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

NASA Astrophysics Data System (ADS)

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

2016-07-01

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

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

NASA Astrophysics Data System (ADS)

Oropeza, D.

2016-12-01

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

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

NASA Astrophysics Data System (ADS)

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.

Rapid screening of heavy metals and trace elements in environmental samples using portable X-ray fluorescence spectrometer, A comparative study

PubMed Central

McComb, Jacqueline Q.; Rogers, Christian; Han, Fengxiang X.; Tchounwou, Paul B.

2014-01-01

With industrialization, great amounts of trace elements and heavy metals have been excavated and released on the surface of the earth and dissipated into the environments. Rapid screening technology for detecting major and trace elements as well as heavy metals in variety of environmental samples is most desired. The objectives of this study were to determine the detection limits, accuracy, repeatability and efficiency of a X-ray fluorescence spectrometer (Niton XRF analyzer) in comparison with the traditional analytical methods, inductively coupled plasma optical emission spectrometer (ICP-OES) and inductively coupled plasma optical emission spectrometer (ICP-MS) in screening of major and trace elements of environmental samples including estuary soils and sediments, contaminated soils, and biological samples. XRF is a fast and non-destructive method in measuring the total concentration of multi--elements simultaneously. Contrary to ICP-OES and ICP-MS, XRF analyzer is characterized by the limited preparation required for solid samples, non-destructive analysis, increased total speed and high throughout, the decreased production of hazardous waste and the low running costs as well as multi-elemental determination and portability in the fields. The current comparative study demonstrates that XRF is a good rapid non-destructive method for contaminated soils, sediments and biological samples containing higher concentrations of major and trace elements. Unfortunately, XRF does not have sensitive detection limits of most major and trace elements as ICP-OES or ICP-MS but it may serve as a rapid screening tool for locating hot spots of uncontaminated field soils and sediments. PMID:25861136

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

PubMed

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

2008-01-01

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

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

NASA Astrophysics Data System (ADS)

Zhang, Gai; Tian, Min

2015-04-01

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

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

PubMed

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

2015-07-23

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

Improved documentation of spectral lines for inductively coupled plasma emission spectrometry

NASA Astrophysics Data System (ADS)

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.

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

PubMed

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

2016-12-01

Analytical methods for the determination of rare earth elements (REE) in natural waters by plasma spectrochemical techniques often require sample preparation procedures for analytes preconcentration as well as for removing matrix constituents, that may interfere on the analytical measurements. In the present work, calcium alginate (CA) beads were used for the first time aiming at Ce, La and Nd preconcentration from groundwater samples for further determination by inductively coupled plasma optical emission spectrometry (ICP OES). Test samples were analyzed in batch mode by transferring a 40mL test portion (pH=5±0.2) into a 50mL polyethylene flask containing 125mg CA beads. After 15min contact, the analytes were quantitatively extracted from the loaded CA beads with 2.0mL of 1.0molL -1 HCl solution for further determination by ICP OES, using Ce (II) 456.236, La (II) 379.478 and Nd (II) 430.358nm emission lines. The proposed approach is a reliable alternative for REE single-stage preconcentration from aqueous samples, as it provided accurate results based on the addition and recovery analysis of groundwater. The results obtained by the proposed method were also compared with those from reference method based on inductively coupled plasma mass spectrometry (ICP-MS) and no significant differences were observed after applying the Student's t-test at 95% confidence level. Copyright © 2016 Elsevier B.V. All rights reserved.

Real-time measurement of size-resolved elemental composition ratio for flame synthesized composite nanoparticle aggregates using a tandem SMPS-ICP-OES

PubMed Central

Reed, Nathan; Fang, Jiaxi; Chavalmane, Sanmathi; Biswas, Pratim

2017-01-01

Composite nanoparticles find application in catalysis, drug delivery, and energy storage and require increasingly fine control of their physical properties and composition. While composite nanoparticles have been widely synthesized and characterized, little work has systematically correlated the initial concentration of precursors and the final composition of flame synthesized composite nanoparticles. This relationship is explored in a diffusion flame aerosol reactor by coupling a scanning mobility particle sizer (SMPS) with an inductively coupled plasma optical emission spectrometer (ICP-OES). A framework for studying the relationship between the initial precursor concentrations of different elements and the final nanoparticle composition is explored. The size-resolved elemental composition was measured by directly injecting size-selected fractions of aggregated magnetite and silicon dioxide composite nanoparticles into the ICP-OES plasma. This work showed a correlation between precursor molar ratio and the measured elemental ratio in the mobility size range of 50 to 140 nm. Building on previous work studying size resolved elemental composition of engineered nanoparticles, the analysis is extended to flame synthesized composite nanoparticle aggregates in this work. PMID:28435179

Real-time measurement of size-resolved elemental composition ratio for flame synthesized composite nanoparticle aggregates using a tandem SMPS-ICP-OES.

PubMed

Reed, Nathan; Fang, Jiaxi; Chavalmane, Sanmathi; Biswas, Pratim

2017-01-01

Composite nanoparticles find application in catalysis, drug delivery, and energy storage and require increasingly fine control of their physical properties and composition. While composite nanoparticles have been widely synthesized and characterized, little work has systematically correlated the initial concentration of precursors and the final composition of flame synthesized composite nanoparticles. This relationship is explored in a diffusion flame aerosol reactor by coupling a scanning mobility particle sizer (SMPS) with an inductively coupled plasma optical emission spectrometer (ICP-OES). A framework for studying the relationship between the initial precursor concentrations of different elements and the final nanoparticle composition is explored. The size-resolved elemental composition was measured by directly injecting size-selected fractions of aggregated magnetite and silicon dioxide composite nanoparticles into the ICP-OES plasma. This work showed a correlation between precursor molar ratio and the measured elemental ratio in the mobility size range of 50 to 140 nm. Building on previous work studying size resolved elemental composition of engineered nanoparticles, the analysis is extended to flame synthesized composite nanoparticle aggregates in this work.

Profiling of patterned metal layers by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS)

NASA Astrophysics Data System (ADS)

Bi, Melody; Ruiz, Antonio M.; Gornushkin, Igor; Smith, Ben W.; Winefordner, James D.

2000-02-01

Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was used for profiling patterned thin metal layers on a polymer/silicon substrate. The parameters of the laser and ICP-MS operating conditions have been studied and optimized for this purpose. A new laser ablation chamber was designed and built to achieve the best spatial resolution. The results of the profiling by LA-ICP-MS were compared to those obtained from a laser ablation optical emission spectrometry (LA-OES) instrument, which measured the emission of the plasma at the sample surface, and thus, eliminated the time delay caused by the sample transport into the ICP-MS system. Emission spectra gave better spatial resolution than mass spectra. However, LA-ICP-MS provided much better sensitivity and was able to profile thin metal layers (on the order of a few nanometers) on the silicon surface. A lateral spatial resolution of 45 μm was achieved.

[Determination of tungsten and cobalt in the air of workplace by ICP-OES].

PubMed

Zhang, J; Ding, C G; Li, H B; Song, S; Yan, H F

2017-08-20

Objective: To establish the inductively coupled plasma optical emission spectrometry (ICP-OES) method for determination of cobalt and tungsten in the air of workplace. Methods: The cobalt and tungsten were collected by filter membrane and then digested by nitric acid, inductively coupled plasma optical emission spectrometry (ICP-OES) was used for the detection of cobalt and tungsten. Results: The linearity of tungsten was good at the range of 0.01-1 000 μg/ml with a correlation coefficient of 0.999 9, the LOD and LOQ were 0.006 7 μg/ml and 0.022 μg/ml, respectively. The recovery was ranged from 98%-101%, the RSD of intra-and inter-batch precision were 1.1%-3.0% and 2.1%-3.8%, respectively. The linearity of cobalt was good at the range of 0.01-100 μg/ml with a correlation coefficient of 0.999 9, the LOD and LOQ were 0.001 2 μg/ml and 0.044 μg/ml, respectively. The recovery was ranged from 95%-97%, the RSD of intra-and inter-batch precision were 1.1%-2.4% and 1.1%-2.9%, respectively. The sampling efficiency of tungsten and cobalt were higher than 94%. Conclusion: The linear range, sensitivity and precision of the method was suitable for the detection of tungsten and cobalt in the air of workplace.

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

PubMed

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

2012-06-01

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

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

PubMed

Sert, Şenol

2013-07-01

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

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

PubMed

Ohata, Masaki

2016-01-01

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

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

PubMed Central

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

2014-01-01

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

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

PubMed

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

2014-01-01

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

In vivo testing for gold nanoparticle toxicity.

PubMed

Simpson, Carrie A; Huffman, Brian J; Cliffel, David E

2013-01-01

A technique for measuring the toxicity of nanomaterials using a murine model is described. Blood samples are collected via submandibular bleeding while urine samples are collected on cellophane sheets. Both biosamples are then analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES) for nanotoxicity. Blood samples are further tested for immunological response using a standard Coulter counter. The major organs of interest for filtration are also digested and analyzed via ICP-OES, producing useful information regarding target specificity of the nanomaterial of interest. Collection of the biosamples and analysis afterward is detailed, and the operation of the technique is described and illustrated by analysis of the nanotoxicity of an injection of a modified tiopronin monolayer-protected cluster.

Accurate quantitation standards of glutathione via traceable sulfur measurement by inductively coupled plasma optical emission spectrometry and ion chromatography

PubMed Central

Rastogi, L.; Dash, K.; Arunachalam, J.

2013-01-01

The quantitative analysis of glutathione (GSH) is important in different fields like medicine, biology, and biotechnology. Accurate quantitative measurements of this analyte have been hampered by the lack of well characterized reference standards. The proposed procedure is intended to provide an accurate and definitive method for the quantitation of GSH for reference measurements. Measurement of the stoichiometrically existing sulfur content in purified GSH offers an approach for its quantitation and calibration through an appropriate characterized reference material (CRM) for sulfur would provide a methodology for the certification of GSH quantity, that is traceable to SI (International system of units). The inductively coupled plasma optical emission spectrometry (ICP-OES) approach negates the need for any sample digestion. The sulfur content of the purified GSH is quantitatively converted into sulfate ions by microwave-assisted UV digestion in the presence of hydrogen peroxide prior to ion chromatography (IC) measurements. The measurement of sulfur by ICP-OES and IC (as sulfate) using the “high performance” methodology could be useful for characterizing primary calibration standards and certified reference materials with low uncertainties. The relative expanded uncertainties (% U) expressed at 95% confidence interval for ICP-OES analyses varied from 0.1% to 0.3%, while in the case of IC, they were between 0.2% and 1.2%. The described methods are more suitable for characterizing primary calibration standards and certifying reference materials of GSH, than for routine measurements. PMID:29403814

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

PubMed

Lech, Teresa

2014-04-01

In this work, a case of deliberate self-poisoning is presented. A 14-year-old girl suddenly died during one of the several hospitalizations. Abdominal computer tomography showed a large number of metallic particles in the large intestine. Analysis of blood and internal organs for mercury and other toxic metals carried out by inductively coupled plasma optical emission spectrometry (ICP OES) revealed high concentrations of mercury in kidneys and liver (64,200 and 2470ng/g, respectively), less in stomach (90ng/g), and none in blood. Using cold vapor-atomic absorption spectrometry (CV AAS), high levels of mercury were confirmed in all examined materials, including blood (87ng/g), and additionally in hair. The results of analysis obtained by two techniques revealed that the exposure to mercury was considerable (some time later, it was stated that the mercury originated from thermometers that had been broken over the course of about 1 year, because of Münchausen syndrome). CV AAS is a more sensitive technique, particularly for blood samples (negative results using ICP OES), and tissue samples - with LOQ: 0.63ng/g of Hg (CV AAS) vis-à-vis 70ng/g of Hg (ICP OES). However, ICP OES may be used as a screening technique for autopsy material in acute poisoning by a heavy metal, even one as volatile as mercury. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Surface Modification of Polyimide for Improving Adhesion Strength by Inductively Coupled Plasma

NASA Astrophysics Data System (ADS)

Byun, Tae Joon; Kim, Sung Il; Kim, Youn Joon; Choi, Yoon Suk; Choi, In Sik; Setsuhara, Yuichi; Geon Han, Jeon

2009-08-01

This study examined the effect of an inductively coupled plasma (ICP) treatment using an argon and helium gas mixture on the adhesion between polyimide and a copper film. Optical emission spectroscopy (OES) of the ICP revealed the emission intensity of helium and argon at various intensities with the helium mixing ratio. The treated polyimide surface was analyzed using a contact angle analyzer, Atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The contact angle and RMS roughness ranged from 66 to 31° and 2.3 to 4.1 nm, respectively. XPS showed an increase in C-O bonding. The highest peel strength was 0.43 kgf/cm at a 40% of helium mixing ratio, which contained the highest level of activate species. Overall, an ICP treatment of a polyimide surface with a 40% helium gas mixture improves the adhesion strength between copper and polyimide significantly.

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

NASA Astrophysics Data System (ADS)

Menegário, Amauri A.; Fernanda Giné, Maria

2001-10-01

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

Multielement analysis and antioxidant capacity of Merlot wine clones developed in Montenegro.

PubMed

Đorđević, Neda O; Pejin, Boris; Novaković, Miroslav M; Stanković, Dalibor M; Mutić, Jelena J; Pajović, Snežana B; Tešević, Vele V

2018-02-01

The overall aim of this paper was to compare the multielement composition and antioxidant capacity of two Montenegrin Merlot wines obtained from specific vine clones (VCR1 and VCR 101) along with commercial Merlot wine throughout the consecutive vintages in 2010 and 2011. Elemental composition was analysed using inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). Additionally, antioxidant capacity was assessed by cyclic voltammetry. VCR 1 wine from 2011 stood out for its elemental composition. On the other hand, antioxidant capacity of VCR 101 wines was the highest one for the both vintages. According to the experimental data obtained, all three wines are good source of essential elements and products with a significant antioxidant activity and specific geographical origin.

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

PubMed

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

2014-09-01

To determine the contents of 22 inorganic elements in different parts of Lantana camara by inductively coupled plasma optical emission spectroscopy (ICP-OES). HNO3-H2 02 digested system was used to completely decomposed the organic compounds effectually by microwave digestion. 22 inorganic elements such as K, Ca, Mg, Fe, Al, Na, Zn, Mn and Cr were determined by ICP-OES under set up working conditions. The contents of K, Ca and Mg were the most in different parts of Lantana camrnara; The contents of K, Ca, Mg, Mn, Sr and Cu in the leaves of Lantana camara were more than that in the root and the branch. The contents of Fe and Na in the root of Lantana camara were more than that in the leaves and the branch. The contents of Pb and Cd were higher than the national standard and Cr had high content in different parts of Lantana camara. The determination method is quick, easy and accurate with high sensitivity,which can determine the contents of 22 inorganic elements accurately in different parts of Lantana camara.

Simultaneous trace multielement determination by ICP-OES after solid phase extraction with modified octadecyl silica gel.

PubMed

Karbasi, Mohamad-Hadi; Jahanparast, Babak; Shamsipur, Mojtaba; Hassan, Jalal

2009-10-15

Multielement simultaneous determination of 35 trace elements in environmental samples was carried out by inductively coupled plasma emission spectrometry (ICP-OES) after preconcentration with octadecyl silicagel, modified with aurin tricarboxylic acid (Aluminon). Optimal experimental conditions including pH of sample solution, sample volume, sample and eluent flow rate, type, concentration and volume of eluent and foreign ions effect were investigated and established. Trace element ions in aqueous solution were quantitatively adsorbed onto octadecyl silicagel modified with aurin tricarboxylic acid at pH 8.0 with a flow rate of 11.0 mL min(-1). The adsorbed element ions were eluted with 3-5 mL of 0.5 mol L(-1) HNO(3) at a flow rate of 10.0 mL min(-1) and analyzed by ICP-OES simultaneously. The proposed method has at least preconcentration factor of 100 in water samples, which results high sensitive detection of ultra-trace and trace analysis. The present methodology gave recoveries better than 70% and RSD less than 16%.

Determination of cobalt species in nutritional supplements using ICP-OES after microwave-assisted extraction and solid-phase extraction.

PubMed

Bartosiak, Magdalena; Jankowski, Krzysztof; Giersz, Jacek

2018-06-05

Cobalt content (as vitamin B 12 and inorganic cobalt) in two nutritional supplements, namely Spirulina platensis and Saccharomyces cerevisiae known as a "superfood", has been determined using inductively coupled plasma optical emission spectrometry (ICP-OES). Several sample pre-treatment protocols have been applied and compared. Microwave-assisted acid digestion efficiently decomposed all cobalt-containing compounds, thus allowed obtaining total cobalt content in supplements examined. Vitamin B 12 was extracted from the samples with acetate buffer and potassium cyanide solution exposed to mild microwave radiation for 30 min, and cyanocobalamin was separated from the extract by on-column solid phase extraction using C-18 modified silica bed. About 100% of cobalt species was extracted using the triple microwave-assisted extraction procedure. Total cobalt content was 20-fold greater in Spirulina tablets than the declared cobalamin content (as Co). The ICP-OES method precision was about 3% and detection limit was 1.9 and 2.7 ng Co mL -1 for inorganic cobalt or cyanocobalamin, respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

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

PubMed

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.

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

PubMed

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

2015-07-23

Due to their outstanding analytical performances, inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are widely used for multi-elemental measurements and also for isotopic characterization in the case of ICP-MS. While most studies are carried out in aqueous matrices, applications involving organic/hydro-organic matrices become increasingly widespread. This kind of matrices is introduced in ICP based instruments when classical "matrix removal" approaches such as acid digestion or extraction procedures cannot be implemented. Due to the physico-chemical properties of organic/hydro-organic matrices and their associated effects on instrumentation and analytical performances, their introduction into ICP sources is particularly challenging and has become a full topic. In this framework, numerous theoretical and phenomenological studies of these effects have been performed in the past, mainly by ICP-OES, while recent literature is more focused on applications and associated instrumental developments. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP-OES and ICP-MS. The present Part I, provides theoretical considerations in connection with the physico-chemical properties of organic/hydro-organic matrices, in order to better understand the induced phenomena. This focal point is divided in four chapters highlighting: (i) the impact of organic/hydro-organic matrices from aerosol generation to atomization/excitation/ionization processes; (ii) the production of carbon molecular constituents and their spatial distribution in the plasma with respect to analytes repartition; (iii) the subsequent modifications of plasma fundamental properties; and (iv) the resulting spectroscopic and non spectroscopic interferences. This first part of this tutorial review is addressed either to beginners or to more experienced scientists who are interested in the analysis of organic/hydro-organic matrices by ICP sources and would like to consider the theoretical background of effects induced by such matrices. The second part of this tutorial review will be dedicated to more practical consideration on instrumentation, such as adapted introductions devices, as well as instrumental and operating parameters optimization. The analytical strategies for elemental quantification in such matrices will also be addressed. Copyright © 2015 Elsevier B.V. All rights reserved.

A comparison of reliability of soil Cd determination by standard spectrometric methods

PubMed Central

McBride, M.B.

2015-01-01

Inductively coupled plasma emission spectrometry (ICP-OES) is the most common method for determination of soil Cd, yet spectral and matrix interferences affect measurements at the available analytical wavelengths for this metal. This study evaluated the severity of the interference over a range of total soil Cd by comparing ICP-OES and ICP-MS measurements of Cd in acid digests. ICP-OES using the emission at 226.5 nm generally unable to quantify soil Cd at low (near-background) levels, and gave unreliable values compared to ICP-MS. Using the line at 228.nm, a marked positive bias in Cd measurement (relative to the 226.5 nm measurement) was attributable to As interference even at soil As concentrations below 10 mg/kg. This spectral interference in ICP-OES was severe in As-contaminated orchard soils, giving a false value for soil total Cd near 2 mg kg−1 when soil As was 100–150 mg kg−1. In attempting to avoid these ICP emission-specific interferences, we evaluated a method to estimate total soil Cd using 1 M HNO3 extraction followed by determination of Cd by flame atomic absorption (FAA), either with or without pre-concentration of Cd using an Aliquat-heptanone extractant. The 1 M HNO3 extracted an average of 82% of total soil Cd. The FAA method had no significant interferences, and estimated the total Cd concentrations in all soils tested with acceptable accuracy. For Cd-contaminated soils, the Aliquat-heptanone pre-concentration step was not necessary, as FAA sensitivity was adequate for quantification of extractable soil Cd and reliable estimation of total soil Cd. PMID:22031569

Stoichiometry determination of (Pb,La)(Zr,Ti)O3-type nano-crystalline ferroelectric ceramics by wavelength-dispersive X-ray fluorescence spectrometry.

PubMed

Sitko, Rafał; Zawisza, Beata; Kita, Andrzej; Płońska, Małgorzata

2006-07-01

Analysis of small samples of lanthanum-doped lead zirconate titanate (PLZT) by wavelength-dispersive X-ray fluorescence spectrometry (WDXRF) is presented. The powdered material in ca. 30 mg was suspended in water and collected on the membrane filter. The pure oxide standards (PbO, La2O3, ZrO2 and TiO2) were used for calibration. The matrix effects were corrected using a theoretical influence coefficients algorithm for intermediate-thickness specimens. The results from XRF method were compared with the results from the inductively coupled plasma optical emission spectrometry (ICP-OES). Agreement between XRF and ICP-OES analysis was satisfactory and indicates the usefulness of XRF method for stoichiometry determination of PLZT.

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

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

The endpoint detection technique for deep submicrometer plasma etching

NASA Astrophysics Data System (ADS)

Wang, Wei; Du, Zhi-yun; Zeng, Yong; Lan, Zhong-went

2009-07-01

The availability of reliable optical sensor technology provides opportunities to better characterize and control plasma etching processes in real time, they could play a important role in endpoint detection, fault diagnostics and processes feedback control and so on. The optical emission spectroscopy (OES) method becomes deficient in the case of deep submicrometer gate etching. In the newly developed high density inductively coupled plasma (HD-ICP) etching system, Interferometry endpoint (IEP) is introduced to get the EPD. The IEP fringe count algorithm is investigated to predict the end point, and then its signal is used to control etching rate and to call end point with OES signal in over etching (OE) processes step. The experiment results show that IEP together with OES provide extra process control margin for advanced device with thinner gate oxide.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rubio, R.; Peralta, I.; Alberti, J.

1993-01-01

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

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

NASA Astrophysics Data System (ADS)

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.

Using ICP-OES and SEM-EDX in biosorption studies

PubMed Central

Chojnacka, Katarzyna; Marycz, Krzysztof

2010-01-01

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

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

PubMed

Michalak, Izabela; Chojnacka, Katarzyna; Marycz, Krzysztof

2011-02-01

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

Determination of Microelements in Human Milk and Infant Formula Without Digestion by ICP-OES.

PubMed

Đurović, Dijana; Milisavljević, Branka; Nedović-Vuković, Mirjana; Potkonjak, Branislav; Spasić, Snežana; Vrvić, Miroslav

2017-06-01

The concentrations of zinc (Zn), iron (Fe) and copper (Cu) in both human milk and infant formula were determined using a new sample preparation method, by inductively coupled plasma - optical emission spectometry (ICP-OES) and flame atomic absorption spectrometry (FAAS). Human milk samples were diluted in ultrapure water. The infant formula of powder samples (suitable for an infant 1-6 months of age) and standard reference material (SRM-1849) were analyzed in parallel. The results have shown that FAAS method was more sensitive for Fe determination in human milk while ICP-OES was more sensitive for both Zn and Cu detection. The limit of quantification for both Zn and Cu was 5 μg L-1 and 10 μg L-1 for Fe and the recovery for Zn, Fe and Cu was ranged from 90% to 94%, 97% to 103% and 90% to 102%, respectively. Mean concentrations of Zn, Fe, and Cu in human milk samples were 5.35, 0.47 and 0.83 mg L-1, respectively while these values in infant formula were ranged from 3.52-4.75 mg L-1, 3.37-4.56 mg L-1 and 0.28-0.41 mg L-1, respectively. Despite the sample complexity, the proposed method using dilution of milk samples with water was simple, rapid, effective and accurate. ICP-OES was a better method for Zn determination while FAAS was a better method for Fe determination. In the case of Cu both methods were comparable.

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

PubMed Central

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

2016-01-01

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

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

PubMed

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

2014-10-01

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

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

PubMed

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

2015-01-01

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

Effect of sample preparation procedure for the determination of As, Sb and Se in fruit juices by HG-ICP-OES.

PubMed

Welna, Maja; Szymczycha-Madeja, Anna

2014-09-15

Various sample preparation procedures for the simultaneous determination of As, Sb and Se in fruit juices by hydride generation inductively coupled plasma optical emission spectrometry (HG-ICP-OES) were examined. Applicability of total wet digestion with HNO3/H2O2, partial decomposition (solubilisation in aqua regia), 1:1 dilution with 2% (v/v) HNO3 and direct analysis were evaluated. Hydrides were generated in the reaction of an acidified sample with NaBH4 after pre-reduction with KI-ascorbic acid for total As and Sb, and boiling with HCl for total Se. Best results, i.e. limits of detection (LODs) of 0.51-0.73 ng mL(-1), precision (RSD) within 1.7-3.6% and recoveries for spiked samples between 101% and 106% were found using aqua regia treatment. This procedure simplifying and improving sample preparation step prior to As, Sb and Se measurements in fruit juices by HG-ICP-OES, thus could be adequate for the routine analysis in terms of the quality control of these drinks. Copyright © 2014 Elsevier Ltd. All rights reserved.

Biomonitoring of boron: Development and characterization of a simple, reliable and quality controlled biomonitoring method.

PubMed

Michalke, Bernhard

2017-03-01

Boron exposure is of interest and concern from an occupational point of view. Usual daily boron intake is related to boron blood plasma concentration <1mg/L and to <3mg/L in urine, but after exposure urine concentrations are quickly elevated. Reliable boron biomonitoring, typically in urine, thus is mandatory for occupational health control institutions. This paper reports on the development of a simple, fast and reliable boron determination procedure based on inductively coupled plasma - optical emission spectrometry (ICP-OES). Major aims for this method were simplicity in sample preparation, low risk for artifacts and interferences, high precision and accuracy, possibly low costs, including lower costs for element selective detection, short total analysis time and suitability for occupational health laboratories. Precision data (serial or day-to-day) from urine and doped urine were very good: <1.5 or <2%. Accuracy was calculated from analysis of a certified reference material (ERM-CD 281), as 99% or according to recoveries of doped concentrations ranging from 102 to 109% recovery. For cross-checking ICP-OES determinations, samples were analyzed also by quadrupole ICP-qMS and by sectorfield ICP-sf-MS at low and medium resolution. Both systems confirmed ICP-OES measurements when using 11 B for quantification. Determinations based on 10 B however showed some bias, except with ICP-sf-MS at medium resolution. The observed elevated signals are discussed with respect to the known Ne ++ interference (as an impurity in Ar), which is not separated in low resolving quadrupole ICP-MS systems or ICP-sf-MS at low resolution. Copyright © 2016 Elsevier GmbH. All rights reserved.

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

PubMed

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

2016-04-01

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

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

PubMed

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

2014-12-01

A procedure is developed for the analysis of sub-μg L(-1) levels of arsenic, antimony and selenium after preconcentration of their hydrides. The study highlights the capability of an aqueous suspension of a nanometer-sized magnetic ceria, in the presence of iodide, to function as a sorbent for the in situ trapping and preconcentration of the hydrides of certain metalloids. After extraction, the material is magnetically separated from the trapping solution and analyzed. A slurry suspension sampling approach with inductively coupled plasma-optical emission spectrometry (ICP-OES) is employed for measurements, as the quantitative elution of the adsorbed metalloids is not feasible. The whole analytical procedure consists of five steps: (i) pre-reduction of As, Sb and Se, (ii) generation of the hydrides AsH3, SbH3 and SeH2, (iii) in situ collection in the trapping suspension of magnetic ceria, (iv) isolation of the particles by applying a magnetic field, and (v) measurement of As, Sb and Se concentrations using ICP-OES. Under the established experimental conditions, the efficiency of trapping accounted for 94 ± 2%, 89 ± 2% and 98 ± 3% for As, Sb and Se, respectively, signifying the effective implementation of the overall procedure. The applicability of the procedure has been demonstrated by analyzing tap and lake water and a reference material (soft drinking water). The obtained analytical figures of merit were satisfactory for the analysis of the above metalloids in natural waters by ICP-OES. Copyright © 2014 Elsevier B.V. All rights reserved.

Rapid Analysis of Inorganic Species in Herbaceous Materials Using Laser-Induced Breakdown Spectroscopy

PubMed Central

Emerson, Rachel M.

2015-01-01

Abstract Inorganic compounds in biomass, often referred to as ash, are known to be problematic in the thermochemical conversion of biomass to bio-oil or syngas and, ultimately, hydrocarbon fuels because they negatively influence reaction pathways, contribute to fouling and corrosion, poison catalysts, and impact waste streams. The most common ash-analysis methods, such as inductively coupled plasma-optical emission spectrometry/mass spectrometry (ICP-OES/MS), require considerable time and expensive reagents. Laser-induced breakdown spectroscopy (LIBS) is emerging as a technique for rapid analysis of the inorganic constituents in a wide range of biomass materials. This study compares analytical results using LIBS data to results obtained from three separate ICP-OES/MS methods for 12 samples, including six standard reference materials. Analyzed elements include aluminum, calcium, iron, magnesium, manganese, phosphorus, potassium, sodium, and silicon, and results show that concentrations can be measured with an uncertainty of approximately 100 parts per million using univariate calibration models and relatively few calibration samples. These results indicate that the accuracy of LIBS is comparable to that of ICP-OES methods and indicate that some acid-digestion methods for ICP-OES may not be reliable for Na and Al. These results also demonstrate that germanium can be used as an internal standard to improve the reliability and accuracy of measuring many elements of interest, and that LIBS can be used for rapid determination of total ash in biomass samples. Key benefits of LIBS include little sample preparation, no reagent consumption, and the generation of meaningful analytical data instantaneously. PMID:26733765

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

NASA Astrophysics Data System (ADS)

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

2015-03-01

A systematic study was performed for the determination of inorganic contaminants in polymeric waste from electrical and electronic equipment (EEE) for achieving an efficient digestion to minimize interferences in determination using plasma-based techniques. The determination of As, Br, Cd, Co, Cr, Cu, Ni, Pb, Sb, and Zn by inductively coupled plasma mass spectrometry (ICP-MS) and also by inductively coupled plasma optical emission spectrometry (ICP OES) was carried out after digestion using microwave-induced combustion (MIC). Arsenic and Hg were determined by flow-injection chemical vapor generation inductively coupled plasma mass spectrometry (FI-CVG-ICP-MS). Dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) with ammonia was also used for Cr determination. The suitability of MIC for digestion of sample masses up to 400 mg was demonstrated using microcrystalline cellulose as aid for combustion of polymers from waste of EEEs that usually contain flame retardants that impair the combustion. The composition and concentration of acid solutions (HNO3 or HNO3 plus HCl) were evaluated for metals and metalloids and NH4OH solutions were investigated for Br absorption. Accuracy was evaluated by comparison of results with those obtained using high pressure microwave-assisted wet digestion (HP-MAWD) and also by the analysis of certified reference material (CRM) of polymer (EC680k-low-density polyethylene). Bromine determination was only feasible using digestion by MIC once losses were observed when HP-MAWD was used. Lower limits of detection were obtained for all analytes using MIC (from 0.005 μg g- 1 for Co by ICP-MS up to 3.120 μg g-1 for Sb by ICP OES) in comparison to HP-MAWD due to the higher sample mass that can be digested (400 mg) and the use of diluted absorbing solutions. The combination of HNO3 and HCl for digestion showed to be crucial for quantitative recovery of some elements, as Cr and Sb. In addition, suitable agreement of Cr to CRM value was only obtained by mixing NH4Cl to samples before combustion. No statistical difference (95% confidence level) was observed between the results obtained for As, Cd, Co, Cr, Cu, Hg, Ni, Pb, Sb, and Zn by MIC and HP-MAWD methods. Agreement with certified values was better than 96% using MIC for all inorganic contaminants. Particularly for Br, MIC was the method of choice for digestion due to the possibility of using diluted alkaline solutions for analyte absorption. Based on the obtained results, MIC can be considered as a suitable method for digestion of polymers from waste of EEEs for further plasma based determination of inorganic contaminants.

Monitoring of Cr, Cu, Pb, V and Zn in polluted soils by laser induced breakdown spectroscopy (LIBS).

PubMed

Dell'Aglio, Marcella; Gaudiuso, Rosalba; Senesi, Giorgio S; De Giacomo, Alessandro; Zaccone, Claudio; Miano, Teodoro M; De Pascale, Olga

2011-05-01

Laser Induced Breakdown Spectroscopy (LIBS) is a fast and multi-elemental analytical technique particularly suitable for the qualitative and quantitative analysis of heavy metals in solid samples, including environmental ones. Although LIBS is often recognised in the literature as a well-established analytical technique, results about quantitative analysis of elements in chemically complex matrices such as soils are quite contrasting. In this work, soil samples of various origins have been analyzed by LIBS and data compared to those obtained by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). The emission intensities of one selected line for each of the five analytes (i.e., Cr, Cu, Pb, V, and Zn) were normalized to the background signal, and plotted as a function of the concentration values previously determined by ICP-OES. Data showed a good linearity for all calibration lines drawn, and the correlation between ICP-OES and LIBS was confirmed by the satisfactory agreement obtained between the corresponding values. Consequently, LIBS method can be used at least for metal monitoring in soils. In this respect, a simple method for the estimation of the soil pollution degree by heavy metals, based on the determination of an anthropogenic index, was proposed and determined for Cr and Zn.

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

PubMed

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

2017-09-01

The treatment of corpses with extremely acid or basic liquids is sometimes performed in criminal contexts. A thorough characterization by chemical analysis may provide further help to macroscopic and microscopic analysis; 63 porcine bone samples were treated with solutions at different pH (1-14) for immersion periods up to 70 days, as well as in extremely acidic sulfuric acid solutions (9 M/18 M) and extremely basic sodium hydroxide. Inductively coupled optical emission spectrometry (ICP-OES)/plasma mass spectrometry (ICP-MS), Fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray analysis (EDX), X-ray powder diffraction (XRPD), and scanning electron microscopy (SEM) showed that only the sulfuric acid solution 18 M was able to completely dissolve the sample. In addition, chemical analysis allowed to recognize the contact between bone and substances. Hydrated calcium sulfate arose from extreme pH. The possibility of detecting the presence of human material within the residual solution was demonstrated, especially with FT-IR, ICP-OES, and EDX. © 2017 American Academy of Forensic Sciences.

Final report on CCQM-K125: elements in infant formula

NASA Astrophysics Data System (ADS)

Merrick, J.; Saxby, D.; Dutra, E. S.; Sena, R. C.; Araújo, T. O.; Almeida, M. D.; Yang, L.; Pihillagawa, I. G.; Mester, Z.; Sandoval, S.; Wei, C.; Castillo, M. E. D.; Oster, C.; Fisicaro, P.; Rienitz, O.; Pape, C.; Schulz, U.; Jährling, R.; Görlitz, V.; Lampi, E.; Kakoulides, E.; Sin, D. W. M.; Yip, Y. C.; Tsoi, Y. T.; Zhu, Y.; Okumu, T. O.; Yim, Y. H.; Heo, S. W.; Han, M.; Lim, Y.; Osuna, M. A.; Regalado, L.; Uribe, C.; Buzoianu, M. M.; Duta, S.; Konopelko, L.; Krylov, A.; Shin, R.; Linsky, M.; Botha, A.; Magnusson, B.; Haraldsson, C.; Thiengmanee, U.; Klich, H.; Can, S. Z.; Coskun, F. G.; Tunc, M.; Entwisle, J.; O'Reilly, J.; Hill, S.; Goenaga-Infante, H.; Winchester, M.; Rabb, S. A.; Pérez, R.

2017-01-01

CCQM-K125 was organized by the Inorganic Analysis Working Group (IAWG) of CCQM to assess and document the capabilities of the national metrology institutes (NMIs) or the designated institutes (DIs) to measure the mass fractions of trace elements (K, Cu and I) in infant formula. Government Laboratory, Hong Kong SAR (GLHK) acted as the coordinating laboratory. In CCQM-K125, 25 institutes submitted the results for potassium, 24 institutes submitted the results for copper and 8 institutes submitted the results for iodine. For examination of potassium and copper, most of the participants used microwave-assisted acid digestion methods for sample dissolution. A variety of instrumental techniques including inductively coupled plasma mass spectrometry (ICP-MS), isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS), inductively coupled plasma optical emission spectrometry (ICP-OES), atomic absorption spectrometry (AAS), flame atomic emission spectrometry (FAES) and microwave plasma atomic emission spectroscopy (MP-AES) were employed by the participants for determination. For analysis of iodine, most of the participants used alkaline extraction methods for sample preparation. ICP-MS and ID-ICP-MS were used by the participants for the determination. Generally, the participants' results of CCQM-K125 were found consistent for all measurands according to their equivalence statements. Except with some extreme values, most of the participants obtained the values of di/U(di) within +/- 1 for the measurands. Main text To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

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

PubMed

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

2013-10-01

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

Development of routines for simultaneous in situ chemical composition and stable Si isotope ratio analysis by femtosecond laser ablation inductively coupled plasma mass spectrometry.

PubMed

Frick, Daniel A; Schuessler, Jan A; von Blanckenburg, Friedhelm

2016-09-28

Stable metal (e.g. Li, Mg, Ca, Fe, Cu, Zn, and Mo) and metalloid (B, Si, Ge) isotope ratio systems have emerged as geochemical tracers to fingerprint distinct physicochemical reactions. These systems are relevant to many Earth Science questions. The benefit of in situ microscale analysis using laser ablation (LA) over bulk sample analysis is to use the spatial context of different phases in the solid sample to disclose the processes that govern their chemical and isotopic compositions. However, there is a lack of in situ analytical routines to obtain a samples' stable isotope ratio together with its chemical composition. Here, we evaluate two novel analytical routines for the simultaneous determination of the chemical and Si stable isotope composition (δ(30)Si) on the micrometre scale in geological samples. In both routines, multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) is combined with femtosecond-LA, where stable isotope ratios are corrected for mass bias using standard-sample-bracketing with matrix-independent calibration. The first method is based on laser ablation split stream (LASS), where the laser aerosol is split and introduced simultaneously into both the MC-ICP-MS and a quadrupole ICP-MS. The second method is based on optical emission spectroscopy using direct observation of the MC-ICP-MS plasma (LA-MC-ICP-MS|OES). Both methods are evaluated using international geological reference materials. Accurate and precise Si isotope ratios were obtained with an uncertainty typically better than 0.23‰, 2SD, δ(30)Si. With both methods major element concentrations (e.g., Na, Al, Si, Mg, Ca) can be simultaneously determined. However, LASS-ICP-MS is superior over LA-MC-ICP-MS|OES, which is limited by its lower sensitivity. Moreover, LASS-ICP-MS offers trace element analysis down to the μg g(-1)-range for more than 28 elements due to lower limits of detection, and with typical uncertainties better than 15%. For in situ simultaneous stable isotope measurement and chemical composition analysis LASS-ICP-MS in combination with MC-ICP-MS is the method of choice. Copyright © 2016 Elsevier B.V. All rights reserved.

Spatial distribution and historical trends of heavy metals in the sediments of petroleum producing regions of the Beibu Gulf, China.

PubMed

Yang, Jichao; Wang, Weiguo; Zhao, Mengwei; Chen, Bin; Dada, Olusegun A; Chu, Zhihui

2015-02-15

The concentrations of As, Sb, Hg, Pb, Cd, and Ba in the surface and core sediments of the oil and gas producing region of the Beibu Gulf were measured by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), Inductively Coupled Plasma Mass Spectrometry (ICP-MS) and Atomic Fluorescence Spectrometry (AFS), and the spatial distribution and historical trends of these elements are discussed. The results show that the concentrations of these elements are highest near the platforms. The results of Enrichment Factor (EF) and Potential Ecological Risk Index (PERI) also reveal significantly higher enrichment around the platforms, which imply that the offshore petroleum production was the cause of the unusual distribution and severe enrichment of these elements in the study area. The environment around the platforms was highly laden with toxic elements, thereby representing a very high ecological risk to the environment of the study area. Copyright © 2014 Elsevier Ltd. All rights reserved.

Rapid Detection of Transition Metals in Welding Fumes Using Paper-Based Analytical Devices

PubMed Central

Volckens, John

2014-01-01

Metals in particulate matter (PM) are considered a driving factor for many pathologies. Despite the hazards associated with particulate metals, personal exposures for at-risk workers are rarely assessed due to the cost and effort associated with monitoring. As a result, routine exposure assessments are performed for only a small fraction of the exposed workforce. The objective of this research was to evaluate a relatively new technology, microfluidic paper-based analytical devices (µPADs), for measuring the metals content in welding fumes. Fumes from three common welding techniques (shielded metal arc, metal inert gas, and tungsten inert gas welding) were sampled in two welding shops. Concentrations of acid-extractable Fe, Cu, Ni, and Cr were measured and independently verified using inductively coupled plasma-optical emission spectroscopy (ICP-OES). Results from the µPAD sensors agreed well with ICP-OES analysis; the two methods gave statistically similar results in >80% of the samples analyzed. Analytical costs for the µPAD technique were ~50 times lower than market-rate costs with ICP-OES. Further, the µPAD method was capable of providing same-day results (as opposed several weeks for ICP laboratory analysis). Results of this work suggest that µPAD sensors are a viable, yet inexpensive alternative to traditional analytic methods for transition metals in welding fume PM. These sensors have potential to enable substantially higher levels of hazard surveillance for a given resource cost, especially in resource-limited environments. PMID:24515892

Rapid detection of transition metals in welding fumes using paper-based analytical devices.

PubMed

Cate, David M; Nanthasurasak, Pavisara; Riwkulkajorn, Pornpak; L'Orange, Christian; Henry, Charles S; Volckens, John

2014-05-01

Metals in particulate matter (PM) are considered a driving factor for many pathologies. Despite the hazards associated with particulate metals, personal exposures for at-risk workers are rarely assessed due to the cost and effort associated with monitoring. As a result, routine exposure assessments are performed for only a small fraction of the exposed workforce. The objective of this research was to evaluate a relatively new technology, microfluidic paper-based analytical devices (µPADs), for measuring the metals content in welding fumes. Fumes from three common welding techniques (shielded metal arc, metal inert gas, and tungsten inert gas welding) were sampled in two welding shops. Concentrations of acid-extractable Fe, Cu, Ni, and Cr were measured and independently verified using inductively coupled plasma-optical emission spectroscopy (ICP-OES). Results from the µPAD sensors agreed well with ICP-OES analysis; the two methods gave statistically similar results in >80% of the samples analyzed. Analytical costs for the µPAD technique were ~50 times lower than market-rate costs with ICP-OES. Further, the µPAD method was capable of providing same-day results (as opposed several weeks for ICP laboratory analysis). Results of this work suggest that µPAD sensors are a viable, yet inexpensive alternative to traditional analytic methods for transition metals in welding fume PM. These sensors have potential to enable substantially higher levels of hazard surveillance for a given resource cost, especially in resource-limited environments.

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

PubMed

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

2008-11-01

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

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

NASA Astrophysics Data System (ADS)

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

2009-06-01

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

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

PubMed

Vijayaraghavan, K; Joshi, U M

2013-01-01

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

[Determination of Fe, Ti and V in vanadium and titanium magnetite by ICP-OES and microwave-assisted digestion].

PubMed

Zhu, Xia-ping; Yin, Ji-xian; Chen, Wei-dong; Hu, Zi-Wen; Liang, Qing-xun; Chen, Tie-yao

2010-08-01

The method of determination of iron, titanium and vanadium in indissolvable vanadium and titanium magnetite has been established by inductively coupled plasma atomic emission spectroscopy through adding the complexant A and using microwave-assisted digestion. The optimal conditions are confirmed by orthogonal experiment: 0.1 g vanadium and titanium magnetite, 0.04 g complexant A, 12 mL concentrated HC1, 10 min digestion time, and 385 W microwave power. The newly-established method has been applied to digest vanadium and titanium magnetite of Panzhihua Iron and Steel Institute (GBW07226). The iron, titanium and vanadium were detected by ICP-OES, and both comparative error (Er%) and comparative standard deviation (RSD%) met the demand of analytical chemistry, and the complexant A can significantly accelerate the dissolution of vanadium and titanium magnetite through the complexation with the dissolved metal ions, and making the surface of sample and hydrochloric acid medium to update constantly. The determination of the main and trace elements of digestion solution at the same time was achieved by ICP-OES. The method has the advantages of less use of reagents, economy, rapidness, and being friendly to environment, and it meets the requirement for rapid and volume determination. So the method has the value of practical application for the entry-exit inspection and quarantine department of the state and other relevant inspection units.

