The significance of metals in life and their epidemiological effects necessitate the development of a direct, efficient, and rapid method of analysis. The matrix assisted laser desorption/ionization technique is on the horns of a dilemma of metal analysis as the conventional matrixes have high background in the low mass range. An organic salt, NEDC (N-naphthylethylenediamine dihydrochloride), is applied as a matrix for identification of metal ions in the negative ion mode in the present work. Sixteen metal ions, Ba(2+), Ca(2+), Cd(2+), Ce(3+), Co(2+), Cu(2+), Fe(3+), Hg(2+), K(+), Mg(2+), Mn(2+), Na(+), Ni(2+), Pb(2+), Sn(2+) and Zn(2+), in the form of their chloride-adducted clusters were systematically tested. Mass spectra can provide unambiguous identification through accurate mass-to-charge ratios and characteristic isotope patterns. Compared to ruthenium ICP standard solution, tris(2,2'-bipyridyl)dichlororuthenium(ii) (C30H24N6Cl2Ru) can form organometallic chloride adducts to discriminate from the inorganic ruthenium by this method. After evaluating the sensitivity for Ca, Cu, Mg, Mn, Pb and Zn and plotting their quantitation curves of signal intensity versus concentration, we determined magnesium concentration in lake water quantitatively to be 5.42 mg L(-1) using the standard addition method. There is no significant difference from the result obtained with ICP-OES, 5.8 mg L(-1). Human urine and blood were also detected to ascertain the multi-metal analysis ability of this strategy in complex samples. At last, we explored its applicability to tissue slice and visualized sodium and potassium distribution by mass spectrometry imaging in the normal Kunming mouse brain.

  7. Effect of fuel injection parameters on combustion stability and emissions of a mineral diesel fueled partially premixed charge compression ignition (PCCI) engine

    International Nuclear Information System (INIS)

    Jain, Ayush; Singh, Akhilendra Pratap; Agarwal, Avinash Kumar

    2017-01-01

    Highlights: • NOx and PM emissions were lowest at 700 bar fuel injection pressure (FIP). • PCCI showed lower knocking than compression ignition combustion mode. • Increasing FIP reduced emissions of nitrogen oxides and smoke opacity in PCCI mode. • Increasing FIP reduced nucleation mode particle concentration. • Increasing FIP with advanced main injection timings improved PCCI combustion. - Abstract: This experimental study focuses on developing new combustion concept for compression ignition (CI) engines by achieving partially homogeneous charge, leading to low temperature combustion (LTC). Partially premixed charge compression ignition (PCCI) combustion is a single-stage phenomenon, with combustion shifting towards increasingly premixed combustion phase, resulting in lower in-cylinder temperatures. PCCI leads to relatively lower emissions of oxides of nitrogen (NOx) and particulate matter (PM) simultaneously. To investigate combustion, performance and emission characteristics of the PCCI engine, experiments were performed in a mineral diesel fueled single cylinder research engine, which was equipped with flexible fuel injection equipment (FIE). Effects of fuel injection pressure (FIP) were investigated by changing the FIP from 400 bar to 1000 bar. Experiments were carried out by varying start of main injection (SoMI) timings (from 12° to 24° before top dead center (bTDC)), when using single pilot injection. This experimental study included detailed investigations of particulate characteristics such as particulate number-size distribution using engine exhaust particle sizer (EEPS), particulate bound trace metal analysis using inductively coupled plasma-optical emission spectrometer (ICP-OES), and soot morphology using transmission electron microscopy (TEM). PCCI combustion improved with increasing FIP (up to 700 bar) due to superior fuel atomization however further increasing FIP deteriorated PCCI combustion and engine performance due to intense

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

    International Nuclear Information System (INIS)

    Carrion, Nereida; Murillo, Miguel; Montiel, Edie; Diaz, Dorfe

    2003-01-01

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

  9. Establishing the link between health effects and tire pyrolysis emissions through X RF spectrometry of particulate matter in the 2.5 range

    International Nuclear Information System (INIS)

    Santos, Flora L.; Pabroa, Preciosa Corazon B.; Bautista VII, Angel T.; Bucal, Camille Grace DL.

    2011-01-01

    In July 2009, several tire pyrolysis facility started operations in Angat, Bulacan. Very soon after the facility in Pulong Yantok started operations, nearby residents noted oily effluents contaminating the surrounding area including a nearby creek and adjacent rice fields; sacks of dark ash stacked close just outside the facility; dark layers of soot on the ground, foliage and rooftops. Residents complained that they could no longer save rainwater for drinking because their rain gutters were contaminated by soot. The residents also complained of foul odor emanating from the facility. many of them has to stay indoors and close their windows to keep away tire pyrolysis emissions. In January, 2010, people became alarmed on realizing that they were exhibiting a communal reaction to airborne substances which they suspected were coming from the tire pyrolysis facility. Symptoms experienced were: tightening of the chest, asthma, excessive phlegm formation, coughing, allergic rhinitis, eye and skin irritation, headaches, stomach ache and even fever. At the time the exact nature of the facility was not yet clear to stake holders. Assistance was sought from the Philippine Nuclear Research Institute (PNRI) for the conduct of air particulate monitoring, in order to generate preliminary information on the nature of airborne pollutants. PM2.5 and PM10-2.5 monitoring was undertaken with the Gent sampler and subsequent elemental analysis by X RF spectrometry, in an attempt to identify possible signature elements. PM2.5 and PM10 levels were much below the WHO guideline values. Elements present above one percent in PM2.5 were: Black C, Na, S, Si, K, Ca, Al and Mg. Those present below one percent in PM2.5 were: Fe, Zn, Pb, P, and Ni, Ti, V, Cr, Mn and Cu were below detection limits. A drop in concentration was noted for elements present in tires (Zn, S, Pb, Al, Si, Mg and Black C) when the facility stopped operations after the implementation of the Cease and Desist Order (CDO). Zn

  10. Determination of essential trace elements in wine by neutron activation analysis

    International Nuclear Information System (INIS)

    Daniele, Anna Paula

    2016-01-01

    Several studies have been carried out for determining essential elements in foodstuffs, including wine, due to its important nutritional role in human body functions. It was shown that daily consumption of wine in moderation contributes significantly to the needs of essential elements in human body such as Ca, Co, Cr, Fe, K, Mg, Mn, Zn, V, among others, and has health benefits in the prevention of numerous diseases and longer life expectancy, related in particular to the intake of antioxidants such as polyphenolic compounds. Trace elements are good indicators of origin of wines and their concentrations can be used as criteria to ensure authenticity, quality and show that the tolerance limits established by law were respected throughout the production process. However, although Brazilian wine industry is among the 15 largest in the world, analytical studies for organic and inorganic compounds of wine content are still small when compared to other major producers. In this sense, this study aimed to evaluate some procedures of wine sample preparation to determine essential elements by Instrumental Neutron Activation Analysis (INAA) and compare the results with those determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP OES). Three sample preparation procedures were studied: freeze-drying, evaporation and dry ashing. The parameters studied were precision, accuracy and detection limit. ANOVA and Tukey-Kramer tests were applied to verify the statistical differences between the mean values obtained by the three wine preparation procedures for INAA with those means obtained by ICP OES. It was noticed that about 60% of results obtained by freeze-drying agreed with those obtained by ICP OES. (author)

  11. Determination of essential trace elements in wine by neutron activation analysis; Determinacao de elementos essenciais em vinhos por analise por ativacao com neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Daniele, Anna Paula

    2016-07-01

    Several studies have been carried out for determining essential elements in foodstuffs, including wine, due to its important nutritional role in human body functions. It was shown that daily consumption of wine in moderation contributes significantly to the needs of essential elements in human body such as Ca, Co, Cr, Fe, K, Mg, Mn, Zn, V, among others, and has health benefits in the prevention of numerous diseases and longer life expectancy, related in particular to the intake of antioxidants such as polyphenolic compounds. Trace elements are good indicators of origin of wines and their concentrations can be used as criteria to ensure authenticity, quality and show that the tolerance limits established by law were respected throughout the production process. However, although Brazilian wine industry is among the 15 largest in the world, analytical studies for organic and inorganic compounds of wine content are still small when compared to other major producers. In this sense, this study aimed to evaluate some procedures of wine sample preparation to determine essential elements by Instrumental Neutron Activation Analysis (INAA) and compare the results with those determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP OES). Three sample preparation procedures were studied: freeze-drying, evaporation and dry ashing. The parameters studied were precision, accuracy and detection limit. ANOVA and Tukey-Kramer tests were applied to verify the statistical differences between the mean values obtained by the three wine preparation procedures for INAA with those means obtained by ICP OES. It was noticed that about 60% of results obtained by freeze-drying agreed with those obtained by ICP OES. (author)

  12. Assessment and modifications of digestion procedures to determine trace elements in urine of hypertensive and diabetes mellitus patients

    Directory of Open Access Journals (Sweden)

    Awad Abdalla Momen

    2013-01-01

    Full Text Available Context: There is accumulating evidence that the metabolism of several trace elements like Cr, Cu, Pb, Cd, Co, Mn and Zn might have specific roles in the pathogenesis and progress of many diseases like hypertension (HTN and diabetes mellitus (DM. Objectives: To provide a fast, efficient, sensitive, and reliable analytical procedure for trace element determination in urine samples of HTN and DM patients using inductively coupled plasma optical emission spectrometry (ICP-OES. Setting and Design: The ICP-OES operating conditions were optimised and carefully selected in order to maximise the sensitivity, precision and accuracy. Factors affecting analytical and biological variability of the concentrations under study were discussed and carefully optimised. Materials and Methods: Different digestion procedures with acids and oxidising reagents were tested. The suitable procedure ICP-OES was selected, carefully modified and applied. The validity and accuracy of the different elements were determined by spiking of samples with known amounts of multi-element standard solution. Statistical Analysis: Student t-test and analysis of variance (ANOVA test were used for analysis. Microsoft Excel was used to assess the significance of the difference between variables. The concentrations obtained were expressed as mean value ± standard deviation (P = 0.05. Results: The results of this study showed that the mean concentrations of Cd, Zn, Pb, Cu, Cr and Mn in urine from both HTN (study group A and DM (study group B patients were higher than the corresponding values observed in the control group. However, while the mean value of Co was low as compared to the control group, the differences found were not significant (P = 0.05. Conclusion: The method used had excellent sensitivity, multi-element data could be obtained with very short acquisition time. The elements Cr, Cd, Pb and Zn might have specific roles in the pathogenesis and progress of HTN and DM. Further

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    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 NH 4 OH 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 NH 4 OH 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

  14. Comparison of the samples injection systems with ultrasonic nebulizer and with pneumatic nebulizer for the metal determination in water by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Marin, Sergio R; Pismante, Paola A

    2005-01-01

    The natural waters, depending on their use, must fulfill the exigencies and requirements that fix national and international norms. These establish conditions with respect to the concentration levels that must be some metals. In this work the development of inductively coupled plasma emission optical spectrometry with ultrasonic injection system is presented. The determination of aluminum, arsenic, barium, cadmium, zinc, cobalt, chromium, copper, iron, manganese, molybdenum, nickel, lead, strontium and vanadium, at levels of ultra-trace in water samples is studied by this technique. The wavelengths that represented better sensitivity and minors spectral interferences, were selected from the Literature specialized in the analysis of this type of material. Also the conditions of work for the ultrasonic nebulization: temperature, pressure, flow speed of argon, and flow speed of sample was determined. The greater sensitivity of the injection system by ultrasonic nebulization forehead to the injection system by pneumatic nebulization, is verified when comparing the spectral intensity of the selected wavelengths. Also the limits of detection and quantification was obtained by both systems. The validity of the results obtained in this method is verified applying the test of Fisher, who determines the degree of homogeneity of the variances, and the test of Student, to determine the trazability obtained with these values. For these studies, the certified material of reference TM-24.2 of National Water Research Institute Environment Canada (NWRI), was used. The positive answer to the criteria of evaluation E and Z-Score, obtained by this technique, allows to verify that it fulfills the exigencies to be used in the determination of metals at the required levels (au)

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

    KAUST Repository

    Patole, Shashikant P.

    2015-10-21

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

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

    Science.gov (United States)

    Masuck, Ines; Hutzler, Christoph; Luch, Andreas

    2010-04-30

    In the revised European toy safety directive 2009/48/EC the application of fragrance allergens in children's toys is restricted. The focus of the present work lies on the instrumental analytics of 13 banned fragrance allergens, as well as on 11 fragrance allergens that require declaration when concentrations surpass 100 microg per gram material. Applying a mixture of ethyl acetate and toluene solid/liquid extraction was performed prior to quantitative analysis of mass contents of fragrances in scented toys. In addition, an easy-to-perform method for the determination of emitted fragrances at 23 degrees C (handling conditions) or at 40 degrees C (worst case scenario) has been worked out to allow for the evaluation of potential risks originating from inhalation of these compounds during handling of or playing with toys. For this purpose a headspace solid-phase microextraction (HS-SPME) technique was developed and coupled to subsequent gas chromatography-mass spectrometry (GC-MS) analysis. Fragrance allergens were adsorbed (extracted) from the gas phase onto an 85 microm polyacrylate fiber while incubating pieces of the scented toys in sealed headspace vials at 23 degrees C and 40 degrees C. Quantification of compounds was performed via external calibration. The newly developed headspace method was subsequently applied to five perfumed toys. As expected, the emission of fragrance allergens from scented toys depends on the temperature and on the content of fragrance allergens present in those samples. In particular at conditions mimicking worst case (40 degrees C), fragrance allergens in toys may pose a risk to children since considerable amounts of compound might be absorbed by lung tissue via breathing of contaminated air. 2010 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-10-03

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

  18. High Precision Seawater Sr/Ca Measurements in the Florida Keys by Inductively Coupled Plasma Atomic Emission Spectrometry: Analytical Method and Implications for Coral Paleothermometry

    Science.gov (United States)

    Khare, A.; Kilbourne, K. H.; Schijf, J.

    2017-12-01

    Standard methods of reconstructing past sea surface temperatures (SSTs) with coral skeletal Sr/Ca ratios assume the seawater Sr/Ca ratio is constant. However, there is little data to support this assumption, in part because analytical techniques capable of determining seawater Sr/Ca with sufficient accuracy and precision are expensive and time consuming. We demonstrate a method to measure seawater Sr/Ca using inductively coupled plasma atomic emission spectrometry where we employ an intensity ratio calibration routine that reduces the self- matrix effects of calcium and cancels out the matrix effects that are common to both calcium and strontium. A seawater standard solution cross-calibrated with multiple instruments is used to correct for long-term instrument drift and any remnant matrix effects. The resulting method produces accurate seawater Sr/Ca determinations rapidly, inexpensively, and with a precision better than 0.2%. This method will make it easier for coral paleoclimatologists to quantify potentially problematic fluctuations in seawater Sr/Ca at their study locations. We apply our method to test for variability in surface seawater Sr/Ca along the Florida Keys Reef Tract. We are collecting winter and summer samples for two years in a grid with eleven nearshore to offshore transects across the reef, as well as continuous samples collected by osmotic pumps at four locations adjacent to our grid. Our initial analysis of the grid samples indicates a trend of decreasing Sr/Ca values offshore potentially due to a decreasing groundwater influence. The values differ by as much as 0.05 mmol/mol which could lead to an error of 1°C in mean SST reconstructions. Future work involves continued sampling in the Florida Keys to test for seasonal and interannual variability in seawater Sr/Ca, as well as collecting data from small reefs in the Virgin Islands to test the stability of seawater Sr/Ca under different geologic, hydrologic and hydrographic environments.