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

PubMed

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

2012-10-01

A mobile sampling and measurement system for the analysis of gaseous and liquid samples in the field was developed. An inductively coupled plasma optical emission spectrometer (ICP-OES), which is built into a van, was used as detector. The analytical system was calibrated with liquid and/or gaseous standards. It was shown that identical mass flows of either gaseous or liquid standards resulted in identical ICP-OES signal intensities. In a field measurement campaign trace and minor elements in the raw flue gas of a waste wood combustor were monitored. Sampling was performed with a highly transport efficient liquid quench system, which allowed to observe temporal variations in the elemental process gas composition. After a change in feedstock an immediate change of the element concentrations in the flue gas was detected. A comparison of the average element concentrations during the combustion of the two feedstocks showed a high reproducibility for matrix elements that are expected to be present in similar concentrations. On the other hand elements that showed strong differences in their concentration in the feedstock were also represented by a higher concentration in the flue gas. Following the temporal variations of different elements revealed strong correlations between a number of elements, such as chlorine with sodium, potassium and zinc, as well as arsenic with lead, and calcium with strontium. Copyright © 2012 Elsevier Ltd. All rights reserved.

Using Gamma ray and Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) to Evaluate Elemental Sequences in Cap-carbonates and Cap-like Carbonates of the Death Valley Region

NASA Astrophysics Data System (ADS)

Holter, S. A.; Theissen, K. M.; Hickson, T. A.; Bostick, B.

2004-12-01

The Snowball Earth theory of Hoffman et al. (1998) proposes dramatic post-glacial chemical weathering as large concentrations of carbon were removed from the atmosphere. This would result in a large input of terrigenous material into the oceans; hence, we might expect that carbonates formed under these conditions would demonstrate elevated K, U, Th levels in comparison to carbonates formed under more typical conditions. In January of 2004 we collected spectral gamma data (K, U, Th) and hand samples from cap carbonates (Noonday Dolomite) and cap-like carbonates (Beck Spring Dolomite) of the Death Valley region in order to explore elemental changes in post-snowball Earth oceans. Based on our spectral gamma results, Th/U ratio trends suggested variations in the oxidation state of the Precambrian ocean. We pursued further investigations of trace elements to ascertain the reliability of these results by using ICP-OES. A suite of 25 trace elements was measured, most notably including U and Th. The ICP-OES data not only allow us to compare elemental changes between cap-carbonates and cap-like carbonates, but they also allow for a comparison of optical emission spectrometry and hand held gamma spectrometry methods. Both methods show similar trends in U and Th values for both the cap-carbonates and cap-like carbonates.

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

USGS Publications Warehouse

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

1989-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2013-08-01

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

Identification and characterization of gadolinium(III) complexes in biological tissue extracts.

PubMed

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.

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

PubMed

Pereira, João B; Dantas, Kelly G F

2016-04-01

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

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

PubMed

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

2015-01-01

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

Characterization of Hatay honeys according to their multi-element analysis using ICP-OES combined with chemometrics.

PubMed

Yücel, Yasin; Sultanoğlu, Pınar

2013-09-01

Chemical characterisation has been carried out on 45 honey samples collected from Hatay region of Turkey. The concentrations of 17 elements were determined by inductively coupled plasma optical emission spectrometry (ICP-OES). Ca, K, Mg and Na were the most abundant elements, with mean contents of 219.38, 446.93, 49.06 and 95.91 mg kg(-1) respectively. The trace element mean contents ranged between 0.03 and 15.07 mg kg(-1). Chemometric methods such as principal component analysis (PCA) and cluster analysis (CA) techniques were applied to classify honey according to mineral content. The first most important principal component (PC) was strongly associated with the value of Al, B, Cd and Co. CA showed eight clusters corresponding to the eight botanical origins of honey. PCA explained 75.69% of the variance with the first six PC variables. Chemometric analysis of the analytical data allowed the accurate classification of the honey samples according to origin. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wellinger, Marco, E-mail: marco.wellinger@gmail.com; Ecole Polytechnique Federale de Lausanne; Wochele, Joerg

2012-10-15

Highlights: Black-Right-Pointing-Pointer Simultaneous measurements of 23 elements in process gases of a waste wood combustor. Black-Right-Pointing-Pointer Mobile ICP spectrometer allows measurements of high quality at industrial plants. Black-Right-Pointing-Pointer Continuous online measurements with high temporal resolution. Black-Right-Pointing-Pointer Linear correlations among element concentrations in the raw flue gas were detected. Black-Right-Pointing-Pointer Novel sampling and calibration methods for ICP-OES analysis of process gases. - Abstract: A mobile sampling and measurement system for the analysis of gaseous and liquid samples in the field was developed. An inductively coupled plasma optical emission spectrometer (ICP-OES), which is built into a van, was used as detector. Themore » 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.« less

Modeling the Effect of a Hydrophobic Concrete Admixture on Chloride Ingress: Contractors Supplemental Report for CPC Project F09-AR05A

DTIC Science & Technology

2017-12-01

of acronyms  ASTM: American Society for Testing and Materials  CSA: Canadian Standard Association  FA: fly ash  GU: general use ( cement )  ICP...OES: inductively coupled plasma optical emission spectrometry  OPC: Ordinary Portland cement  RH: relative humidity  UFGS: Unified Facilities Guide...Specifications  w/b: water-to-binder ratio  w/c: water-to- cement ratio SIMCO Technologies Inc. 2013 Page | 3 1 Executive summary SIMCO

[Performance comparison of material tests for cadmium and lead in food contact plastics].

PubMed

Mutsuga, Motoh; Abe, Tomoyuki; Abe, Yutaka; Ishii, Rie; Itoh, Yuko; Ohno, Hiroyuki; Ohno, Yuichiro; Ozaki, Asako; Kakihara, Yoshiteru; Kaneko, Reiko; Kawamura, Yoko; Shibata, Hiroshi; Sekido, Haruko; Sonobe, Hironori; Takasaka, Noriko; Tajima, Yoshiyasu; Tanaka, Aoi; Nomura, Chie; Hikida, Akinori; Matsuyama, Sigetomo; Murakami, Ryo; Yamaguchi, Miku; Wada, Takenari; Watanabe, Kazunari; Akiyama, Hiroshi

2014-01-01

Based on the Japanese Food Sanitation Law, the performances of official and alternative material test methods for cadmium (Cd) and lead (Pb) in food contact plastics were compared. Nineteen laboratories participated to an interlaboratory study, and quantified Cd and Pb in three PVC pellets. in the official method, a sample is digested with H2SO4, taken up in HCl, and evaporated to dryness on a water bath, then measured by atomic absorption spectrometry (AAS) or inductively coupled plasma-optical emission spectrometry (ICP-OES). Statistical treatment revealed that the trueness, repeatability (RSDr) and reproducibility (RSDr) were 86-95%, 3.1-9.4% and 8.6-22.1%, respectively. The values of the performance parameters fulfilled the requirements , and the performances met the test specifications. The combination of evaporation to dryness on a hot plate and measurement by AAS or ICP-OES is applicable as an alternative method. However, the trueness and RSDr were inferior to those of the official method. The performance parameters obtained by using the microwave digestion method (MW method) to prepare test solution were better than those of the official method. Thus, the MW method is available as an alternative method. Induced coupled plasma-mass spectrometry (ICP-MS) is also available as an alternative method. However, it is necessary to ensure complete digestion of the sample.

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

PubMed

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

2014-01-01

Lung cancer ranks as the fifth largest of all cancer cases in Thailand. However, it is the first leading cancer in the northern part of Thailand (data from 2003-2007). There are several predisposing causes that lead to lung cancer and one important inducement is particulate matters (PMs). Lampang Province in Thailand is famous for the ceramic industry, where there are over 200 ceramic industrial factories. PMs are produced during the ceramic manufacturing process and spread throughout all of the working areas. It is very possible that workers could directly inhale PM-contaminated air during working hours. This study focuses on the toxic effects of PMs collected from ceramic factories on genes and lungs of rats. PMs collected from six ceramic factories in Lampang Province were extracted using dimethyl sulfoxide (DMSO). The inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES) were used to analyze the chemical elements at lower and higher concentrations, respectively. Then, the toxicity of PMs on the genes was examined by the Ames test, and subsequently, the effect of PMs on DNA was examined by quantifying the amount of 8-hydroxy-2'-deoxyguanosine (8-OHdG). Finally, the toxicity of the PMs on rat's lungs was examined by histology. As chemical elements of lower concentrations, cadmium, chromium, nickel, copper, and lead were detected by ICP-MS. As chemical elements of higher concentrations, manganese, magnesium, zinc, iron, potassium, calcium, and sodium were detected by ICP-OES. No mutagenicity in Salmonella typhimurium was found in the PM extracts from all six factories by utilizing the Ames test. In the histological study, the reduction in spaces of alveolar ducts and sacs, and terminal bronchioles, the thickening of interstitial connective tissues were noted by PM extracts in high amounts (100 and 350 µg). Female rats were more sensitive to PM extracts than males in terms of their pulmonary damages. PMs were not mutagenic to S. typhimurium but can damage the lung tissue of rats.

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

PubMed

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

2014-04-01

A slurry suspension sampling technique is developed and optimized for the rapid microextraction of heavy metals and analysis using nanometer-sized ceria-coated silica-iron oxide particles and inductively coupled plasma optical emission spectrometry (ICP-OES). Magnetic-silica material is synthesized by a co-precipitation and sol-gel method followed by ceria coating through a precipitation. The large particles are removed using a sedimentation-fractionation procedure and a magnetic homogeneous colloidal suspension of ceria-modified iron oxide-silica is produced for microextraction. The nanometer-sized particles are separated from the sample solution magnetically and analyzed with ICP-OES using a slurry suspension sampling approach. The ceria-modified iron oxide-silica does not contain any organic matter and this probably justifies the absence of matrix effect on plasma atomization capacity, when increased concentrations of slurries are aspirated. The As, Be, Mo, Cr, Cu, Pb, Hg, Sb, Se and V can be preconcentrated by the proposed method at pH 6.0 while Mn, Cd, Co and Ni require a pH ≥ 8.0. Satisfactory values are obtained for the relative standard deviations (2-6%), recoveries (88-102%), enrichment factors (14-19) and regression correlation coefficients as well as detectability, at sub-μg L(-1) levels. The applicability of magnetic ceria for the microextraction of metal ions in combination with the slurry introduction technique using ICP is substantiated by the analysis of environmental water and urine samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Antibacterial Ag/a-C nanocomposite coatings: The influence of nano-galvanic a-C and Ag couples on Ag ionization rates

NASA Astrophysics Data System (ADS)

Manninen, N. K.; Calderon, S.; Carvalho, I.; Henriques, M.; Cavaleiro, A.; Carvalho, S.

2016-07-01

Biofilm formation has been pointed as a major concern in different industrial applications, namely on biomedical implants and surgical instruments, which has prompted the development of new strategies for production of efficient antimicrobial surfaces. In this work, nano-galvanic couples were created to enhance the antibacterial properties of silver, by embedding it into amorphous carbon (a-C) matrix. The developed Ag/a-C nanocomposite coatings, deposited by magnetron sputtering, revealed an outstanding antibacterial activity against Staphylococcus epidermidis, promoting a total reduction in biofilm formation with no bacteria counts in all dilution. The open circuit potential (OCP) tests in 0.9% NaCl confirmed that a-C shows a positive OCP value, in contrast to Ag coating, thus enhancing the ionization of biocidal Ag+ due to the nano-galvanic couple activation. This result was confirmed by the inductively coupled plasma-optical emission spectroscopy (ICP-OES), which revealed a higher Ag ionization rate in the nanocomposite coating in comparison with the Ag coating. The surface of Ag/a-C and Ag coatings immersed in 0.9% NaCl were monitored by scanning electron microscopy (SEM) over a period of 24 h, being found that the Ag ionization determined by ICP-OES was accompanied by an Ag nanoparticles coalescence and agglomeration in Ag/a-C coating.

Concentrations of mercury and other metals in black bass (Micropterus spp.) from Whiskeytown Lake, Shasta County, California, 2005

USGS Publications Warehouse

May, Jason T.; Hothem, Roger L.; Bauer, Marissa L.; Brown, Larry R.

2012-01-01

This report presents the results of a reconnaissance study conducted by the U.S. Geological Survey (USGS) to determine mercury (Hg) and other selected metal concentrations in Black bass (Micropterus spp.) from Whiskeytown Lake, Shasta County, California. Total mercury concentrations were determined by cold-vapor atomic absorption spectroscopy (CVAAS) in fillets and whole bodies of each sampled fish. Selected metals scans were performed on whole bodies (less the fillets) by inductively coupled plasma–mass spectroscopy (ICP-MS) and inductively coupled plasma–optical emission spectroscopy (ICP-OES). Mercury concentrations in fillet samples ranged from 0.06 to 0.52 micrograms per gram (μg/g) wet weight (ww). Total mercury (HgT) in the same fish whole-body samples ranged from 0.04 to 0.37 (μg/g, ww). Mercury concentrations in 17 percent of "legal catch size" (≥305 millimeters in length) were above the U.S. Environmental Protection Agency water-quality criterion for the protection of human health of 0.30 μg/g (ww). These data will serve as a baseline for future monitoring efforts within Whiskeytown Lake.

Destructive versus non-destructive methods for geochemical analyses of ceramic artifacts: comparison of portable XRF and ICP-MS data on Bronze Age ceramics from Failaka Island (Kuwait) and Bahrain

NASA Astrophysics Data System (ADS)

Stremtan, Ciprian; Ashkanani, Hasan; Tykot, Robert H.

2013-04-01

The study of bi-phase (i.e. matrix and clasts) geochemical composition of ceramic artifacts is a very powerful tool in fingerprinting the raw materials used by ancient manufacturers (clay sources, tempering materials, coloring agents, etc.), as well as in understanding the physical parameters of the manufacturing techniques. Reliable datasets often require the deployment of destructive techniques that will irremediably damage the artifact. Recent advances in portable X-ray fluorescence instrumentation (pXRF) allow for quick measurements of a range of chemical elements that not too long ago were available only through complicated and often destructive means of analytical chemistry (instrumental neutron activation analysis - INAA, inductively coupled plasma mass spectrometry - ICP-MS, direct coupled plasma-optical emission spectroscopy - DCP-OES etc.). In this contribution we present a comparison of datasets acquired by means of pXRF, DCP-OES, and ICP-MS on Bronze Age ceramics from Failaka Island (Kuwait) and Bahrain. The samples chosen for this study are fine grained, with very well sorted mineral components, and lack any visible organic material fragments. The sample preparation for ICP-MS and DCP-OES analyses was carried out on powdered samples, by using LiBO2 flux fusion and Ge (for the DCP-OES) and In (for ICP-MS) were used as internal standards. The measurements were calibrated against certified reference materials ranging from shales to rhyolites (SGR-1, SDo-1, JA-2, and JR-1) and performed at Univerity of South Florida's Center for Geochemical Analyses. The analytical errors for major elements was smaller than 5 %, while for selected trace elements the error was usually smaller than 3 %. The same set of elements was measured on the same samples at University of South Florida's Anthropology Department using a pXRF device equipped with obsidian filter. Each sample was measured three times and the values were averaged. Two certified reference materials (NIST-612 glass and MACS-3 pressed powder) were also measured to check for accuracy and precision. Our preliminary data shows that most of the major and trace elemental data acquired by both methods are consistent. Some transition metals (e.g. Y, Fe, and Mn) yielded overall lower values when measured with pXRF device (ranging from 27 to 60 % difference), while Ni and Ba showed systematically higher values (20 to 53 %). If samples are chosen properly for pXRF measurements (i.e. thoroughly cleaned, fine grained, well sorted) and the device is properly calibrated, the results are comparable with DCP-OES and ICP-MS data, thus being suitable to use for geochemical fingerprinting

Investigation of a measure of robustness in inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Makonnen, Yoseif; Beauchemin, Diane

2015-01-01

In industrial/commercial settings where operators often have minimal expertise in inductively coupled plasma (ICP) mass spectrometry (MS), there is a prevalent need for a response factor indicating robust plasma conditions, which is analogous to the Mg II/Mg I ratio in ICP optical emission spectrometry (OES), whereby a Mg II/Mg I ratio of 10 constitutes robust conditions. While minimizing the oxide ratio usually corresponds to robust conditions, there is no specific target value that is widely accepted as indicating robust conditions. Furthermore, tuning for low oxide ratios does not necessarily guarantee minimal matrix effects, as they really address polyatomic interferences. From experiments, conducted in parallel for both MS and OES, there were some element pairs of similar mass and very different ionization potential that were exploited for such a purpose, the rationale being that, if these elements were ionized to the same extent, then that could be indicative of a robust plasma. The Be II/Li I intensity ratio was directly related to the Mg II/Mg I ratio in OES. Moreover, the 9Be+/7Li+ ratio was inversely related to the CeO+/Ce+ and LaO+/La+ oxide ratios in MS. The effects of different matrices (i.e. 0.01-0.1 M Na) were also investigated and compared to a conventional argon plasma optimized for maximum sensitivity. The suppression effect of these matrices was significantly reduced, if not eliminated in the case of 0.01 M Na, when the 9Be+/7Li+ ratio was around 0.30 on the Varian 820 MS instrument. Moreover, a very similar ratio (0.28) increased robustness to the same extent on a completely different ICP-MS instrument (PerkinElmer NEXION). Much greater robustness was achieved using a mixed-gas plasma with nitrogen in the outer gas and either nitrogen or hydrogen as a sheathing gas, as the 9Be+/7Li+ ratio was then around 1.70. To the best of our knowledge, this is the first report on using a simple analyte intensity ratio, 9Be+/7Li+, to gauge plasma robustness.

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

PubMed

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

2015-09-01

Methyltin mercaptide is widely used as one of the best heat stabilizer in the polyvinylchloride (PVC) thermal processing due to its excellent stability, good transparency, high compatibility and weather resistance. The content of sulfur and tin significantly affects its quality and performance, so it is of great significance to develop an analytical method for the simultaneous determination of sulfur and tin. Inductively coupled plasma atomic emission spectrometry (ICP-OES) has been a powerful analytical tool for a myriad of complex samples owing to its advantages of the low detection limits, rapid and precise determinations over wide dynamic ranges, freedom from chemical inter-element interferences, the high sample throughput and above all, simultaneous multi-elements analysis. Microwave technique as a well-developed method for sample preparation can dramatically reduce the digestion time and the loss of volatile elements compared with the traditional open digestion. Hereby, a microwave-assisted acid digestion (MW-AAD) procedure followed by inductively coupled plasma optical emission spectroscopy (ICP-OES) analysis was developed for the simultaneous determination of Sn and S in methyltin mercaptide. This method has the advantages of simplicity, rapidness, good accuracy, green and less use of samples. Parameters affecting the MW-AAD such as the digestion solution and digestion time were optimized by using a chemical analyzed reference sample (DX-181) to attain tin and sulfur quantitative recoveries. HNO3-HCl-HClO4 (v/v/v=9:3:1) and 10 min were the optimum digestion solution and digestion time, respectively. Under optimum conditions, the standard addition method and the standard calibration curve method were both been used to detect Sn and S in DX-181. There was no significant difference between two methods and the relative deviations to the chemical analysis values were both less than 2%. Additionally, the accuracy of the MW-AAD method was examined by analyzing three methyltin mercaptide samples (DX-181, DX-990, DX-960). The results were satisfactory with the relative deviations (<3%) and the recoveries of standard addition (99%~102%).

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

PubMed

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

2017-01-01

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

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

PubMed Central

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

2017-01-01

The determination of trace rare-earth elements (REEs) can be used for the assessment of environmental pollution, and is of great significance to the study of toxicity and toxicology in animals and plants. N, N, N′, N′-tetraoctyl diglycolamide (TODGA) is an environmental friendly extractant that is highly selective to REEs. In this study, an analytical method was developed for the simultaneous determination of 16 trace REEs in simulated water samples by inductively coupled plasma optical emission spectroscopy (ICP-OES). With this method, TODGA was used as the extractant to perform the liquid-liquid extraction (LLE) sample pretreatment procedure. All 16 REEs were extracted from a 3 M nitric acid medium into an organic phase by a 0.025 M TODGA petroleum ether solution. A 0.03 M ethylenediaminetetraacetic acid disodium salt (EDTA) solution was used for back-extraction to strip the REEs from the organic phase into the aqueous phase. The aqueous phase was concentrated using a vacuum rotary evaporator and the concentration of the 16 REEs was detected by ICP-OES. Under the optimum experimental conditions, the limits of detection (3σ, n = 7) for the REEs ranged from 0.0405 ng mL-1 (Nd) to 0.5038 ng mL-1 (Ho). The relative standard deviations (c = 100 ng mL-1, n = 7) were from 0.5% (Eu) to 4.0% (Tm) with a linear range of 4–1000 ng mL-1 (R2 > 0.999). The recoveries of 16 REEs ranged from 95% to 106%. The LLE-ICP-OES method established in this study has the advantages of simple operation, low detection limits, fast analysis speed and the ability to simultaneously determine 16 REEs, thereby acting as a viable alternative for the simultaneous detection of trace amounts of REEs in water samples. PMID:28945788

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

PubMed

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

2017-06-01

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

The determination of trace elements in crude oil and its heavy fractions by atomic spectrometry

NASA Astrophysics Data System (ADS)

Duyck, Christiane; Miekeley, Norbert; Porto da Silveira, Carmem L.; Aucélio, Ricardo Q.; Campos, Reinaldo C.; Grinberg, Patrícia; Brandão, Geisamanda P.

2007-09-01

A literature review on the determination of trace elements in crude oil and heavy molecular mass fractions (saturates, aromatics, resins and asphaltenes) by ICP-MS, ICP OES and AAS is presented. Metal occurrences, forms and distributions are examined as well as their implications in terms of reservoir geochemistry, oil refining and environment. The particular analytical challenges for the determination of metals in these complex matrices by spectrochemical techniques are discussed. Sample preparation based on ashing, microwave-assisted digestion and combustion decomposition procedures is noted as robust and long used. However, the introduction of non-aqueous solvents and micro-emulsions into inductively coupled plasmas is cited as a new trend for achieving rapid and accurate analysis. Separation procedures for operationally defined fractions in crude oil are more systematically applied for the observation of metal distributions and their implications. Chemical speciation is of growing interest, achieved by the coupling of high efficiency separation techniques (e.g., HPLC and GC) to ICP-MS instrumentation, which allows the simultaneous determination of multiple organometallic species of geochemical and environmental importance.

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

PubMed

Zhou, Hui; Tan, Qian; Gao, Ya-ling; Sang, Shi-hua; Chen, Wen

2015-10-01

Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), Flame Atomic Absorption Spectrometry (FAAS) and Visible Spectrometry (VS) was applied for determination of Ag and Li in lithium-aluminium alloy standard sample and test sample, their respective advantages and disadvantages were compared, the excellent selectivity of ICP-OES was confirmed by analyses of certified standard sample. Three different sample digestion methods were compared and discussed in this study. It was found that the better accuracy would be obtained by digesting sample with chloroazotic acid while the content of Li was measured by FAAS, and it was better to digest sample with hydrochloric acid and hydrogen peroxide while determining Ag and Li by ICP-OES simultaneously and determining Ag by FAAS and VS. The interference of co-existing elements and elimination methods was detailedly discussed. Ammonium hydroxide was added to adjust the sample solution into alkalescent and Al, Ti, Zr was precipitated by forming hydroxide precipitation, Mg and Cu was formed complex precipitation with 8-hydroxyquinoline in this condition, then the interference from matrix element to determinate Ag by FAAS was eliminated. In addition, phosphate was used to precipitate Ti to eliminate its interference for determination of Li by FAAS. The same treatment of determination for Ag by FAAS was used to eliminate the interference of matrix element for determination of Ag by VS, the excess of nitrate was added into sample and heated to release Ag+ from silver chloride complex, and the color of 8-hydroxyquinoline was eliminated because of decomposed by heating. The accuracy of analysis result for standard sample was conspicuously improved which confirms the efficient of the method to eliminate interference in this study. The optimal digestion method and eliminate interference method was applied to lithium-aluminium alloy samples. The recovery of samples was from 100.39% to 103.01% by ICP-OES determination for Ag, and from 100.42% to 103.01% by ICP-OES determination for Li. The recovery ranged from 95.91% to 99.98% by FAAS determination for Ag, and ranged from 98.04% to 99.98% for FAAS determination of Li. The recovery was from 98.00% to 101.00 by VS determination for Ag, the analysis results all meet the analysis requirement.

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

PubMed

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

2012-11-15

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

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

PubMed

Faraji, Mohammad; Yamini, Yadollah; Shariati, Shahab

2009-07-30

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

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

PubMed

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.

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

NASA Astrophysics Data System (ADS)

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

2017-01-01

The CCQM-K123 key comparison was organized by the Inorganic Analysis Working Group (IAWG) of CCQM to assess and document the capabilities of the national metrology institutes (NMIs) or the designated institutes (DIs) to measure the mass fractions of sodium, calcium, potassium, magnesium phosphorous and sulfur in biodiesel fuel (BDF). National Metrology Institute of Japan (NMIJ) and National Institute of Standards and Technology (NIST) acted as the coordinating laboratories. Results were submitted by 11 NMIs and DIs. Most of the participants used inductively coupled plasma-mass spectrometry (ICP-MS), isotope dilution technique with ICP-MS and inductively coupled plasma-optical emission spectrometry (ICP-OES) with microwave acid digestion. Accounting for relative expanded uncertainty, comparability of measurement results for each of Na, Ca, K, Mg and P was successfully demonstrated by the participants. Concerning S, the variation in results between participants, particularly those using IDMS methods was observed. According to the additional evaluation and investigation, the revised results were overlapping between IDMS measurements at the k = 2 level. However, this KC does not support S measurements. Main text To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

[Studies on six heavy metal elements dissolution characteristics of Andrographis herb by ICP-OES].

PubMed

Tang, Rui; Li, Tian-Peng; Gu, Xue-Shi; Li, Yong-Jian; Yang, Yi

2010-02-01

A simple and accurate method for the simultaneous determination of As, Ba, Cd, Cr, Cu and Pb in andrographis herb by inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. The samples were digested by HNO3-HClO4. The digestion-determination method was evaluated with the relative standard deviations for all these elements between 2.1% and 4.6%, and the recoveries were between 92.0% and 103.2%. The measuring method was proved to be simple, reliable and highly sensitive. The dissolution characteristics of the 6 heavy metal elements in different solvents and with different extraction methods such as refluxing, soaking, and ultrasonic assisted extraction were studied. The experimental results showed that Ba was in the highest concentration followed by Cu and Cr, and the concentration of As, Pb and Cd was relatively lower in the herb. With the increase in ethanol concentration, the dissolution amount of Ba decreased but that of Cu and Cr increased, and the highest concentration of Cd was dissolved in acidic solution. Overall, Cd and Pb were difficult to dissolve out with 85% ethanol refluxing, but As dissolved comparatively more under the same condition. Comparing the extraction methods, the higher concentration of these 6 metals was obtained by refluxing water or alkaline water than that by 85% ethanol maceration. These differences might be related to the existent forms of these six elements in the herb. The determination and study on dissolution characteristics of these elements by using ICP-OES was important for rational using medicinal resources and ensuring the safety of drugs.

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

PubMed

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

2015-10-01

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

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

PubMed

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

2015-01-01

A method has been developed for the determination of traces of arsenic, boron, bismuth, gallium, germanium, phosphorus, lead, antimony, selenium, silicon and tellurium in nickel matrix. The sample was dissolved in HClO4 (~ 150°C) and nickel was settled as crystalline nickelperchlorate [Ni(ClO4)2] on cooling. The mixture was ultrasonicated and after the separation of Ni(ClO4)2, analytes of interest were determined in the supernatant using ICP-OES. Similarly, it was also found that, after the dissolution of nickel in perchloric acid, when the solution temperature was maintained at ~ 100°C, long needle like crystals of nickel perchlorate were formed. The crystals were separated from the mixture and trace elements in the supernatant were determined using ICP-OES. In both methods the matrix removal was >99% and the recoveries of analytes were in the range 92-97%. The limits of detection for As, B, Bi, Ga, Ge, P, Pb, Sb, Se, Si and Te were found to be 0.18, 0.21, 0.07, 0.06, 0.25, 0.11, 0.09, 0.10, 0.17, 0.20 and 0.07 μg g(-1) respectively. The procedure was applied for the analysis of a standard reference material nickel oxide (SRM 761, Nickel Oxide No.1, NBS, USA) and the values obtained are in close agreement with the certified values. Copyright © 2014 Elsevier B.V. All rights reserved.

Screening of trace elements in hair of the female population with different types of cancers in Wielkopolska region of Poland.

PubMed

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

2014-01-01

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

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

PubMed Central

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

2014-01-01

Background: Lung cancer ranks as the fifth largest of all cancer cases in Thailand. However, it is the first leading cancer in the northern part of Thailand (data from 2003–2007). There are several predisposing causes that lead to lung cancer and one important inducement is particulate matters (PMs). Lampang Province in Thailand is famous for the ceramic industry, where there are over 200 ceramic industrial factories. PMs are produced during the ceramic manufacturing process and spread throughout all of the working areas. It is very possible that workers could directly inhale PM-contaminated air during working hours. Objective: This study focuses on the toxic effects of PMs collected from ceramic factories on genes and lungs of rats. Methods: PMs collected from six ceramic factories in Lampang Province were extracted using dimethyl sulfoxide (DMSO). The inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES) were used to analyze the chemical elements at lower and higher concentrations, respectively. Then, the toxicity of PMs on the genes was examined by the Ames test, and subsequently, the effect of PMs on DNA was examined by quantifying the amount of 8-hydroxy-2′-deoxyguanosine (8-OHdG). Finally, the toxicity of the PMs on rat’s lungs was examined by histology. Results: As chemical elements of lower concentrations, cadmium, chromium, nickel, copper, and lead were detected by ICP-MS. As chemical elements of higher concentrations, manganese, magnesium, zinc, iron, potassium, calcium, and sodium were detected by ICP-OES. No mutagenicity in Salmonella typhimurium was found in the PM extracts from all six factories by utilizing the Ames test. In the histological study, the reduction in spaces of alveolar ducts and sacs, and terminal bronchioles, the thickening of interstitial connective tissues were noted by PM extracts in high amounts (100 and 350 μg). Female rats were more sensitive to PM extracts than males in terms of their pulmonary damages. Conclusions: PMs were not mutagenic to S. typhimurium but can damage the lung tissue of rats. PMID:24390747

Membrane solid phase microextraction with alumina hollow fiber on line coupled with ICP-OES for the determination of trace copper, manganese and nickel in environmental water samples.

PubMed

Cui, Chao; He, Man; Hu, Bin

2011-03-15

A novel alumina hollow fiber was synthesized by sol-gel template method and was characterized by scanning electron microscopy, N(2) adsorption technique and X-ray diffraction. With the use of prepared alumina hollow fiber as extraction membrane, a new method of flow injection (FI)-membrane solid phase microextraction (MSPME) on-line coupled to inductively coupled plasma-optical emission spectrometry (ICP-OES) was developed for simultaneous determination of trace metals (Cu, Mn and Ni) in environmental water samples. The adsorption capacities of the alumina hollow fiber for Cu, Mn and Ni were found to be 6.6, 8.7 and 13.3 mg g(-1), respectively. With a preconcentration factor of 10, the limits of detection (LODs) for Cu, Mn and Ni were found to be 0.88, 0.61 and 0.38 ng mL(-1), respectively, and the relative standard deviations (RSDs) were ranging from 6.2 to 7.9% (n = 7, c = 10 ng mL(-1)). To validate the accuracy, the proposed method was applied to the analysis of certified reference material GSBZ50009-88 environmental water and the determined values are in good agreement with the certified values. The developed method was also employed for the analysis of Yangtze River water and East Lake water, and the recoveries for the spiked samples were in the range of 87.4-110.2%. Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

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

2005-12-01

The members of the committee NMP 264 "Chemical analysis of non-oxidic raw and basic materials" of the German Standards Institute (DIN) have organized two interlaboratory comparisons for multielement determination of trace elements in silicon carbide (SiC) powders via direct solid sampling methods. One of the interlaboratory comparisons was based on the application of inductively coupled plasma optical emission spectrometry with electrothermal vaporization (ETV ICP OES), and the other on the application of optical emission spectrometry with direct current arc (DC arc OES). The interlaboratory comparisons were organized and performed in the framework of the development of two standards related to "the determination of mass fractions of metallic impurities in powders and grain sizes of ceramic raw and basic materials" by both methods. SiC powders were used as typical examples of this category of material. The aim of the interlaboratory comparisons was to determine the repeatability and reproducibility of both analytical methods to be standardized. This was an important contribution to the practical applicability of both draft standards. Eight laboratories participated in the interlaboratory comparison with ETV ICP OES and nine in the interlaboratory comparison with DC arc OES. Ten analytes were investigated by ETV ICP OES and eleven by DC arc OES. Six different SiC powders were used for the calibration. The mass fractions of their relevant trace elements were determined after wet chemical digestion. All participants followed the analytical requirements described in the draft standards. In the calculation process, three of the calibration materials were used successively as analytical samples. This was managed in the following manner: the material that had just been used as the analytical sample was excluded from the calibration, so the five other materials were used to establish the calibration plot. The results from the interlaboratory comparisons were summarized and used to determine the repeatability and the reproducibility (expressed as standard deviations) of both methods. The calculation was carried out according to the related standard. The results are specified and discussed in this paper, as are the optimized analytical conditions determined and used by the authors of this paper. For both methods, the repeatability relative standard deviations were <25%, usually ~10%, and the reproducibility relative standard deviations were <35%, usually ~15%. These results were regarded as satifactory for both methods intended for rapid analysis of materials for which decomposition is difficult and time-consuming. Also described are some results from an interlaboratory comparison used to certify one of the materials that had been previously used for validation in both interlaboratory comparisons. Thirty laboratories (from eight countries) participated in this interlaboratory comparison for certification. As examples, accepted results are shown from laboratories that used ETV ICP OES or DC arc OES and had performed calibrations by using solutions or oxides, respectively. The certified mass fractions of the certified reference materials were also compared with the mass fractions determined in the interlaboratory comparisons performed within the framework of method standardization. Good agreement was found for most of the analytes.

Development of a certified reference material (NMIJ CRM 7505-a) for the determination of trace elements in tea leaves.

PubMed

Zhu, Yanbei; Narukawa, Tomohiro; Inagaki, Kazumi; Kuroiwa, Takayoshi; Chiba, Koichi

2011-01-01

A certified reference material (CRM) for trace elements in tea leaves has been developed in National Metrology Institute of Japan (NMIJ). The CRM was provided as a dry powder (<90 µm) after frozen pulverization of washed and dried fresh tea leaves from a tea plant farm in Shizuoka Prefecture, Japan. Characterization of the property value for each element was carried out exclusively by NMIJ with at least two independent analytical methods, including inductively coupled plasma mass spectrometry (ICP-MS), high-resolution (HR-) ICP-MS, isotope-dilution (ID-) ICP-MS, inductively coupled plasma optical emission spectrometry (ICP-OES), graphite-furnace atomic-absorption spectrometry (GF-AAS) and flame atomic-absorption spectrometry (FAAS). Property values were provided for 19 elements (Ca, K, Mg, P, Al, B, Ba, Cd, Cu, Fe, Li, Mn, Na, Ni, Pb, Rb, Sr, Zn and Co) and informative values for 18 elements (Ti, V, Cr, Y, and all of the lanthanides, except for Pm whose isotopes are exclusively radioactive). The concentration ranges of property values and informative values were from 1.59% (mass) of K to 0.0139 mg kg(-1) of Cd and from 0.6 mg kg(-1) of Ti to 0.0014 mg kg(-1) of Lu, respectively. Combined relatively standard uncertainties of the property values were estimated by considering the uncertainties of the homogeneity, analytical methods, characterization, calibration standard, and dry-mass correction factor. The range of the relative combined standard uncertainties was from 1.5% of Mg and K to 4.1% of Cd.

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

PubMed

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

2017-08-15

Cosmetics are part of the daily life of most of the people. Thus, a complete characterization of the products we applied in our skin is necessary. In this work, an analytical investigation of a wide variety of cosmetics from the point of view of total element content and metallic nanoparticles (NPs) has been performed. Firstly, we analyzed the total element content by ICP-MS and ICP-OES after acid digestion as an assessment of the presence of metal impurities. Prohibited elements in cosmetics, according to the European Commission regulation No 1223/2009, were not detected, and only elements mentioned in the label were found (e.g. Al, Fe, Ti and Si). Secondly, a screening of the presence of NPs has been performed by Dynamic Light Scattering (DLS) and Single Particle Inductively-Coupled Plasma Mass Spectrometry (SP-ICP-MS). Two sample preparation procedures were applied. The first protocol consisted in the preparation of suspensions in 0.1% w/v SDS and the second based on defatting with hexane followed by resuspension in water. DLS was employed as a routine method for a fast analysis of NPs, but this technique showed limitations due to the lack of specificity. SP-ICP-MS analyses were then performed, first as a screening technique to evaluate the presence of TiO 2 and Au NPs in cosmetics suspensions prepared in SDS; and second, when a positive answer was obtained about the presence of NPs from the screening, SP-ICP-MS was used for particle size determination. Results showed that only TiO 2 NPs were present in two sunscreens, one anti-wrinkle day cream, one lip balm protector labeled as 'nano' and in one brand of toothpaste not labeled as 'nano'. Sizes obtained for both sample preparations were compared and ranged from 30 to 120nm in most of the samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis of alkyl phosphates in petroleum samples by comprehensive two-dimensional gas chromatography with nitrogen phosphorus detection and post-column Deans switching.

PubMed

Nizio, Katie D; Harynuk, James J

2012-08-24

Alkyl phosphate based gellants used as viscosity builders for fracturing fluids used in the process of hydraulic fracturing have been implicated in numerous refinery-fouling incidents in North America. In response, industry developed an inductively coupled plasma optical emission spectroscopy (ICP-OES) based method for the analysis of total volatile phosphorus in distillate fractions of crude oil; however, this method is plagued by poor precision and a high limit of detection (0.5±1μg phosphorus mL(-1)). Furthermore this method cannot provide speciation information, which is critical for developing an understanding of the challenge of alkyl phosphates at a molecular level. An approach using comprehensive two-dimensional gas chromatography with nitrogen phosphorus detection (GC×GC-NPD) and post-column Deans switching is presented. This method provides qualitative and quantitative profiles of alkyl phosphates in industrial petroleum samples with increased precision and at levels comparable to or below those achievable by ICP-OES. A recovery study in a fracturing fluid sample and a profiling study of alkyl phosphates in four recovered fracturing fluid/crude oil mixtures (flowback) are also presented. Copyright © 2012 Elsevier B.V. All rights reserved.

Determination of Pd, Pt and Rh in vehicles escape fumes by GF-AAS and ICP-OES.

PubMed

Goncalves, Antonio; Domínguez, José R; Alvarado, José

2008-04-15

Automotive exhaust gases from vehicles using catalytic converters were filtered through cellulose filter papers to collect suspended particles expulsed along with the engine's escape fumes. A specially designed sample collector was used for supporting the filter papers during collection. The collector was manufactured from a new car's exhaust pipe. A cellulose circular paper filter, 11 cm diameter, was attached to one end of the pipe and kept centered by pressing it against the borders of the pipe by means of a perforated aluminum cap, slightly wider than the pipe, used to cover this end of the collector. Filter papers loaded with the solid particles were acid-digested using a modified domestic microwave oven to bring the solid material into solution. The resulting solutions were analyzed for Pt by graphite furnace atomic absorption spectrometry (GF-AAS) and for Pd and Rh by inductively coupled plasma (ICP-OES). Results indicate that concentration of these analytes in the particulate is higher for new vehicles, having new catalytic converters, than for old ones. Maximum Pd, Pt and Rh in the samples analyzed were found to be 5.36, 12.60 and 1.03 microg g(-1), respectively.

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

PubMed

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

2016-06-05

St. John's wort (SJW) (Hypericum perforatum) is a herbal remedy commonly used to treat mild depression. The elemental profiles of 54 samples (i.e., dry herbs, tablets and capsules) were evaluated by monitoring 25 elements using Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). The major elemental constituents in the SJW samples were Ca (300-199,000μg/g), Mg (410-3,530μg/g), Al (4.4-900μg/g), Fe (1.154-760μg/g), Mn (2.4-261μg/g), Sr (0.88-83.6μg/g), and Zn (7-64μg/g). For the sixteen elements that could be reliably quantified, principal component analysis (PCA) was used to investigate underlying patterns in the data. PCA models identified 7 key elements (i.e., Ba, Ca, Cd, Mg, Mo, Ni and Y), which described 85% of the variance in the dataset in the first three principal components. The PCA approach resulted in a general delineation between the three different formulations and provides a basis for monitoring product quality in this manner. Copyright © 2016 Elsevier B.V. All rights reserved.

Investigation on mechanical behavior and material characteristics of various weight composition of SiCp reinforced aluminium metal matrix composite

NASA Astrophysics Data System (ADS)

Pichumani, Sivachidambaram; Srinivasan, Raghuraman; Ramamoorthi, Venkatraman

2018-02-01

Aluminium - silicon carbide (Al - SiC) metal matrix composite is produced with following wt % of SiC reinforcement (4%, 8% & 12%) using stir casting method. Mechanical testing such as micro hardness, tensile testing and bend testing were performed. Characterizations, namely micro structure, X-ray diffraction (XRD) analysis, inductive coupled plasma - optical emission spectroscopy (ICP-OES) and scanning electron microscopy (SEM) analysis, were carried out on Al - SiC composites. The presence of SiC on Al - SiC composite is confirmed through XRD technique and microstructure. The percentage of SiC was confirmed through ICP-OES technique. Increase in weight percentage of SiC tends to increase micro hardness, ultimate strength & yield strength but it reduces the bend strength and elongation (%) of the material. SEM factrography of tensile tested fractured samples of Al - 8% SiC & Al - 12% SiC showed fine dimples on fractured surface & coarse dimples fractured surface respectively. This showed significant fracture differences between Al - 8% SiC & Al - 12% SiC. From the above experiment, Al - 8% SiC had good micro hardness, ultimate strength & yield strength without significant loss in elongation (%) & bend strength.

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

PubMed

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

2013-06-01

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

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

PubMed

Welna, Maja; Szymczycha-Madeja, Anna

2014-04-01

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

On-line preconcentration/determination of lead in Ilex paraguariensis samples (mate tea) using polyurethane foam as filter and USN-ICP-OES.

PubMed

Marchisio, P F; Sales, A; Cerutti, S; Marchevski, E; Martinez, L D

2005-09-30

The present paper proposes an on-line preconcentration procedure for lead determination in Ilex paraguariensis (St. Hilaire) samples by ultrasonic nebulization associated to inductively coupled plasma optical emission spectrometry (USN-ICP-OES). It is based on the precipitation of lead(II) ion on a minicolumn packed with polyurethane foam using 2-(5-bromo-2-pyridilazo)-5-diethylaminophenol (5-Br-PADAP) as precipitating reagent. The collected analyte precipitate was quantitatively eluted from the minicolumn with 20% (v/v) nitric acid. An enhancement factor of 225-fold was obtained (15 for USN and 15 for preconcentration). The detection limit (DL) value for the preconcentration of 10.0 ml of sample was 40.0 ng/l. The relative standard deviation (R.S.D.) was 3.0% for a Pb concentration of 1 microg/l, calculated from the peak heights obtained. The calibration graph using the preconcentration system for lead was linear with a correlation coefficient of 0.9997, at levels near the detection limits up to at least 100 microg/l. The preconcentration procedure was successfully applied to the determination of lead in mate tea samples.

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

PubMed Central

Baytak, Sıtkı; Arslan, Zikri

2015-01-01

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

Comparison of analytical performances of inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry for trace analysis of bismuth and bismuth oxide

NASA Astrophysics Data System (ADS)

Medvedev, Nickolay S.; Shaverina, Anastasiya V.; Tsygankova, Alphiya R.; Saprykin, Anatoly I.

2018-04-01

The paper presents а comparison of analytical performances of inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) for trace analysis of high purity bismuth and bismuth oxide. Matrix effects in the ICP-MS and ICP-AES methods were studied as a function of Bi concentration, ICP power and nebulizer flow rate. For ICP-MS the strong dependence of the matrix effects versus the atomic mass of analytes was observed. For ICP-AES the minimal matrix effects were achieved for spectral lines of analytes with low excitation potentials. The optimum degree of sample dilution providing minimum values of the limits of detection (LODs) was chosen. Both methods let us to reach LODs from n·10-7 to n·10-4 wt% for more than 50 trace elements. For most elements the LODs of ICP-MS were lower in comparison to ICP-AES. Validation of accuracy of the developed techniques was performed by "added-found" experiments and by comparison of the results of ICP-MS and ICP-AES analysis of high-purity bismuth oxide.