  19. Recent Studies on the Speciation and Determination of Mercury in Different Environmental Matrices Using Various Analytical Techniques

    Directory of Open Access Journals (Sweden)

    Lakshmi Narayana Suvarapu

    2017-01-01

    Full Text Available This paper reviews the current research on the speciation and determination of mercury by various analytical techniques, including the atomic absorption spectrometry (AAS, voltammetry, inductively coupled plasma optical emission spectrometry (ICP-OES, ICP-mass spectrometry (MS, atomic fluorescence spectrometry (AFS, spectrophotometry, spectrofluorometry, and high performance liquid chromatography (HPLC. Approximately 96 research papers on the speciation and determination of mercury by various analytical instruments published in international journals since 2015 were reviewed. All analytical parameters, including the limits of detection, linearity range, quality assurance and control, applicability, and interfering ions, evaluated in the reviewed articles were tabulated. In this review, we found a lack of information in speciation studies of mercury in recent years. Another important conclusion from this review was that there were few studies regarding the concentration of mercury in the atmosphere.

  20. Uranium determination using atomic spectrometric techniques: An overview

    International Nuclear Information System (INIS)

    Santos, Juracir S.; Teixeira, Leonardo S.G.; Santos, Walter N.L. dos; Lemos, Valfredo A.; Godoy, Jose M.; Ferreira, Sergio L.C.

    2010-01-01

    This review focuses on the determination of uranium using spectroanalytical techniques that are aimed at total determination such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), inductively coupled plasma optical emission spectrometry (ICP-OES); and inductively coupled plasma mass spectrometry (ICP-MS) that also enables the determination of uranium isotopes. The advantages and shortcomings related to interferences, precision, accuracy, sample type and equipment employed in the analysis are taken into account, as well as the complexity and costs (i.e., acquisition, operation and maintenance) associated with each of the techniques. Strategies to improve their performance that employ separation and/or preconcentration steps are considered, with an emphasis given to solid-phase extraction because of its advantages compared to other preconcentration procedures.

  1. Experimental half-life determination of 176Lu

    International Nuclear Information System (INIS)

    Kossert, Karsten; Jörg, Gerhard; Gostomski, Christoph Lierse v.

    2013-01-01

    The half-life of the naturally occurring long-lived rare earth isotope 176 Lu was determined by a combination of highly sophisticated experimental procedures in order to further improve the reliability and the precision of literature data. The amount of lutetium in the samples was determined by inductively coupled plasma optical emission spectrometry (ICP-OES) using a NIST reference standard. The isotopic ratio N( 176 Lu)/N(Lu) in the samples was measured by means of inductively coupled plasma high resolution mass spectrometry (ICP-HRMS). The activity divided by the mass of Lu was determined by applying liquid scintillation (LS) counting. The LS counting efficiency of the beta/gamma emitter 176 Lu was determined with the CIEMAT/NIST efficiency tracing technique with low uncertainty. The influences of colour quenching and background effects are discussed in this paper. The half-life was found to be 3.640(35)×10 10 y. The result is in good agreement with other evaluations and the relative standard uncertainty of 0.95% is among the lowest of previously published data. - Highlights: • The half-life of 176 Lu was determined by ICP-OES, ICP-HRMS and LSC. • The LSC efficiency was determined with the CIEMAT/NIST method. • The half-life was found to be 3.640(35)×10 10 y

  2. Rapid Analysis of Ash Composition Using Laser-Induced Breakdown Spectroscopy (LIBS)

    Energy Technology Data Exchange (ETDEWEB)

    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.

  3. Assessment of metal concentrations in sediment samples from Billings Reservoir, Rio Grande tributary, Sao Paulo, Brazil

    International Nuclear Information System (INIS)

    Bostelmann, Eleine

    2006-01-01

    The present study chemically characterized sediment samples from the Billings reservoir, Rio Grande tributary, in the Metropolitan region of Sao Paulo, by determining metal concentration and other elements of interest. The chosen chemical parameters for this characterization were Aluminum, Arsenic, Barium, Cadmium, Copper, Chromium, Iron, Lead, Manganese, Mercury, Nickel, Selenium and Zinco. These parameters are also used in the water quality index, with the exception of Selenium. The concentrations were determined through different analytical techniques such as atomic absorption spectrometry (FAAS, GFAAS and CVAAS), optical emission spectrometry (ICP OES) and neutron activation analysis. These analytical methodologies were assessed for precision, accuracy and detection and/or quantification limits for the sediment elements in question. Advantages and disadvantages of each technique for each element and its concentration were also discussed. From these assessments the most adequate technique was selected for the routine analysis of sediment samples for each element concentration determination. This assessment verified also that digestion in a closed microwave system with nitric acid is efficient for the evaluation of extracted metals of environmental interest. The analytical techniques chosen were equally efficient for metals determination. In the case of Cd and Pb, the FAAS technique was selected due to better results than ICP OES, as it does not present matrix interference. The concentration values obtained for metals As, Cd, Cu, Cr, Hg, Ni, Pb and Zn in the sediment samples were compared to Canadian Council of Minister of the Environment (CCME) TEL and PEL values. (author)

  4. Assessment of metal concentrations in sediment samples from Billings reservoir, Rio Grande tributary, Sao Paulo, Brazil

    International Nuclear Information System (INIS)

    Bostelmann, Eleine

    2006-01-01

    The present study chemically characterized sediment samples from the Billings reservoir, Rio Grande tributary, in the Metropolitan region of Sao Paulo, by determining metal concentration and other elements of interest. The chosen chemical parameters for this characterization were Aluminum, Arsenic, Barium, Cadmium, Copper, Chromium, Iron, Lead, Manganese, Mercury, Nickel, Selenium and Zinc. These parameters are also used in the water quality index, with the exception of Selenium. The concentrations were determined through different analytical techniques such as atomic absorption spectrometry (FAAS, GFAAS and CVAAS), optical emission spectrometry (ICP OES) and neutron activation analysis. These analytical methodologies were assessed for precision, accuracy and detection and/or quantification limits for the sediment elements in question. Advantages and disadvantages of each technique for each element and its concentration were also discussed. From these assessment the most adequate technique was selected for the routine analysis of sediment samples for each element concentration determination. This assessment verified also that digestion in a closed microwave system with nitric acid is efficient for the evaluation of extracted metals of environmental interest. The analytical techniques chosen were equally efficient for metals determination. In the case of Cd and Pb, the FAAS technique was selected due to better results than ICP OES, as it does not present matrix interference. The concentration values obtained for metals As, Cd, Cu, Cr, Hg, Ni, Pb and Zn in the sediment samples were compared to Canadian Council of Minister of the Environment (CCME) TEL and PEL values. (author)

  5. Assessment of metal concentrations in sediment samples from Billings Reservoir, Rio Grande tributary, Sao Paulo, Brazil; Avaliacao da concentracao de metais em amostras de sedimento do Reservatorio Billings, Braco Rio Grande, Sao Paulo, Brasil

    Energy Technology Data Exchange (ETDEWEB)

    Bostelmann, Eleine

    2006-07-01

    The present study chemically characterized sediment samples from the Billings reservoir, Rio Grande tributary, in the Metropolitan region of Sao Paulo, by determining metal concentration and other elements of interest. The chosen chemical parameters for this characterization were Aluminum, Arsenic, Barium, Cadmium, Copper, Chromium, Iron, Lead, Manganese, Mercury, Nickel, Selenium and Zinco. These parameters are also used in the water quality index, with the exception of Selenium. The concentrations were determined through different analytical techniques such as atomic absorption spectrometry (FAAS, GFAAS and CVAAS), optical emission spectrometry (ICP OES) and neutron activation analysis. These analytical methodologies were assessed for precision, accuracy and detection and/or quantification limits for the sediment elements in question. Advantages and disadvantages of each technique for each element and its concentration were also discussed. From these assessments the most adequate technique was selected for the routine analysis of sediment samples for each element concentration determination. This assessment verified also that digestion in a closed microwave system with nitric acid is efficient for the evaluation of extracted metals of environmental interest. The analytical techniques chosen were equally efficient for metals determination. In the case of Cd and Pb, the FAAS technique was selected due to better results than ICP OES, as it does not present matrix interference. The concentration values obtained for metals As, Cd, Cu, Cr, Hg, Ni, Pb and Zn in the sediment samples were compared to Canadian Council of Minister of the Environment (CCME) TEL and PEL values. (author)

  6. Identification and characterization of gadolinium(III) complexes in biological tissue extracts.

    Science.gov (United States)

    Kahakachchi, Chethaka L; Moore, Dennis A

    2010-07-01

    The gadolinium species present in a rat kidney following intravenous administration of a gadolinium-based magnetic resonance contrast agent (Optimark™, Gadoversetamide injection) to a rat was examined in the present study. The major gadolinium species in the supernatant of the rat kidney tissue extracts was determined by reversed-phase liquid chromatography with online inductively coupled plasma optical emission spectrometry (HPLC-ICP-OES). The identity of the compound was established by liquid chromatography electrospray ionization mass spectrometry (LC-ESI-MS) detection. The principal gadolinium(III) complex in a rat kidney tissue extract was identified as Gd-DTPA-BMEA 24 Hrs and 7 days after a single intravenous injection of Optimark™ (gadoversetamide; Gd-DTPA-BMEA) at a dose of 5 mmol Gd/kg body weight. The study demonstrated for the first time the feasibility of the use of two complementary techniques, HPLC-ICP-OES and HPLC-ESI-MS to study the in vivo behavior of gadolinium-based magnetic resonance contrast media.

  7. Sample Preprocessing For Atomic Spectrometry

    International Nuclear Information System (INIS)

    Kim, Sun Tae

    2004-08-01

    This book gives descriptions of atomic spectrometry, which deals with atomic absorption spectrometry such as Maxwell-Boltzmann equation and Beer-Lambert law, atomic absorption spectrometry for solvent extraction, HGAAS, ETASS, and CVAAS and inductively coupled plasma emission spectrometer, such as basic principle, generative principle of plasma and device and equipment, and interferences, and inductively coupled plasma mass spectrometry like device, pros and cons of ICP/MS, sample analysis, reagent, water, acid, flux, materials of experiments, sample and sampling and disassembling of sample and pollution and loss in open system and closed system.

  8. Effects of air exchange, temperature and slurry management on odorant emissions from pig production units and slurry tanks studied by proton-transfer-reaction mass spectrometry (PTR-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Feilberg, A.; Adamsen, A.P.S.; Liu, D.; Hansen, M.J.; Bildsoe, P. [Aarhus Univ., Tjele (Denmark). Dept. of Biosystems Engineering

    2010-07-01

    The factors affecting the variability of odorant emissions from intensive pig production facilities were examined using proton-transfer-reaction mass spectrometry (PTR-MS) to monitor emissions of odorants. Quantitative and time-resolved results for protonated ions representing hydrogen sulphide (H{sub 2}S), volatile organic sulphur compounds, organic amines, volatile carboxylic acids, carbonyls, phenols and indoles can be obtained. This study presented the results from PTRMS measurements of odorant emissions from finisher pig houses and finisher manure storage tanks. The measurements were performed at an experimental full-scale pig section with mechanical ventilation and at an experimental manure storage facility with controlled air exchange. Field measurements were taken during variable air exchange rates and temperatures, during finisher growth, and during emptying of the slurry pit. The results revealed a pronounced diurnal variation in emissions of odorants from the pig section with peaks in daytime coinciding with the highest ventilation rates and highest room temperatures. The highest emission rates were observed for H{sub 2}S and carboxylic acids. Based on odour threshold values, methanethiol and 4-methylphenol were estimated to contribute considerably to the odour nuisance. Discharging of the slurry pit led to reduced H{sub 2}S emissions, but peaks of H{sub 2}S were observed during manure handling.

  9. Determination of boron in graphite, boron carbide and glass by ICP-MS, ICP-OES and conventional wet chemical methods

    International Nuclear Information System (INIS)

    Venkatesh, K.; Kamble, Granthali S.; Venkatesh, Manisha; Kumar, Sanjukta A.; Reddy, A.V.R.

    2014-01-01

    Boron is an important element of interest in nuclear reactor materials due to its high neutron absorption cross section (σ 0 =3837 barns for 10 B). In the present paper, R and D work and routinely used methods have been described for the analysis of case samples (1) Graphite where boron is present at trace levels, (2) Boron Carbide having boron concentration of about 80% and (3) Glass containing 4-6 % boron. (author)

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

    DEFF Research Database (Denmark)

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

    2013-01-01

    for quantitation of As, Cd, Cu, Cr, Fe, Hg, Ir, Mn, Mo, Ni, Os, Pb, Pd, Pt, Rh, Ru, V and Zn in tablets according to the new USP chapters was developed. Sample preparation was performed by microwave-assisted acid digestion using a mixture of 65% HNO3 and 37% HCl (3:1, v/v). Limits of detection and quantitation...

  11. Analysis of human serum and whole blood for mineral content by ICP-MS and ICP-OES: development of a mineralomics method.

    Science.gov (United States)

    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.

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

    Directory of Open Access Journals (Sweden)

    Hadi M. Marwani

    2016-06-01

    Full Text Available 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.

  13. Investigating the Effect of Glass Ion Release on the Cytocompatibility, Antibacterial Eflcacy and Antioxidant Activity of Y2O3 / CeO2 doped SiO2-SrO-Na2O glasses

    Directory of Open Access Journals (Sweden)

    Placek L. M.

    2018-02-01

    Full Text Available The effect on ion release and cytocompatibility of Yttrium (Y and Cerium (Ce are investigated when substituted for Sodium (Na in a 0.52SiO2-0.24SrO-0.24-Na2OMOglass series (where MO= Y2O3 or CeO2. Glass leaching was evaluated through pH measurements and Inductive Coupled Plasma-Optical Emission Spectrometry (ICP-OES analysiswhere the extract pH increased during incubation (11.2 - 12.5. Ion release of Silicon (Si, Na and Strontium (Sr from the Con glass was at higher than that of glasses containing Y or Ce, and reached a limit after 1 day. Ion release from Y and Ce containing glasses reached a maximum of 1800 μg/mL, 1800 μg/mL, and 10 μg/mL for Si, Na, and Sr, respectively. Release of Y and Cewas below the ICP- OES detection limit 75% of bacteria at a 9% extract concentration. Antioxidant capacity (mechanism for neuroprotection was evaluated using the ABTS assay. All glasses had inherent radical oxygen species (ROS scavenging capability with Con reaching 9.5 mMTE.

  14. Fe{sub 3}O{sub 4}/salicylic acid nanoparticles versatility in magnetic mediated vascular nanoblockage

    Energy Technology Data Exchange (ETDEWEB)

    Mîndrilă, I., E-mail: tutu0101@yahoo.com [University of Medicine and Pharmacy of Craiova, Faculty of Medicine (Romania); Buteică, S. A. [University of Medicine and Pharmacy of Craiova, Faculty of Pharmacy (Romania); Mihaiescu, D. E.; Badea, G.; Fudulu, A. [Politehnica University of Bucharest, Faculty of Applied Chemistry and Material Science (Romania); Mărgăritescu, D. N. [University of Medicine and Pharmacy of Craiova, Faculty of Medicine (Romania)

    2016-01-15

    An aqueous dispersion of Fe{sub 3}O{sub 4}/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 Fe{sub 3}O{sub 4} 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. Determination of the mineral compositions of some selected oil-bearing seeds and kernels using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES

    Directory of Open Access Journals (Sweden)

    Musa Özcan, M.