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

NASA Astrophysics Data System (ADS)

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

2009-06-01

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

The Effect of Mustard Gas on Salivary Trace Metals (Zn, Mn, Cu, Mg, Mo, Sr, Cd, Ca, Pb, Rb)

PubMed Central

Zamani Pozveh, Elham; Seif, Ahmad; Ghalayani, Parichehr; Maleki, Abbas; Mottaghi, Ahmad

2015-01-01

We have determined and compared trace metals concentration in saliva taken from chemical warfare injures who were under the exposure of mustard gas and healthy subjects by means of inductively coupled plasma optical emission spectroscopy (ICP-OES) for the first time. The influence of preliminary operations on the accuracy of ICP-OES analysis, blood contamination, the number of restored teeth in the mouth, salivary flow rate, and daily variations in trace metals concentration in saliva were also considered. Unstimulated saliva was collected at 10:00–11:00 a.m. from 45 subjects in three equal groups. The first group was composed of 15 healthy subjects (group 1); the second group consisted of 15 subjects who, upon chemical warfare injuries, did not use Salbutamol spray, which they would have normally used on a regular basis (group 2); and the third group contained the same number of patients as the second group, but they had taken their regular medicine (Salbutamol spray; group 3). Our results showed that the concentration of Cu in saliva was significantly increased in the chemical warfare injures compared to healthy subjects, as follows: healthy subjects 15.3± 5.45(p.p.b.), patients (group 2) 45.77±13.65, and patients (Salbutamol spray; group 3) 29 ±8.51 (P <0.02). In contrast, zinc was significantly decreased in the patients, as follows: healthy subjects 37 ± 9.03(p.p.b.), patients (group 2) 12.2 ± 3.56, and patients (Salbutamol spray; group 3) 20.6 ±10.01 (P < 0.01). It is important to note that direct dilution of saliva samples with ultrapure nitric acid showed the optimum ICP-OES outputs. PMID:25965704

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

PubMed

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.

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.

PubMed

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.

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

PubMed

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

2015-11-01

A method for the simultaneous determination of Ni, V and S in petroleum coke by inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave-assisted ultraviolet digestion (MW-UV) in closed vessels was proposed. Digestion was performed using electrodeless discharge lamps positioned inside quartz vessels and turned on by microwave radiation. The following parameters were evaluated: HNO3 concentration (15 mL of 1, 4, 7, 10 or 14.4 mol L(-1)), volume of H2O2 (30%, 1 or 3 mL), sample mass (100, 250 or 500 mg) and heating time (40 or 60 min) with or without the use of UV lamps. Digestion efficiency was evaluated by the determination of the residual carbon content (RCC) in digests. Using UV lamps lower RCC was obtained and the combination of 4 mol L(-1) HNO3 with 3 mL of H2O2 and 60 min of heating allowed a suitable digestion of up to 500 mg of petroleum coke (RCC< 21%). The agreement with the reference values for Ni, V and S (obtained by digestion of petroleum coke by microwave-induced combustion) and with a certified reference material of petroleum coke was between 96 and 101%. The proposed method was considered as advantageous when compared to American Society for Testing and Materials method because it allowed the simultaneous determination of Ni, V and S with lower limit of detection (0.22, 0.12 and 8.7 µg g(-1) for Ni, V and S, respectively) avoiding the use of concentrated nitric acid and providing digests suitable for routine analysis by ICP-OES. Copyright © 2015 Elsevier B.V. All rights reserved.

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

NASA Technical Reports Server (NTRS)

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

2006-01-01

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

Road Environments: Impact of Metals on Human Health in Heavily Congested Cities of Poland

PubMed Central

Adamiec, Ewa

2017-01-01

Road dust as a by-product of exhaust and non-exhaust emissions can be a major cause of systemic oxidative stress and multiple disorders. Substantial amounts of road dust are repeatedly resuspended, in particular at traffic lights and junctions where more braking is involved, causing potential threat to pedestrians, especially children. In order to determine the degree of contamination in the heavily traffic-congested cities of Poland, a total of 148 samples of road dust (RD), sludge from storm drains (SL) and roadside soil (RS) were collected. Sixteen metals were analysed using inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectroscopy (ICP-OES) and atomic absorption spectroscopy (AAS) in all samples. Chemical evaluation followed by Principal Component Analysis (PCA) revealed that road environments have been severely contaminated with traffic-related elements. Concentration of copper in all road-environment samples is even higher, exceeding even up to 15 times its average concentrations established for the surrounding soils. Non-carcinogenic health risk assessment revealed that the hazard index (HI) for children in all road-environment samples exceeds the safe level of 1. Therefore, greater attention should be paid to potential health risks caused by the ingestion of traffic-related particles during outdoor activities. PMID:28661464

Road Environments: Impact of Metals on Human Health in Heavily Congested Cities of Poland.

PubMed

Adamiec, Ewa

2017-06-29

Road dust as a by-product of exhaust and non-exhaust emissions can be a major cause of systemic oxidative stress and multiple disorders. Substantial amounts of road dust are repeatedly resuspended, in particular at traffic lights and junctions where more braking is involved, causing potential threat to pedestrians, especially children. In order to determine the degree of contamination in the heavily traffic-congested cities of Poland, a total of 148 samples of road dust (RD), sludge from storm drains (SL) and roadside soil (RS) were collected. Sixteen metals were analysed using inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectroscopy (ICP-OES) and atomic absorption spectroscopy (AAS) in all samples. Chemical evaluation followed by Principal Component Analysis (PCA) revealed that road environments have been severely contaminated with traffic-related elements. Concentration of copper in all road-environment samples is even higher, exceeding even up to 15 times its average concentrations established for the surrounding soils. Non-carcinogenic health risk assessment revealed that the hazard index (HI) for children in all road-environment samples exceeds the safe level of 1. Therefore, greater attention should be paid to potential health risks caused by the ingestion of traffic-related particles during outdoor activities.

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

PubMed

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

2011-09-01

The first study on the high efficiency of triocarbohydrazide modified attapulgite as solid-phase extractant for preconcentration of trace Au(III) prior to the measurement by inductively coupled plasma optical emission spectrometry (ICP-OES) has been reported. Experimental conditions for effective adsorption of trace levels of Au(III) were optimized with respect to different experimental parameters using batch and column procedures in detail. At pH 3, Au(III) could be quantitatively adsorbed on the new sorbent, and the adsorbed Au(III) could be completely eluted from the sorbent surface by 2.0mL 1.0molL(-1) of HCl+2% CS(NH(2))(2) solution. An enrichment factor of 150 was accomplished. Moreover, common interfering ions did not interfere in both separation and determination. The maximum adsorption capacity of the sorbent for Au(III) was found to be 66.7mgg(-1). The detection limit (3σ) of this method was 0.32μgL(-1) and the relative standard deviation (RSD) was 3.3% (n=8). The method, with high selectivity, sensitivity and reproducibility, was validated using certified reference materials, and had been applied for the determination of trace Au(III) with satisfactory results. Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

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

2014-01-01

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

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

PubMed Central

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

2014-01-01

The biomass of Vaucheria sessilis forms algal mats in many freshwaters. There is a need to find the method of algal biomass utilization. Vaucheria sessilis is a rich source of micro- and macronutrients and can be used as a soil amendment. In the paper, the elemental composition of enriched, via bioaccumulation process, macroalga was investigated. For this purpose, two independent techniques were used: scanning electron microscopy with an energy dispersive X-ray analytical system (SEMEDX) and inductively coupled plasma optical emission spectroscopy (ICP-OES). The biomass was exposed to two microelemental solutions, with Cu(II) and Zn(II) ions. After two weeks of the experiment, macroalga accumulated 98.5 mg of Zn(II) ions in 1 g of dry biomass and 68.9 mg g−1 of Cu(II) ions. Micrographs performed by SEM proved that bioaccumulation occurred. Metal ions were bound on the surface and in the interior of cells. Mappings of all cations showed that in the case of the surface of biomass (biosorption), the elements constituted aggregations and in the case of the cross section (bioaccumulation) they were evenly distributed. The algal biomass with permanently bound microelements can find an application in many branches of the industry (feed, natural fertilizers, etc.). PMID:25180212

Report of the CCQM-K124: trace elements and chromium speciation in drinking water—part A: trace elements in drinking water, part B: chromium speciation in drinking water

NASA Astrophysics Data System (ADS)

Kuroiwa, T.; Fung, W. H.; Zhu, Y.; Inagaki, K.; Sin, D. W. M.; Chu, H. S.; Saxby, D.; Merrick, J.; White, I.; Araujo, T.; Almeida, M. D.; Rodrigues, J.; Yang, L.; Pihillagawa, I. G.; Mester, Z.; Riquelme, S. S.; Pérez, L.; Barriga, R.; Núñez, C.; Chao, J.; Wang, J.; Wang, Q.; Shi, N.; Lu, H.; Song, P.; Nüykki, T.; Aho, T. Sara; Labarraque, G.; Oster, C.; Rienitz, O.; Jührling, R.; Pape, C.; Lampi, E.; Kakoulides, E.; Ketrin, R.; Mardika, E.; Komalasari, I.; Okumu, T. O.; Kang'iri, J. N.; Yim, Y. H.; Heo, S. W.; Lee, K. S.; Suh, J. K.; Lim, Y.; Manzano, J. V. L.; Uribe, C.; Carrasco, E.; Tayag, E. D.; Dablio, A. R. C.; Encarnacion, E. K. P.; Damian, R. L.; Konopelko, L.; Krylov, A.; Vadim, S.; Shin, R.; Peng, S. L.; Juan, W.; Chang, X.; Dewi, F.; Horvat, M.; Zuliani, T.; Taebunpakul, S.; Yafa, C.; Kaewkhomdee, N.; Thiengmanee, U.; Klich, H.; Can, S. Z.; Ari, B.; Cankur, O.; Goenaga Infante, H.; Ferreira, E.; Pérez, R.; E Long, S.; Kassim, B. L.; E Murphy, K.; Molloy, J. L.; Butler, T. A.

2017-01-01

CCQM-K124 was organized by the Inorganic Analysis Working Group (IAWG) of CCQM to assess and document the capabilities of the national metrology institutes (NMIs) or the designated institutes (DIs) to measure the mass fractions of trace elements (As, B, Cd, Ca, Cr, Hg and Mo) and hexavalent chromium (Cr(VI)) in drinking water. The National Metrology Institute of Japan (NMIJ) and the Government Laboratory, Hong Kong SAR (GLHK) acted as the coordinating laboratories. This comparison is divided into two parts. Part A was organized by the NMIJ and the trace elements were the analytes, and Part B was organised by the GLHK and Cr(VI) was the analyte. In Part A, results were submitted by 14 NMIs and nine DIs. The participants used different measurement methods, though most of them used direct measurement using inductively coupled plasma-optical emission spectrometry (ICP-OES), inductively coupled plasma-mass spectrometry (ICP-MS), and isotope dilution technique with ICP-MS. The results of As, B, Cd, Ca and Cr show good agreement with the exception of some outliers. Concerning Hg, instability was observed when the sample was stored in the light. And some participants observed instability of Mo. Therefore, it was agreed to abandon the Hg and Mo analysis as this sample was not satisfactory for KC. In Part B, results were submitted by six NMIs and one DI. The methods applied were direct measurement using 1,5-diphenylcarbazide (DPC) derivatisation UV-visible spectrophotometry, standard addition using ion chromatography-UV-visible spectrophotometry or HPLC—inductively coupled plasma-mass spectrometry (ICP-MS) and isotope dilution technique with ion chromatography—ICP-MS. The results of all participants show good agreement. Accounting for relative expanded uncertainty, comparability of measurement results for each of As, B, Cd, Ca, Cr and Cr(VI) was successfully demonstrated by the participating NMIs or DIs. Main text To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

Technological study of ancient ceramics produced in Casteldurante (central Italy) during the Renaissance

NASA Astrophysics Data System (ADS)

Padeletti, G.; Fermo, P.; Gilardoni, S.; Galli, A.

In order to recover the ancient tradition concerning the materials used for the decoration, majolica shards produced during the Renaissance period in Casteldurante, a famous centre for ceramic production in Italy (Marche), have been examined. In the present study, pigments used for the decorations have been investigated by means of inductively coupled plasma optical emission spectrometry (ICP-OES), scanning electron microscopy/energy-dispersive X-ray spectroscopy (SEM-EDX) and diffuse-reflectance UV-Vis spectroscopy. Ochre, lead antimonate yellow, copper-based pigment and smalt have been used as colourants to obtain respectively yellow-orange, yellow, green and blue decorations in accordance with what is reported by the ancient recipes.

Metal concentrations of wild edible mushrooms from Turkey.

PubMed

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

2012-01-01

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

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

NASA Astrophysics Data System (ADS)

Salas, Antonio; Ramírez, Estele

2009-01-01

After the successful completion of the pilot study, CCQM-P65 [1], the Inorganic Analysis Working Group of CCQM agreed to conduct key comparison CCQM-K57, Chemical composition of clay, in Paris, April 2006. The natural mass fraction levels of five elements—Si, Ca, Fe, Al and Mg—were measured and reported as oxides in clay. Six national metrology institutes participated in CCQM K57, and CENAM (Querétaro, Mexico) coordinated. The methods employed were isotope dilution mass spectrometry (IDMS), inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-optical emission spectrometry (ICP-OES) using the dehydration method and condensation method, gravimetric analysis, neutron activation analysis (NAA), prompt gamma activation analysis (PGAA) and x-ray fluorescence spectrometry (XRF) with the reconstitution method and external calibration. This final report presents the capability of the participant institutes, based on the KCRV, which was approved at the IAWG spring meeting in 2008, and the equivalence statements regarding the KCRV, approved at its autumn meeting. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (MRA).

Lithium loss in the solid electrolyte interphase: Lithium quantification of aged lithium ion battery graphite electrodes by means of laser ablation inductively coupled plasma mass spectrometry and inductively coupled plasma optical emission spectroscopy

NASA Astrophysics Data System (ADS)

Schwieters, Timo; Evertz, Marco; Mense, Maximilian; Winter, Martin; Nowak, Sascha

2017-07-01

In this work we present a new method using LA-ICP-MS to quantitatively determine the lithium content in aged graphite electrodes of a lithium ion battery (LIB) by performing total depth profiling. Matrix matched solid external standards are prepared using a solid doping approach to avoid elemental fractionation effects during the measurement. The results are compared and matched to the established ICP-OES technique for bulk quantification after performing a microwave assisted acid digestion. The method is applied to aged graphite electrodes in order to determine the lithium immobilization (= "Li loss") in the solid electrolyte interphase after the first cycle of formation. For this, different samples including a reference sample are created to obtain varying thicknesses of the SEI covering the electrode particles. By applying defined charging voltages, an initial lithiation process is performed to obtain specific graphite intercalation compounds (GICs, with target stoichiometries of LiC30, LiC18, LiC12 and LiC6). Afterwards, the graphite electrode is completely discharged to obtain samples without mobile, thus active lithium in its lattice. Taking the amount of lithium into account which originates from the residues of the LiPF6 (dissolved in the carbon components containing electrolyte), it is possible to subtract the amount of lithium in the SEI.

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

NASA Astrophysics Data System (ADS)

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

2009-06-01

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

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

PubMed

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

2017-05-01

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

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

PubMed

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

2014-05-01

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

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

PubMed Central

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

2014-01-01

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

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

PubMed

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

2012-09-15

This article reports a method that is used for the preconcentration and determination of Cd(2+) and Co(2+) in vegetables, using Pleurotus eryngii immobilized Amberlite XAD-16 as a solid-phase biosorbent. The concentrations of metals were determined by inductively coupled plasma-optical spectrometry (ICP-OES). Critical parameters, such as the pH of the solution, flow rate, the amount of biosorbent, type and volume of eluent, and the sample volume, that affect the solid-phase extraction (SPE) procedure were optimized. The optimum extraction conditions were determined as being a pH of 6.0 for Cd(2+) and of 5.0 for Co(2+); a sample flow rate of 2.0 mL min(-1); 200.0mg of biosorbent; and 5.0 mL of 1.0 mol L(-1) HCl as eluent. The capacities of the biosorbent for metal uptake were found to be 11.3 and 9.8 mg g(-1) for Cd(2+) and Co(2+) ions, respectively. Limit of quantitations (LOQs) were found to be 0.67 and 0.82 ng mL(-1), respectively, for Cd(2+) and Co(2+). The linear working curves were observed to be in the linear range from 1.0 to 50.0 ng mL(-1), and possessed high correlation coefficients. The use of the SPE method showed 50.7- and 35.7-fold improvements in the sensitivities of ICP-OES. The developed method was successfully applied to NCS ZC-73014 (a certified reference tea sample). Relative standard deviations (RSD) were lower than 5.0%. The Cd(2+) and Co(2+) concentrations in the different parts (leave, root, stem, and fruit) of purslane, onion, rocket, okra, and aubergine were determined after microwave digestion and solid-phase extraction by P. eryngii immobilized on Amberlite XAD-16. Copyright © 2012 Elsevier B.V. All rights reserved.

Multivariate optimization of a procedure employing microwave-assisted digestion for the determination of nickel and vanadium in crude oil by ICP OES.

PubMed

Dos Anjos, Shirlei L; Alves, Jeferson C; Rocha Soares, Sarah A; Araujo, Rennan G O; de Oliveira, Olivia M C; Queiroz, Antonio F S; Ferreira, Sergio L C

2018-02-01

This work presents the optimization of a sample preparation procedure using microwave-assisted digestion for the determination of nickel and vanadium in crude oil employing inductively coupled plasma optical emission spectrometry (ICP OES). The optimization step was performed utilizing a two-level full factorial design involving the following factors: concentrated nitric acid and hydrogen peroxide volumes, and microwave-assisted digestion temperature. Nickel and vanadium concentrations were used as responses. Additionally, a multiple response based on the normalization of the concentrations by the highest values was built to establish a compromise condition between the two analytes. A Doehlert matrix optimized the instrumental conditions of the ICP OE spectrometer. In this design, the plasma robustness was used as chemometric response. The experiments were performed using a digested oil sample solution doped with magnesium(II) ions, as well as a standard magnesium solution. The optimized method allows for the determination of nickel and vanadium with quantification limits of 0.79 and 0.20μgg -1 , respectively, for a digested sample mass of 0.1g. The precision (expressed as relative standard deviations) was determined using five replicates of two oil samples and the results obtained were 1.63% and 3.67% for nickel and 0.42% and 4.64% for vanadium. Bismuth and yttrium were also tested as internal standards, and the results demonstrate that yttrium allows for a better precision for the method. The accuracy was confirmed by the analysis of the certified reference material trace element in fuel oil (CRM NIST 1634c). The proposed method was applied for the determination of nickel and vanadium in five crude oil samples from Brazilian Basins. The metal concentrations found varied from 7.30 to 33.21μgg -1 for nickel and from 0.63 to 19.42μgg -1 for vanadium. Copyright © 2017. Published by Elsevier B.V.

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

PubMed

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

2005-05-01

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

Final Report on Jobin Yvon Contained Inductively Coupled Plasma Emission Spectrometer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pennebaker, F.M.

2003-03-17

A new Inductively Coupled Plasma -- Emission Spectrometer (ICP-ES) was recently purchased and installed in Lab B-147/151 at SRTC. The contained JY Model Ultima 170-C ICP-ES has been tested and compared to current ADS ICP-ES instrumentation. The testing has included both performance tests to evaluate instrumental ability, and the measurement of matrix standards commonly analyzed by ICP-ES at Savannah River. In developing operating procedures for this instrument, we have implemented the use of internal standards and off-peak background subtraction. Both of these techniques are recommended by EPA SW-846 ICP-ES methods and are common to current ICP-ES operations. Based on themore » testing and changes, the JY Model Ultima 170-C ICP-ES provides improved performance for elemental analysis of radioactive samples in the Analytical Development Section.« less

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

PubMed

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

2014-06-15

Inductively coupled plasma mass spectrometry and optical emission were used to determine the multi-element composition of 272 bottled Slovenian wines. To achieve geographical classification of the wines by their elemental composition, principal component analysis (PCA) and counter-propagation artificial neural networks (CPANN) have been used. From 49 elements measured, 19 were used to build the final classification models. CPANN was used for the final predictions because of its superior results. The best model gave 82% correct predictions for external set of the white wine samples. Taking into account the small size of whole Slovenian wine growing regions, we consider the classification results were very good. For the red wines, which were mostly represented from one region, even-sub region classification was possible with great precision. From the level maps of the CPANN model, some of the most important elements for classification were identified. Copyright © 2013 Elsevier Ltd. All rights reserved.

ARO - Terrestrial Research Program, Methodologies and Protocols for Characterization of Geomaterials

DTIC Science & Technology

2015-05-14

of ice involves melting, digestion, and analysis using inductively coupled plasma – mass spectrometry (ICPMS). ICP-MS analysis established elemental...4] have distinct chemical compositions. Knowledge of the chemical composition of the mineral assemblage present in a rock is critical to...activation analysis (INAA), to inductively-coupled plasma analysis and mass spectrometry (ICP & ICP-MS), mass spectrometry (MS), and laser-ablation

Behaviour of aluminium in forest soils with different lithology and herb vegetation cover.

PubMed

Hubová, Petra; Tejnecký, Václav; Češková, Michaela; Borůvka, Luboš; Němeček, Karel; Drábek, Ondřej

2018-04-01

The aim of this study was to determine the content, distribution and behaviour of Al in soils under beech forest with different parent rock, and to assess the role of herbaceous vegetation on soil Al behaviour. We hypothesize that the contents of elements in the soil sorption complex (Al etc.) are strongly influenced by vegetation cover. Also, low molecular mass organic acids (LMMOA) can be considered as an indicator of soil organic matter (SOM) decomposition and vegetation litter turnover. Speciation of LMMOA, nutrition content (PO 4 3- , Ca 2+ , K + ) and element composition in aqueous extracts were determined by means of ion chromatography and inductively coupled plasma - optical emission spectrometry (ICP-OES) respectively. Active and exchangeable pH, sorption characteristics and exchangeable Al (Al ex ) were determined in BaCl 2 extracts by ICP-OES. Elemental composition of parent rocks was assessed by means of X-ray fluorescence spectroscopy. Herb-poor localities showed lower pH, less nutrients (PO 4 3- , Ca 2+ , K + ), less LMMOA, a larger stock of SOM and greater cation exchange capacity. There was also lower mobilisation of Al in organic horizons, which explains the larger pools of Al. Generally, we can conclude that LMMOA, and thus soil vegetation cover, play an important role in the Al soil cycle. Copyright © 2017 Elsevier Inc. All rights reserved.

Uncertainty Estimation for the Determination of Ni, Pb and Al in Natural Water Samples by SPE-ICP-OES

NASA Astrophysics Data System (ADS)

Ghorbani, A.; Farahani, M. Mahmoodi; Rabbani, M.; Aflaki, F.; Waqifhosain, Syed

2008-01-01

In this paper we propose uncertainty estimation for the analytical results we obtained from determination of Ni, Pb and Al by solidphase extraction and inductively coupled plasma optical emission spectrometry (SPE-ICP-OES). The procedure is based on the retention of analytes in the form of 8-hydroxyquinoline (8-HQ) complexes on a mini column of XAD-4 resin and subsequent elution with nitric acid. The influence of various analytical parameters including the amount of solid phase, pH, elution factors (concentration and volume of eluting solution), volume of sample solution, and amount of ligand on the extraction efficiency of analytes was investigated. To estimate the uncertainty of analytical result obtained, we propose assessing trueness by employing spiked sample. Two types of bias are calculated in the assessment of trueness: a proportional bias and a constant bias. We applied Nested design for calculating proportional bias and Youden method to calculate the constant bias. The results we obtained for proportional bias are calculated from spiked samples. In this case, the concentration found is plotted against the concentration added and the slop of standard addition curve is an estimate of the method recovery. Estimated method of average recovery in Karaj river water is: (1.004±0.0085) for Ni, (0.999±0.010) for Pb and (0.987±0.008) for Al.

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

EPA Pesticide Factsheets

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

Identification and quantification of indoor air pollutant sources within a residential academic campus.

PubMed

Suryawanshi, Shalini; Chauhan, Amit Singh; Verma, Ritika; Gupta, Tarun

2016-11-01

There is a growing concern regarding the adverse health effects due to indoor air pollution in developing countries including India. Hence, it becomes important to study the causes and sources of indoor air pollutants. This study presents the indoor concentrations of PM0.6 (particles with aerodynamic diameter less than 0.6μm) and identifies sources leading to indoor air pollution. Indoor air samples were collected at IIT Kanpur campus. Ninety-eight PM0.6 samples were collected during November 2013 to September 2014. PM0.6 concentration was measured using a single stage impactor type PM0.6 sampler. The average PM0.6 concentration indoor was about 94.44μg/m(3). Samples collected were then analysed for metal concentrations using ICP-OES (Inductively Coupled Plasma - Optical Emission Spectrometer). Eight metals Ba, Ca, Cr, Cu, Fe, Mg, Ni and Pb were quantified from PM samples using ICP-OES. Positive Matrix Factorization (PMF) was used for source apportionment of indoor air pollution. PMF is a factor analysis tool which helps in resolving the profile and contribution of the sources from an unknown mixture. Five possible sources of indoor pollutants were identified by factor analysis - (1) Coal combustion (21.8%) (2) Tobacco smoking (9.8%) (3) Wall dust (25.7%) (4) Soil particles (17.5%) (5) Wooden furniture/paper products (25.2%). Copyright © 2016 Elsevier B.V. All rights reserved.

Analytical performance of benchtop total reflection X-ray fluorescence instrumentation for multielemental analysis of wine samples

NASA Astrophysics Data System (ADS)

Dalipi, Rogerta; Marguí, Eva; Borgese, Laura; Bilo, Fabjola; Depero, Laura E.

2016-06-01

Recent technological improvements have led to a widespread adoption of benchtop total reflection X-ray fluorescence systems (TXRF) for analysis of liquid samples. However, benchtop TXRF systems usually present limited sensitivity compared with high-scale instrumentation which can restrict its application in some fields. The aim of the present work was to evaluate and compare the analytical capabilities of two TXRF systems, equipped with low power Mo and W target X-ray tubes, for multielemental analysis of wine samples. Using the Mo-TXRF system, the detection limits for most elements were one order of magnitude lower than those attained using the W-TXRF system. For the detection of high Z elements like Cd and Ag, however, W-TXRF remains a very good option due to the possibility of K-Lines detection. Accuracy and precision of the obtained results have been evaluated analyzing spiked real wine samples and comparing the TXRF results with those obtained by inductively coupled plasma emission spectroscopy (ICP-OES). In general, good agreement was obtained between ICP-OES and TXRF results for the analysis of both red and white wine samples except for light elements (i.e., K) which TXRF concentrations were underestimated. However, a further achievement of analytical quality of TXRF results can be achieved if wine analysis is performed after dilution of the sample with de-ionized water.

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

PubMed

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

2016-07-01

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

Rapid Analysis of Ash Composition Using Laser-Induced Breakdown Spectroscopy (LIBS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

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 thesemore » 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.« less

Gas and liquid chromatography with inductively coupled plasma mass spectrometry detection for environmental speciation analysis — advances and limitations

NASA Astrophysics Data System (ADS)

Szpunar, Joanna; McSheehy, Shona; Połeć, Kasia; Vacchina, Véronique; Mounicou, Sandra; Rodriguez, Isaac; Łobiński, Ryszard

2000-07-01

Recent advances in the coupling of gas chromatography (GC) and high performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP MS) and their role in trace element speciation analysis of environmental materials are presented. The discussion is illustrated with three research examples concerning the following topics: (i) development and coupling of multicapillary microcolumn GC with ICP MS for speciation of organotin in sediment and biological tissue samples; (ii) speciation of arsenic in marine algae by size-exclusion-anion-exchange HPLC-ICP MS; and (iii) speciation of cadmium in plant cell cultures by size-exclusion HPLC-ICP MS. Particular attention is paid to the problem of signal identification in ICP MS chromatograms; the potential of electrospray MS/MS for this purpose is highlighted.

Quantification of elemental area densities in multiple metal layers (Au/Ni/Cu) on a Cr-coated quartz glass substrate for certification of NMIJ CRM 5208-a.

PubMed

Ariga, Tomoko; Zhu, Yanbei; Ito, Mika; Takatsuka, Toshiko; Terauchi, Shinya; Kurokawa, Akira; Inagaki, Kazumi

2018-04-01

Area densities of Au/Ni/Cu layers on a Cr-coated quartz substrate were characterized to certify a multiple-metal-layer certified reference material (NMIJ CRM5208-a) that is intended for use in the analysis of the layer area density and the thickness by an X-ray fluorescence spectrometer. The area densities of Au/Ni/Cu layers were calculated from layer mass amounts and area. The layer mass amounts were determined by using wet chemical analyses, namely inductively coupled plasma mass spectrometry (ICP-MS), isotope-dilution (ID-) ICP-MS, and inductively coupled plasma optical emission spectrometry (ICP-OES) after dissolving the layers with diluted mixture of HCl and HNO 3 (1:1, v/v). Analytical results of the layer mass amounts obtained by the methods agreed well with each another within their uncertainty ranges. The area of the layer was determined by using a high-resolution optical scanner calibrated by Japan Calibration Service System (JCSS) standard scales. The property values of area density were 1.84 ± 0.05 μg/mm 2 for Au, 8.69 ± 0.17 μg/mm 2 for Ni, and 8.80 ± 0.14 μg/mm 2 for Cu (mean ± expanded uncertainty, coverage factor k = 2). In order to assess the reliability of these values, the density of each metal layer calculated from the property values of the area density and layer thickness measured by using a scanning electron microscope were compared with available literature values and good agreement between the observed values and values obtained in previous studies.

PIXE as a complement to ICP-OES trace metal analysis in Sudanese medicinal plants.

PubMed

Mubark Ebrahim, Ammar; Etayeb, M A; Khalid, H; Noun, Manale; Roumie, M; Michalke, B

2014-08-01

This paper compares trace element concentrations (Ca, K, Sr, Fe, Mn, Zn, Ni, Cu, Co and Cr) in 27 Sudanese medical plants determined in parallel by PIXE and ICP-OES to get information on which technique is preferable at different matrices and element concentrations. PIXE correlates well to ICP-OES for Sr, Mn, Ca, K, Zn and Fe determinations. ICP-OES seems to be the superior technique over PIXE when measuring low concentrated elements (chromium, cobalt, nickel and copper) in the medicinal plants. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

USGS Publications Warehouse

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

2011-01-01

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

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

PubMed

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

2010-02-10

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

Removal of uranium from soil samples for ICP-OES analysis of RCRA metals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wero, M.; Lederer-Cano, A.; Billy, C.

1995-12-01

Soil samples containing high levels of uranium present unique analytical problems when analyzed for toxic metals (Ag, As, Ba, Cd, Cr, Cu, Ni, Pb, Se and Tl) because of the spectral interference of uranium in the ICP-OES emission spectrometer. Methods to remove uranium from the digestates of soil samples, known to be high in uranium, have been developed that reduce the initial uranium concentration (1-3%) to less than 500 ppm. UTEVA ion exchange columns, used as an ICP-OES analytical pre-treatment, reduces uranium to acceptable levels, permitting good analytical results of the RCRA metals by ICP-OES.

Dispersed particle extraction--a new procedure for trace element enrichment from natural aqueous samples with subsequent ICP-OES analysis.

PubMed

Bauer, Gerald; Neouze, Marie-Alexandra; Limbeck, Andreas

2013-01-15

A novel sample pre-treatment method for multi trace element enrichment from environmental waters prior to optical emission spectrometry analysis with inductively coupled plasma (ICP-OES) is proposed, based on dispersed particle extraction (DPE). This method is based on the use of silica nanoparticles functionalized with strong cation exchange ligands. After separation from the investigated sample solution, the nanoparticles used for the extraction are directly introduced in the ICP for measurement of the adsorbed target analytes. A prerequisite for the successful application of the developed slurry approach is the use of sorbent particles with a mean size of 500 nm instead of commercially available μm sized beads. The proposed method offers the known advantages of common bead-injection (BI) techniques, and further circumvents the elution step required in conventional solid phase extraction procedures. With the use of 14.4 mL sample and addition of ammonium acetate buffer and particle slurry limits of detection (LODs) from 0.03 μg L(-1) for Be to 0.48 μg L(-1) for Fe, with relative standard deviations ranging from 1.7% for Fe and 5.5% for Cr and an average enrichment factor of 10.4 could be achieved. By implementing this method the possibility to access sorbent materials with irreversible bonding mechanisms for sample pre-treatment is established, thus improvements in the selectivity of sample pre-treatment procedures can be achieved. The presented procedure was tested for accuracy with NIST standard reference material 1643e (fresh water) and was applied to drinking water samples from the vicinity of Vienna. Copyright © 2012 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-09-06

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

[Determination of Total Iron and Fe2+ in Basalt].

PubMed

Liu, Jian-xun; Chen, Mei-rong; Jian, Zheng-guo; Wu, Gang; Wu, Zhi-shen

2015-08-01

Basalt is the raw material of basalt fiber. The content of FeO and Fe2O3 has a great impact on the properties of basalt fibers. ICP-OES and dichromate method were used to test total Fe and Fe(2+) in basalt. Suitable instrument parameters and analysis lines of Fe were chosen for ICP-OES. The relative standard deviation (RSD) of ICP-OES is 2.2%, and the recovery is in the range of 98%~101%. The method shows simple, rapid and highly accurate for determination of total Fe and Fe(2+) in basalt. The RSD of ICP-OES and dichromate method is 0.42% and 1.4%, respectively.

Sulfur analysis by inductively coupled plasma-mass spectrometry: A review

NASA Astrophysics Data System (ADS)

Giner Martínez-Sierra, J.; Galilea San Blas, O.; Marchante Gayón, J. M.; García Alonso, J. I.

2015-06-01

In recent years the number of applications of sulfur (S) analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. In this article we describe in some depth the application of ICP-MS for S analysis with emphasis placed on the sulfur-specific detection by hyphenated techniques such as LC, GC, CE and LA coupled on-line to ICP-MS. The different approaches available for sulfur isotope ratio measurements by ICP-MS are also detailed. Particular attention has been paid to the quantification of peptides/proteins and the analysis of metallopeptides/metalloproteins via sulfur by LC-ICP-MS. Likewise, the speciation analysis of metal-based pharmaceuticals and metallodrugs and non-metal selective detection of pharmaceuticals via S are highlighted. Labeling procedures for metabolic applications are also included. Finally, the measurement of natural variations in S isotope composition with multicollector ICP-MS instruments is also covered in this review.

Boron determination in steels by Inductively-Coupled Plasma spectometry (ICP)

NASA Technical Reports Server (NTRS)

Coedo, A. G.; Lopez, M. T. D.

1986-01-01

The sample is treated with 5N H2SO4 followed by concentrated HNO3 and the diluted mixture is filtered. Soluble B is determined in the filtrate by Inductively-Coupled Plasma (ICP) spectrometry after addition HCl and extraction of Fe with ethyl-ether. The residue is fused with Na2CO3 and, after treatment with HCl, the insoluble B is determined by ICP spectrometry as before. The method permits determination of ppm amounts of B in steel.

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

NASA Astrophysics Data System (ADS)

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.

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

PubMed

Lech, Teresa

2013-05-01

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

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

PubMed

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).

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

PubMed

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.

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

PubMed

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

2013-01-30

We have prepared calcined CuO microsheets (MSs) by a wet-chemical process using reducing agents in alkaline medium and characterized by UV/vis., fourier transform infrared (FT-IR) spectroscopy, powder X-ray diffraction (XRD), and field-emission scanning electron microscopy (FESEM) etc. The detailed structural, compositional, and optical characterizations of the MSs were evaluated by XRD pattern, FT-IR, X-ray photoelectron spectroscopy (XPS), and UV-vis spectroscopy, respectively which confirmed that the obtained MSs are well-crystalline CuO and possessed good optical properties. The CuO MSs morphology was investigated by FESEM, which confirmed that the calcined nanomaterials were sheet-shaped and grown in large-quantity. Here, the efficiency of the CuO MS was applied for a selective adsorption of gold(III) ion prior to its detection by inductively coupled plasma-optical emission spectrometry (ICP-OES). The selectivity of CuO MSs towards various metal ions, including Au(III), Cd(II), Co(II), Cr(III), Fe(III), Pd(II), and Zn(II) was analyzed. Based on the adsorption isotherm study, it was confirmed that the selectivity of MSs phase was mostly towards Au(III) ion. The static adsorption capacity for Au(III) was calculated to be 57.0 mg g(-1). From Langmuir adsorption isotherm, it was confirmed that the adsorption process was mainly monolayer-adsorption onto a surface containing a finite number of adsorption sites. Copyright © 2012 Elsevier B.V. All rights reserved.

Factorial design optimization of experimental variables in the on-line separation/preconcentration of copper in water samples using solid phase extraction and ICP-OES determination.

PubMed

Escudero, Luis A; Cerutti, S; Olsina, R A; Salonia, J A; Gasquez, J A

2010-11-15

An on-line preconcentration procedure using solid phase extraction (SPE) for the determination of copper in different water samples by inductively coupled plasma optical emission spectrometry (ICP-OES) is proposed. The copper was retained on a minicolumn filled with ethyl vinyl acetate (EVA) at pH 8.0 without using any complexing reagent. The experimental optimization step was performed using a two-level full factorial design. The results showed that pH, sample loading flow rate, and their interaction (at the tested levels) were statistically significant. In order to determine the best conditions for preconcentration and determination of copper, a final optimization of the significant factors was carried out using a central composite design (CCD). The calibration graph was linear with a regression coefficient of 0.995 at levels near the detection limit up to at least 300 μg L(-1). An enrichment factor (EF) of 54 with a preconcentration time of 187.5 s was obtained. The limit of detection (3σ) was 0.26 μg L(-1). The sampling frequency for the developed methodology was about 15 samples/h. The relative standard deviation (RSD) for six replicates containing 50 μg L(-1) of copper was 3.76%. The methodology was successfully applied to the determination of Cu in tap, mineral, river water samples, and in a certified VKI standard reference material. Copyright © 2010 Elsevier B.V. All rights reserved.

Nucleotides, micro- and macro-nutrients, limonoids, flavonoids, and hydroxycinnamates composition in the phloem sap of sweet orange

PubMed Central

Hijaz, Faraj; Manthey, John A.; Van der Merwe, Deon; Killiny, Nabil

2016-01-01

ABSTRACT Currently, the global citrus production is declining due to the spread of Huanglongbing (HLB). HLB, otherwise known as citrus greening, is caused by Candidatus Liberibacter asiaticus (CLas) and is transmitted by the Asian citrus psyllids (ACP), Diaphorina citri Kuwayama. ACP transmits CLas bacterium while feeding on the citrus phloem sap. Multiplication of CLas in the phloem of citrus indicates that the sap contains all the essential nutrients needed for CLas. In this study, we investigated the micro- and macro-nutrients, nucleotides, and others secondary metabolites of phloem sap from pineapple sweet orange. The micro- and macro-nutrients were analyzed using inductively coupled plasma-mass spectroscopy (ICP-MS) and inductively coupled plasma-optical emission spectroscopy (ICP-OES). Nucleotides and other secondary metabolites analysis was accomplished by reversed phase HPLC coupled with UV, fluorescence detection, or negative mode electrospray ionization mass spectrometry (ESI-MS). Calcium (89 mM) was the highest element followed by potassium (38.8 mM) and phosphorous (24 mM). Magnesium and sulfur were also abundant and their concentrations were 15 and 9 mM, respectively. The rest of the elements were found in low amounts (< 2mM). The concentrations of ATP, ADP, and AMP were 16, 31, and 3 µ mole/Kg fwt, respectively. GTP, GMP. NAD, FMN, FAD, and riboflavin were found at concentrations below (3 µ mole/Kg fwt). The phloem was rich in nomilin 124 mM and limonin 176 µ mole/Kg fwt. Hesperidin, vicenin-2, sinensetin, and nobiletin were the most predominant flavonoids. In addition, several hydroxycinnamates were detected. The results of this study will increase our knowledge about the nature and the chemical composition of citrus phloem sap. PMID:27171979

Nucleotides, micro- and macro-nutrients, limonoids, flavonoids, and hydroxycinnamates composition in the phloem sap of sweet orange.

PubMed

Hijaz, Faraj; Manthey, John A; Van der Merwe, Deon; Killiny, Nabil

2016-06-02

Currently, the global citrus production is declining due to the spread of Huanglongbing (HLB). HLB, otherwise known as citrus greening, is caused by Candidatus Liberibacter asiaticus (CLas) and is transmitted by the Asian citrus psyllids (ACP), Diaphorina citri Kuwayama. ACP transmits CLas bacterium while feeding on the citrus phloem sap. Multiplication of CLas in the phloem of citrus indicates that the sap contains all the essential nutrients needed for CLas. In this study, we investigated the micro- and macro-nutrients, nucleotides, and others secondary metabolites of phloem sap from pineapple sweet orange. The micro- and macro-nutrients were analyzed using inductively coupled plasma-mass spectroscopy (ICP-MS) and inductively coupled plasma-optical emission spectroscopy (ICP-OES). Nucleotides and other secondary metabolites analysis was accomplished by reversed phase HPLC coupled with UV, fluorescence detection, or negative mode electrospray ionization mass spectrometry (ESI-MS). Calcium (89 mM) was the highest element followed by potassium (38.8 mM) and phosphorous (24 mM). Magnesium and sulfur were also abundant and their concentrations were 15 and 9 mM, respectively. The rest of the elements were found in low amounts (< 2mM). The concentrations of ATP, ADP, and AMP were 16, 31, and 3 µ mole/Kg fwt, respectively. GTP, GMP. NAD, FMN, FAD, and riboflavin were found at concentrations below (3 µ mole/Kg fwt). The phloem was rich in nomilin 124 mM and limonin 176 µ mole/Kg fwt. Hesperidin, vicenin-2, sinensetin, and nobiletin were the most predominant flavonoids. In addition, several hydroxycinnamates were detected. The results of this study will increase our knowledge about the nature and the chemical composition of citrus phloem sap.

Non-Aqueous Sol-Gel Synthesis of FePt Nanoparticles in the Absence of In Situ Stabilizers

PubMed Central

Preller, Tobias; Knickmeier, Saskia; Porsiel, Julian Cedric; Temel, Bilal

2018-01-01

The synthesis of FePt nanocrystals is typically performed in an organic solvent at rather high temperatures, demanding the addition of the in situ stabilizers oleic acid and oleylamine to produce monomodal particles with well-defined morphologies. Replacing frequently-used solvents with organic media bearing functional moieties, the use of the stabilizers can be completely circumvented. In addition, various morphologies and sizes of the nanocrystals can be achieved by the choice of organic solvent. The kinetics of particle growth and the change in the magnetic behavior of the superparamagnetic FePt nanocrystals during the synthesis with a set of different solvents, as well as the resulting morphologies and stoichiometries of the nanoparticles were determined by powder X-ray diffraction (PXRD), small-angle X-ray scattering (SAXS), transmission electron microscopy (TEM), inductively coupled plasma optical emission spectroscopy (ICP-OES)/mass spectrometry (ICP-MS), and superconducting quantum interference device (SQUID) measurements. Furthermore, annealing of the as-prepared FePt nanoparticles led to the ordered L10 phase and, thus, to hard magnetic materials with varying saturation magnetizations and magnetic coercivities. PMID:29751508

Flow-through dynamic microextraction system for automatic in vitro assessment of chyme bioaccessibility in food commodities.

PubMed

Souza, Lais A; Rosende, María; Korn, Maria Graças A; Miró, Manuel

2018-10-05

An automatic flow-through dynamic extraction method is proposed for the first time for in vitro exploration, with high temporal resolution, of the transit of the chyme from the gastric to the duodenal compartment using the Versantvoort's fed-state physiologically relevant extraction test. The flow manifold was coupled on-line to an inductively coupled plasma optical emission spectrometer (ICP OES) for real-time elucidation of the bioaccessible elemental fraction of micronutrients (viz., Cu, Fe and Mn) in food commodities across the gastrointestinal tract. The simulated intestinal and bile biofluid (added to the gastric phase) was successively pumped at 1.0 mL min -1 through a large-bore column (maintained at 37.0 ± 2.0 °C) initially loaded with a weighed amount of linseed (250 mg) using a PVDF filter membrane (5.0 μm pore size) for retaining of the solid sample and in-line filtration of the extracts. The lack of bias (trueness) of the on-line gastrointestinal extraction method coupled to ICP OES was confirmed using mass balance validation following microwave assisted digestion of the residual (non-bioaccessible) elemental fraction. Mass balance validation yielded absolute recoveries spanning from 79 to 121% for the overall analytes and samples. On-line dynamic extraction was critically appraised against batch counterparts for both gastric and gastrointestinal compartments. Due to the lack of consensus in the literature regarding the agitation method for batch oral bioaccessibility testing, several extraction approaches (viz., magnetic stirring, end-over-end rotation and orbital shaking) were evaluated. Improved gastric extractability of Fe along with bioaccessible data comparable to the dynamic counterpart based on the continuous displacement of the extraction equilibrium was obtained with batchwise magnetic stirring, which is deemed most appropriate for ascertaining worst-case/maximum bioaccessibility scenarios. Copyright © 2018 Elsevier B.V. All rights reserved.

A critical review of inductively coupled plasma-mass spectrometry for geoanalysis, geochemistry and hydrology, Part 1. Analytical performance

USGS Publications Warehouse

Brenner, I.B.; Taylor, Howard E.