    2006-06-01

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

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

    Science.gov (United States)

    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

    2011-02-01

    In microdose studies, the pharmacokinetic 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 pharmacokinetic 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 pharmacokinetic profile of the model drug verapamil in plasma and brain of humans. In order to assess pharmacokinetic dose linearity of verapamil, data were acquired and compared after administration of an intravenous microdose and after an intravenous microdose administered concomitantly with an oral therapeutic dose. Six healthy male subjects received an intravenous microdose [0.05 mg] (period 1) and an intravenous microdose administered concomitantly with an oral therapeutic dose [80 mg] of verapamil (period 2) in a randomized, crossover, two-period study design. The intravenous dose was a mixture of (R/S)-[14C]verapamil and (R)-[11C]verapamil and the oral dose was unlabelled racaemic verapamil. Brain distribution of radioactivity was measured with PET whereas plasma pharmacokinetics of (R)- and (S)-verapamil were determined with AMS. PET data were analysed by pharmacokinetic modelling to estimate the rate constants for transfer (k) of radioactivity across the blood-brain barrier. Most pharmacokinetic parameters of (R)- and (S)-verapamil as well as parameters describing exchange of radioactivity between plasma and brain (influx rate constant [K(1)] = 0.030 ± 0.003 and 0.031 ± 0.005 mL/mL/min and efflux rate constant [k(2)] = 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 nonlinear pharmacokinetics for the (R)-enantiomer. On the other hand, all

  17. Characterization of used lubricating oil by spectrometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Andressa Moreira de, E-mail: andressa@ctaa.embrapa.br [Embrapa Agroindustria de Alimentos, Guaratiba, Rio de Janeiro, RJ (Brazil); Correa, Sergio Machado [Faculdade de Engenharia. Universidade do Estado do Rio de Janeiro (UERJ), Resende, RJ (Brazil); Silva, Glauco Correa da [Instituto de Engenharia Nuclear (IEN/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

    2011-07-01

    Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-Elmer{sup R} OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX Shimadzu{sup R} model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100{mu}A, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics

  18. Characterization of used lubricating oil by spectrometric techniques

    International Nuclear Information System (INIS)

    Souza, Andressa Moreira de; Correa, Sergio Machado; Silva, Glauco Correa da

    2011-01-01

    Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-Elmer R OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX Shimadzu R model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100μA, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics Using GC

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

    Science.gov (United States)

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

  20. Improvement of the detection limits in radio-frequency-powered glow discharge optical emission spectrometry associated with bias-current conduction method; Jiko bias denryu donyuho ni yoru koshuha glow hoden hakko bunseki ni okeru kenshutsu genkai no kaizen

    Energy Technology Data Exchange (ETDEWEB)

    Wagatsuma, K. [Tohoku University, Sendai (Japan). Research Institute for Materials

    1999-01-01

    A d.c. bias current driven by the self-bias voltage which is conducted through the r.f.-powered glow discharge plasma varies the emission characteristics drastically, leading to improvement of the detection power in the optical emission spectrometry. By conducting the bias currents of 20-30 mA, the emission intensities of the atomic resonance lines were 10-20 times larger than those obtained with conventional r.t.- powered plasmas. The detection limits for determination of alloyed elements in the re-based binary alloy samples were estimated to be l.6 x 10{sup -3}% Cr for CrI 425.43nm, 7 x 10{sup -4}% Mn for MnI 403.10nm, 1.9>10{sup -3}% Cu for CuI 327.40nm, 1.1 x 10{sup -3}% Al for AlI 396.16nm, and 6.6 x 10{sup -3}% Ni for NiI 352.45 nm. (author)

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

    Science.gov (United States)

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

    2006-11-01

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

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

    Directory of Open Access Journals (Sweden)

    F. Reyes

    2006-01-01

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

  3. Comparison of ultra-violet and inductively coupled plasma-atomic emission spectrometry for the on-line quantification of selenium species after their separation by reversed-phase liquid chromatography

    International Nuclear Information System (INIS)

    Tsopelas, Fotios N.; Ochsenkuehn-Petropoulou, Maria Th.; Mergias, Ioannis G.; Tsakanika, Lambrini V.

    2005-01-01

    An analytical approach for selenium speciation using liquid chromatography (LC) coupled with ultra-violet (UV) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) was developed. The separation of the investigated selenium species, selenites, selenates, selenomethionine, selenocystine, selenocystamine and dimethyldiselenide was accomplished in less than 6 min on a BIO Wide Pore RP-18 column using sodium salt of n-octanesulfonic acid as ion-pairing modifier. The on-line detection of the separated selenium species was performed using UV spectrometry at the optimum wavelength of 192 nm, obtained by the UV spectra of the investigated individual selenium species. ICP-AES was also used as element specific on-line detector, after its coupling with the chromatographic system. The UV and ICP-AES detectors were compared for their suitability, including sensitivity and detection limits, for the on-line quantification of the six selenium species. The developed LC-UV as well as LC-ICP-AES techniques were successfully applied to a selenized yeast candidate reference material, after its enzymatic extraction with protease XIV. It was found that the described LC-UV technique is suitable for the determination of selenomethionine, the main selenium compound in the yeast, with an accuracy of 5%, although the UV detector is not element specific and it is rarely used for selenium speciation. This finding can prove valuable for routine laboratories to perform selenium speciation in such materials

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

    Directory of Open Access Journals (Sweden)

    Anju Mathew

    2013-01-01

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

  5. Spatially and temporally resolved detection of arsenic in a capillary dielectric barrier discharge by hydride generation high-resolved optical emission spectrometry

    Czech Academy of Sciences Publication Activity Database

    Burhenn, S.; Kratzer, Jan; Svoboda, Milan; Klute, F. D.; Michels, A.; Veža, D.; Franzke, J.

    2018-01-01

    Roč. 90, MAR (2018), s. 3424-3429 ISSN 0003-2700 R&D Projects: GA ČR GA17-04329S Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * optical emission spectroscopy * arsenic hydride Subject RIV: CB - Analytical Chemistry , Separation OBOR OECD: Analytical chemistry Impact factor: 6.320, year: 2016

  6. Spatially and temporally resolved detection of arsenic in a capillary dielectric barrier discharge by hydride generation high-resolved optical emission spectrometry

    Czech Academy of Sciences Publication Activity Database

    Burhenn, S.; Kratzer, Jan; Svoboda, Milan; Klute, F. D.; Michels, A.; Veža, D.; Franzke, J.

    2018-01-01

    Roč. 90, MAR (2018), s. 3424-3429 ISSN 0003-2700 R&D Projects: GA ČR GA17-04329S Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * optical emission spectroscopy * arsenic hydride Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 6.320, year: 2016

  7. Spectrometry techniques for radioactivity measurements

    International Nuclear Information System (INIS)

    Anilkumar, S.

    2016-01-01

    The energy of the radiation emission following the nuclear decay is unique and the characteristic of the radio nuclide which undergoes decay. Thus measurement of the energy of the radiation offers a method of identifying the radio nuclides. The prime requirement of the energy measurement is a suitable detector which shows response proportional to the energy of the radiation rather than the presence of the radiation. The response from such detectors are suitably processed and distributed with respect to the signal strength which is proportional to incident energy. This distribution is normally referred as energy spectrum and is recorded in the multichannel analyser. The measurement of energy and intensity of radiation from the spectrum is called radiation spectrometry. Thus the radiation spectrometry allows the identification and quantification of radioactive isotopes in variety of matrices. The radiation spectrometry has now become a popular radioanalytical technique in wide area of nuclear fuel cycle programs. The popular spectrometry techniques commonly used for the radioactivity measurement and analysis are Alpha spectrometry, Gamma ray spectrometry and Beta spectrometry

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

    Science.gov (United States)

    Yassaa, Noureddine; Williams, Jonathan

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

  9. Mass spectrometry

    DEFF Research Database (Denmark)

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

    2010-01-01

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

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2009-04-01

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

  12. Do consumption of Kargi Tulum cheese meet daily requirements for minerals and trace elements?

    Directory of Open Access Journals (Sweden)

    Seval Sevgi Kirdar

    2015-07-01

    Full Text Available The mineral and trace elements of Kargı Tulum cheese are investigated during the ripening period of 90 days. Calcium, potassium, phosphorus, sodium, magnesium, manganese, copper, zinc and iron quantities were determined by simultaneous inductively coupled plasma optical emission spectrometry (ICP-OES. The effect of maturation time on the sodium, phosphor and potassium content of cheese samples has been found to be statistically significant (p<0.05. Magnesium and calcium levels during ripening period showed significant statistical difference (p<0.01. Copper values of cheese samples demonstrated an increase throughout 90-day maturation time. The effect of maturation time on manganese and zinc value has been found to be statistically significant (p<0.05. According to obtained data, by consuming 100 g Kargı Tulum cheese in daily period, an adult can provide a remarkable portion of his/her minerals needs.

  13. Zeolites as possible biofortifiers in Maitake cultivation

    Directory of Open Access Journals (Sweden)

    Vunduk Jovana

    2014-01-01

    Full Text Available The levels of Ni, Cu and Mg in Grifola frondosa (also known as Maitake mushroom fruit body produced on zeolite Minazel Plus (MG-supplemented substrate were measured with inductively coupled plasma optical emission spectrometry (ICP-OES. Two different concentrations of MG were added to the substrate for mushroom cultivation. Levels of selected metals were measured in cultivated dry carpophores. The content of Ni increased in fruit bodies produced on supplemented substrate, while in case of Cu, a pronounced decrease was observed. When two different concentrations of MG were implemented, the Mg level showed both positive and negative trend, depending on the applied concentration of zeolite. MG in a concentration of 1% showed the strongest influence on the observed elements in the cultivated fruiting body of Maitake mushroom. [Projekat Ministarstva nauke Republike Srbije, br. 46010

  14. Uranium determination by UV-Vis spectrophotometry in organic matrix

    International Nuclear Information System (INIS)

    Iwaki, Leonardo E.O.; Silva, Ieda S.; Oliveira, Luis C.

    2013-01-01

    Concentrations of uranium in the process samples provide essential information required for nuclear process monitoring. A large number of techniques have been developed to allow uranium determination, but each technique possesses some advantages and disadvantages and cannot be applied without difficulty to all samples. The ultraviolet visible spectrophotometry (UV-Vis) is widely method used in analytical industrial processes due to its simplicity, rapidity, low costs, low generation of analytical waste, easy calibration and operation. In this study, we describe a simple and fast quantification method to determination of a high amount of uranium in organic phase (TBP/kerosene) using UV-Vis spectrophotometry. The process sample was analyzed in UV-Vis and compared with inductively coupled plasma optical emission spectrometry (ICP OES) showing similar results in both methods. The statistical tests (Student-t and Fischer) showed that the both techniques they are equivalent. (author)

  15. Multi-element analysis, bioavailability and fractionation of herbal tea products

    International Nuclear Information System (INIS)

    Szymczycha-Madeja, Anna; Welna, Maja; Zyrnicki, Wieslaw

    2013-01-01

    Herbal teas (Mentha piperitae foliumand mixture Marticaria chamomilla flos with Lavandula officinalis flos) were compared considering the total contents of micro (Al, Ba, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Sr, Ti, V) and macro (C, H, N, S, Ca, Mg, P) elements, bioavailability and fractionation. Different methods (inductively coupled plasma optical emission spectrometry (ICP OES), Fourier transform infrared spectroscopy (FTIR) and CHNS elemental analysis) were applied. The microwave-assisted digestion procedure was found to be more effective than the hot-plate heating for the wet acid digestion of tea. The application of the modified BCR (Community Bureau of Reference) sequential extraction procedure exhibited differences in the concentrations of metal bound to reducible and oxidizable fractions. The accuracy of method was verified by analysis of certified reference material INCT-TL -1 Tea Leaves. The daily intake of all elements from the analyzed herbal tea infusion did not exceed the maximum permissible levels and does not constitute health risk. (author)

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

    International Nuclear Information System (INIS)

    Fernandes, Andrea P.; Santos, Mirian C.; Lemos, Sherlan G.; Ferreira, Marcia M.C.; Nogueira, Ana Rita A.; Nobrega, Joaquim A.

    2005-01-01

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

  17. Sweet chemistry: a green way for obtaining selenium nanoparticles active against cancer cells

    International Nuclear Information System (INIS)

    Vieira, Adriana P.; Stein, Erika M.; Ferreira, Ana Maria D.C.; Colepicolo, Pio; Andreguetti, Daniel X.; Cebrián-Torrejón, Gerardo; Doménech-Carbó, Antonio

    2017-01-01

    We present an environment friendly synthesis of selenium nanoparticles and the study of their cytotoxic activity against uterine sarcoma cancer and fibroblasts cells. Amorphous selenium (a-SeNPs) and trigonal selenium (t-SeNPs) were synthesized using D-fructose as the reducing agent and characterized by high-resolution transmission electron microscopy (HRTEM), energy dispersive X-ray spectroscopy (EDX), powder X-ray diffraction analysis (XRD), inductively coupled plasma optical emission spectrometry (ICP OES), dynamic light scattering (DLS) to obtain zeta potential values and cyclic voltammetry (CV). Particularly, a-SeNPs presented high toxicity toward the resistant cancer cell line MES-SA/Dx5 and its parental MES-SA line. However, they are not toxic against P4 fibroblast cells in comparative studies. (author)

  18. Total-reflection X-ray fluorescence: An alternative tool for the analysis of magnetic ferrofluids

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez-Ruiz, R. [Servicio Interdepartamental de Investigacion (SIdI), Facultad de Ciencias, Universidad Autonoma de Madrid, Cantoblanco, E-28049, Madrid (Spain)], E-mail: ramon.fernandez@uam.es; Costo, R.; Morales, M.P.; Bomati-Miguel, O.; Veintemillas-Verdaguer, S. [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, E-28049, Madrid (Spain)

    2008-12-15

    This work presents the first application of the total-reflection X-ray fluorescence (TXRF) to the compositional study of magnetic ferrofluids. With the aims of validating the best analytical conditions and also, limitations of the TXRF in the compositional study of these materials, an alternative empirical method, based in the use of angle-dependence TXRF (AD-TXRF) measurements, is proposed. Three kinds of ferromagnetic nanoparticles, with different morphologies, have been studied. The techniques of inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectroscopy (ICP-OES) have been used to validate the TXRF results. In contrast with the plasma techniques, the developed TXRF procedure need not of previous chemical acid digestion. Additionally, two procedures of magnetic nanoparticles synthesis, co-precipitation and laser-pyrolysis, have been checked for the contaminants trace metals Zn, Mn and Cr. It has been found that the method of laser-pyrolysis produces nanoparticles of higher purity.