1992-01-01

Present-day inductively coupled plasma-mass spectrometry (ICP-MS) instrumentation is described briefly. Emphasis is placed on performance characteristics for geoanalysis, geochemistry, and hydrology. Applications where ICP-MS would be indispensable are indicated. Determination of geochemically diagnostic trace elements (such as the rare earth elements [REE], U and Th), of isotope ratios for fingerprinting, tracer and other geo-isotope applications, and benchmark isotope dilution determinations are considered to be typical priority applications for ICP-MS. It is concluded that ICP-MS furnishes unique geoanalytical and environmental data that are not readily provided by conventional spectroscopic (emission and absorption) techniques.

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

PubMed

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

2012-01-15

A fast and simple method for analysis of trace amounts of Cr(III), Cu(II), Pb(II) and Zn(II) in environmental and biological samples was developed by combining magnetic solid phase extraction (MSPE) with inductively coupled plasma-optical emission spectrometry (ICP-OES) detection. Dithizone modified silica-coated magnetic Fe(3)O(4) nanoparticles (H(2)Dz-SCMNPs) were prepared and used for MSPE of trace amounts of Cr(III), Cu(II), Pb(II) and Zn(II). The prepared magnetic nanoparticles were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). The factors affecting the extraction of the target metal ions such as pH, sample volume, eluent, and interfering ions had been investigated and the adsorption mechanism of the target metals on the self-prepared H(2)Dz-SCMNPs was investigated by FT-IR and X-ray photo electron spectroscopy (XPS). Under the optimized conditions, the detection limits of the developed method for Cr(III), Cu(II), Pb(II) and Zn(II) were 35, 11, 62, and 8ngL(-1), respectively, with the enrichment factor of 100. The relative standard deviations (RSDs, c=10μgL(-1), n=7) were in the range of 1.7-3.1% and the linear range was 0.1-100μgL(-1). The proposed method had been validated by two certified reference materials (GSBZ50009-88 environmental water and GBW07601 human hair), and the determined values were in good agreement with the certified values. The method was also applied for the determination of trace metals in real water and human hair samples with recoveries in the range of 85-110% for the spiked samples. The developed MSPE-ICP-OES method has the advantages of simplicity, rapidity, selectivity, high extraction efficiency and is suitable for the analysis of samples with large volume and complex matrix. Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

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

2017-09-01

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

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

NASA Astrophysics Data System (ADS)

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

2008-07-01

Herein, we present the development of a procedure for the determination of total sulfur in petroleum-derived products (gasoline, kerosene and diesel fuel) employing inductively coupled plasma optical emission spectrometry (ICP OES). For this procedure, samples were prepared as emulsions that were made using concentrated nitric acid, Triton X-100, sample, and ultra pure water in proportions of 5/10/7/78% (v/v), respectively. Sample volumes were weighed because of the density differences, and oxygen was added to the sheat gas entrance of the ICP OES in order to decrease carbon deposition in the torch and to minimize background effects. A Doehlert design was applied as an experimental matrix to investigate the flow ratios of argon (sheat and plasma gas) and oxygen in relation to the signal-to-background ratio. A comparative study among the slopes of the analytical curves built in aqueous media, surfactant/HNO 3, and by spike addition for several sample emulsions indicates that a unique solution of surfactant in acidic media can be employed to perform the external calibration for analysis of the emulsions. The developed procedure allows for the determination of the total sulfur content in petroleum derivatives with a limit of detection (LOD) and limit of quantification (LOQ) of 0.72 and 2.4 μg g - 1 , respectively. Precision values, expressed as the relative standard deviations (% RSD, n = 10) for 12 and 400 μg g - 1 , were 2.2% and 1.3%, respectively. The proposed procedure was applied toward the determination of total sulfur in samples of gasoline, kerosene, and diesel fuel commercialized in the city of Niterói/RJ, Brazil. The accuracy of the proposed method was evaluated by the determination of the total sulfur in three different standard reference materials (SRM): NIST 2723a (sulfur in diesel fuel oil), NIST 1616b (sulfur in kerosene), and NIST 2298 (sulfur in gasoline). The data indicate that the methodology can be successfully applied to these types of samples. Spiking tests, conducted with the analyzed samples, indicate that recoveries are between 97 and 103%.

Multi-elemental analysis of aqueous geochemical samples by quadrupole inductively coupled plasma-mass spectrometry (ICP-MS)

USGS Publications Warehouse

Wolf, Ruth E.; Adams, Monique

2015-01-01

Typically, quadrupole inductively coupled plasma-mass spectrometry (ICP-MS) is used to determine as many as 57 major, minor, and trace elements in aqueous geochemical samples, including natural surface water and groundwater, acid mine drainage water, and extracts or leachates from geological samples. The sample solution is aspirated into the inductively coupled plasma (ICP) which is an electrodeless discharge of ionized argon gas at a temperature of approximately 6,000 degrees Celsius. The elements in the sample solution are subsequently volatilized, atomized, and ionized by the ICP. The ions generated are then focused and introduced into a quadrupole mass filter which only allows one mass to reach the detector at a given moment in time. As the settings of the mass analyzer change, subsequent masses are allowed to impact the detector. Although the typical quadrupole ICP-MS system is a sequential scanning instrument (determining each mass separately), the scan speed of modern instruments is on the order of several thousand masses per second. Consequently, typical total sample analysis times of 2–3 minutes are readily achievable for up to 57 elements.

Effects of copper sulfate on seedlings of Prosopis pubescens (screwbean mesquite).

PubMed

Zappala, Marian N; Ellzey, Joanne T; Bader, Julia; Peralta-Videa, Jose R; Gardea-Torresdey, Jorge

2014-01-01

Phytoextraction is an established method of removal of heavy metals from contaminated soils worldwide. Phytoextraction is most efficient if local plants are used in the contaminated site. We propose that Prosopis pubescens (Screw bean mesquite) would be a successful phytoextractor of copper in our local soils. In order to determine the feasibility of using Screw bean mesquite, we utilized inductively-coupled plasma-optical emission spectroscopy (ICP-OES) and elemental analysis to observe the uptake of copper and the effects on macro and micro nutrients within laboratory-grown seedlings. We have previously shown that P. pubescens is a hyperaccumulator of copper in soil-grown seedlings. Light and transmission electron microscopy demonstrated death of root cells and ultrastructural changes due to the presence of copper from 50 mg/L - 600 mg/L. Ultrastructural changes included plasmolysis, starch accumulation, increased vacuolation and swollen chloroplasts with disarranged thylakoid membranes in cotyledons. Inductively coupled plasma-optical emission spectroscopy analyses of macro- and micro-nutrients revealed that the presence of copper sulfate in the growth medium of Petri-dish grown Prosopis pubescens seedlings resulted in dramatic decreases of magnesium, potassium and phosphorus. At 500-600 mg/L of copper sulfate, a substantial increase of sulfur was present in roots.

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

PubMed

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

2009-11-15

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

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

PubMed

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.

Determination of 241Am in sediments by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS).

PubMed

Agarande, M; Benzoubir, S; Bouisset, P; Calmet, D

2001-08-01

Trace levels (pg kg(-1)) of 241Am in sediments were determined by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS) using a microconcentric nebulizer. 241Am was isolated from major elements like Ca and Fe by different selective precipitations. In further steps. Am was first separated from other transuranic elements and purified by anion exchange and extraction chromatography prior to the mass spectrometric measurements. The ID HR ICP-MS results are compared with isotope dilution alpha spectrometry.

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

PubMed

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

2015-01-01

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

Development of certified reference materials for electrolytes in human serum (GBW09124-09126).

PubMed

Feng, Liuxing; Wang, Jun; Cui, Yanjie; Shi, Naijie; Li, Haifeng; Li, Hongmei

2017-05-01

Three reference materials, at relatively low, middle, and high concentrations, were developed for analysis of the mass fractions of electrolytes (K, Ca, Na, Mg, Cl, and Li) in human serum. The reference materials were prepared by adding high purity chloride salts to normal human serum. The concentration range of the three levels is within ±20% of normal human serum. It was shown that 14 units with duplicate analysis is enough to demonstrate the homogeneity of these candidate reference materials. The statistical results also showed no significant trends in both short-term stability test for 1 week at 40 °C and long-term stability test for 14 months. The certification methods of the six elements include isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS), inductively coupled plasma optical emission spectroscopy (ICP-OES), atomic absorption spectroscopy (AAS), ion chromatography (IC), and ion-selective electrode (ISE). The certification methods were validated by international comparisons among a number of national metrology institutes (NMIs). The combined relative standard uncertainties of the property values were estimated by considering the uncertainties of the analytical methods, homogeneity, and stability. The range of the expanded uncertainties of all the elements is from 2.2% to 3.9%. The certified reference materials (CRMs) are primarily intended for use in the calibration and validation of procedures in clinical analysis for the determination of electrolytes in human serum or plasma. Graphical Abstract Certified reference materials for K, Ca, Mg, Na, Cl and Li in human serum (GBW09124-09126).

In vitro element release and biological aspects of base–metal alloys for metal-ceramic applications

PubMed Central

Holm, Charlotta; Morisbak, Else; Kalfoss, Torill; Dahl, Jon E.

2015-01-01

Abstract Objective: The aims of this study were to investigate the release of element from, and the biological response in vitro to, cobalt–chromium alloys and other base–metal alloys used for the fabrication of metal-ceramic restorations. Material and methods: Eighteen different alloys were investigated. Nine cobalt–chromium alloys, three nickel–chromium alloys, two cobalt–chromium–iron alloys, one palladium–silver alloy, one high-noble gold alloy, titanium grade II and one type III copper–aluminium alloy. Pure copper served as positive control. The specimens were prepared according to the ISO standards for biological and corrosion testing. Passive leaching of elements was measured by using Inductively Coupled Plasma – Mass Spectrometry (ICP-MS) after incubation in cell culture media, MEM, for 3 days. Corrosion testing was carried out in 0.9% sodium chloride (NaCl) and 1% lactic acid for 7 days, and the element release was measured by Inductively Coupled Plasma – Optical Emission Spectroscopy (ICP-OES). The biological response from the extract solutions was measured though MTT cytotoxicity testing and the Hen's egg test-chorio-allantoic membrane (HET-CAM) technique for irritationt. Results: The corrosion test showed similar element release from base-metal alloys compared to noble alloys such as gold. Apart from the high-copper alloy, all alloys expressed low element release in the immersion test, no cytotoxic effect in the MTT test, and were rated non-irritant in the HET-CAM test. Conclusions: Minimal biological response was observed for all the alloys tested, with the exception of the high-copper alloy. PMID:28642904

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.

NASA Astrophysics Data System (ADS)

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.

Hydraulic Evolution of Karst Microfracture

NASA Astrophysics Data System (ADS)

Windom, L. M.; Dragila, M. I.; Weisbrod, N.

2017-12-01

Karst terrain comprises an astounding 25% of our planet's potable water resources, yet the evolution of these systems from micro-fracture to open channel is poorly understood. Focusing on the unsaturated portion of an evolving karst system, we present a conceptual model for the hydraulic evolution of micro-fractures into larger conduits. Tensional micro-fractures (< 1mm thick) under unsaturated conditions may be eroded by water flowing either as seepage films or as capillary rivulets. In addition to general erosion, the narrow width of capillary rivulets may etch the beginning of preferential paths within the tensional micro-fractures that will lead to tubular channels. Both fluid mechanisms, seepage and rivulets, were tested in the laboratory, and data of the resulting geochemical erosion rates are presented in the form of calcium dissolution rates measured by inductively coupled plasma atomic emission spectroscopy (ICP-OES).

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

NASA Astrophysics Data System (ADS)

Ma, Yinbiao; Wei, Xiaojuan

2017-04-01

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

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

PubMed

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

2017-05-01

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

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

PubMed

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

2005-03-30

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

Electrodeposition and characterisation of Al-W alloy films from ionic liquid

NASA Astrophysics Data System (ADS)

Höhlich, D.; Wachner, D.; Müller, M.; Scharf, I.; Lampke, T.

2018-06-01

Al–W alloy films were prepared by electrodeposition using anhydrous 1-ethyl-3-methylimidazolium chloride (EMIMCl) ionic-liquid solution with aluminium chloride in a ratio of 1:1.5. As a commercially available tungsten precursor, tungsten hexachloride was used. The metal is dissolved in the ionic liquid at concentrations up to 0.06 mol/l. The deposition took place outside the glove box with a continuous argon stream over the electrolyte at a temperature of 60 °C with a current density of 1 A/m2. Resulting alloys show a tungsten content higher than 20 wt% (3.5 at%). The phase composition of Al-W alloys was observed by X-ray diffraction (XRD), and the chemical composition was characterised by scanning electron microscopy (SEM) and inductively-coupled plasma optical emission spectroscopy (ICP-OES).

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

NASA Astrophysics Data System (ADS)

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

2013-12-01

Coral reefs near their latitudinal and ecological limits may be affected disproportionately by global climate changes, especially by changing sea surface temperatures (SST's). One such reef is Kure Atoll, the northernmost reef in the Hawaiian chain. Kure Atoll experiences dramatic temperature and seasonal differences throughout the year. Tracking these fluctuations is important for understanding recent physical forces affecting coral growth in such marginal reefs, and for predicting likely responses to future climate and oceanic changes. We used Sr/Ca ratios of a 50cm Porites evermanni coral core collected in Kure (September 2002) as a SST proxy for reconstructing a temperature timescale spanning the length of the core (~62 years). After cutting a 5 mm thick slab through the center growth axis and X-raying it to identify annual density banding, we extracted 4 equally-spaced samples from each annual increment to quantify, seasonal, inter-annual, and decadal SST patterns. We measured Sr and Ca concentrations by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). We then converted Sr/Ca ratios (mmol/mol) to SST using published equations, and calibrated the more recent SST estimates against satellite-based SST imagery and instrumental records from Midway Atoll (ca. 90 km to SE). We coupled the ICP-OES data with Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) scans along the core to provide higher temporal resolution for interpreting intra-seasonal and inter-seasonal trends. Higher resolution of temperature dating can help us interpret strong inter-seasonal changes not readily seen with low resolution measurements, giving us the ability to track temperature anomalies at interannual and decadal timescales, such as El Niño/Southern Oscillation or La Niña/North Pacific Decadal Oscillation. Further, the SST signature from the Sr/Ca analyses are being used in conjunction with bomb radiocarbon signals in order to establish a complete timeline of when carbon isotope spikes appear in this region from large scale atomic testing. Changes in 14C along the length of our core have important implications for understanding regional oceanic circulation, and for the life history age validation of marine organisms, including long-lived fishes whose calcareous otoliths retain a 14C signal. These results have direct application for improved management of commercially important reef and bottom fishes of Hawaii. By tracing the bomb 14C signal in the otolith (ear bone) of regional fishes, important population parameters can be validated (e.g. age of maturity and longevity). At present, the bomb 14C record is incomplete for the Hawaiian Archipelago, but the work presented will fill the void.

Fundamental and methodological investigations for the improvement of elemental analysis by inductively coupled plasma mass soectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ebert, Christopher Hysjulien

This dissertation describes a variety of studies meant to improve the analytical performance of inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation (LA) ICP-MS. The emission behavior of individual droplets and LA generated particles in an ICP is studied using a high-speed, high frame rate digital camera. Phenomena are observed during the ablation of silicate glass that would cause elemental fractionation during analysis by ICP-MS. Preliminary work for ICP torch developments specifically tailored for the improvement of LA sample introduction are presented. An abnormal scarcity of metal-argon polyatomic ions (MAr{sup +}) is observed during ICP-MS analysis. Evidence shows thatmore » MAr{sup +} ions are dissociated by collisions with background gas in a shockwave near the tip of the skimmer cone. Method development towards the improvement of LA-ICP-MS for environmental monitoring is described. A method is developed to trap small particles in a collodion matrix and analyze each particle individually by LA-ICP-MS.« less

High intensity ion beams from an atmospheric pressure inductively coupled plasma

NASA Astrophysics Data System (ADS)

Al Moussalami, S.; Chen, W.; Collings, B. A.; Douglas, D. J.

2002-02-01

This work is directed towards substantially improving the sensitivity of an inductively coupled plasma mass spectrometer (ICP-MS). Ions produced in the ICP at atmospheric pressure have been extracted with comparatively high current densities. The conventional approach to ion extraction, based on a skimmed molecular beam, has been abandoned, and a high extraction field arrangement has been adopted. Although the new approach is not optimized, current densities more than 180 times greater than that of a conventional interface have been extracted and analyte sensitivities ˜10-100× greater than those reported previously for quadrupole ICP-MS have been measured.

Flow-field differences and electromagnetic-field properties of air and N2 inductively coupled plasmas

NASA Astrophysics Data System (ADS)

Yu, Minghao; Yamada, Kazuhiko; Takahashi, Yusuke; Liu, Kai; Zhao, Tong

2016-12-01

A numerical model for simulating air and nitrogen inductively coupled plasmas (ICPs) was developed considering thermochemical nonequilibrium and the third-order electron transport properties. A modified far-field electromagnetic model was introduced and tightly coupled with the flow field equations to describe the Joule heating and inductive discharge phenomena. In total, 11 species and 49 chemical reactions of air, which include 5 species and 8 chemical reactions of nitrogen, were employed to model the chemical reaction process. The internal energy transfers among translational, vibrational, rotational, and electronic energy modes of chemical species were taken into account to study thermal nonequilibrium effects. The low-Reynolds number Abe-Kondoh-Nagano k-ɛ turbulence model was employed to consider the turbulent heat transfer. In this study, the fundamental characteristics of an ICP flow, such as the weak ionization, high temperature but low velocity in the torch, and wide area of the plasma plume, were reproduced by the developed numerical model. The flow field differences between the air and nitrogen ICP flows inside the 10-kW ICP wind tunnel were made clear. The interactions between the electromagnetic and flow fields were also revealed for an inductive discharge.

Demonstration/Validation of the Snap Sampler Passive Groundwater Sampling Device at the Former McClellan Air Force Base

DTIC Science & Technology

2011-02-01

and Development Center Fe Iron gpd Gallons per Day HDPE High Density Polyethylene Hg Mercury ICP Inductively Coupled Plasma ICP/MS...Inductively Coupled Plasma Mass Spectrometry IROD Interim Record of Decision ITRC Interstate Technology and Regulatory Council K Potassium Kow...alkaline earth metals, alkali metals, and a metalloid, were sampled. This particular demonstration took place at the McClellan Air Force Base (AFB) in

Ion sampling and transport in Inductively Coupled Plasma Mass Spectrometry

NASA Astrophysics Data System (ADS)

Farnsworth, Paul B.; Spencer, Ross L.

2017-08-01

Quantitative accuracy and high sensitivity in inductively coupled plasma mass spectrometry (ICP-MS) depend on consistent and efficient extraction and transport of analyte ions from an inductively coupled plasma to a mass analyzer, where they are sorted and detected. In this review we examine the fundamental physical processes that control ion sampling and transport in ICP-MS and compare the results of theory and computerized models with experimental efforts to characterize the flow of ions through plasma mass spectrometers' vacuum interfaces. We trace the flow of ions from their generation in the plasma, into the sampling cone, through the supersonic expansion in the first vacuum stage, through the skimmer, and into the ion optics that deliver the ions to the mass analyzer. At each stage we consider idealized behavior and departures from ideal behavior that affect the performance of ICP-MS as an analytical tool.

Novel and versatile solid-state chemiluminescence sensor based on TiO2-Ru(bpy)32+ nanoparticles for pharmaceutical drugs detection

NASA Astrophysics Data System (ADS)

Al-Hetlani, Entesar; Amin, Mohamed O.; Madkour, Metwally

2018-02-01

This work describes a novel and versatile solid-state chemiluminescence sensor for analyte detection using TiO2-Ru(bpy)32+-Ce(IV). Herein, we report the synthesis, characterization, optimization and application of a new type of hybrid nanoparticles (NPs). Mesoporous TiO2-Ru(bpy)32+ NPs were prepared using a modified sol-gel method by incorporating Ru(bpy)32+ into the initial reaction mixture at various concentrations. The resultant bright orange precipitate was characterized via transmission electron microscopy, N2 sorpometry, inductively coupled plasma-optical emission spectrometer (ICP-OES), Raman and UV-Vis spectroscopy techniques. The concentration of Ru(bpy)32+ complex in the NPs was quantified using ICP-OES, and its chemiluminescence (CL) response was measured and compared with the same concentration in the liquid phase using oxalate as model analyte. The results showed that this type of hybrid material exhibited a higher CL signal compared with the liquid phase due to the enlarged surface area of the hybrid NPs ( 149.6 m2/g). The amount of TiO2-Ru(bpy)32+ NPs and the effect of the analyte flow rate were also investigated to optimize the CL signal. The optimized system was further used to detect oxalate and two pharmaceutical drugs, namely, imipramine and promazine. The linear range for both drugs was 1-100 pm with limits of detection (LOD) of 0.1 and 0.5 pm, respectively. This approach is considered to be simple, low cost and facile and can be applied to a wide range of analytes.

Optimized ultrasound-assisted emulsification microextraction for simultaneous trace multielement determination of heavy metals in real water samples by ICP-OES.

PubMed

Sereshti, Hassan; Heravi, Yeganeh Entezari; Samadi, Soheila

2012-08-15

Ultrasonic-assisted emulsification microextraction (USAEME) combined with inductively coupled plasma-optical emission spectrometry (ICP-OES) was used for preconcentration and determination of aluminum, bismuth, cadmium, cobalt, copper, iron, gallium, indium, nickel, lead, thallium and zinc in real water samples. Ammonium pyrrolidine dithiocarbamate (APDC) and carbon tetrachloride (CCl(4)) were used as the chelating agent and extraction solvent, respectively. The effective parameters (factors) of the extraction process such as volume of extraction solvent, pH, sonication time, and concentration of chelating agent were optimized by a small central composite design (CCD). The optimum conditions were found to be 98 μL for extraction solvent, 1476 mg L(-1) for chelating agent, 3.8 for pH and 9 min for sonication time. Under the optimal conditions, the limits of detection (LODs) for Al, Bi, Cd, Co, Cu, Fe, Ga, In, Ni, Pb, Tl and Zn were 0.13, 0.48, 0.19, 0.28, 0.29, 0.27, 0.27, 0.38, 0.44, 0.47, 0.52 and 0.17 μg L(-1), respectively. The linear dynamic range (LDR) was 1-1000 μ gL(-1) with determination coefficients of 0.991-0.998. Relative standard deviations (RSDs, C=200 μg L(-1), n=6) were between 1.87%-5.65%. The proposed method was successfully applied to the extraction and determination of heavy metals in real water samples and the satisfactory relative recoveries (90.3%-105.5%) were obtained. Copyright © 2012 Elsevier B.V. All rights reserved.

Selective divalent cobalt ions detection using Ag2O3-ZnO nanocones by ICP-OES method for environmental remediation.

PubMed

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

2014-01-01

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

Determination of As, Se, and Hg in fuel samples by in-chamber chemical vapor generation ICP OES using a Flow Blurring® multinebulizer.

PubMed

García, Miriam; Aguirre, Miguel Ángel; Canals, Antonio

2017-09-01

In this work, a new and simple analytical methodology based on in-chamber chemical vapor generation has been developed for the spectrochemical analysis of commercial fuel samples. A multiple nebulizer with three nebulization units has been employed for this purpose: One unit was used for sample introduction, while the other two were used for the necessary reagent introduction. In this way, the aerosols were mixed inside the spray chamber. Through this method, analyte transport and, therefore, sensitivity are improved in inductively coupled plasma-optical emission spectrometry. The factors (i.e., variables), influencing chemical vapor generation, have been optimized using a multivariate approach. Under optimum chemical vapor generation conditions ([NaBH 4 ] = 1.39%, [HCl] = 2.97 M, total liquid flow = 936 μL min -1 ), the proposed sample introduction system allowed the determination of arsenic, selenium, and mercury up to 5 μg g -1 with a limit of detection of 25, 140, and 13 μg kg -1 , respectively. Analyzing spiked commercial fuel samples, recovery values obtained were between 96 and 113%, and expanded uncertainty values ranged from 4 to 16%. The most striking practical conclusion of this investigation is that no carbon deposit appears on the plasma torch after extended periods of working. Graphical abstract A new and simple analytical methodology based on in-chamber chemical vapor generation has been developed for the spectrochemical analysis of commercial fuel samples in ICP OES.

Calcium extraction from brine water and seawater using oxalic acid

NASA Astrophysics Data System (ADS)

Natasha, Nadia Chrisayu; Lalasari, Latifa Hanum

2017-01-01

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

Calibration-free quantitative analysis of elemental ratios in intermetallic nanoalloys and nanocomposites using Laser Induced Breakdown Spectroscopy (LIBS).

PubMed

Davari, Seyyed Ali; Hu, Sheng; Mukherjee, Dibyendu

2017-03-01

Intermetallic nanoalloys (NAs) and nanocomposites (NCs) have increasingly gained prominence as efficient catalytic materials in electrochemical energy conversion and storage systems. But their morphology and chemical compositions play critical role in tuning their catalytic activities, and precious metal contents. While advanced microscopy techniques facilitate morphological characterizations, traditional chemical characterizations are either qualitative or extremely involved. In this study, we apply Laser Induced Breakdown Spectroscopy (LIBS) for quantitative compositional analysis of NAs and NCs synthesized with varied elemental ratios by our in-house built pulsed laser ablation technique. Specifically, elemental ratios of binary PtNi, PdCo (NAs) and PtCo (NCs) of different compositions are determined from LIBS measurements employing an internal calibration scheme using the bulk matrix species as internal standards. Morphology and qualitative elemental compositions of the aforesaid NAs and NCs are confirmed from Transmission Electron Microscopy (TEM) images and Energy Dispersive X-ray Spectroscopy (EDX) measurements. LIBS experiments are carried out in ambient conditions with the NA and NC samples drop cast on silicon wafers after centrifugation to increase their concentrations. The technique does not call for cumbersome sample preparations including acid digestions and external calibration standards commonly required in Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) techniques. Yet the quantitative LIBS results are in good agreement with the results from ICP-OES measurements. Our results indicate the feasibility of using LIBS in future for rapid and in-situ quantitative chemical characterizations of wide classes of synthesized NAs and NCs. Copyright © 2016 Elsevier B.V. All rights reserved.

Rapid methodology to screen flame retardants in upholstered furniture for compliance with new California labeling law (SB 1019).

PubMed

Petreas, Myrto; Gill, Ranjit; Takaku-Pugh, Sayaka; Lytle, Eric; Parry, Emily; Wang, Miaomiao; Quinn, John; Park, June-Soo

2016-06-01

In response to concerns regarding the widespread use of flame retardants, the California Legislature passed a law (SB1019) requiring labels on furniture products to indicate whether they do or do not contain flame retardants. To support the enforcement of the new law, our laboratory developed a step-wise, screening approach to test for brominated (BFR) and phosphorus-based flame retardants (OPFRs) in several types of furniture components (foam, fabric, batting, plumage, etc.). We used X-Ray Fluorescence (XRF) to screen for the presence of Br (and other elements) and Inductively Coupled Plasma - Optical Emission Spectrometry (ICP-OES) to identify and measure the concentration of P (and other elements). The same samples were also extracted by dichloromethane using sonication and analyzed by a single injection into a Gas Chromatograph - Tandem Mass Spectrometer to obtain concentrations of specific BFRs and OPFRs. Our approach showed excellent screening potential for Br and Sb by XRF and for P by ICP-OES, with both tests having predictive values of a negative equal to 1. To explore and screen for flame retardants in products not included in our current list of target chemicals, we used Liquid Chromatography/Time-of-Flight Mass Spectrometry operated with electrospray ionization, to identify additional flame retardants to be incorporated in quantitative methods. We are making all our methodologies public to facilitate simple and low cost methods that can help manufacturers and suppliers have their products tested and correctly labeled, ultimately benefitting the consumer. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

PubMed Central

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

2014-01-01

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

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

PubMed

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

2016-06-01

Metals and metalloids are natural components of the biosphere, which are not produced per se by human beings, but whose form and distribution can be affected by human activities. Like all substances, they are a contaminant if present in excess compared to background levels and/or in a form that would not normally occur in the environment. Samples of liver, gills, gonads and muscle from European chub, Squalius cephalus, were analyzed for Al, As, B, Ba, Cr, Cu, Fe, Hg, Mn, Mo, Sr and Zn using inductively coupled plasma optical emission spectrometry (ICP-OES) to highlight the importance of tissue selection in monitoring research. The comet assay or single cell gel electrophoresis (SCGE) was selected as an in vivo genotoxicity assay, a rapid and sensitive method for measuring genotoxic effects in blood, liver and gills of the European chub. Microscopic images of comets were scored using Comet IV Computer Software (Perceptive Instruments, UK). The objective of our study was to investigate two reservoirs, Zlatar and Garasi, and one river, Pestan by: (i) determining and comparing metal and metalloid concentrations in sediment, water and tissues of European chub: liver, gills, muscle and gonads (ii) comparing these findings with genotoxicity of water expressed through DNA damage of fish tissues. A clear link between the level of metals in water, sediment and tissues and between metal and genotoxicity levels at examined sites was not found. This suggests that other xenobiotics (possibly the organic compounds), contribute to DNA damage. Copyright © 2016 Elsevier Ltd. All rights reserved.

Physical chemical effects of zinc on in vitro enamel demineralization.

PubMed

Mohammed, N R; Mneimne, M; Hill, R G; Al-Jawad, M; Lynch, R J M; Anderson, P

2014-09-01

Zinc salts are formulated into oral health products as antibacterial agents, yet their interaction with enamel is not clearly understood. The aim was to investigate the effect of zinc concentration [Zn(2+)] on the in vitro demineralization of enamel during exposure to caries-simulating conditions. Furthermore, the possible mechanism of zinc's action for reducing demineralization was determined. Enamel blocks and synthetic hydroxyapatite (HAp) were demineralized in a range of zinc-containing acidic solutions (0-3565ppm [Zn(2+)]) at pH 4.0 and 37°C. Inductively coupled-plasma optical emission spectroscopy (ICP-OES) was used to measure ion release into solution. Enamel blocks were analysed by Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy (ATR-FTIR), and HAp by X-ray diffraction (XRD) and neutron diffraction (ND). ICP-OES analysis of the acidic solutions showed a decrease in [Ca(2+)] and [PO4(3-)] release with increasing [Zn(2+)]. FTIR revealed a α-hopeite (α-Zn3(PO4)2.4H2O)-like phase on the enamel surfaces at >107ppm [Zn(2+)]. XRD and ND analysis confirmed a zinc-phosphate phase present alongside the HAp. This study confirms that zinc reduces enamel demineralization. Under the conditions studied, zinc acts predominantly on enamel surfaces at PO4(3-) sites in the HAp lattice to possibly form an α-hopeite-like phase. These results have a significant implication on the understanding of the fundamental chemistry of zinc in toothpastes and demonstrate its therapeutic potential in preventing tooth mineral loss. Copyright © 2014 The Authors. Published by Elsevier Ltd.. All rights reserved.

A comparison of lead-isotope measurements on exploration-type samples using inductively coupled plasma and thermal ionization mass spectrometry

USGS Publications Warehouse

Gulson, B.L.; Meier, A.L.; Church, S.E.; Mizon, K.J.

1989-01-01

Thermal ionization mass spectrometry (TI-MS) has long been the method of choice for Pb-isotope determinations. More recently, however, inductively coupled plasma mass spectrometry (ICP-MS) has been used to determine Pb-isotope ratios for mineral exploration. The ICP-MS technique, although not as precise as TI-MS, may promote a wider application of Ph-isotope ratio methods because it allows individual isotopes to be determined more rapidly, generally without need for chemical separation (e.g., Smith et al., 1984; Hinners et al., 1987). To demonstrate the utility of the ICP-MS method, we have conducted a series of Pb-isotope measurements on several suites of samples using both TI-MS and ICP-MS. ?? 1989.

2D elemental mapping of sections of human kidney stones using laser ablation inductively-coupled plasma-mass spectrometry: Possibilities and limitations

NASA Astrophysics Data System (ADS)

Vašinová Galiová, Michaela; Čopjaková, Renata; Škoda, Radek; Štěpánková, Kateřina; Vaňková, Michaela; Kuta, Jan; Prokeš, Lubomír; Kynický, Jindřich; Kanický, Viktor

2014-10-01

A 213 nm Nd:YAG-based laser ablation (LA) system coupled to quadrupole-based inductively coupled plasma-mass spectrometer and an ArF* excimer-based LA-system coupled to a double-focusing sector field inductively coupled plasma-mass spectrometer were employed to study the spatial distribution of various elements in kidney stones (uroliths). Sections of the surfaces of uroliths were ablated according to line patterns to investigate the elemental profiles for the different urolith growth zones. This exploratory study was mainly focused on the distinguishing of the main constituents of urinary calculus fragments by means of LA-ICP-mass spectrometry. Changes in the ablation rate for oxalate and phosphate phases related to matrix density and hardness are discussed. Elemental association was investigated on the basis of 2D mapping. The possibility of using NIST SRM 1486 Bone Meal as an external standard for calibration was tested. It is shown that LA-ICP-MS is helpful for determination of the mineralogical composition and size of all phases within the analyzed surface area, for tracing down elemental associations and for documenting the elemental content of urinary stones. LA-ICP-MS results (elemental contents and maps) are compared to those obtained with electron microprobe analysis and solution analysis ICP-MS.

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

PubMed

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

2008-12-15

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

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

PubMed

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

2015-01-01

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

Phosphorus Concentrations in Sequentially Fractionated Soil Samples as Affected by Digestion Methods

PubMed Central

do Nascimento, Carlos A. C.; Pagliari, Paulo H.; Schmitt, Djalma; He, Zhongqi; Waldrip, Heidi

2015-01-01

Sequential fractionation has helped improving our understanding of the lability and bioavailability of P in soil. Nevertheless, there have been no reports on how manipulation of the different fractions prior to analyses affects the total P (TP) concentrations measured. This study investigated the effects of sample digestion, filtration, and acidification on the TP concentrations determined by ICP-OES in 20 soil samples. Total P in extracts were either determined without digestion by ICP-OES, or ICP-OES following block digestion, or autoclave digestion. The effects of sample filtration, and acidification on undigested alkaline extracts prior to ICP-OES were also evaluated. Results showed that, TP concentrations were greatest in the block-digested extracts, though the variability introduced by the block-digestion was the highest. Acidification of NaHCO3 extracts resulted in lower TP concentrations, while acidification of NaOH randomly increased or decreased TP concentrations. The precision observed with ICP-OES of undigested extracts suggests this should be the preferred method for TP determination in sequentially extracted samples. Thus, observations reported in this work would be helpful in appropriate sample handling for P determination, thereby improving the precision of P determination. The results are also useful for literature data comparison and discussion when there are differences in sample treatments. PMID:26647644

Assessment of Heavy Metals in Municipal Sewage Sludge: A Case Study of Limpopo Province, South Africa

PubMed Central

Shamuyarira, Kudakwashe K.; Gumbo, Jabulani R.

2014-01-01

Heavy metals in high concentrations can cause health and environmental damage. Nanosilver is an emerging heavy metal which has a bright future of use in many applications. Here we report on the levels of silver and other heavy metals in municipal sewage sludge. Five towns in Limpopo province of South Africa were selected and the sludge from their wastewater treatment plants (WWTPs) was collected and analysed. The acid digested sewage sludge samples were analysed using Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) methods. The concentrations of silver found were low, but significant, in the range 0.22 to 21.93 mg/kg dry mass. The highest concentration of silver was found in Louis Trichardt town with a concentration of 21.93 ± 0.38 mg/kg dry mass while the lowest was Thohoyandou with a concentration of 6.13 ± 0.12 mg/kg dry mass. A control sludge sample from a pit latrine had trace levels of silver at 0.22 ± 0.01 mg/kg dry mass. The result showed that silver was indeed present in the wastewater sewage sludge and at present there is no DWAF guideline standard. The average Cd concentration was 3.10 mg/kg dry mass for Polokwane municipality. Polokwane and Louis Trichardt municipalities exhibited high levels of Pb, in excess DWAF guidelines, in sludge at 102.83 and 171.87 mg/kg respectfully. In all the WWTPs the zinc and copper concentrations were in excess of DWAF guidelines. The presence of heavy metals in the sewage sludge in excess of DWAF guidelines presents environmental hazards should the sludge be applied as a soil ameliorant. PMID:24595211

Determination of the post mortem interval in skeletal remains by the comparative use of different physico-chemical methods: Are they reliable as an alternative to 14C?

PubMed

Amadasi, Alberto; Cappella, Annalisa; Cattaneo, Cristina; Cofrancesco, Pacifico; Cucca, Lucia; Merli, Daniele; Milanese, Chiara; Pinto, Andrea; Profumo, Antonella; Scarpulla, Valentina; Sguazza, Emanuela

2017-05-01

The determination of the post-mortem interval (PMI) of skeletal remains is a challenging aspect in the forensic field. Previous studies focused their attention on different macroscopic and morphological aspects but a thorough and complete evaluation of the potential of chemical and physical analyses in this field of research has not been performed. In addition to luminol test and Oxford histology index (OHI) reported in a recent paper, widely spread and accessible methods based on physical aspect and chemical characteristics of skeletal remains have been investigated as potential alternatives to dating by determination of 14 C. The investigation was performed on a total of 24 archeological and forensic bone samples with known PMI, with inductively coupled plasma optical emission spectrometer (ICP-OES), inductively coupled plasma quadruple mass spectrometry (ICP-MS), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive X-ray analysis (EDX), powder X-ray diffraction analysis (XRPD) and scanning electron microscopy (SEM). Finally, the feasibility of such alternative methods was discussed. Some results such as carbonates/phosphates ratio from FT-IR, the amounts of organic and inorganic matter by EDX, crystallite sizes with XRPD, and surface morphology obtained by SEM, showed significant trends along with PMI. Though, from a chemical point of view cut-off values and gold-standard methods still present challenges, and rather different techniques together can provide useful information toward the assessment of the PMI of skeletal remains. It is however clear that in a hypothetical flowchart those methods may be placed practically at the same level and a choice should always consider the evaluation of results by each technique, execution times and a costs/benefits relationship. Copyright © 2017 Elsevier GmbH. All rights reserved.

Gravimetric preparation and characterization of primary reference solutions of molybdenum and rhodium.

PubMed

Kaltenbach, Angela; Noordmann, Janine; Görlitz, Volker; Pape, Carola; Richter, Silke; Kipphardt, Heinrich; Kopp, Gernot; Jährling, Reinhard; Rienitz, Olaf; Güttler, Bernd

2015-04-01

Gravimetrically prepared mono-elemental reference solutions having a well-known mass fraction of approximately 1 g/kg (or a mass concentration of 1 g/L) define the very basis of virtually all measurements in inorganic analysis. Serving as the starting materials of all standard/calibration solutions, they link virtually all measurements of inorganic analytes (regardless of the method applied) to the purity of the solid materials (high-purity metals or salts) they were prepared from. In case these solid materials are characterized comprehensively with respect to their purity, this link also establishes direct metrological traceability to The International System of Units (SI). This, in turn, ensures the comparability of all results on the highest level achievable. Several national metrology institutes (NMIs) and designated institutes (DIs) have been working for nearly two decades in close cooperation with commercial producers on making an increasing number of traceable reference solutions available. Besides the comprehensive characterization of the solid starting materials, dissolving them both loss-free and completely under strict gravimetric control is a challenging problem in the case of several elements like molybdenum and rhodium. Within the framework of the European Metrology Research Programme (EMRP), in the Joint Research Project (JRP) called SIB09 Primary standards for challenging elements, reference solutions of molybdenum and rhodium were prepared directly from the respective metals with a relative expanded uncertainty associated with the mass fraction of U rel(w) < 0.05 %. To achieve this, a microwave-assisted digestion procedure for Rh and a hotplate digestion procedure for Mo were developed along with highly accurate and precise inductively coupled plasma optical emission spectrometry (ICP OES) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) methods required to assist with the preparation and as dissemination tools.

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

PubMed

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

2017-06-01

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

Heavy metals phytoremediation potential of Hevea brasiliensis in Bentong, Malaysia

NASA Astrophysics Data System (ADS)

Yusof, Muhammad Jefri Mohd; Latif, Mohd Talip; Yusoff, Siti Fairus Mohd

2018-04-01

Biomonitoring uses living organisms to assess environmental quality and being preferred over conventional methods that use fully or semi-automatic gauges for its lower cost and practicality. Recently, higher plants are widely used for biomonitoring purposes by means of their species identification simplicity, larger availability of biological substantial, and easy to sample. In this study, samples of Hevea brasiliensis (i.e leaves, barks, and latex as well as surrounding soils) from outskirts of Pelangai, Bentong were tested for heavy metals by using inductively coupled plasma optical emission spectroscopy (ICP-OES). Enrichment factor of soils indicated that some metals (B, Ca, Cu, Mn, Pb, Zn, As and Na) were anthropogenic which most likely originated from traffic emissions. In addition, leaves trapped the most heavy metals compared to barks and latex. The accumulation of pollutants in those samples has identified biomonitoring abilities of Hevea brasiliensis.

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

NASA Astrophysics Data System (ADS)

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

2005-06-01

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

Direct analysis of deodorants for determination of metals by inductively coupled plasma optical emission spectrometry.

PubMed

da Costa, Wiviane Kássia Oliveira Correia; da Silva, Caroline Santos; Figueiredo, José Fernando Dagnone; Nóbrega, Joaquim Araujo; Paim, Ana Paula Silveira

2018-06-05

A fast and simple dilute-and-shoot procedure for determination of Al, As, Ba, Cd, Cu, Fe, Mg, Mn, Ni, Pb, Sc, Ti, V, Zn and Zr in deodorants by inductively coupled plasma optical emission spectrometry (ICP OES) was developed. Sample preparation was carried out by diluting 1 mL of deodorant sample in 1% (v v -1 ) HNO 3 . The accuracy of the analytical procedure was evaluated using addition and recovery experiments, and recoveries ranged from 80 to 119%. The limits of detection varied from 0.001 to 0.76 mg kg -1 . Nine deodorants samples of different brands were analyzed. The maximum concentrations found (mg kg -1 ) were: Fe (1.0), Mn (0.1), Ti (1.02), V (0.33), Zn (255.2) and Zr (0.5); for Al and Mg, determined concentrations varied from 0.01 to 7.0% and from 0.005 to 1.44 mg kg -1 , respectively, showing wide variation depending on the sample type. The developed procedure was adequate for determining these analytes in routine analysis presenting high sample throughput and demonstrated the feasibility of direct analysis measurements after simple dilution step. Copyright © 2018 Elsevier B.V. All rights reserved.

Fluorescence quenching and the "ring-mode" to "red-mode" transition in alkali inductively coupled plasmas

NASA Astrophysics Data System (ADS)

Huang, M.; Bazurto, R.; Camparo, J.

2018-01-01

The ring-mode to red-mode transition in alkali metal inductively coupled plasmas (ICPs) (i.e., rf-discharge lamps) is perhaps the most important physical phenomenon affecting these devices as optical pumping light sources for atomic clocks and magnetometers. It sets the limit on useful ICP operating temperature, thereby setting a limit on ICP light output for atomic-clock/magnetometer signal generation, and it is a temperature region of ICP operation associated with discharge instability. Previous work has suggested that the mechanism driving the ring-mode to red-mode transition is associated with radiation trapping, but definitive experimental evidence validating that hypothesis has been lacking. Based on that hypothesis, one would predict that the introduction of an alkali-fluorescence quenching gas (i.e., N2) into the ICP would increase the ring-mode to red-mode transition temperature. Here, we test that prediction, finding direct evidence supporting the radiation-trapping hypothesis.

Diagnostic studies of ion beam formation in inductively coupled plasma

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jacobs, Jenee L.

2015-01-01

This dissertation describes a variety of studies focused on the plasma and the ion beam in inductively coupled plasma mass spectrometry (ICP-MS). The ability to use ICP-MS for measurements of trace elements in samples requires the analytes to be efficiently ionized. Updated ionization efficiency tables are discussed for ionization temperatures of 6500 K and 7000 K with an electron density of 1 x 10 15 cm -3. These values are reflective of the current operating parameters of ICP-MS instruments. Calculations are also discussed for doubly charged (M 2+) ion formation, neutral metal oxide (MO) ionization, and metal oxide (MO +)more » ion dissociation for similar plasma temperature values. Ionization efficiency results for neutral MO molecules in the ICP have not been reported previously.« less

Inductively Coupled Plasma Mass Spectrometry (ICP-MS) and its Application in Life Sciences

NASA Astrophysics Data System (ADS)

Xu, Gu-feng; Wang, Hong-mei

2001-08-01

Inductively-coupled plasma mass spectrometry (ICP-MS) has made much progress since its birth in the late 1990s. This paper will give a rather systematic overview on the use of this technique in new devices and technologies related to plasma source, sample-introducing device and detecting spectrometer etc. In this overview, an emphasis will be put on the evaluation of the ICP-MS technique in combination with a series of physical, chemical and biological techniques, such as laser ablation (LA), capillary electrophoresis (CE) and high performance liquid chromatograph (HPLC), along with their representative high accuracy and high sensitivity. Finally, comprehensive and fruitful applications of the ICP-MS and its combinative techniques in the detection of trace metallic elements and isotopes in complex biological and environmental samples will be revealed.

Specific activity and isotope abundances of strontium in purified strontium-82

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fitzsimmons, J. M.; Medvedev, D. G.; Mausner, L. F.