  19. Multi-element analysis, bioavailability and fractionation of herbal tea products

    Energy Technology Data Exchange (ETDEWEB)

    Szymczycha-Madeja, Anna; Welna, Maja; Zyrnicki, Wieslaw, E-mail: anna.szymczycha@pwr.wroc.pl [Wroclaw University of Technology, Chemistry Department, Analytical Chemistry Division, Wroclaw (Poland)

    2013-05-15

    Herbal teas (Mentha piperitae foliumand mixture Marticaria chamomilla flos with Lavandula officinalis flos) were compared considering the total contents of micro (Al, Ba, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Sr, Ti, V) and macro (C, H, N, S, Ca, Mg, P) elements, bioavailability and fractionation. Different methods (inductively coupled plasma optical emission spectrometry (ICP OES), Fourier transform infrared spectroscopy (FTIR) and CHNS elemental analysis) were applied. The microwave-assisted digestion procedure was found to be more effective than the hot-plate heating for the wet acid digestion of tea. The application of the modified BCR (Community Bureau of Reference) sequential extraction procedure exhibited differences in the concentrations of metal bound to reducible and oxidizable fractions. The accuracy of method was verified by analysis of certified reference material INCT-TL{sup -1} Tea Leaves. The daily intake of all elements from the analyzed herbal tea infusion did not exceed the maximum permissible levels and does not constitute health risk. (author)

  20. Sweet chemistry: a green way for obtaining selenium nanoparticles active against cancer cells

    Energy Technology Data Exchange (ETDEWEB)

    Vieira, Adriana P.; Stein, Erika M.; Ferreira, Ana Maria D.C.; Colepicolo, Pio, E-mail: apiresvieira@gmail.com [Universidade de São Paulo (USP), São Paulo-SP (Brazil); Andreguetti, Daniel X.; Cebrián-Torrejón, Gerardo; Doménech-Carbó, Antonio [Departament de Química Analítica, Facultat de Química, Universitat de València, Valencia (Spain)

    2017-07-01

    We present an environment friendly synthesis of selenium nanoparticles and the study of their cytotoxic activity against uterine sarcoma cancer and fibroblasts cells. Amorphous selenium (a-SeNPs) and trigonal selenium (t-SeNPs) were synthesized using D-fructose as the reducing agent and characterized by high-resolution transmission electron microscopy (HRTEM), energy dispersive X-ray spectroscopy (EDX), powder X-ray diffraction analysis (XRD), inductively coupled plasma optical emission spectrometry (ICP OES), dynamic light scattering (DLS) to obtain zeta potential values and cyclic voltammetry (CV). Particularly, a-SeNPs presented high toxicity toward the resistant cancer cell line MES-SA/Dx5 and its parental MES-SA line. However, they are not toxic against P4 fibroblast cells in comparative studies. (author)

  1. RECYCLING OF PRINTED CIRCUIT BOARDS AIMING SILVER RECOVERY: A HYDROMETALLURGICAL ROUTE STUDY

    Directory of Open Access Journals (Sweden)

    Marcos Paulo Kohler Caldas

    2015-06-01

    Full Text Available The aim of this paper is characterize printed circuit board of computers and propose a hydrometallurgical route for silver recovery present in its composition. Initially, the printed circuit board was comminuted in both knife and hammer mills. The comminuted material was characterized by sieve analysis, chemical analysis by inductively coupled plasma optical emission spectrometry (ICP-OES and loss on ignition. Leaching tests were conducted in sulfuric acid, sulfuric acid in an oxidizing medium and nitric acid. The results indicated that the printed circuit board is mainly composed of copper (19.42%. Silver content of 0.045% was found. The route for silver recovery was leaching in sulfuric acid at 75°C for 18 hours. Then, leaching in sulfuric acid at 75°C in an oxidizing medium for 6 hours and nitric acid leaching at room temperature for 2 hours. Through of this route, 96.6% of silver was recovered.

  2. Investigation Of The Effects Of Heavy Metal Pollution In Black Sea Seaside Caused From Vehicles By Using Verbascum Sinuatum L. (Scrophulariaceae

    Directory of Open Access Journals (Sweden)

    Neslihan Duru

    2011-12-01

    Full Text Available In this study, the heavy metal pollution caused by vehicle traffic was investigated in the leaves of Verbascum sinuatum L.(Scrophulariaceae collected from the Blacksea coast ranging between Samsun, Ordu, Giresun, Trabzon, Rize and Hopa. Sample collection procedure was made in 23 stations in the related route. Heavy metal concentrations in the leaf samples of each station were determined with Perkin Emler Optic Emission Spectrometry (ICP-OES. Heavy metal concentration in samples was showed an order as Lead (Pb ; Zinc (Zn ; Chromium (Cr ; Nickel (Ni ; Copper (Cu ; Cadmium (Cd. The results of this study showed that the heavy metal accumulation in samples increased with an increase in traffic and V. sinuatum used as a biological indicator of this accumulation.

  3. Metals recovery of spent household batteries using a hydrometallurgical process

    International Nuclear Information System (INIS)

    Souza, K.P.; Tenorio, J.A.S.

    2010-01-01

    The objective of the work is to study a method for metals recovery from a sample composed by a mixture of the main types of spent household batteries. Segregation of the main metals is investigated using a treatment route consisting of the following steps: manual identified and dismantling, grinding, electric furnace reduction, acid leaching and selective precipitation with sodium hydroxide with and without hydrogen peroxide. Before and after precipitations the solutions had been analyzed by Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP/OES) and the precipitated analyzed by Scanning Electron Microscopy (SEM) with Spectrometry of Energy Dispersion Spectroscopy (EDS). The results had indicated that the great majority of metals had been precipitated in pHs studied, also had co-precipitation or simultaneous precipitation of metals in some pHs. (author)

  4. Use of dispersive liquid-liquid microextraction for simultaneous preconcentration of samarium, europium, gadolinium and dysprosium

    International Nuclear Information System (INIS)

    Mallah, M.H.; Atomic Energy Organization of Iran, Tehran; Shemirani, F.; Ghannadi Maragheh, M.

    2008-01-01

    A new preconcentration method of dispersive liquid-liquid microextraction (DLLME) was developed for simultaneous preconcentration of samarium, europium, gadolinium and dysprosium. DLLME technique was successfully used as a sample preparation method. In this preconcentration method, an appropriate mixture of extraction solvent, disperser solvent was injected rapidly into an aqueous solution containing Sm, Eu, Gd and Dy after complex formation using chelating reagent of the 1-(2-pyridylazo)-2-naphthol (PAN). After phase separation, 0.5 mL of the settled phase containing enriched analytes was determined by inductively coupled plasma optical emission spectrometry (ICP-OES). The main factors affected the preconcentration of Sm, Eu, Gd and Dy were extraction and dispersive solvent type and their volume, extraction time, volume of chelating agent (PAN), centrifuge speed and drying temperature of the samples. Under the best operating condition simultaneous preconcentration factors of 80, 100, 103 and 78 were obtained for Sm, Eu, Gd and Dy, respectively. (author)

  5. A Preliminary study of Sr/Ca thermometry in Chang Islands, Gulf of Thailand

    Directory of Open Access Journals (Sweden)

    Wararat Sirianansakul

    2014-10-01

    Full Text Available Variations in ratios of strontium-to-calcium (Sr/Ca for two Porites sp. coral specimens collected from Wai (PW and Loa Ya (PLY islands, part of Chang islands, Gulf of Thailand, were determined. Inductively coupled plasma optimal emission spectrometry (ICP-OES was used to analyze this ratio, which demonstrates annual cycles and the data is assumed to reflect the sea surface temperature (SST. Comparing the ratios with SST data, following Sr/Ca–SST relationships were determined PW: Sr/Ca (mmol/mol = 11.56–0.070×SST, PLY: Sr/Ca (mmol/mol = 11.89–0.081×SST. Our correlations are different from those previously reported; a discrepancy that may involve differences in analytical methods employed and abnormally low sea surface salinity (SSS (<30 psu in the Gulf of Thailand.

  6. Synthesis and Characterization of Chitosan Coated Manganese Zinc Ferrite Nanoparticles as MRI Contrast Agents

    Directory of Open Access Journals (Sweden)

    M. Zahraei

    2015-04-01

    Full Text Available Manganese zinc ferrite nanoparticles (MZF NPs were synthesized by using a direct, efficient and environmental friendly hydrothermal method. To improve the colloidal stability of MZF NPs for biomedical applications, NPs were coated with chitosan by ionic gelation technique using sodium tripolyphosphate (TPP as crosslinker. The synthesized NPs were characterized by X ray diffraction (XRD analysis, inductively coupled plasma optical emission spectrometry (ICP-OES, fourier transform infrared (FTIR spectroscopy, transmission electron microscopy (TEM, vibrating sample magnetometer (VSM and the dynamic light scattering (DLS methods. The results confirmed the spinel ferrite phase formation without any calcination process after synthesis. Mean particle size of bare NPs was around 14 nm. Moreover, certain molar ratio of chitosan to TPP was required for encapsulation of NPs in chitosan. Coated NPs showed hydrodynamic size of 300 nm and polydispersity index about 0.3.

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

    Science.gov (United States)

    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.

  8. Metals recovery of spent household batteries using a hydrometallurgical process; Recuperacao de metais de sucatas de pilhas e baterias pos-consumo utilizando processamento hidrometalurgico

    Energy Technology Data Exchange (ETDEWEB)

    Souza, K.P.; Tenorio, J.A.S., E-mail: kprovazi@gmail.co [Universidade de Sao Paulo (USP), SP (Brazil). Dept. de Engenharia Metalurgica e de Materiais

    2010-07-01

    The objective of the work is to study a method for metals recovery from a sample composed by a mixture of the main types of spent household batteries. Segregation of the main metals is investigated using a treatment route consisting of the following steps: manual identified and dismantling, grinding, electric furnace reduction, acid leaching and selective precipitation with sodium hydroxide with and without hydrogen peroxide. Before and after precipitations the solutions had been analyzed by Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP/OES) and the precipitated analyzed by Scanning Electron Microscopy (SEM) with Spectrometry of Energy Dispersion Spectroscopy (EDS). The results had indicated that the great majority of metals had been precipitated in pHs studied, also had co-precipitation or simultaneous precipitation of metals in some pHs. (author)

  9. Flotation separation of Cd, Co, Cr, Cu, Ni and Tl from calcium minerals and their determination by inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Zajkova-Paneva, Vesna; Stafilov, Trajche; Boev, Blazho

    2003-01-01

    The method of inductively coupled plasma-atomic spectrometry (ICP-AES), is developed for determination of Cd, Co, Cr, Cu, Ni and Tl in traces in calcite and gypsum. The interferences of Ca as matrix element on Co, Cr, Cu, Ni and Tl intensities during their ICP-AES determination are investigated. The results reveal that Ca does not interfere on intensities of Cr, but tends to decrease the intensity of the other elements. To eliminate those matrix interferences of Ca on trace elements intensities a flotation separation method is proposed. Lead(II) hexamethylenedithiocarbamate, Pb(HMDTC) 2 , is applied as a collector for flotation of trace elements from acidic solutions of mineral samples. The most suitable concentrations of calcite and gypsum solutions for flotation are ascertained. The detection limits of ICP-AES method following flotation of elements present in calcite and gypsum as impurities are determined: 0.022 and 0.061 μg·g -1 for Cd, 0.071 and 0.042 μg·g -1 for Co, 0.026 and 0.132 μg·g -1 for Cr, 0.164 and 0.149 μg·g -1 for Cu, 0.289 and 0.095 μg·g -1 for Ni and 0.645 and 0.7666 μg·g -1 for Tl, respectively. (Original)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-03-15

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

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

    International Nuclear Information System (INIS)

    Paredes, Eduardo; Maestre, Salvador E.; Todoli, Jose L.

    2006-01-01

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

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

    Science.gov (United States)

    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.

  13. Determination of fluorine by proton induced gamma ray emission (PIGE) spectrometry in igneous and metamorphic charnockitic rocks from Rogaland (S.W. Norway)

    International Nuclear Information System (INIS)

    Roelandts, I.; Robaye, G.; Weber, G.; Delbrouck, J.M.; Duchesne, J.C.

    1986-01-01

    More than 200 specimens from different occurrences of the Rogaland igneous complex and surrounding granulite facies metamorphic rocks (S.W. Norway) have been analysed by a direct non-destructive proton induced gamma ray emission (PIGE) technique. The fluorine contents vary from < 25 ppm to 3500 ppm. There is a good correlation between the concentration of fluorine and that of phosphorus for igneous rocks, suggesting a control of apatite on the F content. In metamorphic rocks, amphibole and biotite besides apatite are the principal concentrations of fluorine indicating that fluorine in the system is controlled by granulite facies metamorphism conditions. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-09-09

    Highlights: • Automatic oral bioaccessibility tests of trace metals under worst-case scenarios. • Use of intricate and realistic digestive fluids (UBM method). • Analysis of large amounts of soils (≥400 mg) in a flow-based configuration. • Smart interface to inductively coupled plasma atomic emission spectrometry. • Comparison of distinct flow systems mimicking physiological conditions. - Abstract: A novel biomimetic extraction procedure that allows for the in-line handing of ≥400 mg solid substrates is herein proposed for automatic ascertainment of trace element (TE) bioaccessibility in soils under worst-case conditions as per recommendations of ISO norms. A unified bioaccessibility/BARGE method (UBM)-like physiological-based extraction test is evaluated for the first time in a dynamic format for accurate assessment of in-vitro bioaccessibility of Cr, Cu, Ni, Pb and Zn in forest and residential-garden soils by on-line coupling of a hybrid flow set-up to inductively coupled plasma atomic emission spectrometry. Three biologically relevant operational extraction modes mimicking: (i) gastric juice extraction alone; (ii) saliva and gastric juice composite in unidirectional flow extraction format and (iii) saliva and gastric juice composite in a recirculation mode were thoroughly investigated. The extraction profiles of the three configurations using digestive fluids were proven to fit a first order reaction kinetic model for estimating the maximum TE bioaccessibility, that is, the actual worst-case scenario in human risk assessment protocols. A full factorial design, in which the sample amount (400–800 mg), the extractant flow rate (0.5–1.5 mL min{sup −1}) and the extraction temperature (27–37 °C) were selected as variables for the multivariate optimization studies in order to obtain the maximum TE extractability. Two soils of varied physicochemical properties were analysed and no significant differences were found at the 0.05 significance level

  15. 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

    International Nuclear Information System (INIS)

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

    2014-01-01

    Highlights: • Automatic oral bioaccessibility tests of trace metals under worst-case scenarios. • Use of intricate and realistic digestive fluids (UBM method). • Analysis of large amounts of soils (≥400 mg) in a flow-based configuration. • Smart interface to inductively coupled plasma atomic emission spectrometry. • Comparison of distinct flow systems mimicking physiological conditions. - Abstract: A novel biomimetic extraction procedure that allows for the in-line handing of ≥400 mg solid substrates is herein proposed for automatic ascertainment of trace element (TE) bioaccessibility in soils under worst-case conditions as per recommendations of ISO norms. A unified bioaccessibility/BARGE method (UBM)-like physiological-based extraction test is evaluated for the first time in a dynamic format for accurate assessment of in-vitro bioaccessibility of Cr, Cu, Ni, Pb and Zn in forest and residential-garden soils by on-line coupling of a hybrid flow set-up to inductively coupled plasma atomic emission spectrometry. Three biologically relevant operational extraction modes mimicking: (i) gastric juice extraction alone; (ii) saliva and gastric juice composite in unidirectional flow extraction format and (iii) saliva and gastric juice composite in a recirculation mode were thoroughly investigated. The extraction profiles of the three configurations using digestive fluids were proven to fit a first order reaction kinetic model for estimating the maximum TE bioaccessibility, that is, the actual worst-case scenario in human risk assessment protocols. A full factorial design, in which the sample amount (400–800 mg), the extractant flow rate (0.5–1.5 mL min −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

  16. Flow Injection Photochemical Vapor Generation Coupled with Miniaturized Solution-Cathode Glow Discharge Atomic Emission Spectrometry for Determination and Speciation Analysis of Mercury.