2015-11-12

A linear accelerator was used to irradiate a rubidium chloride target with protons to produce strontium-82 (Sr-82), and the Sr-82 was purified by ion exchange chromatography. The amount of strontium associated with the purified Sr-82 was determined by either: ICP-OES or method B which consisted of a summation of strontium quantified by gamma spectroscopy and ICP-MS. The summation method agreed within 10% to the ICP-OES for the total mass of strontium and the subsequent specific activities were determined to be 0.25–0.52 TBq mg -1. Method B was used to determine the isotope abundances by weight% of the purified Sr-82, andmore » the abundances were: Sr-82 (10–20.7%), Sr-83 (0–0.05%), Sr-84 (35–48.5%), Sr-85 (16–25%), Sr-86 (12.5–23%), Sr-87 (0%), and Sr-88 (0–10%). The purified strontium contained mass amounts of Sr-82, Sr-84, Sr-85, Sr-86, and Sr-88 in abundances not associated with natural abundance, and 90% of the strontium was produced by the proton irradiation. A comparison of ICP-OES and method B for the analysis of Sr-82 indicated analysis by ICP-OES would be easier to determine total mass of strontium and comply with regulatory requirements. An ICP-OES analytical method for Sr-82 analysis was established and validated according to regulatory guidelines.« less

Effect of neutral gas heating in argon radio frequency inductively coupled plasma

NASA Astrophysics Data System (ADS)

Chin, O. H.; Jayapalan, K. K.; Wong, C. S.

2014-08-01

Heating of neutral gas in inductively coupled plasma (ICP) is known to result in neutral gas depletion. In this work, this effect is considered in the simulation of the magnetic field distribution of a 13.56 MHz planar coil ICP. Measured electron temperatures and densities at argon pressures of 0.03, 0.07 and 0.2 mbar were used in the simulation whilst neutral gas temperatures were heuristically fitted. The simulated results showed reasonable agreement with the measured magnetic field profile.

Selenium speciation analysis of Misgurnus anguillicaudatus selenoprotein by HPLC-ICP-MS and HPLC-ESI-MS/MS

USDA-ARS?s Scientific Manuscript database

Analytical methods for selenium (Se) speciation were developed using high performance liquid chromatography (HPLC) coupled to either inductively coupled plasma mass spectrometry (ICP-MS) or electrospray ionization tandem mass spectrometry (ESI-MS/MS). Separations of selenomethionine (Se-Met) and sel...

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

NASA Astrophysics Data System (ADS)

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

2014-06-01

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

Investigation of large-area multicoil inductively coupled plasma sources using three-dimensional fluid model

NASA Astrophysics Data System (ADS)

Brcka, Jozef

2016-07-01

A multi inductively coupled plasma (ICP) system can be used to maintain the plasma uniformity and increase the area processed by a high-density plasma. This article presents a source in two different configurations. The distributed planar multi ICP (DM-ICP) source comprises individual ICP sources that are not overlapped and produce plasma independently. Mutual coupling of the ICPs may affect the distribution of the produced plasma. The integrated multicoil ICP (IMC-ICP) source consists of four low-inductance ICP antennas that are superimposed in an azimuthal manner. The identical geometry of the ICP coils was assumed in this work. Both configurations have highly asymmetric components. A three-dimensional (3D) plasma model of the multicoil ICP configurations with asymmetric features is used to investigate the plasma characteristics in a large chamber and the operation of the sources in inert and reactive gases. The feasibility of the computational calculation, the speed, and the computational resources of the coupled multiphysics solver are investigated in the framework of a large realistic geometry and complex reaction processes. It was determined that additional variables can be used to control large-area plasmas. Both configurations can form a plasma, that azimuthally moves in a controlled manner, the so-called “sweeping mode” (SM) or “polyphase mode” (PPM), and thus they have the potential for large-area and high-density plasma applications. The operation in the azimuthal mode has the potential to adjust the plasma distribution, the reaction chemistry, and increase or modulate the production of the radicals. The intrinsic asymmetry of the individual coils and their combined operation were investigated within a source assembly primarily in argon and CO gases. Limited investigations were also performed on operation in CH4 gas. The plasma parameters and the resulting chemistry are affected by the geometrical relation between individual antennas. The aim of this work is to incorporate the technological, computational, dimensional scaling, and reaction chemistry aspects of the plasma under one computational framework. The 3D simulation is utilized to geometrically scale up the reactive plasma that is produced by multiple ICP sources.

Imaging of Selenium by Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) in 2-D Electrophoresis Gels and Biological Tissues.

PubMed

Cruz, Elisa Castañeda Santa; Susanne Becker, J; Sabine Becker, J; Sussulini, Alessandra

2018-01-01

Selenium and selenoproteins are important components of living organisms that play a role in different biological processes. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is a powerful analytical technique that has been employed to obtain distribution maps of selenium in biological tissues in a direct manner, as well as in selenoproteins, previously separated by their molecular masses and isoelectric points using two-dimensional polyacrylamide gel electrophoresis (2-D PAGE). In this chapter, we present the protocols to perform LA-ICP-MS imaging experiments, allowing the distribution visualization and determination of selenium and/or selenoproteins in biological systems.

Quantitative aspects of inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Bulska, Ewa; Wagner, Barbara

2016-10-01

Accurate determination of elements in various kinds of samples is essential for many areas, including environmental science, medicine, as well as industry. Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful tool enabling multi-elemental analysis of numerous matrices with high sensitivity and good precision. Various calibration approaches can be used to perform accurate quantitative measurements by ICP-MS. They include the use of pure standards, matrix-matched standards, or relevant certified reference materials, assuring traceability of the reported results. This review critically evaluates the advantages and limitations of different calibration approaches, which are used in quantitative analyses by ICP-MS. Examples of such analyses are provided. This article is part of the themed issue 'Quantitative mass spectrometry'.

Statistical evaluation of an inductively coupled plasma atomic emission spectrometric method for routine water quality testing

USGS Publications Warehouse

Garbarino, J.R.; Jones, B.E.; Stein, G.P.

1985-01-01

In an interlaboratory test, inductively coupled plasma atomic emission spectrometry (ICP-AES) was compared with flame atomic absorption spectrometry and molecular absorption spectrophotometry for the determination of 17 major and trace elements in 100 filtered natural water samples. No unacceptable biases were detected. The analysis precision of ICP-AES was found to be equal to or better than alternative methods. Known-addition recovery experiments demonstrated that the ICP-AES determinations are accurate to between plus or minus 2 and plus or minus 10 percent; four-fifths of the tests yielded average recoveries of 95-105 percent, with an average relative standard deviation of about 5 percent.

Predictions of ion energy distributions and radical fluxes in radio frequency biased inductively coupled plasma etching reactors

NASA Astrophysics Data System (ADS)

Hoekstra, Robert J.; Kushner, Mark J.

1996-03-01

Inductively coupled plasma (ICP) reactors are being developed for low gas pressure (<10s mTorr) and high plasma density ([e]≳1011 cm-3) microelectronics fabrication. In these reactors, the plasma is generated by the inductively coupled electric field while an additional radio frequency (rf) bias is applied to the substrate. One of the goals of these systems is to independently control the magnitude of the ion flux by the inductively coupled power deposition, and the acceleration of ions into the substrate by the rf bias. In high plasma density reactors the width of the sheath above the wafer may be sufficiently thin that ions are able to traverse it in approximately 1 rf cycle, even at 13.56 MHz. As a consequence, the ion energy distribution (IED) may have a shape typically associated with lower frequency operation in conventional reactive ion etching tools. In this paper, we present results from a computer model for the IED incident on the wafer in ICP etching reactors. We find that in the parameter space of interest, the shape of the IED depends both on the amplitude of the rf bias and on the ICP power. The former quantity determines the average energy of the IED. The latter quantity controls the width of the sheath, the transit time of ions across the sheath and hence the width of the IED. In general, high ICP powers (thinner sheaths) produce wider IEDs.

Rapid and simple determination of selenium in blood serum by inductively coupled plasma-mass spectrometry (ICP-MS).

PubMed

Labat, L; Dehon, B; Lhermitte, M

2003-05-01

An inductively coupled plasma mass spectrometer (ICP-MS) with a rapid sample-preparative procedure was used for the determination of selenium in blood serum. Blood serum was prepared by dilution in an acidic solution consisting of nitric acid (1%), X-triton (0.1%) and 1-butanol (0.8%). A calibration curve was established for 1-40 microg mL(-1) (r(2)>0.99). The limit of detection was 0.5 microg mL(-1). Repeatability and intermediate precision were satisfactory with relative standard deviations (RSD) of 2.0% and 3.2%, respectively. This method was easily applied to reference materials with satisfactory accuracy. Good correlation (r(2)=0.96) was observed between ICP-MS and atomic absorption spectrometry (AAS) for the determination of (82)Se in blood serum from 23 patients. These results suggest that the sample preparative procedure coupled with ICP-MS can be used for the routine determination of (82)Se in human blood serum.

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

NASA Astrophysics Data System (ADS)

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

2009-06-01

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 São 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.

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

PubMed

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

2014-11-01

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

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

NASA Astrophysics Data System (ADS)

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%.

Capillary electrophoresis-high resolution sector field inductively coupled plasma mass spectrometry.

PubMed

Sonke, Jeroen E; Salters, Vincent J M

2007-08-03

The background and applications of high resolution sector field inductively coupled plasma mass spectrometry (HR-ICP-MS) as a detector for capillary (CE) and gel electrophoretic separations are reviewed. Notable progress has been made in the fields of bioinorganic and environmental (geo-) chemistry. Metallomics, the study of metal species interactions and functions in biological systems, puts substantial technical demands on speciation analysis. The combination of high species resolving power (CE) and high sensitivity-high mass resolving power (HR-ICP-MS) provides a solid base to meet such demands.

Quantitative aspects of inductively coupled plasma mass spectrometry

PubMed Central

Wagner, Barbara

2016-01-01

Accurate determination of elements in various kinds of samples is essential for many areas, including environmental science, medicine, as well as industry. Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful tool enabling multi-elemental analysis of numerous matrices with high sensitivity and good precision. Various calibration approaches can be used to perform accurate quantitative measurements by ICP-MS. They include the use of pure standards, matrix-matched standards, or relevant certified reference materials, assuring traceability of the reported results. This review critically evaluates the advantages and limitations of different calibration approaches, which are used in quantitative analyses by ICP-MS. Examples of such analyses are provided. This article is part of the themed issue ‘Quantitative mass spectrometry’. PMID:27644971

Inductively Coupled Plasma Mass Spectrometry (ICP-MS) Applications in Quantitative Proteomics.

PubMed

Chahrour, Osama; Malone, John

2017-01-01

Recent advances in inductively coupled plasma mass spectrometry (ICP-MS) hyphenated to different separation techniques have promoted it as a valuable tool in protein/peptide quantification. These emerging ICP-MS applications allow absolute quantification by measuring specific elemental responses. One approach quantifies elements already present in the structure of the target peptide (e.g. phosphorus and sulphur) as natural tags. Quantification of these natural tags allows the elucidation of the degree of protein phosphorylation in addition to absolute protein quantification. A separate approach is based on utilising bi-functional labelling substances (those containing ICP-MS detectable elements), that form a covalent chemical bond with the protein thus creating analogs which are detectable by ICP-MS. Based on the previously established stoichiometries of the labelling reagents, quantification can be achieved. This technique is very useful for the design of precise multiplexed quantitation schemes to address the challenges of biomarker screening and discovery. This review discusses the capabilities and different strategies to implement ICP-MS in the field of quantitative proteomics. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

External control of electron energy distributions in a dual tandem inductively coupled plasma

NASA Astrophysics Data System (ADS)

Liu, Lei; Sridhar, Shyam; Zhu, Weiye; Donnelly, Vincent M.; Economou, Demetre J.; Logue, Michael D.; Kushner, Mark J.

2015-08-01

The control of electron energy probability functions (EEPFs) in low pressure partially ionized plasmas is typically accomplished through the format of the applied power. For example, through the use of pulse power, the EEPF can be modulated to produce shapes not possible under continuous wave excitation. This technique uses internal control. In this paper, we discuss a method for external control of EEPFs by transport of electrons between separately powered inductively coupled plasmas (ICPs). The reactor incorporates dual ICP sources (main and auxiliary) in a tandem geometry whose plasma volumes are separated by a grid. The auxiliary ICP is continuously powered while the main ICP is pulsed. Langmuir probe measurements of the EEPFs during the afterglow of the main ICP suggests that transport of hot electrons from the auxiliary plasma provided what is effectively an external source of energetic electrons. The tail of the EEPF and bulk electron temperature were then elevated in the afterglow of the main ICP by this external source of power. Results from a computer simulation for the evolution of the EEPFs concur with measured trends.

Inductively coupled plasma mass spectrometry (ICP MS): a versatile tool.

PubMed

Ammann, Adrian A

2007-04-01

Inductively coupled plasma (ICP) mass spectrometry (MS) is routinely used in many diverse research fields such as earth, environmental, life and forensic sciences and in food, material, chemical, semiconductor and nuclear industries. The high ion density and the high temperature in a plasma provide an ideal atomizer and element ionizer for all types of samples and matrices introduced by a variety of specialized devices. Outstanding properties such as high sensitivity (ppt-ppq), relative salt tolerance, compound-independent element response and highest quantitation accuracy lead to the unchallenged performance of ICP MS in efficiently detecting, identifying and reliably quantifying trace elements. The increasing availability of relevant reference compounds and high separation selectivity extend the molecular identification capability of ICP MS hyphenated to species-specific separation techniques. While molecular ion source MS is specialized in determining the structure of unknown molecules, ICP MS is an efficient and highly sensitive tool for target-element orientated discoveries of relevant and unknown compounds. This special-feature, tutorial article presents the principle and advantages of ICP MS, highlighting these using examples from recently published investigations. Copyright 2007 John Wiley & Sons, Ltd.

Provenance establishment of coffee using solution ICP-MS and ICP-AES.

PubMed

Valentin, Jenna L; Watling, R John

2013-11-01

Statistical interpretation of the concentrations of 59 elements, determined using solution based inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma emission spectroscopy (ICP-AES), was used to establish the provenance of coffee samples from 15 countries across five continents. Data confirmed that the harvest year, degree of ripeness and whether the coffees were green or roasted had little effect on the elemental composition of the coffees. The application of linear discriminant analysis and principal component analysis of the elemental concentrations permitted up to 96.9% correct classification of the coffee samples according to their continent of origin. When samples from each continent were considered separately, up to 100% correct classification of coffee samples into their countries, and plantations of origin was achieved. This research demonstrates the potential of using elemental composition, in combination with statistical classification methods, for accurate provenance establishment of coffee. Copyright © 2013 Elsevier Ltd. All rights reserved.

Messenger RNA Detection in Leukemia Cell lines by Novel Metal-Tagged in situ Hybridization using Inductively Coupled Plasma Mass Spectrometry.

PubMed

Ornatsky, Olga I; Baranov, Vladimir I; Bandura, Dmitry R; Tanner, Scott D; Dick, John

2006-01-01

Conventional gene expression profiling relies on using fluorescent detection of hybridized probes. Physical characteristics of fluorophores impose limitations on achieving a highly multiplex gene analysis of single cells. Our work demonstrates the feasibility of using metal-tagged in situ hybridization for mRNA detection by inductively coupled plasma mass spectrometry (ICP-MS). ICP-MS as an analytical detector has a number of unique and relevant properties: 1) metals and their stable isotopes generate non-overlapping distinct signals that can be detected simultaneously; 2) these signals can be measured over a wide dynamic range; 3) ICP-MS is quantitative and very sensitive. We used commercial antibodies conjugated to europium (Eu) and gold together with biotinylated oligonucleotide probes reacted with terbium-labeled streptavidin to demonstrate simultaneous mRNA and protein detection by ICP-MS in leukemia cells.

Messenger RNA Detection in Leukemia Cell lines by Novel Metal-Tagged in situ Hybridization using Inductively Coupled Plasma Mass Spectrometry

PubMed Central

Ornatsky, Olga I.; Baranov, Vladimir I.; Bandura, Dmitry R.; Tanner, Scott D.; Dick, John

2006-01-01

Conventional gene expression profiling relies on using fluorescent detection of hybridized probes. Physical characteristics of fluorophores impose limitations on achieving a highly multiplex gene analysis of single cells. Our work demonstrates the feasibility of using metal-tagged in situ hybridization for mRNA detection by inductively coupled plasma mass spectrometry (ICP-MS). ICP-MS as an analytical detector has a number of unique and relevant properties: 1) metals and their stable isotopes generate non-overlapping distinct signals that can be detected simultaneously; 2) these signals can be measured over a wide dynamic range; 3) ICP-MS is quantitative and very sensitive. We used commercial antibodies conjugated to europium (Eu) and gold together with biotinylated oligonucleotide probes reacted with terbium-labeled streptavidin to demonstrate simultaneous mRNA and protein detection by ICP-MS in leukemia cells. PMID:23662035

Applications of inductively coupled plasma mass spectrometry and laser ablation inductively coupled plasma mass spectrometry in materials science

NASA Astrophysics Data System (ADS)

Becker, Johanna Sabine

2002-12-01

Inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS) have been applied as the most important inorganic mass spectrometric techniques having multielemental capability for the characterization of solid samples in materials science. ICP-MS is used for the sensitive determination of trace and ultratrace elements in digested solutions of solid samples or of process chemicals (ultrapure water, acids and organic solutions) for the semiconductor industry with detection limits down to sub-picogram per liter levels. Whereas ICP-MS on solid samples (e.g. high-purity ceramics) sometimes requires time-consuming sample preparation for its application in materials science, and the risk of contamination is a serious drawback, a fast, direct determination of trace elements in solid materials without any sample preparation by LA-ICP-MS is possible. The detection limits for the direct analysis of solid samples by LA-ICP-MS have been determined for many elements down to the nanogram per gram range. A deterioration of detection limits was observed for elements where interferences with polyatomic ions occur. The inherent interference problem can often be solved by applying a double-focusing sector field mass spectrometer at higher mass resolution or by collision-induced reactions of polyatomic ions with a collision gas using an ICP-MS fitted with collision cell. The main problem of LA-ICP-MS is quantification if no suitable standard reference materials with a similar matrix composition are available. The calibration problem in LA-ICP-MS can be solved using on-line solution-based calibration, and different procedures, such as external calibration and standard addition, have been discussed with respect to their application in materials science. The application of isotope dilution in solution-based calibration for trace metal determination in small amounts of noble metals has been developed as a new calibration strategy. This review discusses new analytical developments and possible applications of ICP-MS and LA-ICP-MS for the quantitative determination of trace elements and in surface analysis for materials science.

Elemental labelling combined with liquid chromatography inductively coupled plasma mass spectrometry for quantification of biomolecules: A review

PubMed Central

Kretschy, Daniela; Koellensperger, Gunda; Hann, Stephan

2012-01-01

This article reviews novel quantification concepts where elemental labelling is combined with flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS) or liquid chromatography inductively coupled plasma mass spectrometry (LC–ICP-MS), and employed for quantification of biomolecules such as proteins, peptides and related molecules in challenging sample matrices. In the first sections an overview on general aspects of biomolecule quantification, as well as of labelling will be presented emphasizing the potential, which lies in such methodological approaches. In this context, ICP-MS as detector provides high sensitivity, selectivity and robustness in biological samples and offers the capability for multiplexing and isotope dilution mass spectrometry (IDMS). Fundamental methodology of elemental labelling will be highlighted and analytical, as well as biomedical applications will be presented. A special focus will lie on established applications underlining benefits and bottlenecks of such approaches for the implementation in real life analysis. Key research made in this field will be summarized and a perspective for future developments including sophisticated and innovative applications will given. PMID:23062431

Liquid chromatography coupled with inductively coupled plasma mass spectrometry in the pharmaceutical industry: selected examples.

PubMed

Marshall, Peter S; Leavens, Bill; Heudi, Olivier; Ramirez-Molina, Cesar

2004-11-12

Both LC and capillary LC (CapLC) have been successfully interfaced with inductively coupled plasma mass spectrometry (ICP-MS). Gradients of acetonitrile and aqueous based solvents have been employed to separate several compounds of pharmaceutical interest. This paper will describe four application areas in the pharmaceutical industry, and examples will be shown where CapLC, LC and gel electrophoresis via laser ablation have been coupled with ICP-MS. The four areas highlighted in this paper are: (1) the use of derivatisation reactions to "make the invisible visible". Methods involving derivatisations with copper and iron will be described that can be used for the analysis of amines and carboxylic acids by ICP-MS. (2) The profiling of metal ion content (in particular bromine) in biological samples such as human plasma, this study will focus on the metabolism of bromine-labelled peptides (e.g. substance P). (3) The analysis of materials derived from single, solid-phase beads used in combinatorial chemistry, and (4) also discussed will be our findings from investigations into the use of laser ablation ICP-MS on the determination of protein phosphorylation on electrophoresis gel blots.

Analysis of Rare Earth Elements in Geologic Samples using Inductively Coupled Plasma Mass Spectrometry; US DOE Topical Report - DOE/NETL-2016/1794

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bank, Tracy L.; Roth, Elliot A.; Tinker, Phillip

2016-04-17

Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is used to measure the concentrations of rare earth elements (REE) in certified standard reference materials including shale and coal. The instrument used in this study is a Perkin Elmer Nexion 300D ICP-MS. The goal of the study is to identify sample preparation and operating conditions that optimized recovery of each element of concern. Additionally, the precision and accuracy of the technique are summarized and the drawbacks and limitations of the method are outlined.

Plasma characteristics of direct current enhanced cylindrical inductively coupled plasma source

NASA Astrophysics Data System (ADS)

Yue, HUA; Jian, SONG; Zeyu, HAO; Chunsheng, REN

2018-06-01

Experimental results of a direct current enhanced inductively coupled plasma (DCE-ICP) source which consists of a typical cylindrical ICP source and a plate-to-grid DC electrode are reported. With the use of this new source, the plasma characteristic parameters, namely, electron density, electron temperature and plasma uniformity, are measured by Langmuir floating double probe. It is found that DC discharge enhances the electron density and decreases the electron temperature, dramatically. Moreover, the plasma uniformity is obviously improved with the operation of DC and radio frequency (RF) hybrid discharge. Furthermore, the nonlinear enhancement effect of electron density with DC + RF hybrid discharge is confirmed. The presented observation indicates that the DCE-ICP source provides an effective method to obtain high-density uniform plasma, which is desirable for practical industrial applications.

Integrated approaches for reducing sample size for measurements of trace elemental impurities in plutonium by ICP-OES and ICP-MS

DOE PAGES

Xu, Ning; Chamberlin, Rebecca M.; Thompson, Pam; ...

2017-10-07

This study has demonstrated that bulk plutonium chemical analysis can be performed at small scales (\\50 mg material) through three case studies. Analytical methods were developed for ICP-OES and ICP-MS instruments to measure trace impurities and gallium content in plutonium metals with comparable or improved detection limits, measurement accuracy and precision. In two case studies, the sample size has been reduced by 109, and in the third case study, by as much as 50009, so that the plutonium chemical analysis can be performed in a facility rated for lower-hazard and lower-security operations.

Integrated approaches for reducing sample size for measurements of trace elemental impurities in plutonium by ICP-OES and ICP-MS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu, Ning; Chamberlin, Rebecca M.; Thompson, Pam

This study has demonstrated that bulk plutonium chemical analysis can be performed at small scales (\\50 mg material) through three case studies. Analytical methods were developed for ICP-OES and ICP-MS instruments to measure trace impurities and gallium content in plutonium metals with comparable or improved detection limits, measurement accuracy and precision. In two case studies, the sample size has been reduced by 109, and in the third case study, by as much as 50009, so that the plutonium chemical analysis can be performed in a facility rated for lower-hazard and lower-security operations.

Developments in ICP-MS: electrochemically modulated liquid chromatography for the clean-up of ICP-MS blanks and reduction of matrix effects by flow injection ICP-MS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gross, Cory Thomas

2008-01-01

The focus of this dissertation is the development of techniques with which to enhance the existing abilities of inductively coupled plasma mass spectrometry (ICP-MS). ICP-MS is a powerful technique for trace metal analysis in samples of many types, but like any technique it has certain strengths and weaknesses. Attempts are made to improve upon those strengths and to overcome certain weaknesses.

Profiles of non-essential trace elements in ewe and goat milk and their yoghurt, Torba yoghurt and whey.

PubMed

Sanal, Hasan; Güler, Zehra; Park, Young W

2011-01-01

The objectives of this study were to determine the profiles of non-essential trace elements in ewes' and goats' milk and manufactured products, such as yoghurt, torba yoghurt and whey, as well as changes in trace element content during Torba yoghurt-making processes. Concentrations of non-essential trace elements in ewe (Awassi) and goat (Damascus) milk and their yoghurt, torba yoghurt and whey were quantitatively determined by simultaneous inductively coupled plasma optical emission spectrometer (ICP-OES), after microwave digestion. Aluminium, antimony, arsenic, boron, beryllium, cadmium, nickel, lead, silver, titanium, thallium and vanadium were determined for both types of milk and their products. Barium was not detected in goats' milk or their products. Among all trace elements, boron was the most abundant and beryllium was least present in milk and the manufactured products. The results showed that goats' and ewes' milk and their manufactured products may be a source of 13 non-essential trace elements.

Lithium Oxysilicate Compounds Final Report.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Apblett, Christopher A.; Coyle, Jaclyn

In this study, the structure and composition of lithium silicate thin films deposited by RF magnetron co-sputtering is investigated. Five compositions ranging from Li2Si2O5 to Li8SiO6 were confirmed by inductively coupled plasma-optical emission spectroscopy (ICP-OES) and structure analysis on the evolution of non-bridging oxygens in the thin films was conducted with fourier transform infrared (FTIR) spectroscopy. It was found that non-bridging oxygens (NBOs) increased as the silicate network breaks apart with increasing lithium content which agrees with previous studies on lithium silicates. Thin film impurities were examined with x-ray photoelectron spectroscopy (XPS) and time of flight secondary ion mass spectroscopymore » (TOFSIMS) and traced back to target synthesis. This study utilizes a unique synthesis technique for lithium silicate thin films and can be referred to in future studies on the ionic conductivity of lithium silicates formed on the surface of silicon anodes in lithium ion batteries.« less

Prosopis pubescens (Screw bean mesquite) seedlings are hyper accumulators of copper

PubMed Central

Zappala, Marian N.; Ellzey, Joanne T.; Bader, Julia; Peralta-Videa, Jose R.; Gardea-Torresdey, Jorge

2013-01-01

Due to health reasons, toxic metals must be removed from soils contaminated by mine tailings and smelter activities. The phytoremediation potential of Prosopis pubescens (screw bean mesquite) was examined by use of inductively-coupled plasma spectroscopy (ICP-OES). Transmission electron microscopy (TEM) was used to observe ultrastructural changes of parenchymal cells of leaves in the presence of copper. Elemental analysis was utilized to localize copper within leaves. A 600 ppm copper sulfate exposure to seedlings for 24 days resulted in 31,000 ppm copper in roots, 17,000 ppm in stems, 11,000 in cotyledons and 20 ppm in the true leaves. In order for a plant to be considered a hyper accumulator, the plant must accumulate a leaf: root ratio of <1. Screw bean mesquite exposed to copper had a leaf: root ratios of 0.355 when cotyledons were included. We showed that Prosopis pubescens grown in soil is a hyper accumulator of copper. We recommend that this plant should be field tested. PMID:23612918

Heavy Metal Detoxification by Different Bacillus Species Isolated from Solar Salterns

PubMed Central

Syed, Shameer; Chinthala, Paramageetham

2015-01-01

The biosorption mechanism is an alternative for chemical precipitation and ultrafiltration which have been employed to treat heavy metal contamination with a limited success. In the present study, three species of Bacillus which were isolated from solar salterns were screened for their detoxification potential of the heavy metals, lead, chromium, and copper, by biosorption. Biosorption potential of each isolate was determined by Atomic Absorption Spectroscopy (AAS), Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES), and Energy Dispersive Spectroscopy (EDS) as the amount of metal present in the medium after the treatment with the isolates. Bacterial isolates, Bacillus licheniformis NSPA5, Bacillus cereus NSPA8, and Bacillus subtilis NSPA13, showed significant level of lead biosorption with maximum of 87–90% by Bacillus cereus NSPA8. The biosorption of copper and chromium was relatively low in comparison with lead. With the obtained results, we have concluded that the bacterial isolates are potential agents to treat metal contamination in more efficient and ecofriendly manner. PMID:26525498

Health and Risk Assessment by ICP-OES of Heavy Metals and Trace Minerals in Commercial Mushrooms Marketed in China.

PubMed

Huang, Mengyi; Zeng, Huansong; Xu, Baojun

2017-01-01

The objectives of this study were to investigate mineral profiles of 35 species of edible mushrooms collected in China; we compared nutritional values and tolerable values with the official recommended daily intakes (RDIs), maximum intake limits, and provisional tolerable weekly intakes. A total of 19 minerals were detected in edible mushrooms by inductively coupled plasma optical emission spectrometry. The results showed that the mushroom samples had a low percentage of RDI for the minerals calcium, iron, magnesium, manganese, zinc, potassium, and sodium and a relatively higher percentage of RDI for copper and molybdenum. The samples also had a very high percentage of RDI for chromium and selenium. The level of heavy metals in a majority of the mushrooms was above the limited level, and only concentrations of copper and zinc were safe in all mushrooms. In conclusion, the mushrooms collected in China are a good source of minerals such as molybdenum and selenium but are badly contaminated with aluminum, arsenic, cadmium, chromium, and lead.

Bioactivity evaluation of titanium/hydroxyapatite composite coating on stainless steel prepared by thermal spraying

NASA Astrophysics Data System (ADS)

Azhar, Nurul Humaira; Talari, Mahesh Kumar; Koong, Chue Keen

2015-08-01

In this study, titanium powder mixed with different wt % of HA was coated on stainless steel (SS) substrate using high velocity oxy-fuel (HVOF) technique to produce composite coating for biomedical applications. As the addition of HA is expected to influence the bioactivity of the coatings, these coatings were investigated for bioactivity by immersing the samples in a simulated body fluid (SBF) solution for 14 days. The apatite growth rate was evaluated by measuring Ca and P concentration in the SBF using Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). The concentrations of Ca and P have decreased over time in the SBF, suggesting a bone like apatite precipitation on the sample surface. It was observed that pH value increased with the increase of immersion time during initial three days and a subsequent drop after 7 days. Microstructure analysis done using FESEM technique showed nucleation and growth of bone-like apatite on the surface of the coating.

Copper-tolerant yeasts: Raman spectroscopy in determination of bioaccumulation mechanism.

PubMed

Radić, Danka S; Pavlović, Vera P; Lazović, Milana M; Jovičić-Petrović, Jelena P; Karličić, Vera M; Lalević, Blažo T; Raičević, Vera B

2017-09-01

Modern, efficient, and cost-effective approach to remediation of heavy metal-contaminated soil is based on the application of microorganisms. In this paper, four isolates from agricultural and urban contaminated soil showed abundant growth in the presence of copper(II) sulfate pentahydrate (CuSO 4 ·5H 2 O) up to 2 mM. Selected yeasts were identified by molecular methods as Candida tropicalis (three isolates) and Schwanniomyces occidentalis (one isolate). C. tropicalis (4TD1101S) showed the highest percentage of bioaccumulation capabilities (94.37%), determined by the inductively coupled plasma optical emission spectrometry (ICP-OES). The Raman spectra of C. tropicalis (4TD1101S) analyzed in a medium with the addition of 2 mM CuSO 4 ·5H 2 O showed certain increase in metallothionein production, which represents a specific response of the yeast species to the stress conditions. These results indicate that soil yeasts represent a potential for practical application in the bioremediation of contaminated environments.

Hydrothermal liquefaction of high- and low-lipid algae: Mass and energy balances.

PubMed

Cheng, Feng; Cui, Zheng; Mallick, Kwonit; Nirmalakhandan, Nagamany; Brewer, Catherine E

2018-06-01

Hydrothermal liquefaction (HTL) of high-lipid microalgae Nannochloropsis salina (N. salina) and low-lipid microalgae Galdieria sulphuraria (G. sulphuraria) were run under subcritical conditions (310-350 °C and 10-17 MPa) in a 1.8 L batch autoclave system. HTL mass and energy balances for both species were compared under different operating conditions to predict the optimum reaction conditions for new algae strains based on their feedstock composition. Bio-crude oils and chars were characterized by bomb calorimetry, elemental analysis, inductively coupled plasma optical emission spectrometry (ICP-OES), and thermogravimetric analysis (TGA). Under the optimized conditions, 59 wt% and 31 wt% bio-crude oil yields were obtained from HTL of N. salina and G. sulphuraria, while 85% and 59% of the feedstock energy were partitioned into N. salina-derived and G. sulphuraria-derived bio-crude oils, respectively. More favorable energy balances were related to shorter reaction times and higher algal solid contents. Copyright © 2018 Elsevier Ltd. All rights reserved.

Habit modification of bis-thiourea zinc chloride (ZTC) semi organic crystals by impurities

NASA Astrophysics Data System (ADS)

Ruby Nirmala, L.; Thomas Joseph Prakash, J.

2013-06-01

Single crystals of bis-thiourea zinc chloride (ZTC) doped with metal ion (Li+) possess excellent nonlinear optical properties. These crystals were grown by slow evaporation solution growth technique. The effect of Li+ dopant on the growth and properties of ZTC single crystal were investigated and reported. The grown crystals were crystallized in orthorhombic structure with non-centro symmetric space group Pn21a through the parent compound. The amount of dopant incorporated in the parent crystal was revealed by the inductively coupled plasma (ICP-OES) studies. The FT-IR spectroscopy study was done for finding and confirming the functional groups present in the compound. The UV-Visible spectral study was carried out to find the optical behavior and transparency nature of the grown crystal. TG/DTA measurements and Vickers microhardness measurements were traced to find out the thermal and mechanical stability of the grown crystals respectively. Using Nd:YAG laser, the Second harmonic generation (SHG) for the grown crystals were confirmed.

Habit modification of bis-thiourea zinc chloride (ZTC) semi organic crystals by impurities.

PubMed

Ruby Nirmala, L; Thomas Joseph Prakash, J

2013-06-01

Single crystals of bis-thiourea zinc chloride (ZTC) doped with metal ion (Li(+)) possess excellent nonlinear optical properties. These crystals were grown by slow evaporation solution growth technique. The effect of Li(+) dopant on the growth and properties of ZTC single crystal were investigated and reported. The grown crystals were crystallized in orthorhombic structure with non-centro symmetric space group Pn21a through the parent compound. The amount of dopant incorporated in the parent crystal was revealed by the inductively coupled plasma (ICP-OES) studies. The FT-IR spectroscopy study was done for finding and confirming the functional groups present in the compound. The UV-Visible spectral study was carried out to find the optical behavior and transparency nature of the grown crystal. TG/DTA measurements and Vickers microhardness measurements were traced to find out the thermal and mechanical stability of the grown crystals respectively. Using Nd:YAG laser, the Second harmonic generation (SHG) for the grown crystals were confirmed. Copyright © 2013 Elsevier B.V. All rights reserved.

Fabrication and characterization of iron oxide ceramic membranes for arsenic removal.

PubMed

Sabbatini, P; Yrazu, F; Rossi, F; Thern, G; Marajofsky, A; Fidalgo de Cortalezzi, M M

2010-11-01

Nanoscale iron oxide particles were synthesized and deposited on porous alumina tubes to develop tubular ceramic adsorbers for the removal of arsenic, which is an extremely toxic contaminant even in very low concentrations. Its natural presence affects rural and low-income populations in developing countries in Latin America and around the world, which makes it essential to develop a user-friendly, low energy demanding and low cost treatment technology. The fabricated ceramic membranes can be operated with minimal trans-membrane pressure difference and do not require pumping. The support tubes and final membrane have been characterized by surface area and porosity measurements, permeability tests and scanning electron microscopy (SEM) imaging. Arsenic concentrations were determined by inductively coupled plasma-optical emission spectroscopy (ICP-OES). Due to its low cost and simple operation, the system can be applied as a point of use device for the treatment of arsenic contaminated groundwaters in developing countries. Copyright © 2010 Elsevier Ltd. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2016-08-01

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

Use of a parallel path nebulizer for capillary-based microseparation techniques coupled with an inductively coupled plasma mass spectrometer for speciation measurements

NASA Astrophysics Data System (ADS)

Yanes, Enrique G.; Miller-Ihli, Nancy J.

2004-06-01

A low flow, parallel path Mira Mist CE nebulizer designed for capillary electrophoresis (CE) was evaluated as a function of make-up solution flow rate, composition, and concentration, as well as the nebulizer gas flow rate. This research was conducted in support of a project related to the separation and quantification of cobalamin (vitamin B-12) species using microseparation techniques combined with inductively coupled plasma mass spectrometry (ICP-MS) detection. As such, Co signals were monitored during the nebulizer characterization process. Transient effects in the ICP were studied to evaluate the suitability of using gradients for microseparations and the benefit of using methanol for the make-up solution was demonstrated. Co signal response changed significantly as a function of changing methanol concentrations of the make-up solution and maximum signal enhancement was seen at 20% methanol with a 15 μl/min flow rate. Evaluation of the effect of changing the nebulizer gas flow rates showed that argon flows from 0.8 to 1.2 l/min were equally effective. The Mira Mist CE parallel path nebulizer was then evaluated for interfacing capillary microseparation techniques including capillary electrophoresis (CE) and micro high performance liquid chromatography (μHPLC) to inductively coupled plasma mass spectrometry (ICP-MS). A mixture of four cobalamin species standards (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5' deoxyadenosylcobalamin) and the corrinoid analogue cobinamide dicyanide were successfully separated using both CE-ICP-MS and μHPLC-ICP-MS using the parallel path nebulizer with a make-up solution containing 20% methanol with a flow rate of 15 μl/min.

Multivariate classification of edible salts: Simultaneous Laser-Induced Breakdown Spectroscopy and Laser-Ablation Inductively Coupled Plasma Mass Spectrometry Analysis

NASA Astrophysics Data System (ADS)

Lee, Yonghoon; Nam, Sang-Ho; Ham, Kyung-Sik; Gonzalez, Jhanis; Oropeza, Dayana; Quarles, Derrick; Yoo, Jonghyun; Russo, Richard E.

2016-04-01

Laser-Induced Breakdown Spectroscopy (LIBS) and Laser-Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS), both based on laser ablation sampling, can be employed simultaneously to obtain different chemical fingerprints from a sample. We demonstrated that this analysis approach can provide complementary information for improved classification of edible salts. LIBS could detect several of the minor metallic elements along with Na and Cl, while LA-ICP-MS spectra were used to measure non-metallic and trace heavy metal elements. Principal component analysis using LIBS and LA-ICP-MS spectra showed that their major spectral variations classified the sample salts in different ways. Three classification models were developed by using partial least squares-discriminant analysis based on the LIBS, LA-ICP-MS, and their fused data. From the cross-validation performances and confusion matrices of these models, the minor metallic elements (Mg, Ca, and K) detected by LIBS and the non-metallic (I) and trace heavy metal (Ba, W, and Pb) elements detected by LA-ICP-MS provided complementary chemical information to distinguish particular salt samples.

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

USGS Publications Warehouse

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

1984-01-01

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

Optoelectronic properties of Black-Silicon generated through inductively coupled plasma (ICP) processing for crystalline silicon solar cells

NASA Astrophysics Data System (ADS)

Hirsch, Jens; Gaudig, Maria; Bernhard, Norbert; Lausch, Dominik

2016-06-01

The optoelectronic properties of maskless inductively coupled plasma (ICP) generated black silicon through SF6 and O2 are analyzed by using reflection measurements, scanning electron microscopy (SEM) and quasi steady state photoconductivity (QSSPC). The results are discussed and compared to capacitively coupled plasma (CCP) and industrial standard wet chemical textures. The ICP process forms parabolic like surface structures in a scale of 500 nm. This surface structure reduces the average hemispherical reflection between 300 and 1120 nm up to 8%. Additionally, the ICP texture shows a weak increase of the hemispherical reflection under tilted angles of incidence up to 60°. Furthermore, we report that the ICP process is independent of the crystal orientation and the surface roughness. This allows the texturing of monocrystalline, multicrystalline and kerf-less wafers using the same parameter set. The ICP generation of black silicon does not apply a self-bias on the silicon sample. Therefore, the silicon sample is exposed to a reduced ion bombardment, which reduces the plasma induced surface damage. This leads to an enhancement of the effective charge carrier lifetime up to 2.5 ms at 1015 cm-3 minority carrier density (MCD) after an atomic layer deposition (ALD) with Al2O3. Since excellent etch results were obtained already after 4 min process time, we conclude that the ICP generation of black silicon is a promising technique to substitute the industrial state of the art wet chemical textures in the solar cell mass production.

Matrix effects in inductively coupled plasma mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Xiaoshan

1995-07-07

The inductively coupled plasma is an electrodeless discharge in a gas (usually Ar) at atmospheric pressure. Radio frequency energy generated by a RF power source is inductively coupled to the plasma gas through a water cooled load coil. In ICP-MS the "Fassel" TAX quartz torch commonly used in emission is mounted horizontally. The sample aerosol is introduced into the central flow, where the gas kinetic temperature is about 5000 K. The aerosol is vaporized, atomized, excited and ionized in the plasma, and the ions are subsequently extracted through two metal apertures (sampler and skimmer) into the mass spectrometer. In ICP-MS,more » the matrix effects, or non-spectroscopic interferences, can be defined as the type of interferences caused by dissolved concomitant salt ions in the solution. Matrix effects can be divided into two categories: (1) signal drift due to the deposition of solids on the sampling apertures; and/or (2) signal suppression or enhancement by the presence of the dissolved salts. The first category is now reasonably understood. The dissolved salts, especially refractory oxides, tend to deposit on the cool tip of the sampling cone. The clogging of the orifices reduces the ion flow into the ICP-MS, lowers the pressure in the first stage of ICP-MS, and enhances the level of metal oxide ions. Because the extent of the clogging increases with the time, the signal drifts down. Even at the very early stage of the development of ICP-MS, matrix effects had been observed. Houk et al. found out that the ICP-MS was not tolerant to solutions containing significant amounts of dissolved solids.« less

A study of GaN-based LED structure etching using inductively coupled plasma

NASA Astrophysics Data System (ADS)

Wang, Pei; Cao, Bin; Gan, Zhiyin; Liu, Sheng

2011-02-01

GaN as a wide band gap semiconductor has been employed to fabricate optoelectronic devices such as light-emitting diodes (LEDs) and laser diodes (LDs). Recently several different dry etching techniques for GaN-based materials have been developed. ICP etching is attractive because of its superior plasma uniformity and strong controllability. Most previous reports emphasized on the ICP etching characteristics of single GaN film. In this study dry etching of GaN-based LED structure was performed by inductively coupled plasmas (ICP) etching with Cl2 as the base gas and BCl3 as the additive gas. The effects of the key process parameters such as etching gases flow rate, ICP power, RF power and chamber pressure on the etching properties of GaN-based LED structure including etching rate, selectivity, etched surface morphology and sidewall was investigated. Etch depths were measured using a depth profilometer and used to calculate the etch rates. The etch profiles were observed with a scanning electron microscope (SEM).

Ultra-Shallow Depth Profiling of Arsenic Implants in Silicon by Hydride Generation-Inductively Coupled Plasma Atomic Emission Spectrometry

NASA Astrophysics Data System (ADS)

Matsubara, Atsuko; Kojima, Hisao; Itoga, Toshihiko; Kanehori, Keiichi

1995-08-01

High resolution depth profiling of arsenic (As) implanted into silicon wafers by a chemical technique is described. Silicon wafers are precisely etched through repeated oxidation by hydrogen peroxide solution and dissolution of the oxide by hydrofluoric acid solution. The etched silicon thickness is determined by inductively-coupled plasma atomic emission spectrometry (ICP-AES). Arsenic concentration is determined by hydride generation ICP-AES (HG-ICP-AES) with prereduction using potassium iodide. The detection limit of As in a 4-inch silicon wafer is 2.4×1018 atoms/cm3. The etched silicon thickness is controlled to less than 4±2 atomic layers. Depth profiling of an ultra-shallow As diffusion layer with the proposed method shows good agreement with profiling using the four-probe method or secondary ion mass spectrometry.