    Science.gov (United States)

    Mo, Jiamei; Li, Qing; Guo, Xiaohong; Zhang, Guoxia; Wang, Zheng

    2017-10-03

    A novel, compact, and green method was developed for the determination and speciation analysis of mercury, based on flow injection photochemical vapor generation (PVG) coupled with miniaturized solution cathode glow discharge-atomic emission spectroscopy (SCGD-AES). The SCGD was generated between a miniature hollow titanium tube and a solution emerging from a glass capillary. Cold mercury vapor (Hg(0)) was generated by PVG and subsequently delivered to the SCGD for excitation, and finally the emission signals were recorded by a miniaturized spectrograph. The detection limits (DLs) of Hg(II) and methylmercury (MeHg) were both determined to be 0.2 μg L -1 . Moreover, mercury speciation analysis could also be performed by using different wavelengths and powers from the UV lamp and irradiation times. Both Hg(II) and MeHg can be converted to Hg(0) for the determination of total mercury (T-Hg) with 8 W/254 nm UV lamp and 60 s irradiation time; while only Hg(II) can be reduced to Hg(0) and determined selectively with 4 W/365 nm UV lamp and 20 s irradiation time. Then, the concentration of MeHg can be calculated by subtracting the Hg(II) from the T-Hg. Because of its similar sensitivity and DL at 8 W/254 nm, the simpler and less toxic Hg(II) was used successfully as a primary standard for the quantification of T-Hg. The novel PVG-SCGD-AES system provides not only a 365-fold improvement in the DL for Hg(II) but also a nonchromatographic method for the speciation analysis of mercury. After validating its accuracy, this method was successfully used for mercury speciation analysis of water and biological samples.

  17. Algal Biomass Analysis by Laser-Based Analytical Techniques—A Review

    Czech Academy of Sciences Publication Activity Database

    Pořízka, P.; Procházková, P.; Procházka, D.; Sládková, L.; Novotný, J.; Petrilak, M.; Brada, M.; Samek, Ota; Pilát, Zdeněk; Zemánek, Pavel; Adam, V.; Kizek, R.; Novotný, K.; Kaiser, J.

    2014-01-01

    Roč. 14, 23 SEP (2014), s. 17725-17752 ISSN 1424-8220 R&D Projects: GA MŠk(CZ) LO1212; GA MŠk ED0017/01/01; GA ČR GAP205/11/1687 Institutional support: RVO:68081731 Keywords : Laser-Induced Breakdown Spectroscopy * LIBS * Laser-Ablation Inductively Coupled Plasma coupled with Mass Spectroscopy and Optical Emission Spectroscopy * LA-ICP-MS * LA-ICP-OES * ICP-OES * Raman spectroscopy * algae * algal biomass * biofuel * bioremediation Subject RIV: BH - Optics, Masers, Lasers Impact factor: 2.245, year: 2014

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-01-15

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

  19. Beta spectrometry

    International Nuclear Information System (INIS)

    Dryak, P.; Zderadicka, J.; Plch, J.; Kokta, L.; Novotna, P.

    1977-01-01

    For the purpose of beta spectrometry, a semiconductor spectrometer with one Si(Li) detector cooled with liquid nitrogen was designed. Geometrical detection efficiency is about 10% 4 sr. The achieved resolution for 624 keV conversion electrons of sup(137m)Ba is 2.6 keV (FWHM). A program was written in the FORTRAN language for the correction of the deformation of the measured spectra by backscattering in the analysis of continuous beta spectra. The method permits the determination of the maximum energy of the beta spectrum with an accuracy of +-5 keV. (author)

  20. Determination of trace amounts of lead, arsenic, nickel and cobalt in high-purity iron oxide pigment by inductively coupled plasma atomic emission spectrometry after iron matrix removal with extractant-contained resin

    International Nuclear Information System (INIS)

    Xu Yuyu; Zhou Jianfeng; Wang Guoxin; Zhou Jinfan; Tao Guanhong

    2007-01-01

    Inductively coupled plasma atomic emission spectrometry (ICP-AES) was applied to the determination of lead, arsenic, nickel and cobalt in high-purity iron oxide pigment. Samples were dissolved with hydrochloric acid and hydrogen peroxide. The digest was passed through a column, which was packed with a polymer resin containing a neutral organophosphorus extractant, tri-n-butylphosphate. Iron was sorbed selectively on the resin and the analytes of interest passed through the column, allowing the effective separation of them from the iron matrix. Conditions of separation were optimized. The detection limits (3σ) in solution were 10, 40, 7 and 5 μg L -1 , and in pigment were 0.2, 0.8, 0.14 and 0.1 mg kg -1 for lead, arsenic, cobalt and nickel, respectively. The recoveries ranged from 95% to 107% when sample digests were spiked with 5 μg of the analytes of interest, and relative standard deviations (n = 6) were 1.5-17.6% for the determination of the spiked samples. The method was successfully applied to the determination of trace amounts of these elements in high-purity iron oxide pigment samples

  1. Investigation of plasma-related matrix effects in inductively coupled plasma-atomic emission spectrometry caused by matrices with low second ionization potentials-identification of the secondary factor

    International Nuclear Information System (INIS)

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

    2006-01-01

    Plasma-related matrix effects induced by a comprehensive list of matrix elements (a total of fifty-one matrices) in inductively coupled plasma-atomic emission spectrometry were investigated and used to confirm that matrix effects caused by elements with a low second ionization potential are more severe than those from matrix elements having a low first ionization potential. Although the matrix effect is correlated unambiguously with the second ionization potential of a matrix, the correlation is not monotonic, which suggests that at least one other factor is operative. Through study of a large pool of matrix elements, it becomes possible to identify another critical parameter that defines the magnitude of the matrix effect; namely the presence of low-lying energy levels in the doubly charged matrix ion. Penning ionization by Ar excited states is proposed as the dominant mechanism for both analyte ionization/excitation and matrix effects; matrices with a low second ionization potential can effectively quench the population of Ar excited states through successive Penning ionization followed by ion-electron recombination and lead to more severe matrix effects

  2. An Investigation on the Extraction and Quantitation of a Hexavalent Chromium in Acrylonitrile Butadiene Styrene Copolymer (ABS) and Printed Circuit Board (PCB) by Ion Chromatography Coupled with Inductively Coupled Plasma Atomic Emission Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nam, Sang Ho; Kim, Yu Na [Mokpo National University, Muan (Korea, Republic of)

    2012-06-15

    A hexavalent chromium (Cr (VI)) is one of the hazardous substances regulated by the RoHS. The determination of Cr (VI) in various polymers and printed circuit board (PCB) has been very important. In this study, the three different analytical methods were investigated for the determination of a hexavalent chromium in Acrylonitrile Butadiene Styrene copolymer (ABS) and PCB. The results by three analytical methods were obtained and compared. An analytical method by UV-Visible spectrometer has been generally used for the determination of Cr (VI) in a sample, but a hexavalent chromium should complex with diphenylcarbazide for the detection in the method. The complexation did make an adverse effect on the quantitative analysis of Cr (VI) in ABS. The analytical method using diphenylcarbazide was also not applicable to printed circuit board (PCB) because PCB contained lots of irons. The irons interfered with the analysis of hexavalent chromium because those also could complex with diphenylcarbazide. In this study, hexavalent chromiums in PCB have been separated by ion chromatography (IC), then directly and selectively detected by inductively coupled plasma atomic emission spectrometry (ICP-AES). The quantity of Cr (VI) in PCB was 0.1 mg/kg

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

    Energy Technology Data Exchange (ETDEWEB)

    Palmieri, H.E.L.; Leonel, L.V. [Comissao Nacional de Energia Nuclear - Centro de Desenvolvimento da Tecnologia Nuclear, Belo Horizonte (Brazil)

    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 (NaBPh{sub 4}) 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 {mu}g/g and 0.1 {mu}g/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. (orig.)

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

    Science.gov (United States)

    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.

  5. A new nebulization device with exchangeable aerosol generation mode as a useful tool to investigate sample introduction processes in inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Grotti, Marco; Lagomarsino, Cristina; Frache, Roberto

    2004-01-01

    A new sample introduction device has been designed in order to differentiate between the effects of the aerosol production and its following desolvation on analytical performances of an inductively coupled plasma optical spectrometer. This research tool allows to easily switch between the pneumatic and ultrasonic aerosol generation mode and to use a joint desolvation chamber. In this way, a real comparison between aerosol production systems may be attained and the influence of aerosol generation process on analytical figures clearly distinguished from that of the desolvation process. In this work, the separate effects of the aerosol generation and desolvation processes on analytical sensitivity and tolerance towards matrix effects have been investigated. Concerning sensitivity, it was found that both the processes play an important role in determining emission intensities, being the increase in sensitivity due to desolvation higher than that due to the improved aerosol generation efficiency. Concerning the matrix effects, a predominant role of the desolvation system was found, while the influence of the aerosol generation mode was much less important. For nitric acid, the decreasing effect was mitigated by the presence of a desolvation system, due to partial removal of the acid. On the contrary, the depressive effect of sulfuric acid was enhanced by the presence of a desolvation system, due to degradation of the solvent removal efficiency and to further decrease in the analyte transport rate caused by clustering phenomena. Concerning the interferences due to sodium and calcium, a depressive effect was observed, which is enhanced by desolvation

  6. The determination of trace elements in commercial human serum albumin solutions by proton-induced X-ray emission spectrometry and neutron activation analysis

    International Nuclear Information System (INIS)

    Maenhaut, W.; De Reu, L.; Tomza, U.; Versieck, J.

    1982-01-01

    Particle induced X-ray emission (p.i.x.e.) and neutron activation analysis (n.a.a.) are proposed for determining the trace element content of human serum albumin. Application of these methods to some commercial albumin solutions provided concentration data for up to 19 elements, most of which were present at a level below a few μg ml -1 . The precision of the p.i.x.e. technique, as determined by irradiating up to 20 targets from one sample, was about 3% for those elements where counting statistics were good. A comparison between the p.i.x.e. and n.a.a. results showed close agreement, indicating that p.i.x.e. can yield data which are accurate to within 10%. Neutron activation showed very good sensitivity for the elements producing long-lived nuclides (tsub(1/2) >= 3 days), but had rather high detection limits for the other elements, unless radiochemical separations were used. (Auth.)

  7. Simultaneous determination of carbohydrates, carboxylic acids, alcohols, and metals in foods by high-performance liquid chromatography inductively coupled plasma atomic emission spectrometry.

    Science.gov (United States)

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

    2006-10-01

    The applicability of the HPLC-ICP-AES coupling for the simultaneous determination of carbohydrates, carboxylic acids, alcohols, and metals in a single chromatographic run has been demonstrated in the present work. Five saccharides, glucose, fructose, sucrose, sorbitol, and lactose; five carboxylic acids, citric, tartaric, malic, lactic, and acetic; and three alcohols, glycerol, ethanol, and methanol, have been determined. A H+ cation exchange column has been used to separate these compounds. The chromatograms have been obtained by monitoring the carbon emission signal at 193.09 nm. The results obtained by HPLC-ICP-AES have been compared against those found with conventional detection systems (i.e., refractive index, UV, and photodyode array detectors). The HPLC-ICP-AES method has shown the following features: (i) organic compounds and metals can be simultaneously determined; (ii) the detection method is universal; (iii) for nonvolatile organic compounds, a complete calibration line can be obtained from a single injection; and (iv) it provides absolute limits of detection similar to or lower than those found with conventional detection systems (i.e., on the order of several tens of nanograms of organic compound). The methodology has been validated through the analysis of food samples such as juices, isotonic beverages, wines, and a certified nonfat milk powder sample.

  8. Multielement detection limits and sample nebulization efficiencies of an improved ultrasonic nebulizer and a conventional pneumatic nebulizer in inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Olson, K.W.; Haas, W.J. Jr.; Fassel, V.A.

    1977-01-01

    Two important aspects of the analytical performance of a newly developed ultrasonic nebulizer and a specially designed pneumatic nebulizer have been compared for use in inductively coupled plasma--atomic emission spectroscopy (ICP-AES). The ultrasonic nebulizer, when combined with a conventional aerosol desolvation apparatus, provided an order of magnitude or more improvement in simultaneous multielement detection limits as compared to those obtained when the pneumatic nebulizer was used either with or without desolvation. Application of a novel method for direct measurement of the overall efficiency of nebulization to the two systems showed that an approximately tenfold greater rate of sample delivery to the plasma torch was primarily responsible for the superior detection limits afforded by the ultrasonic nebulizer. A unique feature of the ultrasonic nebulizer described is the protection against chemical attack which is achieved by completely enclosing the transducer in an acoustically coupled borosilicate glass cylinder. Direct sample introduction, convenient sample change, and rapid cleanout are other important characteristics of the system which make it an attractive alternate to pneumatic nebulizer systems

  9. Multielemental Determination of As, Bi, Ge, Sb, and Sn in Agricultural Samples Using Hydride Generation Coupled to Microwave-Induced Plasma Optical Emission Spectrometry.

    Science.gov (United States)

    Machado, Raquel C; Amaral, Clarice D B; Nóbrega, Joaquim A; Araujo Nogueira, Ana Rita

    2017-06-14

    A microwave-induced plasma optical emission spectrometer with N 2 -based plasma was combined with a multimode sample introduction system (MSIS) for hydride generation (HG) and multielemental determination of As, Bi, Ge, Sb, and Sn in samples of forage, bovine liver, powdered milk, agricultural gypsum, rice, and mineral fertilizer, using a single condition of prereduction and reduction. The accuracy of the developed analytical method was evaluated using certified reference materials of water and mineral fertilizer, and recoveries ranged from 95 to 106%. Addition and recovery experiments were carried out, and the recoveries varied from 85 to 117% for all samples evaluated. The limits of detection for As, Bi, Ge, Sb, and Sn were 0.46, 0.09, 0.19, 0.46, and 5.2 μg/L, respectively, for liquid samples, and 0.18, 0.04, 0.08, 0.19, and 2.1 mg/kg, respectively, for solid samples. The method proposed offers a simple, fast, multielemental, and robust alternative for successful determination of all five analytes in agricultural samples with low operational cost without compromising analytical performance.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-04-01

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

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

    International Nuclear Information System (INIS)

    Weagant, Scott; Dulai, Gurjit; Li, Lu; Karanassios, Vassili

    2015-01-01

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

  12. Chemical characterization of long-range transport biomass burning emissions to the Himalayas: insights from high-resolution aerosol mass spectrometry

    Science.gov (United States)

    Zhang, Xinghua; Xu, Jianzhong; Kang, Shichang; Liu, Yanmei; Zhang, Qi

    2018-04-01

    An intensive field measurement was conducted at a remote, background, high-altitude site (Qomolangma Station, QOMS, 4276 m a.s.l.) in the northern Himalayas, using an Aerodyne high-resolution time-of-flight aerosol mass spectrometer (HR-ToF-AMS) along with other collocated instruments. The field measurement was performed from 12 April to 12 May 2016 to chemically characterize the high time-resolved submicron particulate matter (PM1) and obtain the dynamic processes (emissions, transport, and chemical evolution) of biomass burning (BB), frequently transported from South Asia to the Himalayas during pre-monsoon season. Overall, the average (±1σ) PM1 mass concentration was 4.44 (±4.54) µg m-3 for the entire study, which is comparable with those observed at other remote sites worldwide. Organic aerosol (OA) was the dominant PM1 species (accounting for 54.3 % of total PM1 on average) followed by black carbon (BC) (25.0 %), sulfate (9.3 %), ammonium (5.8 %), nitrate (5.1 %), and chloride (0.4 %). The average size distributions of PM1 species all peaked at an overlapping accumulation mode (˜ 500 nm), suggesting that aerosol particles were internally well-mixed and aged during long-range transport. Positive matrix factorization (PMF) analysis on the high-resolution organic mass spectra identified three distinct OA factors, including a BB-related OA (BBOA, 43.7 %), a nitrogen-containing OA (NOA, 13.9 %) and a more-oxidized oxygenated OA (MO-OOA, 42.4 %). Two polluted episodes with enhanced PM1 mass loadings and elevated BBOA contributions from the west and southwest of QOMS during the study were observed. A typical BB plume was investigated in detail to illustrate the chemical evolution of aerosol characteristics under distinct air mass origins, meteorological conditions, and atmospheric oxidation processes.

  13. Comparison of 4 analytical techniques based on atomic spectrometry for the determination of total tin in canned foodstuffs

    OpenAIRE

    2011-01-01

    Abstract Different techniques for the determination of total tin in beverage and canned food by atomic spectrometry were compared. The performance characteristics of Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Hydride Generation Inductively Coupled Plasma Atomic Emission Spectrometry (HG-ICP-AES), Electrothermal Atomization Atomic Absorption Spectrometry (ETA-AAS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) were determined in term of linearity, ...

  14. Chemical characterization of long-range transport biomass burning emissions to the Himalayas: insights from high-resolution aerosol mass spectrometry

    Directory of Open Access Journals (Sweden)

    X. Zhang

    2018-04-01

    Full Text Available An intensive field measurement was conducted at a remote, background, high-altitude site (Qomolangma Station, QOMS, 4276 m a.s.l. in the northern Himalayas, using an Aerodyne high-resolution time-of-flight aerosol mass spectrometer (HR-ToF-AMS along with other collocated instruments. The field measurement was performed from 12 April to 12 May 2016 to chemically characterize the high time-resolved submicron particulate matter (PM1 and obtain the dynamic processes (emissions, transport, and chemical evolution of biomass burning (BB, frequently transported from South Asia to the Himalayas during pre-monsoon season. Overall, the average (±1σ PM1 mass concentration was 4.44 (±4.54 µg m−3 for the entire study, which is comparable with those observed at other remote sites worldwide. Organic aerosol (OA was the dominant PM1 species (accounting for 54.3 % of total PM1 on average followed by black carbon (BC (25.0 %, sulfate (9.3 %, ammonium (5.8 %, nitrate (5.1 %, and chloride (0.4 %. The average size distributions of PM1 species all peaked at an overlapping accumulation mode (∼ 500 nm, suggesting that aerosol particles were internally well-mixed and aged during long-range transport. Positive matrix factorization (PMF analysis on the high-resolution organic mass spectra identified three distinct OA factors, including a BB-related OA (BBOA, 43.7 %, a nitrogen-containing OA (NOA, 13.9 % and a more-oxidized oxygenated OA (MO-OOA, 42.4 %. Two polluted episodes with enhanced PM1 mass loadings and elevated BBOA contributions from the west and southwest of QOMS during the study were observed. A typical BB plume was investigated in detail to illustrate the chemical evolution of aerosol characteristics under distinct air mass origins, meteorological conditions, and atmospheric oxidation processes.

  15. Chemical quality of bottled mineral waters from markets of Curitiba-PR-Brazil

    Directory of Open Access Journals (Sweden)

    Éder José dos Santos

    Full Text Available ABSTRACT Twenty-seven bottled mineral waters from local markets in Curitiba, State of Paraná, Brazil were analyzed for a number of constituents, including: pH, conductivity, total dissolved solids, hardness, HCO3 - and CO 3 2-, as well as Ca2+, Mg2+, Na+, K+, NH4 + , F-, Cl-, NO3 -, NO2 - and SO4 2- by ion chromatography (IC; Al, Ba, Cd, Cr, Cu, Fe, Li, Mn, Ni, Sr, V and Zn by inductively coupled plasma optical emission spectrometry (ICP OES; Hg by cold vapor generation-ICP OES and As, Pb, Sb and Se by ICP-mass spectrometry (ICP-MS. The obtained limits of quantitation (LOQ were adequate for the determination of all analytes using the various analytical techniques. Results for the analysis of AccuStandard certified reference materials QCS-01-5, QCS-02-R1-5 and TCLP-02-1 as well as spike recoveries to samples show acceptable values, within 90-111 % of expected concentrations with relative standard deviations below 10 %, demonstrating the accuracy of the determinations. Both NO2 - and NO 3 - were above the maximum limits set by Brazilian legislation in two samples, indicating a microbiological contamination. One imported sample presented As (6.1 ± 0.2 µg L-1 near the maximum limit (10 µg L-1 while all other elements of interest were below the values specified by Brazilian legislation. Principal component analysis revealed that four imported samples and one from the Minas Gerais State have the highest mineral concentrations.

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

    International Nuclear Information System (INIS)

    Bauer, Mathieu; Broekaert, Jose A.C.

    2007-01-01

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

  17. Chromium Speciation Analysis by Ion Chromatography Coupled ...

    African Journals Online (AJOL)

    Two methods coupling ion chromatography with inductively coupled plasma - optical emission spectroscopy (ICP-OES) were developed for the simultaneous separation and determination of Cr(III) and Cr(VI) species. In the first method, anion chromatography with sodium bicarbonate/carbonate solution as the eluent was ...

  18. Removal of Uranium from Aqueous Solutions using Ammonium ...

    African Journals Online (AJOL)

    NICOLAAS

    content was determined by Inductively Coupled Plasma Optical Emission Specroscopy (ICP-OES). The removal of uranium ... systems and may influence the surface properties of such adsorbents. .... The high silica content of the natural zeolite makes it more ..... average drop of 24.94 %) due to competition for binding sites.

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

    Science.gov (United States)

    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.

  20. Studies on the preparation of {sup 68}Ge-{sup 68}Ga generator with inorganic materials

    Energy Technology Data Exchange (ETDEWEB)

    Brambilla, Tania P.; Osso Junior, Joao A., E-mail: jaosso@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2011-07-01

    {sup 68}Ga as a positron emitter is of great interest because of some important advantages. It has a physical half-life of 67.71 min, which is compatible with the pharmacokinetics of many radiopharmaceuticals of low molecular weight. Other important characteristic is its cyclotron-independent availability via the {sup 68}Ge-{sup 68}Ga radionuclide generator system. In Brazil only one positron emitter radionuclide is produced, {sup 18}F, and the medical class has a great interest in using {sup 68}Ga labeled molecules, in particular peptides such as DOTA-octriotide. A project for developing a home made {sup 68}Ge-{sup 68}Ga is under way at IPEN-CNEN/SP. The aim of this work is to develop an efficient and simplified generator system of {sup 68}Ge-{sup 68}Ga that offers {sup 68}Ga{sup 3+} adequate for clinical use. Initial results will be reported concerning the behavior of Ge and Ga in adsorbers such as calcined acid and basic Al{sub 2}O{sub 3}, HZO (hydrous zirconium oxide), TiO{sub 2}, microspheres of Zr (Zr mic) and microspheres of Al (Al mic). Adsorption studies were carried out using {gamma}-emitting tracers, {sup 67}Ga and {sup 68}Ga and chemical tracer, GeO{sub 2}. The samples containing {sup 67}/{sup 68}Ga were analysed using a dose calibrator CRC-15R from Capintec and the samples containing Ge were evaluated by the Optical Emission Spectrometry using Inductively Coupled Plasma (ICP-OES). The ICP-OES equipment used was a Varian Vista-MPX from Varian and calibration curves for Ge were constructed in the range of 0.2 to 1.0 {mu}g.mL{sup -1}. The use of basic Al{sub 2}O{sub 3}, TiO{sub 2}, HZO and Zr mic showed the more promising results. (author)

  1. Nuclear techniques for the study of environmental pollution and control: experience and facilities at PINSTECH

    International Nuclear Information System (INIS)

    Rajput, M.U.; Butt, N.M.

    2001-01-01

    Environmental pollution is a worldwide problem. Developed countries have already gone in the clutches of pollution. Now the rapid industrialization and modernization process has also started in the developing countries. This is posing a serious threat to their own environment. One of the important factors in the pollution control measures is to investigate the levels of environmental pollution, from time to time, by effective and reliable methods. Nuclear techniques due to their high sensitivities play an important role in this regard. These techniques have the potential to determine the concentration of pollutants in trace level quantities (ppm and ppb) and for locating the possible pollution sources such as power plants, refineries, municipal waste, industries etc. Pakistan Institute of Nuclear Science and Technology (PINSTECH) has qualified and experienced scientists and has nearly all the major nuclear facilities that are needed for environmental research such as mass spectrometry, tracer techniques, neutron activation analysis (NAA), X-ray fluorescence spectrometry (XRFS), atomic absorption spectrometry (AAS), atomic emission spectrometry (AES), inductively coupled plasma-optical emission spectrometry (ICP-OES) etc. This paper discusses the importance of environmental pollution with a particular reference to the pollution aspects in Pakistan and the associated environmental research experience based on nuclear methods available at PINSTECH. 308 refs. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

    Picoloto, Rochele S. [Núcleo de Química, Universidade Tecnológica Federal do Paraná, 85884-000 Medianeira, PR (Brazil); Doneda, Morgana [Departamento de Química, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Flores, Eder L.M. [Núcleo de Química, Universidade Tecnológica Federal do Paraná, 85884-000 Medianeira, PR (Brazil); Mesko, Marcia F. [Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, 96010-610 Pelotas, RS (Brazil); Flores, Erico M.M. [Departamento de Química, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Mello, Paola A., E-mail: paola.mello@ufsm.br [Departamento de Química, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil)

    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{sup −1}) were investigated as absorbing solutions and accurate results were achieved using a 25 mmol L{sup −1} NH{sub 4}OH 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 NH{sub 4}OH and tetramethylammonium hydroxide solutions. Solutions obtained after digestion by MIC (whole milk powder) presented low carbon content in digests (< 25 mg L{sup −1}) while solutions obtained after alkaline extraction presented up to 10,000 mg L{sup −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{sup −1} for Br and I, respectively, while for MW-AE were 0.1 and 0.05 μg g{sup −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

  3. Routine Isotopic Analysis of 235U by Emission Spectrometry. 1. Interferometry using electrode-less discharge lamps 2. determination of the 235U/238U ratio using a spectrograph and electrode-less lamps

    International Nuclear Information System (INIS)

    Capitini, R.; Ceccaldi, M.; Leicknam, J.P.; Rabec, J.

    1968-01-01

    I. A 'HYPEAC' interferometric apparatus has been used for routine determination of uranium 235. In order to facilitate the examination of non-metallic samples and to reduce the time required for analysis it has been necessary to replace the hollow-cathode light sources usually used by electrode-less discharge lamps. The preparation outside the apparatus of such lamps containing uranium tetrachloride is described; the process is simple and rapid: about ninety minutes for each, and several lamps can be built simultaneously, thus reducing still further the total time required for each analysis. The amount of sample required is about a few milligrams. In order to counteract any spontaneous optical dis-adjustment which could prevent the application of the usual isotopic abundance method, it is necessary to compare the sample spectra with those of standards, all these spectra being recorded successively and alternately. A series of examples of determinations involving over 150 measurements is presented and discussed. For samples with abundances similar to that of natural uranium and up to 5 per cent of the 235 isotope., the reproducibility is of the order of 2 per cent, the relative accuracy being ± 2 to 3 per cent; for samples enriched in uranium 235 (5 to 93 per cent) the relative accuracy can attain ± 0.5 per cent. II. In spite of the large amount of research into the improvement of the accuracy of uranium isotope analyses using optical methods, it has not been possible up to the present to develop a method as good as mass spectrometry. When it is not necessary to have a high accuracy, however, emission spectroscopy which has no memory effect can constitute a complementary method of analysis if it is sufficiently fast and economical; for this to happen it seems to us that it should be possible to apply such a method in laboratories equipped with all the usual spectrochemical analysis equipment. In the present work we have therefore set out to obtain an acceptable

  4. Reactor gamma spectrometry: status

    International Nuclear Information System (INIS)

    Gold, R.; Kaiser, B.J.

    1979-01-01

    Current work is described for Compton Recoil Gamma-Ray Spectrometry including developments in experimental technique as well as recent reactor spectrometry measurements. The current status of the method is described concerning gamma spectromoetry probe design and response characteristics. Emphasis is given to gamma spectrometry work in US LWR and BR programs. Gamma spectrometry in BR environments are outlined by focussing on start-up plans for the Fast Test Reactor (FTR). Gamma spectrometry results are presented for a LWR pressure vessel mockup in the Poolside Critical Assembly (PCA) at Oak Ridge National Laboratory

  5. Ion detection in mass spectrometry

    International Nuclear Information System (INIS)

    Bolbach, Gerard

    2016-03-01

    This course aims at providing some elements for a better understanding of ion detectors used in mass spectrometers, of their operations, and of their limitations. A first part addresses the functions and properties of an ideal detector, how to detect ions in gas phase, and particle detectors and ion detectors used in mass spectrometry. The second part proposes an overview of currently used detectors with respect to their operation principle: detection from the ion charge (Faraday cylinder), detection by inductive effects (FTICR, Fourier Transform Ion Cyclotron Resonance), and detection by secondary electron emission. The third part discusses the specificities of secondary electron emission. The fourth one addresses operating modes and parameters related to detectors. The sixth part proposes a prospective view on future detectors by addressing the following issues: cryo-detector, inductive effect and charge detectors, ion detection and nano materials

  6. 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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-11-15

    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 {mu}L, 1-10 {mu}L and 10-100 {mu}L) 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 {mu}L volumes) expressed in absolute-amounts ranged between 4 pg for Pb to 0.3 fg ({approx} 5 million atoms) for Ca. Detection limits expressed in concentration units (obtained using 100 {mu}L 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

  7. Evaluation of laser induced breakdown spectroscopy for cadmium determination in soils

    International Nuclear Information System (INIS)

    Santos, Dario; Nunes, Lidiane C.; Trevizan, Lilian C.; Godoi, Quienly; Leme, Flavio O.; Braga, Jez Willian B.; Krug, Francisco Jose

    2009-01-01

    Cadmium is known to be a toxic agent that accumulates in the living organisms and present high toxicity potential over lifetime. Efforts towards the development of methods for microanalysis of environmental samples, including the determination of this element by graphite furnace atomic absorption spectrometry (GFAAS), inductively coupled plasma optical emission spectrometry (ICP OES), and inductively coupled plasma-mass spectrometry (ICP-MS) techniques, have been increasing. Laser induced breakdown spectroscopy (LIBS) is an emerging technique dedicated to microanalysis and there is a lack of information dealing with the determination of cadmium. The aim of this work is to demonstrate the feasibility of LIBS for cadmium detection in soils. The experimental setup was designed using a laser Q-switched (Nd:YAG, 10 Hz, λ = 1064 nm) and the emission signals were collimated by lenses into an optical fiber coupled to a high-resolution intensified charge-coupled device (ICCD)-echelle spectrometer. Samples were cryogenically ground and thereafter pelletized before LIBS analysis. Best results were achieved by exploring a test portion (i.e. sampling spots) with larger surface area, which contributes to diminish the uncertainty due to element specific microheterogeneity. Calibration curves for cadmium determination were achieved using certified reference materials. The metrological figures of merit indicate that LIBS can be recommended for screening of cadmium contamination in soils.