Conditions of Mytilus edulis extracellular body fluids and shell composition in a pH-treatment experiment: Acid-base status, trace elements and δ11B

NASA Astrophysics Data System (ADS)

Heinemann, Agnes; Fietzke, Jan; Melzner, Frank; BöHm, Florian; Thomsen, JöRn; Garbe-SchöNberg, Dieter; Eisenhauer, Anton

2012-01-01

Mytilus edulis were cultured for 3 months under six different seawater pCO2 levels ranging from 380 to 4000 μatm. Specimen were taken from Kiel Fjord (Western Baltic Sea, Germany) which is a habitat with high and variable seawater pCO2 and related shifts in carbonate system speciation (e.g., low pH and low CaCO3 saturation state). Hemolymph (HL) and extrapallial fluid (EPF) samples were analyzed for pH and total dissolved inorganic carbon (CT) to calculate pCO2 and [HCO3-]. A second experiment was conducted for 2 months with three different pCO2 levels (380, 1400 and 4000 μatm). Boron isotopes (δ11B) were investigated by LA-MC-ICP-MS (Laser Ablation-Multicollector-Inductively Coupled Plasma-Mass Spectrometry) in shell portions precipitated during experimental treatment time. Additionally, elemental ratios (B/Ca, Mg/Ca and Sr/Ca) in the EPF of specimen from the second experiment were measured via ICP-OES (Inductively Coupled Plasma-Optical Emission Spectrometry). Extracellular pH was not significantly different in HL and EPF but systematically lower than ambient water pH. This is due to high extracellular pCO2 values, a prerequisite for metabolic CO2 excretion. No accumulation of extracellular [HCO3-] was measured. Elemental ratios (B/Ca, Mg/Ca and Sr/Ca) in the EPF increased slightly with pH which is in accordance with increasing growth and calcification rates at higher seawater pH values. Boron isotope ratios were highly variable between different individuals but also within single shells. This corresponds to a high individual variability in fluid B/Ca ratios and may be due to high boron concentrations in the organic parts of the shell. The mean δ11B value shows no trend with pH but appears to represent internal pH (EPF) rather than ambient water pH.

Composition of Atmospheric Dust from Qatar in the Arabian Gulf

NASA Astrophysics Data System (ADS)

Yigiterhan, O.; Al-Ansari, I. S.; Abdel-Moati, M.; Al-Ansi, M.; Paul, B.; Nelson, A.; Turner, J.; Murray, J. W.; Alfoldy, B. Z.; Mahfouz, M. M. K.; Giamberini, M.

2015-12-01

Samples of atmospheric dust from Qatar have been collected and analyzed for major and trace elemental composition. Twenty-one samples were collected in 2014 and 2015 from Doha, Al Khor, Katara, Sealine, and Al Waab by a variety of techniques. Some samples were collected during the megastorms that occurred in April 2015. Back trajectories were determined for each sample using the NOAA HYSPLIT model over a 50 hour time interval. Our samples were about equally divided between northerly (n=12; northern Saudi Arabia, Kuwait or Iraq) and southerly (n=8; SE Saudi Arabia, United Arab Emirates and Oman) sources. One sample originated directly westward, in Saudi Arabia. Samples were microwave-assisted total acid digested (HF+HCl+HNO3) and analyzed by inductively coupled plasma-mass spectroscopy (ICP-MS) and inductively coupled plasma-optical emission spectroscopy (ICP-OES). There are only 12 out of 23 elements for which the Qatari dust was enriched relative to upper continental crust (UCC). Calcium was especially enriched at 400% relative to UCC. About 33% of the total sample mass was CaCO3, reflecting the composition of surface rocks in the source areas. Of the elements typically associated with anthropogenic activity, Ag, Ni and Zn were the most enriched relative to UCC, with enrichment factors of 182%, 233% and 209%, respectively. Others like Pb and V were not significantly enriched, with enrichment factors of 25% and 3%, respectively. The major elements Al, Mn and Fe were depleted relative to UCC because of the strong enrichment in CaCO3, with enrichment factors of -58%, -35% and -45% respectively. We separately averaged the samples with northern and southern origins to see if composition could be used to identify source. Only three elements had a statistical difference. Pb and Na were higher in the samples from the Se while Cr was higher in those from the north.

Laser ablation inductively coupled plasma mass spectrometry for direct isotope ratio measurements on solid samples

NASA Astrophysics Data System (ADS)

Pickhardt, Carola; Dietze, Hans-Joachim; Becker, J. Sabine

2005-04-01

Isotope ratio measurements have been increasingly used in quite different application fields, e.g., for the investigation of isotope variation in nature, in geoscience (geochemistry and geochronology), in cosmochemistry and planetary science, in environmental science, e.g., in environmental monitoring, or by the application of the isotope dilution technique for quantification purposes using stable or radioactive high-enriched isotope tracers. Due to its high sensitivity, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is today a challenging mass spectrometric technique for the direct determination of precise and accurate isotope ratios in solid samples. In comparison to laser ablation quadrupole ICP-MS (LA-ICP-QMS), laser ablation coupled to a double-focusing sector field ICP-MS (LA-ICP-SFMS) with single ion detection offers a significant improvement of sensitivity at low mass resolution, whereby isotope ratios can be measured with a precision to 0.1% relative standard deviation (R.S.D.). In LA-ICP-SFMS, many disturbing isobaric interferences of analyte and molecular ions can be separated at the required mass resolution (e.g., 40Ar16O+ and 56Fe+ for iron isotope ratio measurements). The precision on isotope ratio measurements was improved by one order of magnitude via the simultaneous detection of mass-separated ion currents of isotopes using multiple ion collectors in LA-ICP-MS (LA-MC-ICP-MS). The paper discusses the state of the art, the challenges and limits in isotope ratio measurements by LA-ICP-MS using different instrumentations at the trace and ultratrace level in different fields of application as in environmental and biological research, geochemistry and geochronology with respect to their precision and accuracy.

Application of isotope dilution inductively coupled plasma mass spectrometry to the analysis of marine sediments

DOE Office of Scientific and Technical Information (OSTI.GOV)

McLaren, J.W.; Beauchemin, D.; Berman, S.S.

1987-02-15

Isotope dilution inductively coupled plasma mass spectrometry (ICP-MS) has been applied to the determination of 11 trace elements (Cr, Ni, Zn, Sr, Mo, Cd, Sn, Sb, Tl, Pb, and U) in the marine sediment reference materials MESS-1 and BCSS-1. Accuracy and, especially, precision are better than those that can be easily achieved by other ICP-MS calibration strategies, as long as isotopic equilibration is achieved and the isotopes used for the ratio measurement are free of isobaric interferences by molecular species. The measurement of the isotope ratios on unspiked samples provides a sensitive diagnostic of such interferences.

A concise guide for the determination of less-studied technology-critical elements (Nb, Ta, Ga, In, Ge, Te) by inductively coupled plasma mass spectrometry in environmental samples

NASA Astrophysics Data System (ADS)

Filella, Montserrat; Rodushkin, Ilia

2018-03-01

There is an increasing demand for analytical techniques able to measure so-called 'technology-critical elements', a set of chemical elements increasingly used in technological applications, in environmental matrices. Nowadays, inductively coupled plasma-mass spectrometry (ICP-MS) has become the technique of choice for measuring trace element concentrations. However, its application is often less straightforward than often assumed. The hints and drawbacks of ICP-MS application to the measurement of a set of less-studied technology-critical elements (Nb, Ta, Ga, In, Ge and Te) is discussed here and concise guidelines given.

Elimination of boron memory effect in inductively coupled plasma-mass spectrometry by ammonia gas injection into the spray chamber during analysis

NASA Astrophysics Data System (ADS)

Al-Ammar, Assad S.; Gupta, Rajesh K.; Barnes, Ramon M.

2000-06-01

Injection of 10-20 ml/min of ammonia gas into an inductively coupled plasma-mass spectrometry (ICP-MS) spray chamber during boron determination eliminates the memory effect of a 1 μg/ml B solution within a 2-min washing time. Ammonia gas injection also reduces the boron blank by a factor of four and enhances the sensitivity by 33-90%. Boron detection limits are improved from 12 and 14 to 3 and 4 ng/ml, respectively, for two ICP-MS instruments. Trace boron concentrations in certified reference materials agree well using ammonia gas injection.

Si-compatible cleaning process for graphene using low-density inductively coupled plasma.

PubMed

Lim, Yeong-Dae; Lee, Dae-Yeong; Shen, Tian-Zi; Ra, Chang-Ho; Choi, Jae-Young; Yoo, Won Jong

2012-05-22

We report a novel cleaning technique for few-layer graphene (FLG) by using inductively coupled plasma (ICP) of Ar with an extremely low plasma density of 3.5 × 10(8) cm(-3). It is known that conventional capacitively coupled plasma (CCP) treatments destroy the planar symmetry of FLG, giving rise to the generation of defects. However, ICP treatment with extremely low plasma density is able to remove polymer resist residues from FLG within 3 min at a room temperature of 300 K while retaining the carbon sp(2)-bonding of FLG. It is found that the carrier mobility and charge neutrality point of FLG are restored to their pristine defect-free state after the ICP treatment. Considering the application of graphene to silicon-based electronic devices, such a cleaning method can replace thermal vacuum annealing, electrical current annealing, and wet-chemical treatment due to its advantages of being a low-temperature, large-area, high-throughput, and Si-compatible process.

Inductively coupled plasma mass spectrometry and electrospray mass spectrometry for speciation analysis: applications and instrumentation

NASA Astrophysics Data System (ADS)

Rosen, Amy L.; Hieftje, Gary M.

2004-02-01

To gain an understanding of the function, toxicity and distribution of trace elements, it is necessary to determine not only the presence and concentration of the elements of interest, but also their speciation, by identifying and characterizing the compounds within which each is present. For sensitive detection of compounds containing elements of interest, inductively coupled plasma mass spectrometry (ICP-MS) is a popular method, and for identification of compounds via determination of molecular weight, electrospray ionization mass spectrometry (ESI-MS) is gaining increasing use. ICP-MS and ESI-MS, usually coupled to a separation technique such as chromatography or capillary electrophoresis, have already been applied to a large number of research problems in such diverse fields as environmental chemistry, nutritional science, and bioinorganic chemistry, but a great deal of work remains to be completed. Current areas of research to which ICP-MS and ESI-MS have been applied are discussed, and the existing instrumentation used to solve speciation problems is described.

Improving catchment scale water quality modelling with continuous high resolution monitoring of metals in runoff

NASA Astrophysics Data System (ADS)

Saari, Markus; Rossi, Pekka; Blomberg von der Geest, Kalle; Mäkinen, Ari; Postila, Heini; Marttila, Hannu

2017-04-01

High metal concentrations in natural waters is one of the key environmental and health problems globally. Continuous in-situ analysis of metals from runoff water is technically challenging but essential for the better understanding of processes which lead to pollutant transport. Currently, typical analytical methods for monitoring elements in liquids are off-line laboratory methods such as ICP-OES (Inductively Coupled Plasma Optical Emission Spectroscopy) and ICP-MS (ICP combined with a mass spectrometer). Disadvantage of the both techniques is time consuming sample collection, preparation, and off-line analysis at laboratory conditions. Thus use of these techniques lack possibility for real-time monitoring of element transport. We combined a novel high resolution on-line metal concentration monitoring with catchment scale physical hydrological modelling in Mustijoki river in Southern Finland in order to study dynamics of processes and form a predictive warning system for leaching of metals. A novel on-line measurement technique based on micro plasma emission spectroscopy (MPES) is tested for on-line detection of selected elements (e.g. Na, Mg, Al, K, Ca, Fe, Ni, Cu, Cd and Pb) in runoff waters. The preliminary results indicate that MPES can sufficiently detect and monitor metal concentrations from river water. Water and Soil Assessment Tool (SWAT) catchment scale model was further calibrated with high resolution metal concentration data. We show that by combining high resolution monitoring and catchment scale physical based modelling, further process studies and creation of early warning systems, for example to optimization of drinking water uptake from rivers, can be achieved.

Rhenium Solubility in Borosilicate Nuclear Waste Glass: Implications for the Processing and Immobilization of Technetium-99

DOE Office of Scientific and Technical Information (OSTI.GOV)

McCloy, John S.; Riley, Brian J.; Goel, Ashutosh

2012-10-26

The immobilization of 99Tc in a suitable host matrix has proved to be an arduous task for the researchers in nuclear waste community around the world. At the Hanford site in Washington State, the total amount of 99Tc in low-activity waste (LAW) is ~1300 kg and the current strategy is to immobilize the 99Tc in borosilicate glass with vitrification. In this context, the present article reports on the solubility/retention of rhenium, a nonradioactive surrogate for 99Tc, in a LAW borosilicate glass. Due to the radioactive nature of technetium, rhenium was chosen as a simulant because of the similarity between theirmore » ionic radii and other chemical aspects. The glasses containing Re (0 – 10,000 ppm by mass) were synthesized in vacuum-sealed quartz ampoules in order to minimize the loss of Re by volatilization during melting at 1000 °C. The rhenium was found to predominantly exist as Re (VII) in all the glasses as observed by X-ray absorption near-edge structure (XANES). The solubility of Re in borosilicate glasses was determined to be ~3000 ppm (by mass) with inductively coupled plasma-optical emission spectroscopy (ICP-OES). At higher rhenium concentrations, some additional material was retained in the glasses in the form of crystalline inclusions that were detected by X-ray diffraction (XRD) and laser ablation-ICP mass spectrometry (LA-ICP-MS). The implications of these results on the immobilization of 99Tc from radioactive wastes in borosilicate glasses have been discussed.« less

THE DEVELOPMENT OF IODINE BASED IMPINGER SOLUTIONS FOR THE EFFICIENT CAPTURE OF HG USING DIRECT INJECTION NEBULIZATION - INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY ANALYSIS

EPA Science Inventory

Inductively coupled plasma mass spectrometry (ICP/MS) with direct injection nebulization (DIN) was used to evaluate novel impinger solution compositions capable of capturing elemental mercury (Hgo) in EPA Method 5 type sampling. An iodine based impinger solutoin proved to be ver...

Bioimaging of metallothioneins in ocular tissue sections by laser ablation-ICP-MS using bioconjugated gold nanoclusters as specific tags.

PubMed

Cruz-Alonso, María; Fernandez, Beatriz; Álvarez, Lydia; González-Iglesias, Héctor; Traub, Heike; Jakubowski, Norbert; Pereiro, Rosario

2017-12-18

An immunohistochemical method is described to visualize the distribution of metallothioneins 1/2 (MT 1/2) and metallothionein 3 (MT 3) in human ocular tissue. It is making use of (a) antibodies conjugated to gold nanoclusters (AuNCs) acting as labels, and (b) laser ablation (LA) coupled to inductively coupled plasma - mass spectrometry (ICP-MS). Water-soluble fluorescent AuNCs (with an average size of 2.7 nm) were synthesized and then conjugated to antibody by carbodiimide coupling. The surface of the modified AuNCs was then blocked with hydroxylamine to avoid nonspecific interactions with biological tissue. Immunoassays for MT 1/2 and MT 3 in ocular tissue sections (5 μm thick) from two post mortem human donors were performed. Imaging studies were then performed by fluorescence using confocal microscopy, and LA-ICP-MS was performed in the retina to measure the signal for gold. Signal amplification by the >500 gold atoms in each nanocluster allowed the antigens (MT 1/2 and MT 3) to be imaged by LA-ICP-MS using a laser spot size as small as 4 μm. The image patterns found in retina are in good agreement with those obtained by conventional fluorescence immunohistochemistry which was used as an established reference method. Graphical abstract Gold nanoclusters (AuNCs) conjugated to a primary specific antibody serve as a label for amplified bioimaging of metallothioneins (MTs) by laser ablation coupled to inductively coupled plasma - mass spectrometry (ICP-MS) in human ocular tissue sections.

Evaluation of Hydrodynamic Chromatography Coupled with UV-Visible, Fluorescence and Inductively Coupled Plasma Mass Spectrometry Detectors for Sizing and Quantifying Colloids in Environmental Media

PubMed Central

Philippe, Allan; Schaumann, Gabriele E.

2014-01-01

In this study, we evaluated hydrodynamic chromatography (HDC) coupled with inductively coupled plasma mass spectrometry (ICP-MS) for the analysis of nanoparticles in environmental samples. Using two commercially available columns (Polymer Labs-PDSA type 1 and 2), a set of well characterised calibrants and a new external time marking method, we showed that flow rate and eluent composition have few influence on the size resolution and, therefore, can be adapted to the sample particularity. Monitoring the agglomeration of polystyrene nanoparticles over time succeeded without observable disagglomeration suggesting that even weak agglomerates can be measured using HDC. Simultaneous determination of gold colloid concentration and size using ICP-MS detection was validated for elemental concentrations in the ppb range. HDC-ICP-MS was successfully applied to samples containing a high organic and ionic background. Indeed, online combination of UV-visible, fluorescence and ICP-MS detectors allowed distinguishing between organic molecules and inorganic colloids during the analysis of Ag nanoparticles in synthetic surface waters and TiO2 and ZnO nanoparticles in commercial sunscreens. Taken together, our results demonstrate that HDC-ICP-MS is a flexible, sensitive and reliable method to measure the size and the concentration of inorganic colloids in complex media and suggest that there may be a promising future for the application of HDC in environmental science. Nonetheless the rigorous measurements of agglomerates and of matrices containing natural colloids still need to be studied in detail. PMID:24587393

Evaluation of hydrodynamic chromatography coupled with UV-visible, fluorescence and inductively coupled plasma mass spectrometry detectors for sizing and quantifying colloids in environmental media.

PubMed

Philippe, Allan; Schaumann, Gabriele E

2014-01-01

In this study, we evaluated hydrodynamic chromatography (HDC) coupled with inductively coupled plasma mass spectrometry (ICP-MS) for the analysis of nanoparticles in environmental samples. Using two commercially available columns (Polymer Labs-PDSA type 1 and 2), a set of well characterised calibrants and a new external time marking method, we showed that flow rate and eluent composition have few influence on the size resolution and, therefore, can be adapted to the sample particularity. Monitoring the agglomeration of polystyrene nanoparticles over time succeeded without observable disagglomeration suggesting that even weak agglomerates can be measured using HDC. Simultaneous determination of gold colloid concentration and size using ICP-MS detection was validated for elemental concentrations in the ppb range. HDC-ICP-MS was successfully applied to samples containing a high organic and ionic background. Indeed, online combination of UV-visible, fluorescence and ICP-MS detectors allowed distinguishing between organic molecules and inorganic colloids during the analysis of Ag nanoparticles in synthetic surface waters and TiO₂ and ZnO nanoparticles in commercial sunscreens. Taken together, our results demonstrate that HDC-ICP-MS is a flexible, sensitive and reliable method to measure the size and the concentration of inorganic colloids in complex media and suggest that there may be a promising future for the application of HDC in environmental science. Nonetheless the rigorous measurements of agglomerates and of matrices containing natural colloids still need to be studied in detail.

Iron levels change in larval Heliothis virescens tissues following baculovirus infection

USDA-ARS?s Scientific Manuscript database

Inductively-coupled plasma mass spectrometry (ICP-MS) and 59Fe radiotracers were used to investigate changes in levels of iron (Fe) in the tissues of Heliothis virescens following baculovirus infection. Fe concentrations were determined by ICP-MS in hemolymph collected from 4th instar larvae infect...

Metal dispersion and transportational activities using food crops as biomonitors.

PubMed

Ward, N I; Savage, J M

1994-05-23

The multielement (Al, Ca, Cd, Ce, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Si, and Zn) levels of various common vegetables (bean, broccoli, cabbage, cauliflower, lettuce, marrow, onion, parsnip, spinach, sprouts, sweet corn, and tomato); fruits (grape and strawberry); herbs (garlic, lemon balm, marjoram, mint, rosemary and tarragon); local pasture species and surface soils collected from a commercial garden centre located within a distance of 30 m of the London Orbital Motorway (M25) is presented. Comparative values are given from a background area, namely a domestic garden located in the North Yorkshire Dales National Park area. Analysis was undertaken by inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma-source mass spectrometry (ICP-MS) with quality control assessment using four international biological reference materials; BCR:CRM 62 Olive Leaves, NIST 1575 Pine Needles, NIST 1573 Tomato Leaves, and NIST 1572 Citrus Leaves. Inter-analytical method comparison is given using two methods of ICP-MS; namely conventional pneumatic nebulisation of sample solution, and direct solids analysis by laser ablation; and neutron activation analysis methods (NAA). For the elements listed there is a good precision obtained by ICP-MS and NAA. In particular levels of < +/- 1-10% (rsd) are obtained. Comparison of data with certified values and other analytical methods are generally of very good agreement. Lead levels in background areas ranged from 0.0008 to 0.340 microgram/g (fresh weight) for plant material; with the lead magnitude greater for grasses > herbs > vegetables > cereals > fruits. Measured values are in good agreement with reported literature values. The lowest Pb values are for marrow, lettuce, tomato and sweet corn samples (approximately 0.001-0.021 microgram/g). 'Green' leaf material levels were approximately 0.02-0.10 microgram/g (i.e. sprouts and cabbage). Root vegetables contain higher levels, approximately 0.02-0.125 microgram/g (especially carrot), reflecting possible metal uptake from soil. The highest vegetable Pb values are for leek and onion (approximately 0.35 microgram/g). Background values are also provided for nineteen elements (Al, As, B, Ba, Br, Cd, Co, Cr, Cu, Fe, Li, Mn, Mo, Ni, Rb, Se, Sr, V, and Zn). Exposure to motor vehicle activities at a site some 30 m from the M25 shows only significant increases in Pb for unwashed plant material and surface soils. Typically Pb levels of 40-80% can be removed by washing plant surfaces resulting in metal levels similar to background areas.(ABSTRACT TRUNCATED AT 400 WORDS)

Characterization of Nanomaterials Using Field Flow Fractionation and Single Particle Inductively Coupled Plasma Mass Spectrometery (FFF-ICP-MS and SP-ICP-MS): Scientific Operating Procedure SOP-C

DTIC Science & Technology

2015-04-01

monodisperse particles. ENPs in environmental samples will likely have much broader size distributions and thus FFF-ICP-MS was tested over a greater...Figure 6). Resolution is based on ICP-MS sensitivity, and will likely decrease as the difference in particle diameter decreases. Second, this...Alvarez. 2006. Antibacterial activity of fullerene water suspensions: Effects of preparation method and particle size. Environmental Science

Comparative study of laminar and turbulent flow model with different operating parameters for radio frequency-inductively coupled plasma torch working at 3  MHz frequency at atmospheric pressure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Punjabi, Sangeeta B., E-mail: p.sangeeta@gmail.com; Department of Physics, University of Mumbai, Kalina, Santacruz; Sahasrabudhe, S. N.

2014-01-15

This paper provides 2D comparative study of results obtained using laminar and turbulent flow model for RF (radio frequency) Inductively Coupled Plasma (ICP) torch. The study was done for the RF-ICP torch operating at 50 kW DC power and 3 MHz frequency located at BARC. The numerical modeling for this RF-ICP torch is done using ANSYS software with the developed User Defined Function. A comparative study is done between laminar and turbulent flow model to investigate how temperature and flow fields change when using different operating conditions such as (a) swirl and no swirl velocity for sheath gas flow rate, (b) variationmore » in sheath gas flow rate, and (c) variation in plasma gas flow rate. These studies will be useful for different material processing applications.« less

On the possibility of the multiple inductively coupled plasma and helicon plasma sources for large-area processes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, Jin-Won; Lee, Yun-Seong, E-mail: leeeeys@kaist.ac.kr; Chang, Hong-Young

2014-08-15

In this study, we attempted to determine the possibility of multiple inductively coupled plasma (ICP) and helicon plasma sources for large-area processes. Experiments were performed with the one and two coils to measure plasma and electrical parameters, and a circuit simulation was performed to measure the current at each coil in the 2-coil experiment. Based on the result, we could determine the possibility of multiple ICP sources due to a direct change of impedance due to current and saturation of impedance due to the skin-depth effect. However, a helicon plasma source is difficult to adapt to the multiple sources duemore » to the consistent change of real impedance due to mode transition and the low uniformity of the B-field confinement. As a result, it is expected that ICP can be adapted to multiple sources for large-area processes.« less

Validation of the determination of the B isotopic composition in Roman glasses with laser ablation multi-collector inductively coupled plasma-mass spectrometry

NASA Astrophysics Data System (ADS)

Devulder, Veerle; Gerdes, Axel; Vanhaecke, Frank; Degryse, Patrick

2015-03-01

The applicability of laser ablation multi-collector inductively coupled plasma-mass spectrometry (LA-MC-ICP-MS) for the determination of the B isotopic composition in Roman glasses was investigated. The δ11B values thus obtained provide information on the natron flux used during the glass-making process. The glass samples used for this purpose were previously characterized using pneumatic nebulization (PN) MC-ICP-MS. Unfortunately, this method is time-consuming and labor-intensive and consumes some 100 mg of sample, which is a rather high amount for ancient materials. Therefore, the use of the less invasive and faster LA-MC-ICP-MS approach was explored. In this work, the results for 29 Roman glasses and 4 home-made glasses obtained using both techniques were compared to assess the suitability of LA-MC-ICP-MS in this context. The results are in excellent agreement within experimental uncertainty. No difference in overall mass discrimination was observed between the Roman glasses, NIST SRM 610 reference glass and B6 obsidian. The expanded uncertainty of the LA-MC-ICP-MS approach was estimated to be < 2‰, which is similar to that obtained upon sample digestion and PN-MC-ICP-MS measurement.

Determination and identification of titanium dioxide nanoparticles in confectionery foods, marketed in South Korea, using inductively coupled plasma optical emission spectrometry and transmission electron microscopy.

PubMed

Kim, Namhoon; Kim, Changkyu; Jung, Soyoung; Park, Youngae; Lee, Youngju; Jo, Juyeon; Hong, Misun; Lee, Sangmi; Oh, Younghee; Jung, Kweon

2018-06-18

Food-grade titanium dioxide (TiO 2 ) is a common and widespread food additive in many processed foods, personal care products, and other industrial categories as it boosts the brightness and whiteness of colours. Although it is generally recognised as safe for humans, there is a growing interest in the health risks associated with its oral intake. This study quantified and identified TiO 2 nanoparticles present in confectionery foods, which are children's favourite foods, with inductively coupled plasma optical emission spectrometry (ICP-OES) and transmission electron microscopy (TEM). A reliable digestion method using hot sulphuric acid and a digestion catalyst (K 2 SO 4 :CuSO 4  = 9:1) was suggested for titanium analysis. Validations of the experimental method were quite acceptable in terms of linearity, recoveries, detection limits, and quantification limits. Of all the 88 analysed foods, TiO 2 was detected in 19 products, all except three declared TiO 2 in their labelling. The mean TiO 2 content of candies, chewing gums, and chocolates were 0.36 mg g -1 , 0.04 mg g -1 , and 0.81 mg g -1 , respectively. Whitish particles isolated from the confectionery foods were confirmed as TiO 2 nanoparticles via TEM and energy dispersive X-ray spectroscopy (EDX), in which nanosized particles (<100 nm) were identified.

Numerical study of heating and evaporation processes of quartz particles in RF inductively coupled plasma

NASA Astrophysics Data System (ADS)

Grishin, Yu M.; Miao, Long

2017-05-01

Numerical simulations of heat and evaporation processes of quartz particles in Ar radio frequency inductively coupled plasma (ICP) are investigated. The quartz particles are supplied by the carrier gas into the ICP within gas-cooling. It is shown that with the increase of amplitude of discharge current above critical value there is a toroidal vortex in the ICP torch at the first coil. The conditions for the formation of vortex and the parameters of the vortex tube have been evaluated and determined. The influence of vortex, discharge current, coil numbers and feed rate of carrier gas on the evaporation efficiency of quartz particles have been demonstrated. It was found that the optimal discharge current is close to the critical value when the quartz particles with initial sizes up to 130 μm can be fully vaporized in the ICP torch with thermal power of 10kW. The heat and evaporation processes of quartz particles in the ICP torch have significant importance for the study of one-step plasma chemical reaction method directly producing silicon from silicide (SiO2) in the argon-hydrogen plasma.

[Interest and limits of inductively coupled plasma mass spectrometry (ICP-MS) for urinary diagnosis of radionuclide internal contamination].

PubMed

Lecompte, Yannick; Bohand, Sandra; Laroche, Pierre; Cazoulat, Alain

2013-01-01

After a review of radiometric reference methods used in radiotoxicology, analytical performance of inductively coupled plasma mass spectrometry (ICP-MS) for the workplace urinary diagnosis of internal contamination by radionuclides are evaluated. A literature review (covering the period from 2000 to 2012) is performed to identify the different applications of ICP-MS in radiotoxicology for urine analysis. The limits of detection are compared to the recommendations of the International commission on radiological protection (ICRP 78: "Individual monitoring for internal exposure of workers"). Except one publication describing the determination of strontium-90 (β emitter), all methods using ICP-MS reported in the literature concern actinides (α emitters). For radionuclides with a radioactive period higher than 10(4) years, limits of detection are most often in compliance with ICRP publication 78 and frequently lower than radiometric methods. ICP-MS allows the specific determination of plutonium-239 + 240 isotopes which cannot be discriminated by α spectrometry. High resolution ICP-MS can also measure uranium isotopic ratios in urine for total uranium concentrations lower than 20 ng/L. The interest of ICP-MS in radiotoxicology concerns essentially the urinary measurement of long radioactive period actinides, particularly for uranium isotope ratio determination and 239 and 240 plutonium isotopes discrimination. Radiometric methods remain the most efficient for the majority of other radionuclides.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of whole-water recoverable arsenic, boron, and vanadium using inductively coupled plasma-mass spectrometry

USGS Publications Warehouse

Garbarino, John R.

2000-01-01

Analysis of in-bottle digestate by using the inductively coupled plasma?mass spectrometric (ICP?MS) method has been expanded to include arsenic, boron, and vanadium. Whole-water samples are digested by using either the hydrochloric acid in-bottle digestion procedure or the nitric acid in-bottle digestion procedure. When the hydrochloric acid in-bottle digestion procedure is used, chloride must be removed from the digestate by subboiling evaporation before arsenic and vanadium can be accurately determined. Method detection limits for these elements are now 10 to 100 times lower than U.S. Geological Survey (USGS) methods using hydride generation? atomic absorption spectrophotometry (HG? AAS) and inductively coupled plasma? atomic emission spectrometry (ICP?AES), thus providing lower variability at ambient concentrations. The bias and variability of the methods were determined by using results from spike recoveries, standard reference materials, and validation samples. Spike recoveries in reagent-water, surface-water, ground-water, and whole-water recoverable matrices averaged 90 percent for seven replicates; spike recoveries were biased from 25 to 35 percent low for the ground-water matrix because of the abnormally high iron concentration. Results for reference material were within one standard deviation of the most probable value. There was no significant difference between the results from ICP?MS and HG?AAS or ICP?AES methods for the natural whole-water samples that were analyzed.

Complexation studies with lanthanides and humic acid analyzed by ultrafiltration and capillary electrophoresis-inductively coupled plasma mass spectrometry.

PubMed

Kautenburger, Ralf; Beck, Horst Philipp

2007-08-03

For the long-term storage of radioactive waste, detailed information about geo-chemical behavior of radioactive and toxic metal ions under environmental conditions is necessary. Humic acid (HA) can play an important role in the immobilisation or mobilisation of metal ions due to complexation and colloid formation. Therefore, we investigate the complexation behavior of HA and its influence on the migration or retardation of selected lanthanides (europium and gadolinium as homologues of the actinides americium and curium). Two independent speciation techniques, ultrafiltration and capillary electrophoresis coupled with inductively coupled plasma mass spectrometry (CE-ICP-MS) have been compared for the study of Eu and Gd interaction with (purified Aldrich) HA. The degree of complexation of Eu and Gd in 25 mg l(-1) Aldrich HA solutions was determined with a broad range of metal loading (Eu and Gd total concentration between 10(-6) and 10(-4) mol l(-1)), ionic strength of 10 mM (NaClO4) and different pH-values. From the CE-ICP-MS electropherograms, additional information on the charge of the Eu species was obtained by the use of 1-bromopropane as neutral marker. To detect HA in the ICP-MS and separate between HA complexed and non complexed metal ions in the CE-ICP-MS, we have halogenated the HA with iodine as ICP-MS marker.

Determination of Arsenic in Sinus Wash and Tap Water by Inductively Coupled Plasma-Mass Spectrometry

ERIC Educational Resources Information Center

Donnell, Anna M.; Nahan, Keaton; Holloway, Dawone; Vonderheide, Anne P.

2016-01-01

Arsenic is a toxic element to which humans are primarily exposed through food and water; it occurs as a result of human activities and naturally from the earth's crust. An experiment was developed for a senior level analytical laboratory utilizing an Inductively Coupled Plasma-Mass Spectrometer (ICP-MS) for the analysis of arsenic in household…

Laser Induced Breakdown Spectroscopy (LIBS)

DTIC Science & Technology

2010-03-31

mass spectrometry and laser induced breakdown spectroscopy, Spe T Trejos, A Flores and JR. Almirall, Micro-spectrochemical analysis of document paper...and gel inks by laser ablation inductively coupled plasma mass spectrometry and laser induced breakdown spectroscopy, Spectrochimica Acta Part B...abstracts): 1. *Schenk, E.R. “Elemental analysis of unprocessed cotton by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and laser

Effects of Inductively Coupled Plasma Hydrogen on Long-Wavelength Infrared HgCdTe Photodiodes

NASA Astrophysics Data System (ADS)

Boieriu, P.; Buurma, C.; Bommena, R.; Blissett, C.; Grein, C.; Sivananthan, S.

2013-12-01

Bulk passivation of semiconductors with hydrogen continues to be investigated for its potential to improve device performance. In this work, hydrogen-only inductively coupled plasma (ICP) was used to incorporate hydrogen into long-wavelength infrared HgCdTe photodiodes grown by molecular-beam epitaxy. Fully fabricated devices exposed to ICP showed statistically significant increases in zero-bias impedance values, improved uniformity, and decreased dark currents. HgCdTe photodiodes on Si substrates passivated with amorphous ZnS exhibited reductions in shunt currents, whereas devices on CdZnTe substrates passivated with polycrystalline CdTe exhibited reduced surface leakage, suggesting that hydrogen passivates defects in bulk HgCdTe and in CdTe.

Development of analytical methods for multiplex bio-assay with inductively coupled plasma mass spectrometry.

PubMed

Ornatsky, Olga I; Kinach, Robert; Bandura, Dmitry R; Lou, Xudong; Tanner, Scott D; Baranov, Vladimir I; Nitz, Mark; Winnik, Mitchell A

2008-01-01

Advances in the development of highly multiplexed bio-analytical assays with inductively coupled plasma mass spectrometry (ICP-MS) detection are discussed. Use of novel reagents specifically designed for immunological methods utilizing elemental analysis is presented. The major steps of method development, including selection of elements for tags, validation of tagged reagents, and examples of multiplexed assays, are considered in detail. The paper further describes experimental protocols for elemental tagging of antibodies, immunostaining of live and fixed human leukemia cells, and preparation of samples for ICP-MS analysis. Quantitative analysis of surface antigens on model cell lines using a cocktail of seven lanthanide labeled antibodies demonstrated high specificity and concordance with conventional immunophenotyping.

Investigation of the RF efficiency of inductively coupled hydrogen plasmas at 1 MHz

NASA Astrophysics Data System (ADS)

Rauner, D.; Mattei, S.; Briefi, S.; Fantz, U.; Hatayama, A.; Lettry, J.; Nishida, K.; Tran, M. Q.

2017-08-01

The power requirements of RF heated sources for negative hydrogen ions in fusion are substantial, which poses strong demands on the generators and components of the RF circuit. Consequently, an increase of the RF coupling efficiency would be highly beneficial. Fundamental investigations of the RF efficiency in inductively coupled hydrogen and deuterium discharges in cylindrical symmetry are conducted at the lab experiment CHARLIE. The experiment is equipped with several diagnostics including optical emission spectroscopy and a movable floating double probe to monitor the plasma parameters. The presented investigations are performed in hydrogen at a varying pressure between 0.3 and 10 Pa, utilizing a conventional helical ICP coil driven at a frequency of 1 MHz and a fixed power of 520 W for plasma generation. The coupling efficiency is strongly affected by the variation in pressure, reaching up to 85 % between 1 and 3 Pa while dropping down to only 50 % at 0.3 Pa, which is the relevant operating pressure for negative hydrogen ion sources for fusion. Due to the lower power coupling, also the measured electron density at 0.3 Pa is only 5 . 1016 m-3, while it reaches up to 2.5 . 1017 m-3 with increasing coupling efficiency. In order to gain information on the spatially resolved aspects of RF coupling and plasma heating which are not diagnostically accessible, first simulations of the discharge by an electromagnetic Particle-In-Cell Monte Carlo collision method have been conducted and are compared to the measurement data. At 1 Pa, the simulated data corresponds well to the results of both axially resolved probe measurements and radially resolved emission profiles obtained via OES. Thereby, information regarding the radial distribution of the electron density and mean energy is provided, revealing a radial distribution of the electron density which is well described by a Bessel profile.

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

NASA Astrophysics Data System (ADS)

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.

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.

PubMed

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 error<11%). Two calibrations (aqueous standard and standard addition) procedures were studied and proved that standard addition was preferable for all analytes. Experimental designs for seven factors (HNO(3), H(2)SO(4) and H(2)O(2) volumes, digestion time, 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.

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

PubMed

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

2009-10-15

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

Environmentally friendly microwave-assisted sequential extraction method followed by ICP-OES and ion-chromatographic analysis for rapid determination of sulphur forms in coal samples.

PubMed

Mketo, Nomvano; Nomngongo, Philiswa N; Ngila, J Catherine

2018-05-15

A rapid three-step sequential extraction method was developed under microwave radiation followed by inductively coupled plasma-optical emission spectroscopic (ICP-OES) and ion-chromatographic (IC) analysis for the determination of sulphur forms in coal samples. The experimental conditions of the proposed microwave-assisted sequential extraction (MW-ASE) procedure were optimized by using multivariate mathematical tools. Pareto charts generated from 2 3 full factorial design showed that, extraction time has insignificant effect on the extraction of sulphur species, therefore, all the sequential extraction steps were performed for 5 min. The optimum values according to the central composite designs and counter plots of the response surface methodology were 200 °C (microwave temperature) and 0.1 g (coal amount) for all the investigated extracting reagents (H 2 O, HCl and HNO 3 ). When the optimum conditions of the proposed MW-ASE procedure were applied in coal CRMs, SARM 18 showed more organic sulphur (72%) and the other two coal CRMs (SARMs 19 and 20) were dominated by sulphide sulphur species (52-58%). The sum of the sulphur forms from the sequential extraction steps have shown consistent agreement (95-96%) with certified total sulphur values on the coal CRM certificates. This correlation, in addition to the good precision (1.7%) achieved by the proposed procedure, suggests that the sequential extraction method is reliable, accurate and reproducible. To safe-guard the destruction of pyritic and organic sulphur forms in extraction step 1, water was used instead of HCl. Additionally, the notorious acidic mixture (HCl/HNO 3 /HF) was replaced by greener reagent (H 2 O 2 ) in the last extraction step. Therefore, the proposed MW-ASE method can be applied in routine laboratories for the determination of sulphur forms in coal and coal related matrices. Copyright © 2018 Elsevier B.V. All rights reserved.

Application of infrared thermography for online monitoring of wall temperatures in inductively coupled plasma torches with conventional and low-flow gas consumption

NASA Astrophysics Data System (ADS)

Engelhard, Carsten; Scheffer, Andy; Maue, Thomas; Hieftje, Gary M.; Buscher, Wolfgang

2007-10-01

Inductively coupled plasma (ICP) sources typically used for trace elemental determination and speciation were investigated with infrared (IR) thermography to obtain spatially resolved torch temperature distributions. Infrared thermographic imaging is an excellent tool for the monitoring of temperatures in a fast and non-destructive way. This paper presents the first application of IR thermography to inductively coupled plasma torches and the possibility to investigate temperatures and thermal patterns while the ICP is operating and despite background emission from the plasma itself. A fast and easy method is presented for the determination of temperature distributions and stress features within ICP torches. Two different ICP operating torches were studied: a commercially available Fassel-type ICP unit with 14 L min - 1 total Ar consumption and a SHIP torch with the unusually low Ar flow of 0.6 L min - 1 . Spatially resolved infrared images of both torches were obtained and laterally resolved temperature profiles were extracted. After temperature-resolved calibration of the emissivity (between 0.5 and 0.35 at 873-1323 K) and transmission (20% between 3.75 and 4.02 μm) of the fused quartz used in the torch construction, an image correction was applied. Inhomogeneous temperature distributions with locally defined stress areas in the conventional Fassel-type torch were revealed. As a general trend, it was found that the SHIP torch exhibited higher temperatures ( Tmax = 1580 K) than the conventional torch ( Tmax = 730 K). In the former case, torch sites with efficient and inefficient cooling were discovered and the external flow of cooling air (24-48 m s - 1 ) was identified as the limiting factor.

Inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS for isotope analysis of long-lived radionuclides

NASA Astrophysics Data System (ADS)

Becker, J. Sabine

2005-04-01

For a few years now inductively coupled plasma mass spectrometry has been increasingly used for precise and accurate determination of isotope ratios of long-lived radionuclides at the trace and ultratrace level due to its excellent sensitivity, good precision and accuracy. At present, ICP-MS and also laser ablation ICP-MS are applied as powerful analytical techniques in different fields such as the characterization of nuclear materials, recycled and by-products (e.g., spent nuclear fuel or depleted uranium ammunitions), radioactive waste control, in environmental monitoring and in bioassay measurements, in health control, in geochemistry and geochronology. Especially double-focusing sector field ICP mass spectrometers with single ion detector or with multiple ion collector device have been used for the precise determination of long-lived radionuclides isotope ratios at very low concentration levels. Progress has been achieved by the combination of ultrasensitive mass spectrometric techniques with effective separation and enrichment procedures in order to improve detection limits or by the introduction of the collision cell in ICP-MS for reducing disturbing interfering ions (e.g., of 129Xe+ for the determination of 129I). This review describes the state of the art and the progress of ICP-MS and laser ablation ICP-MS for isotope ratio measurements of long-lived radionuclides in different sample types, especially in the main application fields of characterization of nuclear and radioactive waste material, environmental research and health controls.

Numerical and Experimental Investigation on the Attenuation of Electromagnetic Waves in Unmagnetized Plasmas Using Inductively Coupled Plasma Actuator

NASA Astrophysics Data System (ADS)

Lin, Min; Xu, Haojun; Wei, Xiaolong; Liang, Hua; Song, Huimin; Sun, Quan; Zhang, Yanhua

2015-10-01

The attenuation of electromagnetic (EM) waves in unmagnetized plasma generated by an inductively coupled plasma (ICP) actuator has been investigated both theoretically and experimentally. A numerical study is conducted to investigate the propagation of EM waves in multilayer plasma structures which cover a square flat plate. Experimentally, an ICP actuator with dimensions of 20 cm×20 cm×4 cm is designed to produce a steady plasma slab. The attenuation of EM waves in the plasma generated by the ICP actuator is measured by a reflectivity arch test method at incident waves of 2.3 GHz and 10.1 GHz, respectively. A contrastive analysis of calculated and measured results of these incident wave frequencies is presented, which suggests that the experiment accords well with our theory. As expected, the plasma slab generated by the ICP actuator can effectively attenuate the EM waves, which may have great potential application prospects in aircraft stealth. supported by National Natural Science Foundation of China (Nos. 51276197, 11472306 and 11402301)

Effect of silane/hydrogen ratio on microcrystalline silicon thin films by remote inductively coupled plasma

NASA Astrophysics Data System (ADS)

Guo, Y. N.; Wei, D. Y.; Xiao, S. Q.; Huang, S. Y.; Zhou, H. P.; Xu, S.

2013-05-01

Hydrogenated microcrystalline silicon (μc-Si:H) thin films were prepared by remote low frequency inductively coupled plasma (ICP) chemical vapor deposition system, and the effect of silane/hydrogen ratio on the microstructure and electrical properties of μc-Si:H films was systematically investigated. As silane/hydrogen ratio increases, the crystalline volume fraction Fc decreases and the ratio of the intensity of (220) peak to that of (111) peak drops as silane flow rate is increased. The FTIR result indicates that the μc-Si:H films prepared by remote ICP have a high optical response with a low hydrogen content, which is in favor of reducing light-induced degradation effect. Furthermore, the processing window of the phase transition region for remote ICP is much wider than that for typical ICP. The photosensitivity of μc-Si:H films can exceed 100 at the transition region and this ensures the possibility of the fabrication of microcrystalline silicon thin film solar cells with a open-circuit voltage of about 700 mV.

Influence of methane addition on selenium isotope sensitivity and their spectral interferences.

PubMed

Floor, Geerke H; Millot, Romain; Iglesias, Mónica; Négrel, Philippe

2011-02-01

The measurements of stable selenium (Se) isotopic signatures by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) are very challenging, due to the presence of spectral interferences and the low abundance of Se in environmental samples. We systematically investigated the effect of methane addition on the signal of Se isotopes and their interferences. It is the first time that the effect of methane addition has been assessed for all Se isotopes and its potential interferences using hydride generator multi-collector inductively coupled plasma mass spectrometry (HG-MC-ICP-MS). Our results show that a small methane addition increases the sensitivity. However, the response differs between a hydride generator and a standard introduction system, which might be related to differences in the ionization processes. Both argon and hydrogen-based interferences, the most common spectral interferences on selenium isotopes in HG-MC-ICP-MS, decrease with increasing methane addition. Therefore, analyte-interference ratios and precision are improved. Methane addition has thus a high potential for the application to stable Se isotopes ratios by HG-MC-ICP-MS. Copyright © 2011 John Wiley & Sons, Ltd.

Determination of the rare-earth elements in geological materials by inductively coupled plasma mass spectrometry

USGS Publications Warehouse

Lichte, F.E.; Meier, A.L.; Crock, J.G.

1987-01-01

A method of analysis of geological materials for the determination of the rare-earth elements using the Inductively coupled plasma mass spectrometric technique (ICP-MS) has been developed. Instrumental parameters and factors affecting analytical results have been first studied and then optimized. Samples are analyzed directly following an acid digestion, without the need for separation or preconcentration with limits of detection of 2-11 ng/g, precision of ?? 2.5% relative standard deviation, and accuracy comparable to inductively coupled plasma emission spectrometry and instrumental neutron activation analysis. A commercially available ICP-MS instrument is used with modifications to the sample introduction system, torch, and sampler orifice to reduce the effects of high salt content of sample solutions prepared from geologic materials. Corrections for isobaric interferences from oxide ions and other diatomic and triatomic ions are made mathematically. Special internal standard procedures are used to compensate for drift in metahmetal oxide ratios and sensitivity. Reference standard values are used to verify the accuracy and utility of the method.

Determination of 20 trace elements and arsenic species for a realgar-containing traditional Chinese medicine Niuhuang Jiedu tablets by direct inductively coupled plasma-mass spectrometry and high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

PubMed

Jin, Pengfei; Liang, Xiaoli; Xia, Lufeng; Jahouh, Farid; Wang, Rong; Kuang, Yongmei; Hu, Xin

2016-01-01

Niuhuang Jiedu tablet (NHJDT) is a realgar-containing traditional Chinese medicine. A direct inductively coupled plasma-mass spectrometry (ICP-MS) method for the simultaneous determination of 20 trace elements (Mg, K, Ca, Na, Fe, As, Zn, Sr, Ba, Cu, Mn, Ni, Pb, V, Cr, Se, Co, Mo, Cd, Hg) in NHJDT, as well as in water, gastric fluid and intestinal fluid was established. Meanwhile, a high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) method was developed for the determination of arsenite (As(III)), arsenate (As(V)), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA) and for the identification of arsenobetaine (AsB) and arsenocholine (AsC) in these extracts. Both methods were fully validated in the respect of linearity, sensitivity, precision, stability and accuracy. The reliability of the ICP-MS method was further evaluated using a certified standard reference material prepared from dried tomato leaves (NIST, SRM 1572a). The analysis showed that some manufacturers formulated lower amount of realgar than required in the Chinese Pharmacopoeia (ChP) in their preparations. In addition, almost same extraction profiles for total As and inorganic As were found in water and in gastrointestinal fluids, while higher extraction rates for other 19 elements were observed in gastrointestinal fluids. Our findings show that the toxicities of Hg, Cu, Cd and Pb in NHJDP are low, while the real As toxicity in NHJDT should be deeply investigated. Copyright © 2015 Elsevier GmbH. All rights reserved.

Reduction of matrix effects in inductively coupled plasma mass spectrometry by flow injection with an unshielded torch.

PubMed

Gross, Cory T; McIntyre, Sally M; Houk, R S

2009-06-15

Solution samples with matrix concentrations above approximately 0.1% generally present difficulties for analysis by inductively coupled plasma mass spectrometry (ICP-MS) because of cone clogging and matrix effects. Flow injection (FI) is coupled to ICP-MS to reduce deposition from samples such as 1% sodium salts (as NaCl) and seawater (approximately 3% dissolved salts). Surprisingly, matrix effects are also less severe during flow injection, at least for some matrix elements on the particular instrument used. Sodium chloride at 1% Na and undiluted seawater cause only 2 to 29% losses of signal for typical analyte elements. A heavy matrix element (Bi) at 0.1% also induces only approximately 14% loss of analyte signal. However, barium causes a much worse matrix effect, that is, approximately 90% signal loss at 5000 ppm Na. Also, matrix effects during FI are much more severe when a grounded metal shield is inserted between the load coil and the torch, which is the most common mode of operation for the particular ICP-MS device used.

Development of a novel low-flow ion source/sampling cone geometry for inductively coupled plasma mass spectrometry and application in hyphenated techniques

NASA Astrophysics Data System (ADS)

Pfeifer, Thorben; Janzen, Rasmus; Steingrobe, Tobias; Sperling, Michael; Franze, Bastian; Engelhard, Carsten; Buscher, Wolfgang

2012-10-01

A novel ion source/sampling cone device for inductively coupled plasma mass spectrometry (ICP-MS) especially operated in the hyphenated mode as a detection system coupled with different separation modules is presented. Its technical setup is described in detail. Its main feature is the very low total argon consumption of less than 1.5 L min- 1, leading to significant reduction of operational costs especially when time-consuming speciation analysis is performed. The figures of merit of the new system with respect to sensitivity, detection power, long-term stability and working range were explored. Despite the profound differences of argon consumption of the new system in comparison to the conventional ICP-MS system, many of the characteristic features of the conventional ICP-MS could be maintained to a great extent. To demonstrate the ion source's capabilities, it was used as an element-selective detector for gas (GC) and high performance liquid chromatography (HPLC) where organic compounds of mercury and cobalt, respectively, were separated and detected with the new low-flow ICP-MS detection system. The corresponding chromatograms are shown. The applicability for trace element analysis has been validated with the certified reference material NIST 1643e.

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION AND MAINTENANCE OF THE JOBIN-YVON MODEL 70 INDUCTIVELY COUPLED PLASMA ATOMIC ABSORPTION SPECTROMETER (BCO-L-7.1)

EPA Science Inventory

The purpose of this SOP is to detail the operation and maintenance of an Instruments, SA Inc., Jobin-Yvon Model 70 (JY-70) inductively coupled plasma atomic emissions spectrometry (ICP-AES). This procedure was followed to ensure consistent data retrieval during the Arizona NHEXA...

A novel strategy to evaluate the degradation of quantum dots: identification and quantification of CdTe quantum dots and corresponding ionic species by CZE-ICP-MS.

PubMed

Meng, Peijun; Xiong, Yamin; Wu, Yingting; Hu, Yue; Wang, Hui; Pang, Yuanfeng; Jiang, Shuqing; Han, Sihai; Huang, Peili

2018-05-09

In view of the significance and urgency of the speciation analysis of quantum dots (QDs) and their degradation products for clarifying their degradation rules and toxicity mechanisms, a method for the identification and quantification of CdTe QDs and corresponding ionic species in complex matrices was developed using capillary zone electrophoresis (CZE) coupled to inductively coupled plasma-mass spectrometry (ICP-MS). The quality assessment of commercial CdTe QDs and serum pharmacokinetics of synthesized CdTe QDs in rats were successfully undertaken using the developed CZE-ICP-MS method.

Observation of collisionless heating of low energy electrons in low pressure inductively coupled argon plasmas

NASA Astrophysics Data System (ADS)

Lee, Min-Hyong; Lee, Hyo-Chang; Chung, Chin-Wook

2008-12-01

Collisionless heating of low energy electrons was observed in low pressure argon rf-biased inductively coupled plasmas (ICPs) by measurement of the electron energy distribution function (EEDF). When only capacitive power (bias) was supplied, the EEDF in the discharge was a bi-Maxwellian distribution with two electron groups. It was found that the low energy electrons were heated up significantly even with a little inductive power (<20 W) even when the discharge was in E mode. Due to the low gas pressure and low temperature of low energy electrons (close to the energy of the Ramsauer minimum), the collisional heating of low energy electrons appears to be negligible. Therefore, this effective heating of the low energy electrons showed a direct experimental evidence of the collisionless heating by inductive field. The significant heating of low energy electrons in E mode indicates that collisionless heating in the skin layer is an important electron heating mechanism of low pressure ICP even when the discharge is in E mode.

Mapping of lead, magnesium and copper accumulation in plant tissues by laser-induced breakdown spectroscopy and laser-ablation inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Kaiser, J.; Galiová, M.; Novotný, K.; Červenka, R.; Reale, L.; Novotný, J.; Liška, M.; Samek, O.; Kanický, V.; Hrdlička, A.; Stejskal, K.; Adam, V.; Kizek, R.

2009-01-01

Laser-Induced Breakdown Spectroscopy (LIBS) and Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) were utilized for mapping the accumulation of Pb, Mg and Cu with a resolution up to 200 μm in a up to cm × cm area of sunflower ( Helianthus annuus L.) leaves. The results obtained by LIBS and LA-ICP-MS are compared with the outcomes from Atomic Absorption Spectrometry (AAS) and Thin-Layer Chromatography (TLC). It is shown that laser-ablation based analytical methods can substitute or supplement these techniques mainly in the cases when a fast multi-elemental mapping of a large sample area is needed.

Considerations in As analysis and speciation

USGS Publications Warehouse

Edwards, M.; Patel, S.; McNeil, L.; Chen, H.W.; Frey, M.; Eaton, A.D.; Antweiler, Ronald C.; Taylor, Howard E.

1998-01-01

This article summarizes recent experiences in arsenic (As) quantification, preservation, and speciation developed during AWWA Research Foundation (AWWARF) and Water Industry Technical Action Fund (WITAF) projects. The goal of this article is to alert analysts and decision-makers to potential problems in As analysis and speciation, because there appear to be several unresolved problems with routine analytical approaches. In true split drinking water samples As was quantified by three accepted analytical methods in three laboratories. The techniques used were graphite furnace atomic absorption spectrometry (GFAAS), inductively coupled plasma mass spectrometry (ICP-MS), and hydride generation inductively coupled plasma-emission spectrometry (HG-ICP-AES). Experimental findings are organized into sections on As analysis, particulate As in water supplies, and examination of As speciation methods.

Development of analytical methods for multiplex bio-assay with inductively coupled plasma mass spectrometry

PubMed Central

Ornatsky, Olga I.; Kinach, Robert; Bandura, Dmitry R.; Lou, Xudong; Tanner, Scott D.; Baranov, Vladimir I.; Nitz, Mark; Winnik, Mitchell A.

2008-01-01

Advances in the development of highly multiplexed bio-analytical assays with inductively coupled plasma mass spectrometry (ICP-MS) detection are discussed. Use of novel reagents specifically designed for immunological methods utilizing elemental analysis is presented. The major steps of method development, including selection of elements for tags, validation of tagged reagents, and examples of multiplexed assays, are considered in detail. The paper further describes experimental protocols for elemental tagging of antibodies, immunostaining of live and fixed human leukemia cells, and preparation of samples for ICP-MS analysis. Quantitative analysis of surface antigens on model cell lines using a cocktail of seven lanthanide labeled antibodies demonstrated high specificity and concordance with conventional immunophenotyping. PMID:19122859

Measurement of low radioactivity background in a high voltage cable by high resolution inductively coupled plasma mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vacri, M. L. di; Nisi, S.; Balata, M.

2013-08-08

The measurement of naturally occurring low level radioactivity background in a high voltage (HV) cable by high resolution inductively coupled plasma mass spectrometry (HR ICP MS) is presented in this work. The measurements were performed at the Chemistry Service of the Gran Sasso National Laboratory. The contributions to the radioactive background coming from the different components of the heterogeneous material were separated. Based on the mass fraction of the cable, the whole contamination was calculated. The HR ICP MS results were cross-checked by gamma ray spectroscopy analysis that was performed at the low background facility STELLA (Sub Terranean Low Levelmore » Assay) of the LNGS underground lab using HPGe detectors.« less

Exchangeable Ions Are Responsible for the In Vitro Antibacterial Properties of Natural Clay Mixtures

PubMed Central

Otto, Caitlin C.; Haydel, Shelley E.

2013-01-01

We have identified a natural clay mixture that exhibits in vitro antibacterial activity against a broad spectrum of bacterial pathogens. We collected four samples from the same source and demonstrated through antibacterial susceptibility testing that these clay mixtures have markedly different antibacterial activity against Escherichia coli and methicillin-resistant Staphylococcus aureus (MRSA). Here, we used X-ray diffraction (XRD) and inductively coupled plasma – optical emission spectroscopy (ICP-OES) and – mass spectrometry (ICP-MS) to characterize the mineralogical and chemical features of the four clay mixture samples. XRD analyses of the clay mixtures revealed minor mineralogical differences between the four samples. However, ICP analyses demonstrated that the concentrations of many elements, Fe, Co, Cu, Ni, and Zn, in particular, vary greatly across the four clay mixture leachates. Supplementation of a non-antibacterial leachate containing lower concentrations of Fe, Co, Ni, Cu, and Zn to final ion concentrations and a pH equivalent to that of the antibacterial leachate generated antibacterial activity against E. coli and MRSA, confirming the role of these ions in the antibacterial clay mixture leachates. Speciation modeling revealed increased concentrations of soluble Cu2+ and Fe2+ in the antibacterial leachates, compared to the non-antibacterial leachates, suggesting these ionic species specifically are modulating the antibacterial activity of the leachates. Finally, linear regression analyses comparing the log10 reduction in bacterial viability to the concentration of individual ion species revealed positive correlations with Zn2+ and Cu2+ and antibacterial activity, a negative correlation with Fe3+, and no correlation with pH. Together, these analyses further indicate that the ion concentration of specific species (Fe2+, Cu2+, and Zn2+) are responsible for antibacterial activity and that killing activity is not solely attributed to pH. PMID:23691149

RHENIUM SOLUBILITY IN BOROSILICATE NUCLEAR WASTE GLASS IMPLICATIONS FOR THE PROCESSING AND IMMOBILIZATION OF TECHNETIUM-99 (AND SUPPORTING INFORMATION WITH GRAPHICAL ABSTRACT)

DOE Office of Scientific and Technical Information (OSTI.GOV)

AA KRUGER; A GOEL; CP RODRIGUEZ

2012-08-13

The immobilization of 99Tc in a suitable host matrix has proved a challenging task for researchers in the nuclear waste community around the world. At the Hanford site in Washington State in the U.S., the total amount of 99Tc in low-activity waste (LAW) is {approx} 1,300 kg and the current strategy is to immobilize the 99Tc in borosilicate glass with vitrification. In this context, the present article reports on the solubility and retention of rhenium, a nonradioactive surrogate for 99Tc, in a LAW sodium borosilicate glass. Due to the radioactive nature of technetium, rhenium was chosen as a simulant becausemore » of previously established similarities in ionic radii and other chemical aspects. The glasses containing target Re concentrations varying from 0 to10,000 ppm by mass were synthesized in vacuum-sealed quartz ampoules to minimize the loss of Re by volatilization during melting at 1000 DC. The rhenium was found to be present predominantly as Re7 + in all the glasses as observed by X-ray absorption near-edge structure (XANES). The solubility of Re in borosilicate glasses was determined to be {approx}3,000 ppm (by mass) using inductively coupled plasma-optical emission spectroscopy (ICP-OES). At higher rhenium concentrations, some additional material was retained in the glasses in the form of alkali perrhenate crystalline inclusions detected by X-ray diffraction (XRD) and laser ablation-ICP mass spectrometry (LA-ICP-MS). Assuming justifiably substantial similarities between Re7 + and Tc 7+ behavior in this glass system, these results implied that the processing and immobilization of 99Tc from radioactive wastes should not be limited by the solubility of 99Tc in borosilicate LAW glasses.« less

Improving Alpha Spectrometry Energy Resolution by Ion Implantation with ICP-MS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dion, Michael P.; Liezers, Martin; Farmer, Orville T.

2015-01-01

We report results of a novel technique using an Inductively Coupled Plasma Mass Spectrometer (ICP-MS) as a method of source preparation for alpha spectrometry. This method produced thin, contaminant free 241Am samples which yielded extraordinary energy resolution which appear to be at the lower limit of the detection technology used in this research.

Mineral Analysis of Pine Nuts (Pinus spp.) Grown in New Zealand

PubMed Central

Vanhanen, Leo P.; Savage, Geoffrey P.

2013-01-01

Mineral analysis of seven Pinus species grown in different regions of New Zealand; Armand pine (Pinus armandii Franch), Swiss stone pine (Pinus cembra L.), Mexican pinyon (Pinus cembroides Zucc. var. bicolor Little), Coulter pine (Pinus coulteri D. Don), Johann’s pine (Pinus johannis M.F. Robert), Italian stone pine (Pinus pinea L.) and Torrey pine (Pinus torreyana Parry ex Carrière), was carried out using an inductively coupled plasma optical emission spectrophotometer (ICP-OES) analysis. Fourteen different minerals (Al, B, Ca, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, P, S and Zn) were identified in all seven varieties, except that no Al or Na was found in Pinus coulteri D. Don. New Zealand grown pine nuts are a good source of Cu, Mg, Mn, P and Zn, meeting or exceeding the recommended RDI for these minerals (based on an intake of 50 g nuts/day) while they supplied between 39%–89% of the New Zealand RDI for Fe. Compared to other commonly eaten tree-nuts New Zealand grown pine nuts are an excellent source of essential minerals. PMID:28239104

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

NASA Astrophysics Data System (ADS)

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

2015-12-01

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

Removal of metals from aqueous solution and sea water by functionalized graphite nanoplatelets based electrodes.

PubMed

Mishra, Ashish Kumar; Ramaprabhu, S

2011-01-15

In the present wok, we have demonstrated the simultaneous removal of sodium and arsenic (pentavalent and trivalent) from aqueous solution using functionalized graphite nanoplatelets (f-GNP) based electrodes. In addition, these electrodes based water filter was used for multiple metals removal from sea water. Graphite nanoplatelets (GNP) were prepared by acid intercalation and thermal exfoliation. Functionalization of GNP was done by further acid treatment. Material was characterized by different characterization techniques. Performance of supercapacitor based water filter was analyzed for the removal of high concentration of arsenic (trivalent and pentavalent) and sodium as well as for desalination of sea water, using cyclic voltametry (CV) and inductive coupled plasma-optical emission spectroscopy (ICP-OES) techniques. Adsorption isotherms and kinetic characteristics were studied for the simultaneous removal of sodium and arsenic (both trivalent and pentavalent). Maximum adsorption capacities of 27, 29 and 32 mg/g for arsenate, arsenite and sodium were achieved in addition to good removal efficiency for sodium, magnesium, calcium and potassium from sea water. Copyright © 2010 Elsevier B.V. All rights reserved.

Incense and joss stick making in small household factories, Thailand.

PubMed

Siripanich, S; Siriwong, W; Keawrueang, P; Borjan, M; Robson, M

2014-07-01

Incense and joss stick are generally used in the world. Most products were made in small household factories. There are many environmental and occupational hazards in these factories. To evaluate the workplace environmental and occupational hazards in small household incense and joss stick factories in Roi-Et, Thailand. Nine small household factories in rural areas of Roi-Et, Thailand, were studied. Dust concentration and small aerosol particles were counted through real time exposure monitoring. The inductively coupled plasma optical emission spectrometry (ICP-OES) was used for quantitative measurement of heavy metal residue in incense products. Several heavy metals were found in dissolved dye and joss sticks. Those included barium, manganese, and lead. Rolling and shaking processes produced the highest concentration of dust and aerosols. Only 3.9% of female workers used personal protection equipment. Dust and chemicals were major threats in small household incense and joss stick factories in Thailand. Increasing awareness towards using personal protection equipment and emphasis on elimination of environmental workplace hazards should be considered to help the workers of this industry.

Electrochemical determination of copper ions in spirit drinks using carbon paste electrode modified with biochar.

PubMed

Oliveira, Paulo Roberto; Lamy-Mendes, Alyne C; Rezende, Edivaltrys Inayve Pissinati; Mangrich, Antonio Sálvio; Marcolino, Luiz Humberto; Bergamini, Márcio F

2015-03-15

This work describes for first time the use of biochar as electrode modifier in combination with differential pulse adsorptive stripping voltammetric (DPAdSV) techniques for preconcentration and determination of copper (II) ions in spirit drinks samples (Cachaça, Vodka, Gin and Tequila). Using the best set of the experimental conditions a linear response for copper ions in the concentration range of 1.5 × 10(-6) to 3.1 × 10(-5) mol L(-1) with a Limit of Detection (LOD) of 4.0 × 10(-7) mol L(-1). The repeatability of the proposed sensor using the same electrode surface was measured as 3.6% and 6.6% using different electrodes. The effect of foreign species on the voltammetric response was also evaluated. Determination of copper ions content in different samples of spirit drinks samples was also realized adopting inductively coupled plasma optical emission spectroscopy (ICP-OES) and the results achieved are in agreement at a 95% of confidence level. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

PubMed

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

2017-09-01

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

Thermodynamic modeling of solid solutions between monosulfate and monochromate 3CaO Bullet Al{sub 2}O{sub 3} Bullet Ca[(CrO{sub 4}){sub x}(SO{sub 4}){sub 1-x}] Bullet nH{sub 2}O

DOE Office of Scientific and Technical Information (OSTI.GOV)

Leisinger, Sabine M., E-mail: sabine.leisinger@eawag.ch; Institute of Biogeochemistry and Pollutant Dynamics, ETH, CH-8092 Zurich; Lothenbach, Barbara

2012-01-15

In hydrated cement paste AFm-phases are regarded to play an important role in the binding of the toxic contaminant chromate through isomorphic substitution with sulfate. Solid solutions formation can lower the solubility of the solids, thus reducing chromate leaching concentrations. Solid solutions between monosulfate and monochromate were synthesized and characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDX) and inductive coupled plasma optical emission spectroscopy (ICP-OES). Based on the measured ion concentrations in solution total solubility products of the solid solution series were determined. For pure monochromate a logK = - 28.4more » {+-} 0.7 was determined. Results from solid and solution analysis showed that limited solid solutions exist. Based on XRD diffractograms a solid solution with a miscibility gap 0.15 < Crx < 0.85 with a dimensionless Guggenheim parameter of 2.43 was proposed.« less

Mineral Analysis of Pine Nuts (Pinus spp.) Grown in New Zealand.

PubMed

Vanhanen, Leo P; Savage, Geoffrey P

2013-04-03

Mineral analysis of seven Pinus species grown in different regions of New Zealand; Armand pine ( Pinus armandii Franch), Swiss stone pine ( Pinus cembra L.), Mexican pinyon ( Pinus cembroides Zucc. var. bicolor Little), Coulter pine ( Pinus coulteri D. Don), Johann's pine ( Pinus johannis M.F. Robert), Italian stone pine ( Pinus pinea L.) and Torrey pine ( Pinus torreyana Parry ex Carrière), was carried out using an inductively coupled plasma optical emission spectrophotometer (ICP-OES) analysis. Fourteen different minerals (Al, B, Ca, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, P, S and Zn) were identified in all seven varieties, except that no Al or Na was found in Pinus coulteri D. Don. New Zealand grown pine nuts are a good source of Cu, Mg, Mn, P and Zn, meeting or exceeding the recommended RDI for these minerals (based on an intake of 50 g nuts/day) while they supplied between 39%-89% of the New Zealand RDI for Fe. Compared to other commonly eaten tree-nuts New Zealand grown pine nuts are an excellent source of essential minerals.

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

PubMed

Kojta, Anna K; Falandysz, Jerzy

2016-06-01

The aim of this study was to investigate and compare the levels of eight metallic elements in the fruiting bodies of Bay Bolete (Boletus badius; current name Imleria badia) collected from ten sites in Poland to understand better the value of this popular mushroom as an organic food. Bay Bolete fruiting bodies were collected from the forest area near the towns and villages of Kętrzyn, Poniatowa, Bydgoszcz, Pelplin, Włocławek, Żuromin, Chełmno, Ełk and Wilków communities, as well as in the Augustów Primeval Forest. Elements such as Ca, Fe, K, Mg, Mn, Na and Zn were analyzed by inductively coupled plasma atomic emission spectroscopy (ICP-OES), and mercury by cold vapor atomic absorption spectrometry (CV-AAS). This made it possible to assess the nutritional value of the mushroom, as well as possible toxicological risks associated with its consumption. The results were subjected to statistical analysis (Kruskal-Wallis test, cluster analysis, principal component analysis). Copyright © 2016 Elsevier Ltd. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2016-10-01

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

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

PubMed Central

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

2016-01-01

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

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

PubMed

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

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

Chemical and biological assessment of sediments and water of Khalid Khor, Sharjah, United Arab Emirates.

PubMed

Samara, Fatin; Elsayed, Yehya; Soghomonian, Balik; Knuteson, Sandra L

2016-10-15

Water and sediments were collected on March 2013 and April 2014 from Khalid Khor creek area in United Arab Emirates to assess their quality parameters. The pH and alkalinity of the water samples were measured and their values were similar to those of shallow saltwater ecosystems. In addition, elemental analyses and organic compounds were done using Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) and Gas Chromatography-Mass Spectroscopy (GC-MS), respectively. The concentration of heavy and trace metals in the water samples were within the acceptable limits except for lead which showed high values, while the concentrations of metals in the sediment samples were relatively high and ranged from 6517 to 13,768mg/kg. GC-MS analysis showed the presence of polyaromatic heterocyclic (PAHs) compounds in sediments near the shipping area and in amounts classified as highly carcinogenic; however, no polychlorinated biphenyls (PCB) were identified. Moreover, fecal bacterial contamination in water was detected in concentrations that range between 300 and 10,140 organisms/100mL. Copyright © 2016 Elsevier Ltd. All rights reserved.

[Analysis of biological material originating from the body of general Władysław Sikorski for inorganic poisons and diatoms presence].

PubMed

Sadlik, Józefa Krystyna; Brozek-Mucha, Zuzanna

2009-01-01

Results of the analysis of biological materials originating from the body of general Sikorski are presented in the paper. Samples of the liver, kidney, intestine and lung were analysed for metals and As content, and samples of the lung, liver, kidney, stomach, intestine and bone marrow--for diatoms presence. The analysis for metals and As was performed by atomic absorption spectrometry (AAS) and inductively coupled plasma optical emission spectrometry (ICP-OES). Before the analysis, the samples were wet digested by the classic and microwave assisted method. The analysis did not result in detecting the presence of As, Co, Ni, and Tl in any of the studied materials, while Hg was not revealed in the liver, intestines and lung and Pb in the intestines and lung. The content of Ba, Cd, Cr, Cu, Fe, Mn, Sr and Zn in all the studied materials, Hg in the kidney, and Pb in the liver and kidney did not indicate poisoning by the above-mentioned metals or arsenic. No diatoms were found in the studied materials.

Response to excess copper in the hyperthermophile Sulfolobus solfataricus strain 98/2

PubMed Central

Villafane, Aramis; Voskoboynik, Yekaterina; Cuebas, Mariola; Ruhl, Ilona; Bini, Elisabetta

2009-01-01

Copper is an essential micronutrient, but toxic in excess. Sulfolobus solfataricus cells have the ability to adapt to fluctuations of copper levels in their external environment. To better understand the molecular mechanism behind the organismal response to copper, the expression of the cluster of genes copRTA, which encodes the copper-responsive transcriptional regulator CopR, the copper-binding protein CopT, and CopA, has been investigated and the whole operon has been shown to be cotranscribed at low levels from the copR promoter under all conditions, whereas increased transcription from the copTA promoter occurs in the presence of excess copper. Furthermore, the expression of the copper-transporting ATPase CopA over a 27-hour interval has been monitored by quantitative real-time RT-PCR and compared to the pattern of cellular copper accumulation, as determined in a parallel analysis by Inductively Coupled Plasma Optical Emission spectrometry (ICP-OES). The results provide the basis for a model of the molecular mechanisms of copper homeostasis in Sulfolobus, which relies on copper efflux and sequestration. PMID:19427833

Detection of heavy metals in water in Negeri Sembilan, Malaysia: From source to consumption

NASA Astrophysics Data System (ADS)

Khalaf, Baydaa; Abdullah, Md. Pauzi; Tahrim, Nurfaizah Abu

2018-04-01

Drinking water should be free from harmful levels of impurities, such as heavy metals. The aim of this study is to investigate the heavy metals concentrations in a water reticulation system of Negeri Sembilan. 25 stations were selected along Sungai Linggi (upstream of intake point) and through there reticulation system of Sungai Linggi Water Treatment Plant encompassing raw water through to the last point of use. Sampling activities were carried out in June and July 2016. The samples taken were analysed for heavymetals using an Inductively Coupled Plasma - Optical Emission Spectrometer (ICP-OES). In addition other water quality parameters were measured in situ (pH, water temperature, conductivity and dissolved oxygen) and analysed in the laboratory (BOD, COD, TSS, NH3-N, TOC and residual chlorine). The results showed a high level of Ca in the distribution system, while in the treatment plant it was normal, as well as Fe is decreased. Meanwhile Mn is decreased after treatment processes. The concentrations of DO and temperature in the tap water exceeded the standard concentrations.

Phosphorus Speciation of Sequential Extracts of Organic Amendments using NMR Spectroscopy

NASA Astrophysics Data System (ADS)

Akinremi, O.

2009-04-01

O.O. 1Akinremi Babasola Ajiboye and Donald N. Flaten 1Department of Soil Science, University of Manitoba, Winnipeg, R3T 2NT, Canada We carried out this study in order to determine the forms of phosphorus in various organic amendments using state-of-the art spectroscopic technique. Anaerobically digested biosolids (BIO), hog (HOG), dairy (DAIRY), beef (BEEF) and poultry (POULTRY) manures were subjected to sequential extraction. The extracts were analyzed by solution 31P nuclear magnetic resonance (NMR) spectroscopy. Most of the total P analysed by inductively coupled plasma-optical emission spectroscopy (ICP-OES) in the sequential extracts of organic amendments were orthophosphate, except POULTRY, which was dominated by organic P. The labile P fraction in all the organic amendments, excluding POULTRY, was mainly orthophosphate P from readily soluble calcium and some aluminum phosphates. In the poultry litter, however, Ca phytate was the main P species controlling P solubility. Such knowledge of the differences in the chemical forms of phosphorus in organic amendments are essential for proper management of these amendments for agro-environmental purposes Key words: organic amendments, solution NMR, sequential fractionation, labile phosphorus

Nuclear and analytical methods for investigation of high quality wines

NASA Astrophysics Data System (ADS)

Tonev, D.; Geleva, E.; Grigorov, T.; Goutev, N.; Protohristov, H.; Stoyanov, Ch; Bashev, V.; Tringovska, I.; Kostova, D.

2018-05-01

Nuclear and analytical methods can help to determine the year of production – vintage and the geographical provenance of high quality wines. A complex analytical investigation of Melnik fine wines from “Artarkata” vineyards, Vinogradi village near Melnik in Southwest Bulgaria using different methods and equipment were performed. Nuclear methods, based on measured gamma-ray activity of 137Cs and specific activity of 3H can be used to determine the year of wine production. The specific activity of 137Cs was measured in wines from different vintages using Low-Background High-Resolution Gamma-Spectrometry. Tritium measurements in wine samples were carried out by using a low level liquid scintillation counting in a Packard Tri-Carb 2770 TR/SL liquid scintillation analyzer. The identification of the origin of wines using their chemical fingerprints is of great interest for wine consumers and producers. Determination of 16 chemical elements in samples from soil, wine stems, wine leaves and fine wine from the type Shiroka Melnishka, which are grown in typical Melnik vineyard was made, using Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES).

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

PubMed

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

2015-07-01

In this work, a homogeneity study of a corn flour reference material candidate for inorganic analysis is presented. Seven kilograms of corn flour were used to prepare the material, which was distributed among 100 bottles. The elements Ca, K, Mg, P, Zn, Cu, Fe, Mn and Mo were quantified by inductively coupled plasma optical emission spectrometry (ICP OES) after acid digestion procedure. The method accuracy was confirmed by analyzing the rice flour certified reference material, NIST 1568a. All results were evaluated by analysis of variance (ANOVA) and principal component analysis (PCA). In the study, a sample mass of 400mg was established as the minimum mass required for analysis, according to the PCA. The between-bottle test was performed by analyzing 9 bottles of the material. Subsamples of a single bottle were analyzed for the within-bottle test. No significant differences were observed for the results obtained through the application of both statistical methods. This fact demonstrates that the material is homogeneous for use as a laboratory reference material. Copyright © 2015 Elsevier Ltd. All rights reserved.

A rapid and reliable method for Pb isotopic analysis of peat and lichens by laser ablation-quadrupole-inductively coupled plasma-mass spectrometry for biomonitoring and sample screening.

PubMed

Kylander, M E; Weiss, D J; Jeffries, T E; Kober, B; Dolgopolova, A; Garcia-Sanchez, R; Coles, B J

2007-01-16

An analytical protocol for rapid and reliable laser ablation-quadrupole (LA-Q)- and multi-collector (MC-) inductively coupled plasma-mass spectrometry (ICP-MS) analysis of Pb isotope ratios ((207)Pb/(206)Pb and (208)Pb/(206)Pb) in peats and lichens is developed. This technique is applicable to source tracing atmospheric Pb deposition in biomonitoring studies and sample screening. Reference materials and environmental samples were dry ashed and pressed into pellets for introduction by laser ablation. No binder was used to reduce contamination. LA-MC-ICP-MS internal and external precisions were <1.1% and <0.3%, respectively, on both (207)Pb/(206)Pb and (208)Pb/(206)Pb ratios. LA-Q-ICP-MS internal precisions on (207)Pb/(206)Pb and (208)Pb/(206)Pb ratios were lower with values for the different sample sets <14.3% while external precisions were <2.9%. The level of external precision acquired in this study is high enough to distinguish between most modern Pb sources. LA-MC-ICP-MS measurements differed from thermal ionisation mass spectrometry (TIMS) values by 1% or less while the accuracy obtained using LA-Q-ICP-MS compared to solution MC-ICP-MS was 3.1% or better using a run bracketing (RB) mass bias correction method. Sample heterogeneity and detector switching when measuring (208)Pb by Q-ICP-MS are identified as sources of reduced analytical performance.

Kinetic modeling on CO₂ capture using basic oxygen furnace slag coupled with cold-rolling wastewater in a rotating packed bed.

PubMed

Chang, E-E; Chen, Tse-Lun; Pan, Shu-Yuan; Chen, Yi-Hung; Chiang, Pen-Chi

2013-09-15

In this study, direct and indirect carbonation of basic oxygen furnace slag (BOFS) coupled with cold-rolling wastewater (CRW) was carried out via a rotating packed bed (RPB). The solid products were qualitatively characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) and quantitatively analyzed with thermogravimetric analysis (TGA). The leachate was analyzed with inductively coupled plasma-optical emission spectroscopy (ICP-OES). The results indicate that the maximum achievable carbonation conversion (MACC) of BOFS was 90.7%, corresponding to a capture capacity of 0.277 g CO₂/g of BOFS, by direct carbonation with CRW under a rotation speed of 750 rpm at 30 °C for 20 min. In addition, CO₂ mass balance among the gas, liquid, and solid phases within an RPB was well-developed, with an error less than 10%, to confirm the actual CO₂ capture capacity of BOFS with precision and accuracy. Furthermore, a reaction kinetic model based on mass balance was established to determine the reaction rate constant for various liquid agents (CRW and pure water). It was concluded that co-utilization of alkaline wastes including BOFS and CRW via the RPB is a novel approach for both enhancing CO₂ capture capacity and reducing the environmental impacts of alkaline wastes. Copyright © 2013 Elsevier B.V. All rights reserved.

Atlas of Atomic Spectral Lines of Neptunium Emitted by Inductively Coupled Plasma

DOE Office of Scientific and Technical Information (OSTI.GOV)

DeKalb, E.L. and Edelson, M. C.

1987-08-01

Optical emission spectra from high-purity Np-237 were generated with a glovebox-enclosed inductively coupled plasma (ICP) source. Spectra covering the 230-700 nm wavelength range are presented along with general commentary on the methodology used in collecting the data. The Ames Laboratory Nuclear Safeguards and Security Program has been charged with the task of developing optical spectroscopic methods to analyze the composition of spent nuclear fuels. Such materials are highly radioactive even after prolonged 'cooling' and are chemically complex. Neptunium (Np) is a highly toxic by-product of nuclear power generation and is found, in low abundance, in spent nuclear fuels. This atlasmore » of the optical emission spectrum of Np, as produced by an inductively coupled plasma (ICP) spectroscopic source, is part of a general survey of the ICP emission spectra of the actinide elements. The ICP emission spectrum of the actinides originates almost exclusively from the electronic relaxation of excited, singly ionized species. Spectral data on the Np ion emission spectrum (i.e., the Np II spectrum) have been reported by Tomkins and Fred [1] and Haaland [2]. Tomkins and Fred excited the Np II spectrum with a Cu spark discharge and identified 114 Np lines in the 265.5 - 436.3 nm spectral range. Haaland, who corrected some spectral line misidentifications in the work of Tomkins and Fred, utilized an enclosed Au spark discharge to excite the Np II spectrum and reported 203 Np lines within the 265.4 - 461.0 nm wavelength range.« less

Determination of trace amounts of rare-earth elements in highly pure neodymium oxide by sector field inductively coupled plasma mass spectrometry (ICP-SFMS) and high-performance liquid chromatography (HPLC) techniques

NASA Astrophysics Data System (ADS)

Pedreira, W. R.; Sarkis, J. E. S.; da Silva Queiroz, C. A.; Rodrigues, C.; Tomiyoshi, I. A.; Abrão, A.

2003-02-01

Recently rare-earth elements (REE) have received much attention in fields of geochemistry and industry. Rapid and accurate determinations of them are increasingly required as industrial demands expand. Sector field inductively coupled plasma mass spectrometry (ICP-SFMS) with high-performance liquid chromatography (HPLC) has been applied to the determination of REE. HR ICP-MS was used as an element-selective detector for HPLC in highly pure materials. The separation of REE with HPLC helped to avoid erroneous analytical results due to spectral interferences. Sixteen elements (Sc, Y and 14 lanthanides) were determined selectively with the HPLC/ICP-SFMS system using a concentration gradient methods. The detection limits with the HPLC/ICP-SFMS system were about 0.5-10 pg mL-1. The percentage recovery ranged from 90% to 100% for different REE. The %RSD of the methods varying between 2.5% and 4.5% for a set of five (n=5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two highly pure neodymium oxides samples (IPEN and Johnson Matthey Company) were performed. In short, the IPEN's materials which are highly pure (>99.9%) were successfully analyzed without spectral interferences.

Evaluation of methods for trace-element determination with emphasis on their usability in the clinical routine laboratory.

PubMed

Bolann, B J; Rahil-Khazen, R; Henriksen, H; Isrenn, R; Ulvik, R J

2007-01-01

Commonly used techniques for trace-element analysis in human biological material are flame atomic absorption spectrometry (FAAS), graphite furnace atomic absorption spectrometry (GFAAS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). Elements that form volatile hydrides, first of all mercury, are analysed by hydride generation techniques. In the absorption techniques the samples are vaporized into free, neutral atoms and illuminated by a light source that emits the atomic spectrum of the element under analysis. The absorbance gives a quantitative measure of the concentration of the element. ICP-AES and ICP-MS are multi-element techniques. In ICP-AES the atoms of the sample are excited by, for example, argon plasma at very high temperatures. The emitted light is directed to a detector, and the optical signals are processed to values for the concentrations of the elements. In ICP-MS a mass spectrometer separates and detects ions produced by the ICP, according to their mass-to-charge ratio. Dilution of biological fluids is commonly needed to reduce the effect of the matrix. Digestion using acids and microwave energy in closed vessels at elevated pressure is often used. Matrix and spectral interferences may cause problems. Precautions should be taken against trace-element contamination during collection, storage and processing of samples. For clinical problems requiring the analysis of only one or a few elements, the use of FAAS may be sufficient, unless the higher sensitivity of GFAAS is required. For screening of multiple elements, however, the ICP techniques are preferable.

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION, AND MAINTENANCE OF THE JOBIN-YVON MODEL 70 INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETER (BCO-L-7.1)

EPA Science Inventory

The purpose of this SOP is to detail the operation and maintenance of an Instruments, SA Inc., Jobin-Yvon Model 70 (JY-70) inductively coupled plasma atomic emissions spectrometry (ICP-AES). This procedure was followed to ensure consistent data retrieval during the Arizona NHEXA...

Determination of Total Arsenic and Speciation in Apple Juice by Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry: An Experiment for the Analytical Chemistry Laboratory

ERIC Educational Resources Information Center

He, Ping; Colon, Luis A.; Aga, Diana S.

2016-01-01

A two-part laboratory experiment was designed for upper-level analytical chemistry students to provide hands-on experience in the use of high performance liquid chromatography (HPLC) for separation and inductively coupled plasma mass spectrometry (ICP-MS) for detection. In the first part of the experiment, the students analyze total arsenic in…

Deep inductively coupled plasma etching of ELO-GaN grown with high fill factor

NASA Astrophysics Data System (ADS)

Gao, Haiyong; Lee, Jaesoong; Ni, Xianfeng; Leach, Jacob; Özgür, Ümit; Morkoç, Hadis

2011-02-01

The epitaxial lateral overgrowth (ELO) gallium nitride (GaN) was grown with high fill factor using metal organic chemical vapor deposition (MOCVD). The inductively coupled plasma (ICP) etching of ELO-GaN based on Cl2/Ar/SiCl4 gas mixture was performed. Surface properties of ELO-GaN subjected to ICP etching have been investigated and optimized etching condition in ELO-GaN with ICP etching is presented. Radiofrequency (RF) power and the flow rate of Cl2 gas were modified during the experiments. The window region, wing region and the edge region of ELO-GaN pattern present different etching characteristics. Different etching conditions were studied to get the minimized plasma-induced damage, relatively high etching rates, and excellent surface profiles. Etch depths of the etched ELO-GaN with smooth surface up to about 19 μm were achieved. The most suitable three-step etching condition is discussed with the assessment based on the morphology observation of the etched surface of ELO-GaN patterns.

Characteristics of n-GaN After Cl2/Ar and Cl2/N2 Inductively Coupled Plasma Etching

NASA Astrophysics Data System (ADS)

Han, Yan-Jun; Xue, Song; Guo, Wen-Ping; Sun, Chang-Zheng; Hao, Zhi-Biao; Luo, Yi

2003-10-01

A systematic study on the effect of inductively coupled plasma (ICP) etching on n-type GaN is presented. The optical and electrical properties and surface stoichiometry of n-type GaN are evaluated using room-temperature photoluminescence (PL) and current-voltage (I-V) characteristic measurements, and X-ray photoelectron spectroscopy (XPS), respectively. Investigation of the effect of additive gas (N2 and Ar) and RF power on these characteristics has also been carried out. It is shown that the decrease in the O/Ga ratio after ICP etching can suppress the deterioration of the near-band-edge emission intensity. Furthermore, N vacancy (VN) with a shallow donor nature and Ga vacancy (VGa) with a deep acceptor nature are generated after ICP etching upon the addition of Ar and N2 to Cl2 plasma, respectively. Lower ohmic contact resistance could be obtained when VN or ion-bombardment-induced defect is dominant at the surface. Improved etching conditions have been obtained based on these results.

Isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS) for the certification of lead and cadmium in environmental standard reference materials.

PubMed

Murphy, K E; Beary, E S; Rearick, M S; Vocke, R D

2000-10-01

Lead (Pb) and cadmium (Cd) have been determined in six new environmental standard reference materials (SRMs) using isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS). The SRMs are the following: SRM 1944, New York-New Jersey Waterway Sediment, SRMs 2583 and 2584, Trace Elements in Indoor Dust, Nominal 90 mg/kg and 10,000 mg/kg Lead, respectively, SRMs 2586 and 2587, Trace Elements in Soil Containing Lead from Paint, Nominal 500 mg/kg and 3,000 mg/kg Lead, respectively, and SRM 2782, Industrial Sludge. The capabilities of ID ICP-MS for the certification of Pb and Cd in these materials are assessed. Sample preparation and ratio measurement uncertainties have been evaluated. Reproducibility and accuracy of the established procedures are demonstrated by determination of gravimetrically prepared primary standard solutions and by comparison with isotope dilution thermal ionization mass spectrometry (ID TIMS). Material heterogeneity was readily demonstrated to be the dominant source of uncertainty in the certified values.

Upcycling Waste Lard Oil into Vertical Graphene Sheets by Inductively Coupled Plasma Assisted Chemical Vapor Deposition.

PubMed

Wu, Angjian; Li, Xiaodong; Yang, Jian; Du, Changming; Shen, Wangjun; Yan, Jianhua

2017-10-12

Vertical graphene (VG) sheets were single-step synthesized via inductively coupled plasma (ICP)-enhanced chemical vapor deposition (PECVD) using waste lard oil as a sustainable and economical carbon source. Interweaved few-layer VG sheets, H₂, and other hydrocarbon gases were obtained after the decomposition of waste lard oil. The influence of parameters such as temperature, gas proportion, ICP power was investigated to tune the nanostructures of obtained VG, which indicated that a proper temperature and H₂ concentration was indispensable for the synthesis of VG sheets. Rich defects of VG were formed with a high I D / I G ratio (1.29), consistent with the dense edges structure observed in electron microscopy. Additionally, the morphologies, crystalline degree, and wettability of nanostructure carbon induced by PECVD and ICP separately were comparatively analyzed. The present work demonstrated the potential of our PECVD recipe to synthesize VG from abundant natural waste oil, which paved the way to upgrade the low-value hydrocarbons into advanced carbon material.