  8. Methods of neutron spectrometry

    International Nuclear Information System (INIS)

    Doerschel, B.

    1981-01-01

    The different methods of neutron spectrometry are based on the direct measurement of neutron velocity or on the use of suitable energy-dependent interaction processes. In the latter case the measuring effect of a detector is connected with the searched neutron spectrum by an integral equation. The solution needs suitable unfolding procedures. The most important methods of neutron spectrometry are the time-of-flight method, the crystal spectrometry, the neutron spectrometry by use of elastic collisions with hydrogen nuclei, and neutron spectrometry with the aid of nuclear reactions, especially of the neutron-induced activation. The advantages and disadvantages of these methods are contrasted considering the resolution, the measurable energy range, the sensitivity, and the experimental and computational efforts. (author)

  9. Flow injection analysis in inductively coupled plasma spectrometry

    International Nuclear Information System (INIS)

    Rosias, Maria F.G.G.

    1995-10-01

    The main features of flow injection analysis (FIA) as contribution to the inductively coupled plasma (Icp) spectrometry are described. A systematic review of researches using the combined FIA-Icp and the benefits of this association are presented. Flow systems were proposed to perform on-line Icp solution management for multielemental determination by atomic emission spectrometry (Icp-AES) or mass spectrometry. The inclusion of on-line ion exchangers in flow systems for matrix separation and/or analyte preconcentration are presented. Together with those applications the new advent of instruments with facilities for multielement detection on flow injection signals are described. (author). 75 refs., 19 figs

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-12-15

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

  11. Atomic mass spectrometry

    International Nuclear Information System (INIS)

    Sanz-Medel, A.

    1997-01-01

    The elemental inorganic analysis seems to be dominated today by techniques based on atomic spectrometry. After an evaluation of advantages and limitations of using mass analysers (ion detectors) versus conventional photomultipliers (photon detector) a brief review of the more popular techniques of the emerging Atomic Mass spectrometry is carried out. Their huge potential for inorganic trace analysis is such that in the future we could well witness how this end of the century and millennium marked the fall of the photons empire in Analytical Atomic Spectrometry. (Author)

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

    Science.gov (United States)

    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.

  13. Characterization of acid tars

    International Nuclear Information System (INIS)

    Leonard, Sunday A.; Stegemann, Julia A.; Roy, Amitava

    2010-01-01

    Acid tars from the processing of petroleum and petrochemicals using sulfuric acid were characterized by gas chromatography/mass spectrometry (GC/MS), inductively coupled plasma/optical emission spectrometry (ICP/OES), differential scanning calorimetry (DSC), Fourier transform infrared (FTIR) spectrometry, and scanning electron microscopy/energy dispersive X-ray (SEM/EDX) micro-analysis. Leaching of contaminants from the acid tars in 48 h batch tests with distilled water at a liquid-to-solid ratio 10:1 was also studied. GC/MS results show that the samples contained aliphatic hydrocarbons, cyclic hydrocarbons, up to 12 of the 16 USEPA priority polycyclic aromatic hydrocarbons (PAHs), and numerous other organic groups, including organic acids (sulfonic acids, carboxylic acids and aromatic acids), phenyl, nitrile, amide, furans, thiophenes, pyrroles, and phthalates, many of which are toxic. Metals analysis shows that Pb was present in significant concentration. DSC results show different transition peaks in the studied samples, demonstrating their complexity and variability. FTIR analysis further confirmed the presence of the organic groups detected by GC/MS. The SEM/EDX micro-analysis results provided insight on the surface characteristics of the samples and show that contaminants distribution was heterogeneous. The results provide useful data on the composition, complexity, and variability of acid tars; information which hitherto have been scarce in public domain.

  14. Designing of Synergistic Waste Mixtures for Multiphase Reactive Smelting

    Directory of Open Access Journals (Sweden)

    Vaso Manojlović

    2016-06-01

    Full Text Available Electric arc furnace (EAF dust, together with a mill scale and coke were smelted in a laboratory electric arc furnace. These metallurgical wastes consist of a many different phases and elements, making the reaction process complex. Thermo-chemical analysis of the reactions in metal, slag, and gas phases was done, and used for modeling of the mixture composition and energy consumption required for smelting. Modelling was performed with the software named RikiAlC. The crude ZnO, slag, and metal phase were analyzed using the atomic absorption spectrometry (AAS, the optical emission spectrometry with inductively coupled plasma (ICP-OES, the X-ray diffraction (XRD, the scanning electron microscopy (SEM equipped with energy dispersive spectrometry (EDS, and reflected and transmitted light microscopy. Also, in order to follow the behavior of this process the exhausted gases were monitored. The synergetic effects of the designed mixture may be recognized in minimizing energy consumption for the smelting process, improving the product yield efficiency, and reducing the negative environmental effects.

  15. Investigation of the remaining major and trace elements in clean coal generated by organic solvent extraction

    Energy Technology Data Exchange (ETDEWEB)

    Jie Wang; Chunqi Li; Kinya Sakanishi; Tetsuya Nakazato; Hiroaki Tao; Toshimasa Takanohashi; Takayuki Takarada; Ikuo Saito [National Institute Advanced Industrial Science and Technology (AIST), Ibaraki (Japan). Energy Technology Research Institute

    2005-09-01

    A sub-bituminous Wyodak coal (WD coal) and a bituminous Illinois No. 6 coal (IL coal) were thermally extracted with 1-methylnaphthalene (1-MN) and N-methyl-2-pyrrolidone (NMP) to produce clean extract. A mild pretreatment with acetic acid was also carried out. Major and trace inorganic elements in the raw coals and resultant extracts were determined by means of inductively coupled plasma optical emission spectrometry (ICP-OES), flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS), and cold vapor atomic absorption spectrometry (CV-AAS). It was found that the extraction with 1-MN resulted in 73-100% reductions in the concentration of Li, Be, V, Ga, As, Se, Sr, Cd, Ba, Hg, and Pb. The extraction with NMP yielded more extract than that with 1-MN, but it retained more organically associated major and trace metals in the extracts. In the extraction of WD coal with NMP, the acid pretreatment not only significantly enhanced the extraction yield but also significantly reduced the concentrations of alkaline earth elements such as Be, Ca, Mg, Sr, and Ba in the extract. In addition, the modes of occurrence of trace elements in the coals were discussed according to their extraction behaviors. 30 refs., 2 figs., 5 tabs.

  16. Characterization of acid tars

    Energy Technology Data Exchange (ETDEWEB)

    Leonard, Sunday A., E-mail: sunday.leonard@ucl.ac.uk [Department of Civil Environmental and Geomatic Engineering, University College London, Chadwick Building, Gower Street, London, WC1E 6BT (United Kingdom); Stegemann, Julia A. [Department of Civil Environmental and Geomatic Engineering, University College London, Chadwick Building, Gower Street, London, WC1E 6BT (United Kingdom); Roy, Amitava [J. Bennett Johnston, Sr., Centre for Advance Microstructures and Devices (CAMD), 6980 Jefferson Highway, Louisiana State University, Baton Rouge, LA, 70806 (United States)

    2010-03-15

    Acid tars from the processing of petroleum and petrochemicals using sulfuric acid were characterized by gas chromatography/mass spectrometry (GC/MS), inductively coupled plasma/optical emission spectrometry (ICP/OES), differential scanning calorimetry (DSC), Fourier transform infrared (FTIR) spectrometry, and scanning electron microscopy/energy dispersive X-ray (SEM/EDX) micro-analysis. Leaching of contaminants from the acid tars in 48 h batch tests with distilled water at a liquid-to-solid ratio 10:1 was also studied. GC/MS results show that the samples contained aliphatic hydrocarbons, cyclic hydrocarbons, up to 12 of the 16 USEPA priority polycyclic aromatic hydrocarbons (PAHs), and numerous other organic groups, including organic acids (sulfonic acids, carboxylic acids and aromatic acids), phenyl, nitrile, amide, furans, thiophenes, pyrroles, and phthalates, many of which are toxic. Metals analysis shows that Pb was present in significant concentration. DSC results show different transition peaks in the studied samples, demonstrating their complexity and variability. FTIR analysis further confirmed the presence of the organic groups detected by GC/MS. The SEM/EDX micro-analysis results provided insight on the surface characteristics of the samples and show that contaminants distribution was heterogeneous. The results provide useful data on the composition, complexity, and variability of acid tars; information which hitherto have been scarce in public domain.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  19. HEAVY METALS LEVELS IN LARUS DOMINICANUS. CASE STUDY: COROA GRANDE MANGROVE, SEPETIBA BAY, RIO DE JANEIRO, BRAZIL

    OpenAIRE

    Aldo Pacheco Ferreira

    2011-01-01

    Samples of liver and kidney of Kelp gull (Larus dominicanus) collected on Sepetiba Bay, Rio de Janeiro, Brazil, were analysed for their copper, zinc, cadmium, lead, chromium and nickel content. All the analyses were made using the inductively coupled plasma optical spectrometry method (ICP-OES). The investigation focused on the variability of the elements content in kidney and liver from a number of sampling seabirds and over different seasons. The results were interpreted using the analysis ...

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

    Directory of Open Access Journals (Sweden)

    Leila Amiri

    2016-12-01

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

  1. Software for nuclear spectrometry

    International Nuclear Information System (INIS)

    1998-10-01

    The Advisory Group Meeting (AGM) on Software for Nuclear Spectrometry was dedicated to review the present status of software for nuclear spectrometry and to advise on future activities in this field. Because similar AGM and consultant's meetings had been held in the past; together with an attempt to get more streamlined, this AGM was devoted to the specific field of software for gamma ray spectrometry. Nevertheless, many of the issues discussed and the recommendations made are of general concern for any software on nuclear spectrometry. The report is organized by sections. The 'Summary' gives conclusions and recommendations adopted at the AGM. These conclusions and recommendations resulted from the discussions held during and after presentations of the scientific and technical papers. These papers are reported here in their integral form in the following Sections

  2. Glycomics using mass spectrometry

    OpenAIRE

    Wuhrer, Manfred

    2013-01-01

    Mass spectrometry plays an increasingly important role in structural glycomics. This review provides an overview on currently used mass spectrometric approaches such as the characterization of glycans, the analysis of glycopeptides obtained by proteolytic cleavage of proteins and the analysis of glycosphingolipids. The given examples are demonstrating the application of mass spectrometry to study glycosylation changes associated with congenital disorders of glycosylation, lysosomal storage di...

  3. Ion mobility spectrometry

    CERN Document Server

    Eiceman, GA

    2005-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Mello, Paola A.; Diehl, Lisarb O.; Oliveira, Jussiane S.S.; Muller, Edson I. [Departamento de Química, Universidade Federal de Santa Maria, Av. Roraima, 1000, 97105-900, Santa Maria (Brazil); Mesko, Marcia F. [Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, Campus Capão do Leão, 96900-010 Pelotas, RS (Brazil); Flores, Erico M.M., E-mail: ericommf@gmail.com [Departamento de Química, Universidade Federal de Santa Maria, Av. Roraima, 1000, 97105-900, Santa Maria (Brazil)

    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 (HNO{sub 3} or HNO{sub 3} plus HCl) were evaluated for metals and metalloids and NH{sub 4}OH 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{sup −1} for Co by ICP-MS up to 3.120 μg g{sup −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 HNO{sub 3} and HCl for digestion showed to be crucial for quantitative recovery of some elements, as Cr and Sb

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

    Energy Technology Data Exchange (ETDEWEB)

    Picoloto, Rochele S. [Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil and Instituto Nacional de Ciência e Tecnologia de Bioanalítica, Campinas, SP (Brazil); Wiltsche, Helmar; Knapp, Günter [Institute of Analytical Chemistry and Food Chemistry, Graz University of Technology, Graz (Austria); Mello, Paola A. [Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil and Instituto Nacional de Ciência e Tecnologia de Bioanalítica, Campinas, SP (Brazil); Barin, Juliano S. [Departamento de Tecnologia e Ciência dos Alimentos, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS (Brazil); Flores, Erico M.M., E-mail: ericommf@gmail.com [Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil and Instituto Nacional de Ciência e Tecnologia de Bioanalítica, Campinas, SP (Brazil)

    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 O{sub 2}. Analytes were volatilized from soil during combustion and quantitatively absorbed in a suitable solution: nitric acid (1, 2, 4 or 6 mol L{sup −1}) or a solution of nitric (2 mol L{sup −1}) and hydrochloric (1, 2 or 4 mol L{sup −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{sup −1} HNO{sub 3} and 2 mol L{sup −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{sup −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. - Highlights: ► Microwave-induced combustion method was applied for soil samples. ► Analytes were volatilized during MIC allowing a suitable separation from matrix. ► Matrix interferences during the determination step are minimized. ► As, Cd, Hg and Pb were determined by ICP-MS. ► Diluted acid solutions were

  6. Metal and trace element sediment assessment from Guarapiranga reservoir, Alto Tiete Basin, Sao Paulo, SP, Brazil; Avaliacao da concentracao de metais e elementos traco em amostras de sedimento do reservatorio Guarapiranga, Sao Paulo, SP, Brasil

    Energy Technology Data Exchange (ETDEWEB)

    Guimaraes, Guilherme Moura

    2011-07-01

    The Guarapiranga Reservoir, located in Sao Paulo metropolitan region, Brazil, is responsible for supplying about 20% of the entire population's water needs of this region or approximately 3.7 million people. However, this system has shown significant degradation in water quality, due to untreated domestic sewage and industrial effluents. In this study sediment samples were collected at five points along the reservoir and total concentration of some major (Fe, K and Na), trace (As, Ba, Br, Co, Cr, Cs, Hf, Hg, Rb, Sb, Sc, Ta, Tb, Th, U, V and Zn) and rare earth (Ce, Eu, La, Lu, Nd, Sm, Tb and Yb) elements were determined by instrumental neutron activation analysis (INAA). By inductively coupled plasma optical emission spectrometry (ICP OES) the concentrations of Al, Ba, Be, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, Pb, Ti, V e Zn were determined after digestion procedure following US EPA 3051 methodology. The concentrations of metals Cd and Pb were determined by graphite furnace atomic absorption spectrometry (GFAAS) and total Hg by cold vapor atomic absorption spectrometry (CVAAS). Methodology validation according to precision and accuracy was performed by reference materials analyses for the three different analytical techniques used. Multielemental results obtained by INAA were compared to NASC (North American Shale Composite), Upper Continental Crust (UCC) and soil from Guarapiranga park values. The Enrichment Factor (EF) and Geo accumulation Index (Igeo) were also evaluated for these data. Metal concentration results by ICP OES and AAS in the samples were compared to the TEL and PEL oriented values established by the Canadian Council of Ministers of the Environment and also adopted by CETESB (Environmental Protection Agency of the Sao Paulo State). The results were also compared to regional reference values (VRR) of limnic sediments from the Alto Tiete Basin. From these data an assessment of metal and trace element accumulated in the sediments from the

  7. Metal and trace element sediment assessment from Guarapiranga reservoir, Alto Tiete Basin, Sao Paulo, SP, Brazil

    International Nuclear Information System (INIS)

    Guimaraes, Guilherme Moura

    2011-01-01

    The Guarapiranga Reservoir, located in Sao Paulo metropolitan region, Brazil, is responsible for supplying about 20% of the entire population's water needs of this region or approximately 3.7 million people. However, this system has shown significant degradation in water quality, due to untreated domestic sewage and industrial effluents. In this study sediment samples were collected at five points along the reservoir and total concentration of some major (Fe, K and Na), trace (As, Ba, Br, Co, Cr, Cs, Hf, Hg, Rb, Sb, Sc, Ta, Tb, Th, U, V and Zn) and rare earth (Ce, Eu, La, Lu, Nd, Sm, Tb and Yb) elements were determined by instrumental neutron activation analysis (INAA). By inductively coupled plasma optical emission spectrometry (ICP OES) the concentrations of Al, Ba, Be, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, Pb, Ti, V e Zn were determined after digestion procedure following US EPA 3051 methodology. The concentrations of metals Cd and Pb were determined by graphite furnace atomic absorption spectrometry (GFAAS) and total Hg by cold vapor atomic absorption spectrometry (CVAAS). Methodology validation according to precision and accuracy was performed by reference materials analyses for the three different analytical techniques used. Multielemental results obtained by INAA were compared to NASC (North American Shale Composite), Upper Continental Crust (UCC) and soil from Guarapiranga park values. The Enrichment Factor (EF) and Geo accumulation Index (Igeo) were also evaluated for these data. Metal concentration results by ICP OES and AAS in the samples were compared to the TEL and PEL oriented values established by the Canadian Council of Ministers of the Environment and also adopted by CETESB (Environmental Protection Agency of the Sao Paulo State). The results were also compared to regional reference values (VRR) of limnic sediments from the Alto Tiete Basin. From these data an assessment of metal and trace element accumulated in the sediments from the

  8. Metal and trace element sediment assessment from Guarapiranga reservoir, Alto Tiete Basin, Sao Paulo, SP, Brazil; Avaliacao da concentracao de metais e elementos traco em amostras de sedimento do reservatorio Guarapiranga, Sao Paulo, SP, Brasil

    Energy Technology Data Exchange (ETDEWEB)

    Guimaraes, Guilherme Moura

    2011-07-01

    The Guarapiranga Reservoir, located in Sao Paulo metropolitan region, Brazil, is responsible for supplying about 20% of the entire population's water needs of this region or approximately 3.7 million people. However, this system has shown significant degradation in water quality, due to untreated domestic sewage and industrial effluents. In this study sediment samples were collected at five points along the reservoir and total concentration of some major (Fe, K and Na), trace (As, Ba, Br, Co, Cr, Cs, Hf, Hg, Rb, Sb, Sc, Ta, Tb, Th, U, V and Zn) and rare earth (Ce, Eu, La, Lu, Nd, Sm, Tb and Yb) elements were determined by instrumental neutron activation analysis (INAA). By inductively coupled plasma optical emission spectrometry (ICP OES) the concentrations of Al, Ba, Be, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, Pb, Ti, V e Zn were determined after digestion procedure following US EPA 3051 methodology. The concentrations of metals Cd and Pb were determined by graphite furnace atomic absorption spectrometry (GFAAS) and total Hg by cold vapor atomic absorption spectrometry (CVAAS). Methodology validation according to precision and accuracy was performed by reference materials analyses for the three different analytical techniques used. Multielemental results obtained by INAA were compared to NASC (North American Shale Composite), Upper Continental Crust (UCC) and soil from Guarapiranga park values. The Enrichment Factor (EF) and Geo accumulation Index (Igeo) were also evaluated for these data. Metal concentration results by ICP OES and AAS in the samples were compared to the TEL and PEL oriented values established by the Canadian Council of Ministers of the Environment and also adopted by CETESB (Environmental Protection Agency of the Sao Paulo State). The results were also compared to regional reference values (VRR) of limnic sediments from the Alto Tiete Basin. From these data an assessment of metal and trace element accumulated in the sediments from the

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

    Science.gov (United States)

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

    2013-09-01

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

  10. Acoustic emission

    International Nuclear Information System (INIS)

    Nichols, R.W.

    1976-01-01

    The volume contains six papers which together provide an overall review of the inspection technique known as acoustic emission or stress wave emission. The titles are: a welder's introduction to acoustic emission technology; use of acoustic emission for detection of defects as they arise during fabrication; examples of laboratory application and assessment of acoustic emission in the United Kingdom; (Part I: acoustic emission behaviour of low alloy steels; Part II: fatigue crack assessment from proof testing and continuous monitoring); inspection of selected areas of engineering structures by acoustic emission; Japanese experience in laboratory and practical applications of acoustic emission to welded structures; and ASME acoustic emission code status. (U.K.)

  11. Nanostructured inorganic materials: Synthesis and associated electrochemical properties

    Science.gov (United States)

    Yau, Shali Zhu

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

  12. Quantitative determination of impurities in nuclear grade aluminum by Flame-Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Jat, J.R.; Nayak, A.K.; Balaji Rao, Y.; Ravindra, H.R.

    2013-01-01

    The paper deals with quantitative determination of impurity elements in nuclear grade aluminum, used as fin tubes in research reactors, by Flame-Atomic Absorption Spectrometry (F-AAS). The results have been compared with those obtained by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) method. Experimental conditions used in both the methods are given in the paper. (author)

  13. Forensic Mass Spectrometry

    Science.gov (United States)

    Hoffmann, William D.; Jackson, Glen P.

    2015-07-01

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

  14. Fourier Transform Mass Spectrometry

    Science.gov (United States)

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

    2011-01-01

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

  15. Ambient ionization mass spectrometry

    International Nuclear Information System (INIS)

    Lebedev, A T

    2015-01-01

    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

  16. Velocity-space sensitivity of neutron spectrometry measurements

    DEFF Research Database (Denmark)

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

    2015-01-01

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

  17. Regulatory quality control in the metal and semi metal environmental monitoring program at IPEN/CNEN-SP

    International Nuclear Information System (INIS)

    Faustino, Mainara G.; Silva, Doulgas Batista; Monteiro, Lucilena R.; Dantas, Elizabeth S.K.; Pires, Maria Aparecida F.; Cotrim, Marycel E.B.

    2013-01-01

    The CONAMA's Resolution 430 recently published in May 13 th of 2011, that completes and modifies the Resolution 357/2005, defined new quality standards to perform liquid effluent monitoring essays in order to allow the release in the public sewer system. This Resolution has established that the essay laboratories must be certified by Brazilian National Metrology, Normalization and Industrial Quality Institute - INMETRO and also count with an implemented quality control system. Thereby this publication affected directly IPEN's Environmental Monitoring Program of Stables Chemical Compound (PMA-Q), performed since 2007. In this program, 20 parameters related to the metallic and non-metallic chemical elements content are monitored by using sensitive analytical techniques such as graphite furnace atomic absorption spectrometry - GF-AAS or inductively coupled plasma spectrometry - ICP-OES. Therefore this paper presents improvements to determine the laboratory individual performance performed by GF-AAS and ICP-OES. To achieve the legislation compliance for these parameters, the following actions were implemented: the construction of control charts (internal quality control) and the participation of the laboratory in interlaboratory proficiency tests (external quality control). These actions are presented and discussed with the results of elements such as Arsenic and Lead that are analyzed through GF-AAS as well as Chromium, Cooper, Zinc, Iron and Nickel, that are analyzed through ICP-OES. These actions of quality control allowed the continuous monitoring of laboratory performance, the identification and resolution of analytic problems and interlaboratory differences, provide additional confidence to monitoring program. (author)

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    Highlights: • Itrax is able to detect trace metals using an appropriate exposure time. • Metal pollution levels can be estimated from Itrax peak areas saving time and money. • Marín harbour is highly polluted by Hg, but most of it is bound to organic matter. • Organic matter variations can be quickly detected by using the inc/coh ratio. • Itrax is a fast option for monitoring pollution in harbours and coastal areas. - Abstract: X-ray fluorescence scanners, such as the Itrax™ Core Scanner (Itrax) (Cox Analytical Systems, Mölndal, Sweden), provide high-resolution geochemical data within several hours. However, the semi-quantitative nature of these analysers has hampered their use to study pollution. This study explores Itrax’s capabilities to detect trace metals, such as Hg and Cd, in the Ría de Pontevedra harbour (NW Spain). A set of Itrax detection levels were proposed for each metal after comparison with quantitative measurements obtained from Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) and Vapour Atomic Absorption Spectrometry (CVAAS) analyses. These quantitative data obtained after a sequential extraction were used to evaluate pollutant bioavailability and to determine metal pollution levels exhibiting Hg pollution. The reliability of inc/coh and Br/Cl ratios to assess the total organic matter variability was also evaluated. The results indicated that the Itrax is an efficient and fast option to monitor contamination, thereby avoiding laborious discrete analyses and reducing analytical cost and time

  19. Toxic elements in sediment from two water bodies near Brazilian Multipurpose Reactor: RMB installation area

    International Nuclear Information System (INIS)

    Silva, Tatiane B.S.C. da; Stellato, Thamiris B.; Monteiro, Lucilena R.; Marques, Joyce R.; Faustino, Mainara G.; Santos, Camila F.R.T.T.; Oliveira, Cintia C. de; Miranda, Gabrielle S.; Pires, Maria Aparecida F.; Cotrim, Marycel E.B.

    2017-01-01

    Aquatic ecosystems are directly affected by contaminants, such as, toxic elements that do not remain in sediment in a insoluble form. Anthropogenic and natural actions influence sediment dynamics that could lead to a potential contaminant accumulation. Therefore, to evaluate possible environmental impacts is,in many cases, mandatory. Environmental impact assessment studies are a licensing tool that seeks to control degradation activities, taking into account the legal and regulatory provisions and technical standards applicable to the case. The present study aims to evaluate the sediment quality in the area of influence of the Brazilian Multipurpose Nuclear Reactor (RMB) to be installed in the contiguous area of the Experimental Center of Aramar of the Technological Center of the Navy in São Paulo (CTMSP), located in the city of Iperó - SP. The potentially toxic elements As, Cd and Hg were analyzed by Graphite Furnace Atomic Absorption Spectrometry (GFAAS) and Cr, Cu, Ni and Zn by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). Results were compared with Canadian Council of Ministers of the Environment (CCME) guideline values (TEL and PEL) and the maximum permitted values of Resolution 454/12. These toxic elements (As, Cd, Hg, Cr, Cu, Ni and Zn) were found below maximum allowed concentrations from national and international legislation. This study provides support for RMB post-completion evaluations, in order to prevent these elements to exceed tolerated levels, ensuring ecological, social and economic values. (author)

  20. The recent developments in dispersive liquid–liquid microextraction for preconcentration and determination of inorganic analytes

    Directory of Open Access Journals (Sweden)

    H.M. Al-Saidi

    2014-12-01

    Full Text Available Recently, increasing interest on the use of dispersive liquid–liquid microextraction (DLLME developed in 2006 by Rezaee has been found in the field of separation science. DLLME is miniaturized format of liquid–liquid extraction in which acceptor-to-donor phase ratio is greatly reduced compared with other methods. In the present review, the combination of DLLME with different analytical techniques such as atomic absorption spectrometry (AAS, inductively coupled plasma-optical emission spectrometry (ICP-OES, gas chromatography (GC, and high-performance liquid chromatography (HPLC for preconcentration and determination of inorganic analytes in different types of samples will be discussed. Recent developments in DLLME, e.g., displacement-DLLME, the use of an auxiliary solvent for adjustment of density of extraction mixture, and the application of ionic liquid-based DLLME in determination of inorganic species even in the presence of high content of salts are presented in the present review. Finally, comparison of DLLME with the other liquid-phase microextraction approaches and limitations of this technique are provided.

  1. Recovery of α-Al{sub 2}O{sub 3} from ionizing radiation dosimetric sensors

    Energy Technology Data Exchange (ETDEWEB)

    Sanches, Edgar Aparecido, E-mail: sanches.ufam@gmail.com [Universidade Federal do Amazonas (UFAM), Manaus, AM (Brazil). Dept. de Fisica; Costalonga, Ademir Geraldo Cavallari; Mascarenhas, Yvonne Primerano [Universidade de Sao Paulo (IFSC/USP), Sao Carlos, SP (Brazil). Institute de Fisica; Nascimento, Luana de Freitas [Belgium Nuclear Research Centre, SCK-CEN, Mol (Belgium); Mascarenhas, Yvone Maria [SAPRA S/A Servico de Assessoria e Protecao Radiologica, Sao Carlos, SP, (Brazil)

    2015-01-15

    Corundum, sapphire or α-Al{sub 2}O{sub 3} is an important technological material in many optical and electronic applications such as solid-state lasers, optical windows and, more recently, as a radiation detector. Landauer (Glenwood, IL, USA) accumulated large number of archived and stored Luxel™ dosemeters composed of Al{sub 2}O{sub 3}:C, which were subjected to a recovery process. Due to the importance of this advanced crystalline material in OSL dosimetry, a recovery process was developed based on the dosemeters calcination and Al{sub 2}O{sub 3}:C has been reused in manufacturing of new dosemeters. This paper does not aim to optimize the recovery process, but provides an opportunity to study the involved process parameters and to recover this valuable crystalline material from used dosemeters. To the best of our knowledge no other recovery process involving this dosimetric material was described in scientific literature. Fourier Transform Infrared Spectrometry (FTIR), Thermogravimetry/Differential Thermoanalysis (TG/DTA), Differential Scanning Calorimetry (DSC), X-ray Diffraction (XRD), Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), Optically Stimulated Luminescence (OSL) and Rietveld Refinement were used to characterize the recovered material and to check for the stability of its structural and dosimetric properties. (author)

  2. Multi-element analysis of lubricant oil by WDXRF technique using thin-film sample preparation

    International Nuclear Information System (INIS)

    Scapin, M. A.; Salvador, V. L. R.; Lopes, C. D.; Sato, I. M.

    2006-01-01

    The quantitative analysis of the chemical elements in matrices like oils or gels represents a challenge for the analytical chemists. The classics methods or instrumental techniques such as atomic absorption spectrometry (AAS) and plasma optical emission spectrometry (ICP-OES) need chemical treatments, mainly sample dissolution and degradation processes. X-ray fluorescence technique allows a direct and multi-element analysis without previous sample treatments. In this work, a sensible method for the determination of elements Mg, Al, Si, P, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Mo, Ag, Sn, Ba and Pb in lubricating oil is presented. The x-ray fluorescence (WDXRF) technique using linear regression method and thin film sample preparation was used. The validation of the methodology (repeatability and accuracy) was obtained by the analysis of the standard reference materials SRM Alpha AESAR lot 703527D, applying the Chauvenet, Cochrane, ANOVA and Z-score statistical tests. The method presents a relative standard deviation lower than 10% for all the elements, except for Pb determination (RSD Pb 15%). The Z-score values for all the elements were in the range -2 < Z < 2, indicating a very good accuracy.(Full text)

  3. Chemical elemental distribution and soil DNA fingerprints provide the critical evidence in murder case investigation.

    Directory of Open Access Journals (Sweden)

    Giuseppe Concheri

    Full Text Available 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