High-Temperature Isothermal Capacitance Transient Spectroscopy Study on Inductively Coupled Plasma Etching Damage for p-GaN Surfaces

NASA Astrophysics Data System (ADS)

Aoki, Toshichika; Wakayama, Hisashi; Kaneda, Naoki; Mishima, Tomoyoshi; Nomoto, Kazuki; Shiojima, Kenji

2013-11-01

The effects of the inductively coupled plasma (ICP) etching damage on the electrical characteristics of low-Mg-doped p-GaN Schottky contacts were evaluated by high-temperature isothermal capacitance transient spectroscopy. A large single peak for an acceptor-type surface state was dominantly detected for as-grown samples. The energy level and state density were obtained to be 1.18 eV above the valence band, which is close to a Ga vacancy (VGa), and 1.5×1013 cm-2, respectively. It was speculated that a small portion of Ga atoms were missing from the surface, and a high VGa density was observed in a few surface layers. The peak intensity decreased by 60% upon annealing at 800 °C, and further decrease was found by ICP etching. This decrease is consistent with the suppression of the memory effect in current-voltage characteristics. Upon annealing and ICP etching, since the VGa structure might be disordered, the peak intensity decreased.

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

DOEpatents

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

2010-08-03

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

DPASV analytical technique for ppb level uranium analysis

NASA Astrophysics Data System (ADS)

Pal, Sangita; Singha, Mousumi; Meena, Sher Singh

2018-04-01

Determining uranium in ppb level is considered to be most crucial for reuse of water originated in nuclear industries at the time of decontamination of plant effluents generated during uranium (fuel) production, fuel rod fabrication, application in nuclear reactors and comparatively small amount of effluents obtained during laboratory research and developmental work. Higher level of uranium in percentage level can be analyzed through gravimetry, titration etc, whereas inductively coupled plasma-atomic energy spectroscopy (ICP-AES), fluorimeter are well suited for ppm level. For ppb level of uranium, inductively coupled plasma - mass spectroscopy (ICP-MS) or Differential Pulse Anodic Stripping Voltammetry (DPASV) serve the purpose. High precision, accuracy and sensitivity are the crucial for uranium analysis in trace (ppb) level, which are satisfied by ICP-MS and stripping voltammeter. Voltammeter has been found to be less expensive, requires low maintenance and is convenient for measuring uranium in presence of large number of other ions in the waste effluent. In this paper, necessity of uranium concentration quantification for recovery as well as safe disposal of plant effluent, working mechanism of voltammeter w.r.t. uranium analysis in ppb level with its standard deviation and a data comparison with ICP-MS has been represented.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; preparation procedure for aquatic biological material determined for trace metals

USGS Publications Warehouse

Hoffman, Gerald L.

1996-01-01

A method for the chemical preparation of tissue samples that are subsequently analyzed for 22 trace metals is described. The tissue-preparation procedure was tested with three National Institute of Standards and Technology biological standard reference materials and two National Water Quality Laboratory homogenized biological materials. A low-temperature (85 degrees Celsius) nitric acid digestion followed by the careful addition of hydrogen peroxide (30-percent solution) is used to decompose the biological material. The solutions are evaporated to incipient dryness, reconstituted with 5 percent nitric acid, and filtered. After filtration the solutions were diluted to a known volume and analyzed by inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), and cold vapor-atomic absorption spectrophotometry (CV-AAS). Many of the metals were determined by both ICP-MS and ICP-AES. This report does not provide a detailed description of the instrumental procedures and conditions used with the three types of instrumentation for the quantitation of trace metals determined in this study. Statistical data regarding recovery, accuracy, and precision for individual trace metals determined in the biological material tested are summarized.

Visualizing fossilization using laser ablation-inductively coupled plasma-mass spectrometry maps of trace elements in Late Cretaceous bones

USGS Publications Warehouse

Koenig, A.E.; Rogers, R.R.; Trueman, C.N.

2009-01-01

Elemental maps generated by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) provide a previously unavailable high-resolution visualization of the complex physicochemical conditions operating within individual bones during the early stages of diagenesis and fossilization. A selection of LA-ICP-MS maps of bones collected from the Late Cretaceous of Montana (United States) and Madagascar graphically illustrate diverse paths to recrystallization, and reveal unique insights into geochemical aspects of taphonomic history. Some bones show distinct gradients in concentrations of rare earth elements and uranium, with highest concentrations at external bone margins. Others exhibit more intricate patterns of trace element uptake related to bone histology and its control on the flow paths of pore waters. Patterns of element uptake as revealed by LA-ICP-MS maps can be used to guide sampling strategies, and call into question previous studies that hinge upon localized bulk samples of fossilized bone tissue. LA-ICP-MS maps also allow for comparison of recrystallization rates among fossil bones, and afford a novel approach to identifying bones or regions of bones potentially suitable for extracting intact biogeochemical signals. ?? 2009 Geological Society of America.

Resolution of rare earth element interferences in fossil energy by-product samples using sector-field ICP-MS

DOE PAGES

Thompson, Robert L.; Bank, Tracy; Roth, Elliot; ...

2016-07-30

Here, the supply and price of rare earth elements (REEs) have become a concern to many countries in the world, which has led to renewed interest in exploration and recovery of REEs from secondary or waste sources. Potential high REE waste sources that are of particular interest are coal mining, preparation, combustion, and other fossil energy by-products, including those from natural gas production. In this work, we have examined a set of five solid samples from the treatment of produced and flowback water containing elevated concentrations of barium. In order to confirm the correct concentrations of Eu, we studied thesemore » materials using sector field inductively coupled plasma mass spectrometry (SF-ICP-MS), which is capable of resolving species of nearly identical masses, including Eu and BaO. While the use of quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS) for the REE analysis of most geological sample matrices should pose no problem, the presence of large amounts of Ba, as encountered in water treatment solids from natural gas produced and flowback samples may require SF-ICP-MS for accurate determination of all REEs.« less

Feasibility of Rare Earth Element Determination in Low Concentration in Crude Oil: Direct Sampling Electrothermal Vaporization-Inductively Coupled Plasma Mass Spectrometry.

PubMed

Silva, Jussiane Souza; Schneider Henn, Alessandra; Dressler, Valderi Luiz; Mello, Paola Azevedo; Flores, Erico Marlon Moraes

2018-06-05

A comprehensive study was developed showing the feasibility of determination of rare earth elements (REE) in low concentration in crude oil by using direct sampling electrothermal vaporization system coupled to inductively coupled plasma mass spectrometry (ETV-ICP-MS). The effect of organic modifier on the REE signal was evaluated and the use of 6 mg of citric acid allowed calibration using aqueous reference solutions (selected pyrolysis and vaporization temperatures were 700 and 2200 °C, respectively). Because of the facility of REE in forming refractory compounds inside the graphite furnace during the heating step, the use of a modifier gas (Freon R-12, 3.0 mL min -1 ) was necessary to allow quantitative vaporization of these elements. A flow rate of 0.40 L min -1 was selected for both bypass and carrier gases. Under optimized conditions, the influence of sample mass was evaluated, and even using a relatively high mass of crude oil (up to 18 mg), accurate results were obtained. The accuracy was evaluated by the comparison of results by ETV-ICP-MS with those obtained by ICP-MS with ultrasonic nebulizer (USN) after high-pressure microwave-assisted wet digestion (MAWD) and microwave-induced combustion (MIC) and no statistical difference was observed between the results. The limits of quantification for REE by ETV-ICP-MS were lower (0.02-0.8 ng g -1 ) than those obtained by USN-ICP-MS after MAWD and MIC (0.6-5.1 ng g -1 ). Negligible blank values and relative standard deviations lower than 12% show the feasibility of the proposed ETV-ICP-MS method for routine analysis of crude oil.

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

PubMed

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

2016-12-01

Ionic liquids-β-cyclodextrin polymer (ILs-β-CDCP) was attached on Fe 3 O 4 nanoparticles to prepare magnetic solid phase extraction agent (Fe 3 O 4 @ILs-β-CDCP). The properties and morphology of Fe 3 O 4 @ILs-β-CDCP were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction(XRD), size distribution and magnetic analysis. A new method of magnetic solid phase extraction (MSPE) coupled to ICP-OES for the speciation of Mn(II)/Mn(VII) in water samples was established. The results showed that Mn(VII) and total manganese [Mn(II)+Mn(VII)] were quantitatively extracted after adjusting aqueous sample solution to pH 6.0 and 10.0, respectively. Mn(II) was calculated by subtraction of Mn(VII) from total manganese. Fe 3 O 4 @ILs-β-CDCP showed a higher adsorption capacity toward Mn(II) and Mn(VII). Several factors, such as the pH value, extraction temperature and sample volume, were optimized to achieve the best extraction efficiency. Moreover, the adsorption ability of Fe 3 O 4 @ILs-β-CDCP would not be significantly lower after reusing of 10 times. The accuracy of the developed method was confirmed by analyzing certified reference materials (GSB 07-1189-2000), and by spiking spring water, city water and lake water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Behavior of microorganisms in drinking water treatment by inductively coupled plasma system: Case study in ground water

NASA Astrophysics Data System (ADS)

Desmiarti, Reni; Hazmi, Ariadi; Martynis, Munas; Sutopo, Ulung Muhammad; Li, Fusheng

2018-02-01

Pathogenic bacteria, such as total coliforms (TC), fecal coliforms (FC) and other coliforms (OC), were removed from groundwater by inductively coupled plasma system treatment in continuous flow experiments. The objective of this study is to investigate the effect of flowrate and frequency on the behavior of microorganisms in drinking water treatment using inductively coupled plasma system (ICPS). The results showed that after 120 minutes of ICPS treatment, the removal efficiency with respect to TC, FC and OC decreased with increasing flowrate. The removal efficiency of FC was achieved at 100% in all runs. Compared to FC, the removal efficiencies with respect to TC and FC were lower than those with respect to TC and OC in the following order: FC >OC> TC. The disinfection yield of TC and OC significantly increased when the removal efficiency increased. The electromagnetic flux varied from 8.08±0.46 to 10.54±0.19 W/cm2. The results in the present work can be used to design a new technology for drinking water treatment to remove all pathogenic bacteria without using hazardous chemicals.

Role of laser ablation-inductively coupled plasma-mass spectrometry in cultural heritage research: a review.

PubMed

Giussani, Barbara; Monticelli, Damiano; Rampazzi, Laura

2009-03-02

Cultural heritage represents a bridge between the contemporary society and the past populations, and a strong collaboration between archaeologists, art historians and analysts may lead to the decryption of the information hidden in an ancient object. Quantitative elemental compositional data play a key role in solving questions concerning dating, provenance, technology, use and the relationship of ancient cultures with the environment. Nevertheless, the scientific investigation of an artifact should be carried out complying with some important constraints: above all the analyses should be as little destructive as possible and performed directly on the object to preserve its integrity. Laser ablation sampling coupled to inductively coupled plasma-mass spectrometry (LA-ICP-MS) fulfils these requirements exhibiting comparably strong analytical performance in trace element determination. This review intends to show through the applications found in the literature how valuable is the contribution of LA-ICP-MS in the investigation of ancient materials such as obsidian, glass, pottery, human remains, written heritage, metal objects and miscellaneous stone materials. The main issues related to cultural heritage investigation are introduced, followed by a brief description of the features of this technique. An overview of the exploitation of LA-ICP-MS is then presented. Finally, advantages and drawbacks of this technique are critically discussed: the fit for purpose and prospects of the use of LA-ICP-MS are presented.

Investigation of heavy-metal accumulation in selected plant samples using laser induced breakdown spectroscopy and laser ablation inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Galiová, M.; Kaiser, J.; Novotný, K.; Novotný, J.; Vaculovič, T.; Liška, M.; Malina, R.; Stejskal, K.; Adam, V.; Kizek, R.

2008-12-01

Single-pulse Laser-Induced Breakdown Spectroscopy (LIBS) and Laser-Ablation Inductively Coupled Plasma Mass-Spectrometry (LA-ICP-MS) were applied for mapping the silver and copper distribution in Helianthus Annuus L. samples treated with contaminant in controlled conditions. For Ag and Cu detection the 328.07 nm Ag(I) and 324.75 nm Cu(I) lines were used, respectively. The LIBS experimental conditions (mainly the laser energy and the observation window) were optimized in order to avoid self-absorption effect in the measured spectra. In the LA-ICP-MS analysis the Ag 107 and Cu 63 isotopes were detected. The capability of these two analytical techniques for high-resolution mapping of selected trace chemical elements was demonstrated.

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

USGS Publications Warehouse

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

1987-01-01

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

The use of inductively coupled plasma mass spectrometry (ICP-MS) for the determination of toxic and essential elements in different types of food samples

NASA Astrophysics Data System (ADS)

Voica, C.; Dehelean, A.; Kovacs, M. H.

2012-02-01

Food is the primary source of essential elements for humans and it is an important source of exposure to toxic elements. In this context, levels of essential and toxic elements must be determined routinely in consumed food products. The content of trace elements (As, Pb, Cu, Cd, Zn, Sn, Hg) in different types of food samples (e.g. rice, bread, sugar, cheese, milk, butter, wheat, coffee, chocolate, biscuits pasta, etc.) was determined, using inductively coupled plasma mass spectrometry (ICP-MS). Trace element contents in some foods were higher than maximum permissible levels of toxic metals in human food (Cd in bread, Zn in cheese, Cu in coffee, Hg in carrots and peppers).

Determination of trace-level haloacetic acids in drinking water by ion chromatography-inductively coupled plasma mass spectrometry.

PubMed

Liu, Yongjian; Mou, Shifen; Chen, Dengyun

2004-06-11

A new method for the determination of nine haloacetic acids (HAAs) with ion chromatography (IC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) was developed. With the very hydrophilic anion-exchange column and steep gradient of sodium hydroxide, the nine HAAs could be well separated in 15 min. After suppression with an ASRS suppressor that was introduced in between IC and ICP-MS, the background was much decreased, the interference caused by sodium ion present in eluent was removed, and the sensitivities of HAAs were greatly improved. The chlorinated and brominated HAAs could be detected as 35ClO and 79Br without interference of the matrix due to the elemental selective ICP-MS. The detection limits for mono-, di-, trichloroacetic acids were between 15.6 and 23.6 microg/l. For the other six bromine-containing HAAs, the detection limits were between 0.34 and 0.99 microg/l. With the pretreatment of OnGuard Ag cartridge to remove high concentration of chloride in sample, the developed method could be applied to the determination of HAAs in many drinking water matrices.

Current role of ICP-MS in clinical toxicology and forensic toxicology: a metallic profile.

PubMed

Goullé, Jean-Pierre; Saussereau, Elodie; Mahieu, Loïc; Guerbet, Michel

2014-08-01

As metal/metalloid exposure is inevitable owing to its omnipresence, it may exert toxicity in humans. Recent advances in metal/metalloid analysis have been made moving from flame atomic absorption spectrometry and electrothermal atomic absorption spectrometry to the multi-elemental inductively coupled plasma (ICP) techniques as ICP atomic emission spectrometry and ICP-MS. ICP-MS has now emerged as a major technique in inorganic analytical chemistry owing to its flexibility, high sensitivity and good reproducibility. This in depth review explores the ICP-MS metallic profile in human toxicology. It is now routinely used and of great importance, in clinical toxicology and forensic toxicology to explore biological matrices, specifically whole blood, plasma, urine, hair, nail, biopsy samples and tissues.

The Uranium from Seawater Program at the Pacific Northwest National Laboratory: Overview of Marine Testing, Adsorbent Characterization, Adsorbent Durability, Adsorbent Toxicity, and Deployment Studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gill, Gary A.; Kuo, Li-Jung; Janke, Chris J.

The Pacific Northwest National Laboratory’s (PNNL) Marine Science Laboratory (MSL) located along the coast of Washington State is evaluating the performance of uranium adsorption materials being developed for seawater extraction under realistic marine conditions with natural seawater. Two types of exposure systems were employed in this program: flow-through columns for testing of fixed beds of individual fibers and pellets and a recirculating water flume for testing of braided adsorbent material. Testing consists of measurements of the adsorption of uranium and other elements from seawater as a function of time, typically 42 to 56 day exposures, to determine the adsorbent capacitymore » and adsorption rate (kinetics). Analysis of uranium and other trace elements collected by the adsorbents was conducted following strong acid digestion of the adsorbent with 50% aqua regia using either Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) or Inductively Coupled Plasma Mass Spectrometer (ICP-MS). The ORNL 38H adsorbent had a 56 day adsorption capacity of 3.30 ± 0.68 g U/ kg adsorbent (normalized to a salinity of 35 psu), a saturation adsorption capacity of 4.89 ± 0.83 g U/kg of adsorbent material (normalized to a salinity of 35 psu) and a half-saturation time of 28 ± 10 days. The AF1 adsorbent material had a 56 day adsorption capacity of 3.9 ± 0.2 g U/kg adsorbent material (normalized to a salinity of 35 psu), a saturation capacity of 5.4 ± 0.2 g U/kg adsorbent material (normalized to a salinity of 35 psu) and a half saturation time of 23 ± 2 days. The ORNL amidoxime-based adsorbent materials are not specific for uranium, but also adsorb other elements from seawater. The major doubly charged cations in seawater (Ca and Mg) account for a majority of the cations adsorbed (61% by mass and 74% by molar percent). For the ORNL AF1 adsorbent material, U is the 4th most abundant element adsorbed by mass and 7th most abundant by molar percentage« less

Sediment Source Analysis at Malakoff Diggins State Historic Park, California

NASA Astrophysics Data System (ADS)

Ward, A. J., IV; Monohan, C.; Matiasek, S. J.; Alpers, C. N.; Curtis, J.; Campbell, K. M.; Roth, D. A.; Howle, J.

2016-12-01

This study aims to identify the sources of suspended sediment and trace metals which are discharged during storm events into Humbug Creek from Malakoff Diggins State Historic Park (MDSHP) in Nevada County, California. MDSHP includes a pit where approximately 32,000,000 cubic meters of auriferous Eocene gravel was mined by hydraulic and dredging methods during 1866-1884 and 1893-1910. High erosion rates within the pit contribute to water-quality impairment downstream; Humbug Creek is listed as an impaired water body under section 303(d) of the Clean Water Act because of suspended sediment, copper, mercury, and zinc. Sediment fingerprinting techniques (mineralogy and geochemistry) are being used to identify stratigraphic units in the pit responsible for delivering the greatest volume of sediment to the pit drain at Hiller Tunnel, which flows to Humbug Creek. In-situ sediment samples were collected in 2015 along four vertical transects located in the mine pit. Additionally, surface water samples were collected during 2015 and 2016 within the pit and Hiller Tunnel, targeting drainage networks below the in-situ sampling sites. In-situ and suspended sediment samples were analyzed for grain-size distribution, X-ray diffraction (XRD) to obtain quantitative mineralogy, inductively coupled plasma - mass spectrometry (ICP-MS) for trace elements, and inductively coupled plasma - optical emission spectroscopy (ICP-OES) for major elements. Preliminary XRD data indicate that the fine suspended sediment in Hiller Tunnel is composed predominantly of kaolinite and halloysite, with minor smectite, illite, and muscovite. Kaolinite is abundant in many of the samples from the in-situ vertical transects, but relatively few stratigraphic units have abundant halloysite. Quantitative erosion rates from a time series of terrestrial LiDAR measurements (2014-16) and from historical aerial photos will help to refine possible scenarios regarding sediment sources within the pit. Chemical and physical characterization of the in-situ sediments may reveal key indicators, or fingerprints, which will allow for a more efficient application of mitigation efforts in MDSHP by identifying which stratigraphic units are delivering high amounts of sediment to Humbug Creek.

Determination of phosphorus in small amounts of protein samples by ICP-MS.

PubMed

Becker, J Sabine; Boulyga, Sergei F; Pickhardt, Carola; Becker, J; Buddrus, Stefan; Przybylski, Michael

2003-02-01

Inductively coupled plasma mass spectrometry (ICP-MS) is used for phosphorus determination in protein samples. A small amount of solid protein sample (down to 1 micro g) or digest (1-10 micro L) protein solution was denatured in nitric acid and hydrogen peroxide by closed-microvessel microwave digestion. Phosphorus determination was performed with an optimized analytical method using a double-focusing sector field inductively coupled plasma mass spectrometer (ICP-SFMS) and quadrupole-based ICP-MS (ICP-QMS). For quality control of phosphorus determination a certified reference material (CRM), single cell proteins (BCR 273) with a high phosphorus content of 26.8+/-0.4 mg g(-1), was analyzed. For studies on phosphorus determination in proteins while reducing the sample amount as low as possible the homogeneity of CRM BCR 273 was investigated. Relative standard deviation and measurement accuracy in ICP-QMS was within 2%, 3.5%, 11% and 12% when using CRM BCR 273 sample weights of 40 mg, 5 mg, 1 mg and 0.3 mg, respectively. The lowest possible sample weight for an accurate phosphorus analysis in protein samples by ICP-MS is discussed. The analytical method developed was applied for the analysis of homogeneous protein samples in very low amounts [1-100 micro g of solid protein sample, e.g. beta-casein or down to 1 micro L of protein or digest in solution (e.g., tau protein)]. A further reduction of the diluted protein solution volume was achieved by the application of flow injection in ICP-SFMS, which is discussed with reference to real protein digests after protein separation using 2D gel electrophoresis.The detection limits for phosphorus in biological samples were determined by ICP-SFMS down to the ng g(-1) level. The present work discusses the figure of merit for the determination of phosphorus in a small amount of protein sample with ICP-SFMS in comparison to ICP-QMS.

Authentication of Kalix (N.E. Sweden) vendace caviar using inductively coupled plasma-based analytical techniques: evaluation of different approaches.

PubMed

Rodushkin, I; Bergman, T; Douglas, G; Engström, E; Sörlin, D; Baxter, D C

2007-02-05

Different analytical approaches for origin differentiation between vendace and whitefish caviars from brackish- and freshwaters were tested using inductively coupled plasma double focusing sector field mass spectrometry (ICP-SFMS) and multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). These approaches involve identifying differences in elemental concentrations or sample-specific isotopic composition (Sr and Os) variations. Concentrations of 72 elements were determined by ICP-SFMS following microwave-assisted digestion in vendace and whitefish caviar samples from Sweden (from both brackish and freshwater), Finland and USA, as well as in unprocessed vendace roe and salt used in caviar production. This data set allows identification of elements whose contents in caviar can be affected by salt addition as well as by contamination during production and packaging. Long-term method reproducibility was assessed for all analytes based on replicate caviar preparations/analyses and variations in element concentrations in caviar from different harvests were evaluated. The greatest utility for differentiation was demonstrated for elements with varying concentrations between brackish and freshwaters (e.g. As, Br, Sr). Elemental ratios, specifically Sr/Ca, Sr/Mg and Sr/Ba, are especially useful for authentication of vendace caviar processed from brackish water roe, due to the significant differences between caviar from different sources, limited between-harvest variations and relatively high concentrations in samples, allowing precise determination by modern analytical instrumentation. Variations in the 87Sr/86Sr ratio for vendace caviar from different harvests (on the order of 0.05-0.1%) is at least 10-fold less than differences between caviar processed from brackish and freshwater roe. Hence, Sr isotope ratio measurements (either by ICP-SFMS or by MC-ICP-MS) have great potential for origin differentiation. On the contrary, it was impossible to differentiate between Swedish caviar processed from brackish water roe and Finnish freshwater caviar based solely on 187Os/188Os ratios.

Trace element analysis of synthetic mono- and poly-crystalline CaF 2 by ultraviolet laser ablation inductively coupled plasma mass spectrometry at 266 and 193 nm

NASA Astrophysics Data System (ADS)

Koch, J.; Feldmann, I.; Hattendorf, B.; Günther, D.; Engel, U.; Jakubowski, N.; Bolshov, M.; Niemax, K.; Hergenröder, R.

2002-06-01

The analytical figures of merit for ultraviolet laser ablation-inductively coupled plasma mass spectrometry (UV-LA-ICP-MS) at 266 nm with respect to the trace element analysis of high-purity, UV-transmitting alkaline earth halides are investigated and discussed. Ablation threshold energy density values and ablation rates for mono- and poly-crystalline CaF 2 samples were determined. Furthermore, Pb-, Rb-, Sr-, Ba- and Yb-specific analysis was performed. For these purposes, a pulsed Nd:YAG laser operated at the fourth harmonic of the fundamental wavelength (λ=266 nm) and a double-focusing sector field ICP-MS detector were employed. Depending on the background noise and isotope-specific sensitivity, the detection limits typically varied from 0.7 ng/g for Sr to 7 ng/g in the case of Pb. The concentrations were determined using a glass standard reference material (SRM NIST612). In order to demonstrate the sensitivity of the arrangement described, comparative measurements by means of a commercial ablation system consisting of an ArF excimer laser (λ=193 nm) and a quadrupole-type ICP-MS (ICP-QMS) instrument were carried out. The accuracy of both analyses was in good agreement, whereas ablation at 266 nm and detection using sector-field ICP-MS led to a sensitivity that was one order of magnitude above that obtained at 193 nm with ICP-QMS.

Evaluation of a tunable bandpass reaction cell for an inductively coupled plasma mass spectrometer for the determination of chromium and vanadium in serum and urine

NASA Astrophysics Data System (ADS)

Nixon, David E.; Neubauer, Kenneth R.; Eckdahl, Steven J.; Butz, John A.; Burritt, Mary F.

2002-05-01

A Dynamic Reaction Cell™ inductively coupled argon plasma mass spectrometer (DRC-ICP-MS) was evaluated for the determination of chromium and vanadium in serum and urine. Reaction cell conditions were evaluated for the elimination of ArC + and ClOH + interferences on chromium at mass 52 and OCl + on vanadium at mass 51. A diluent containing only 1% nitric acid and internal standards (Y and Ga) was used to prepare serum and urine for analysis. Instrument response calibration was achieved by using aqueous acidic standards spiked into pooled sera or urine matrices. The slopes of the calibration curves prepared in urine and serum matrices were nearly identical. On average, chromium detection limits are 2.5 times lower using the DRC than Zeeman graphite furnace atomic absorption spectrometry (ZGFAAS). Vanadium detection limits are approximately 50 times lower. Average detection limits achieved with DRC-ICP-MS are 0.075 μg Cr/l and 0.028 μg V/l. Average results for the analysis of National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1598 Bovine Serum (attained over 22 days) are: 0.14 μg Cr/l and 0.068 μg V/l. The reference concentrations for vanadium and chromium in NIST SRM 1598 are (0.06) μg V/l and 0.14±0.08 μg Cr/l, respectively. Results for chromium and vanadium determinations on ICP-MS survey samples from the Toxocologie du Quebec are equivalent to those reported by high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for the same survey samples.

Laser ablation-inductively coupled plasma mass spectrometry: an emerging technology for detecting rare cells in tissue sections.

PubMed

Managh, Amy J; Hutchinson, Robert W; Riquelme, Paloma; Broichhausen, Christiane; Wege, Anja K; Ritter, Uwe; Ahrens, Norbert; Koehl, Gudrun E; Walter, Lisa; Florian, Christian; Schlitt, Hans J; Reid, Helen J; Geissler, Edward K; Sharp, Barry L; Hutchinson, James A

2014-09-01

Administering immunoregulatory cells to patients as medicinal agents is a potentially revolutionary approach to the treatment of immunologically mediated diseases. Presently, there are no satisfactory, clinically applicable methods of tracking human cells in patients with adequate spatial resolution and target cell specificity over a sufficient period of time. Laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS) represents a potential solution to the problem of detecting very rare cells in tissues. In this article, this exquisitely sensitive technique is applied to the tracking of gold-labeled human regulatory macrophages (Mregs) in immunodeficient mice. Optimal conditions for labeling Mregs with 50-nm gold particles were investigated by exposing Mregs in culture to variable concentrations of label: Mregs incubated with 3.5 × 10(9) particles/ml for 1 h incorporated an average of 3.39 × 10(8) Au atoms/cell without loss of cell viability. Analysis of single, gold-labeled Mregs by LA-ICP-MS registered an average of 1.9 × 10(5) counts/cell. Under these conditions, 100% labeling efficiency was achieved, and label was retained by Mregs for ≥36 h. Gold-labeled Mregs adhered to glass surfaces; after 24 h of culture, it was possible to colabel these cells with human-specific (154)Sm-tagged anti-HLA-DR or (174)Yb-tagged anti-CD45 mAbs. Following injection into immunodeficient mice, signals from gold-labeled human Mregs could be detected in mouse lung, liver, and spleen for at least 7 d by solution-based inductively coupled plasma mass spectrometry and LA-ICP-MS. These promising results indicate that LA-ICP-MS tissue imaging has great potential as an analytical technique in immunology. Copyright © 2014 by The American Association of Immunologists, Inc.

Accurate determination of non-metallic impurities in high purity tetramethylammonium hydroxide using inductively coupled plasma tandem mass spectrometry

NASA Astrophysics Data System (ADS)

Fu, Liang; Xie, Hualin; Shi, Shuyun; Chen, Xiaoqing

2018-06-01

The content of non-metallic impurities in high-purity tetramethylammonium hydroxide (HPTMAH) aqueous solution has an important influence on the yield, electrical properties and reliability of the integrated circuit during the process of chip etching and cleaning. Therefore, an efficient analytical method to directly quantify the content of non-metallic impurities in HPTMAH aqueous solutions is necessary. The present study was aimed to develop a novel method that can accurately determine seven non-metallic impurities (B, Si, P, S, Cl, As, and Se) in an aqueous solution of HPTMAH by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS). The samples were measured using a direct injection method. In the MS/MS mode, oxygen and hydrogen were used as reaction gases in the octopole reaction system (ORS) to eliminate mass spectral interferences during the analytical process. The detection limits of B, Si, P, S, Cl, As, and Se were 0.31, 0.48, 0.051, 0.27, 3.10, 0.008, and 0.005 μg L-1, respectively. The samples were analyzed by the developed method and the sector field inductively coupled plasma mass spectrometry (SF-ICP-MS) was used for contrastive analysis. The values of these seven elements measured using ICP-MS/MS were consistent with those measured by SF-ICP-MS. The proposed method can be utilized to analyze non-metallic impurities in HPTMAH aqueous solution. Table S2 Multiple potential interferences on the analytes. Table S3 Parameters of calibration curve and the detection limit (DL). Table S4 Results obtained for 25% concentration high-purity grade TMAH aqueous solution samples (μg L-1, mean ± standard deviation, n = 10).

Inductively Coupled Plasma-Induced Electrical Damage on HgCdTe Etched Surface at Cryogenic Temperatures

NASA Astrophysics Data System (ADS)

Liu, L. F.; Chen, Y. Y.; Ye, Z. H.; Hu, X. N.; Ding, R. J.; He, L.

2018-03-01

Plasma etching is a powerful technique for transferring high-resolution lithographic patterns into HgCdTe material with low etch-induced damage, and it is important for fabricating small-pixel-size HgCdTe infrared focal plane array (IRFPA) detectors. P- to n-type conversion is known to occur during plasma etching of vacancy-doped HgCdTe; however, it is usually unwanted and its removal requires extra steps. Etching at cryogenic temperatures can reduce the etch-induced type conversion depth in HgCdTe via the electrical damage mechanism. Laser beam-induced current (LBIC) is a nondestructive photoelectric characterization technique which can provide information regarding the vertical and lateral electrical field distribution, such as defects and p-n junctions. In this work, inductively coupled plasma (ICP) etching of HgCdTe was implemented at cryogenic temperatures. For an Ar/CH4 (30:1 in SCCM) plasma with ICP input power of 1000 W and RF-coupled DC bias of ˜ 25 V, a HgCdTe sample was dry-etched at 123 K for 5 min using ICP. The sample was then processed to remove a thin layer of the plasma-etched region while maintaining a ladder-like damaged layer by continuously controlling the wet chemical etching time. Combining the ladder etching method and LBIC measurement, the ICP etching-induced electrical damage depth was measured and estimated to be about 20 nm. The results indicate that ICP etching at cryogenic temperatures can significantly suppress plasma etching-induced electrical damage, which is beneficial for defining HgCdTe mesa arrays.

Sedimentation Time Measurements of Soil Particles by Light Scattering and Determination of Chromium, Lead, and Iron in Soil Samples via ICP

ERIC Educational Resources Information Center

Todebush, Patricia Metthe; Geiger, Franz M.

2005-01-01

The study of soil samples, using light scattering and Inductively Coupled Plasma spectrometry (ICP) to determine colloid sedimentation rates and the quantity of chromium, lead, and iron in the sample is described. It shows the physical and chemical behavior of solid components in soil, and how such pollutant binding colloid surfaces directly…

Questa baseline and pre-mining ground-water-quality investigation. 16. Quality assurance and quality control for water analyses

USGS Publications Warehouse

McCleskey, R. Blaine; Nordstrom, D. Kirk; Naus, Cheryl A.

2004-01-01

The Questa baseline and pre-mining ground-water quality investigation has the main objective of inferring the ground-water chemistry at an active mine site. Hence, existing ground-water chemistry and its quality assurance and quality control is of crucial importance to this study and a substantial effort was spent on this activity. Analyses of seventy-two blanks demonstrated that contamination from processing, handling, and analyses were minimal. Blanks collected using water deionized with anion and cation exchange resins contained elevated concentrations of boron (0.17 milligrams per liter (mg/L)) and silica (3.90 mg/L), whereas double-distilled water did not. Boron and silica were not completely retained by the resins because they can exist as uncharged species in water. Chloride was detected in ten blanks, the highest being 3.9 mg/L, probably as the result of washing bottles, filter apparatuses, and tubing with hydrochloric acid. Sulfate was detected in seven blanks; the highest value was 3.0 mg/L, most likely because of carryover from the high sulfate waters sampled. With only a few exceptions, the remaining blank analyses were near or below method detection limits. Analyses of standard reference water samples by cold-vapor atomic fluorescence spectrometry, ion chromatography, inductively coupled plasma-optical emission spectrometry, inductively coupled plasma-mass spectrometry, FerroZine, graphite furnace atomic absorption spectrometry, hydride generation atomic spectrometry, and titration provided an accuracy check. For constituents greater than 10 times the detection limit, 95 percent of the samples had a percent error of less than 8.5. For constituents within 10 percent of the detection limit, the percent error often increased as a result of measurement imprecision. Charge imbalance was calculated using WATEQ4F and 251 out of 257 samples had a charge imbalance less than 11.8 percent. The charge imbalance for all samples ranged from -16 to 16 percent. Spike recoveries were performed by spiking ground-water samples from SC2B, SC3A, SC3B, CC2A, and Hottentot with a mixed-element standard and then analyzing them by ICP-OES. The mean recovery for all the constituents by ICP-OES was 103 percent with a standard deviation of 16 percent. Fifteen surface- and ground-water sequential duplicates were collected from Straight Creek, Hottentot, and the Red River from 2002 to 2003. Except for chloride from well SC5B and low concentrations of iron (<0.05 mg/L) and aluminum (<0.01 mg/L), constituents of sequential duplicates are generally within 10 percent of each other. Analytical results from different methods and different laboratories, with rare exceptions, were within 10 percent. Chromium analyses were in poor agreement when comparing analyses from the USGS and a contract laboratory, but USGS analyses by ICP-OES and ICP-MS were usually within 10 percent for chromium concentrations above 0.03 mg/L and analyses by ICP-OES and GFAAS were usually within 15 percent for chromium concentrations as much as 0.1 mg/L.Filtration studies also were performed to study the effects of filtration apparatuses (Minitan, plate, capsule, and syringe), pore sizes, and timing on dissolved metal concentrations. Except for iron and aluminum, constituents with concentrations greater than about 0.05 mg/L were generally not affected by the filtration apparatus, membrane pore-size, and filtration delays. Iron, aluminum, and some dissolved metals concentrations less than about 0.05 mg/L, especially copper, were generally lowest in filtrates from the tangential flow Minitan system containing a filter membrane with a pore size of 10,000 Daltons. As part of a filtration timing study, grab samples were collected from two sites along the Red River and were processed immediately and then again 1 to 3 hours later. Aluminum and iron colloids formed during the delay in the sample collected at the USGS gaging station and, after the delay, 0.1-ìm filtrate aluminum and iron concentrations approached the ultrafiltrate (Minitan) concentrations. In the upstream site below Fawn Lakes, aluminum in the 0.1-ìm filtrate decreased but did not decrease in the 0.45-ìm filtrate, signifying that the colloids formed during the delay are between 0.1 and 0.45 ìm. Dissolved nickel and pH also decreased in both samples during the delay. Except for ferrous iron and barium, a sequential filtration study 2 demonstrated that water collected from the Red River at the gage did not affect dissolved metal concentrations with increasing sample volume passing through a plate filter with 0.45- or 0.1-ìm membranes. Barium and ferrous iron both slightly decreased in the filtrate from the 0.45-ìm filter.

Simultaneous preconcentration and removal of iron, chromium, nickel with N,N'-etylenebis-(ethane sulfonamide) ligand on activated carbon in aqueous solution and determination by ICP-OES.

PubMed

Karacan, Mehmet Sayim; Aslantaş, Neslihan

2008-07-15

In this study, Fe, Cr and Ni have been preconcentrated and removed by using N,N'-ethylenebis (ethane sulfonamide), (ESEN) ligand on activated carbon (AC) in aqueous solution. For this purpose, complexes between these metals and ligands have been investigated and used in preconcentration and removal studies. Factors which have affected adsorption of metals on activated carbon have been optimized. Adsorbed metals have been preconcentrated 10-fold and determined by ICP-OES. Interferences of Ca, Mg and K to this process have been investigated. The proposed method has been applied to the tap water and Ankara Creek water in order to Fe, Cr, and Ni remediation and preconcentration. Determination of metals by ICP-OES has been checked with standard reference material (NIST 1643e). The proposed method provides the recoveries of 87%, 108% and 106% for Fe, Cr and Ni, respectively, in preconcentration. It also provides the removal of Fe, Cr and Ni by 93%, 100% and 100% removal from waters, respectively.

Potentialities of mass spectrometry (ICP-MS) for actinides determination in urine.

PubMed

Bouvier-Capely, C; Ritt, J; Baglan, N; Cossonnet, C

2004-05-01

The applicability of inductively coupled plasma-mass spectrometry (ICP-MS) for determining actinides in urine was investigated. Performances of ICP-MS including detection limit and analysis time were studied and compared with alpha spectrometry performances. In the field of individual monitoring of workers, the comparison chart obtained in this study can be used as a guide for medical laboratories to select the most adequate procedure to be carried out depending on the case in question (the radioisotope to be measured, the required sensitivity, and the desired response time).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Witte, Travis

This dissertation provides a general introduction to Inductively coupled plasma-mass spectrometry (ICP-MS) and laser ablation (LA) sampling, with an examination of analytical challenges in the employment of this technique. It discusses the origin of metal oxide ions (MO+) in LA-ICP-MS, as well as the effect of introducing helium and nitrogen to the aerosol gas flow on the formation of these polyatomic interferences. It extends the study of polyatomic ions in LA-ICP-MS to metal argide (MAr+) species, an additional source of possible significant interferences in the spectrum. It describes the application of fs-LA-ICP-MS to the determination of uranium isotope ratios inmore » particulate samples.« less

Asymmetrical flow field-flow fractionation coupled to inductively coupled plasma mass spectrometry for sizing SeNPs for packaging applications

NASA Astrophysics Data System (ADS)

Palomo-Siguero, María; Vera, Paula; Echegoyen, Yolanda; Nerin, Cristina; Cámara, Carmen; Madrid, Yolanda

2017-06-01

This paper describes the application of Asymmetrical Flow Field-Flow Fractionation (AF4) coupled to diode array detector (DAD) and inductively coupled plasma mass spectrometry (AF4-UV-ICP-MS) to characterize selenium nanoparticles (SeNPs) in an aqueous acrylic adhesive to be used in a multilayer food packaging material. SeNPs were synthesized using a solution-phase approach based on the reduction of selenite with ascorbic acid in presence of different stabilizers compatible with food industry such as polysaccharides (chitosan (poly(D-glucosamine) and hydroxyethylcellulose (HEC)) and non-ionic surfactants (Triton X-100 (t-octylphenoxypolyethoxyethanol), 2,4,7,9-tetramethyl 5decyne-4,7-diol ethoxylate, and isotridecanol ethoxylate). Several parameters such as pH, ascorbic acid and stabilizers concentration, and compatibility of the stabilizer with the adhesive were evaluated. SeNPs suspensions with spherical morphology were obtained except when isotridecanol ethoxylate was employed which provides SeNPs with a nanorod morphology. AF4-DAD-ICP-MS was further applied for sizing the different SeNPs preparations. DAD was used as detector for selecting the best AF4 separation conditions before coupling to ICP-MS to ensure unequivocal identification of NPs. AF4 calibration with polystyrene latex (PSL) beads of known sizes allowed size determination of the different SeNPs. The following estimated hydrodynamic sizes (expressed as the mean ± standard deviation, n = 6 replicates) were found: chitosan-SeNPs- (26 ± 3 nm), TritonX100-SeNPs (22 ± 10 nm) HEC- SeNPs (91 ± 8 nm) and 2,4,7,9-tetramethyl 5decyne-4,7-diol ethoxylate- SeNPs (59 ± 4 nm). The proposed methodology was successfully applied to the characterization in terms of size of aqueous acrylic adhesives containing SeNPs Results from AF4-ICP-MS and TEM shown that only those SeNPs obtained with non-ionic surfactants and HEC were compatible with the adhesive. The results reported here evidence the usefulness of AF4-ICP-MS as analytical tool for controlling those manufacturing process involving nanoparticles which opens new frontiers in applicability of AF4-ICP-MS.

Uniformity studies of inductively coupled plasma etching in fabrication of HgCdTe detector arrays

NASA Astrophysics Data System (ADS)

Bommena, R.; Velicu, S.; Boieriu, P.; Lee, T. S.; Grein, C. H.; Tedjojuwono, K. K.

2007-04-01

Inductively coupled plasma (ICP) chemistry based on a mixture of CH 4, Ar, and H II was investigated for the purpose of delineating HgCdTe mesa structures and vias typically used in the fabrication of second and third generation infrared photo detector arrays. We report on ICP etching uniformity results and correlate them with plasma controlling parameters (gas flow rates, total chamber pressure, ICP power and RF power). The etching rate and surface morphology of In-doped MWIR and LWIR HgCdTe showed distinct dependences on the plasma chemistry, total pressure and RF power. Contact stylus profilometry and cross-section scanning electron microscopy (SEM) were used to characterize the anisotropy of the etched profiles obtained after various processes and a standard deviation of 0.06 μm was obtained for etch depth on 128 x 128 format array vias. The surface morphology and the uniformity of the etched surfaces were studied by plan view SEM. Atomic force microscopy was used to make precise assessments of surface roughness.

Invention of the Annular Inductively Coupled Plasma as a Spectroscopic Source

NASA Astrophysics Data System (ADS)

Greenfield, Stanley

2000-05-01

This paper shows how experiments with electrical discharges from the 18th century onward led to their use as sources in atomic spectroscopy and how the invention of the annular inductively coupled plasma (ICP) some 30 years ago arose from the need to solve a problem that necessitated the use of a high-temperature source. The search for such a source followed a fairly logical pattern involving dc plasma jets and an ICP such as had been used by T. B. Reed for crystal growing. The ellipsoidal plasma used by Reed was not entirely suitable as a spectroscopic source, since the analytical sample either mixed with the plasma gases or passed around the plasma, resulting in matrix effects and a diminution in the emission. It is shown how suitable modification of the plasma torch with attention to gas flows made it possible to produce an annular or tunnel plasma through which the sample aerosol could be passed, resulting in an annular ICP with greatly improved spectroscopic properties. The further refinements to the source and ancillary equipment are also discussed.

Isotope ratio analysis of individual sub-micrometer plutonium particles with inductively coupled plasma mass spectrometry.

PubMed

Esaka, Fumitaka; Magara, Masaaki; Suzuki, Daisuke; Miyamoto, Yutaka; Lee, Chi-Gyu; Kimura, Takaumi

2010-12-15

Information on plutonium isotope ratios in individual particles is of great importance for nuclear safeguards, nuclear forensics and so on. Although secondary ion mass spectrometry (SIMS) is successfully utilized for the analysis of individual uranium particles, the isobaric interference of americium-241 to plutonium-241 makes difficult to obtain accurate isotope ratios in individual plutonium particles. In the present work, an analytical technique by a combination of chemical separation and inductively coupled plasma mass spectrometry (ICP-MS) is developed and applied to isotope ratio analysis of individual sub-micrometer plutonium particles. The ICP-MS results for individual plutonium particles prepared from a standard reference material (NBL SRM-947) indicate that the use of a desolvation system for sample introduction improves the precision of isotope ratios. In addition, the accuracy of the (241)Pu/(239)Pu isotope ratio is much improved, owing to the chemical separation of plutonium and americium. In conclusion, the performance of the proposed ICP-MS technique is sufficient for the analysis of individual plutonium particles. Copyright © 2010 Elsevier B.V. All rights reserved.

Inductively and capacitively coupled plasmas at interface: A comparative study towards highly efficient amorphous-crystalline Si solar cells

NASA Astrophysics Data System (ADS)

Guo, Yingnan; Ong, Thiam Min Brian; Levchenko, I.; Xu, Shuyan

2018-01-01

A comparative study on the application of two quite different plasma-based techniques to the preparation of amorphous/crystalline silicon (a-Si:H/c-Si) interfaces for solar cells is presented. The interfaces were fabricated and processed by hydrogen plasma treatment using the conventional plasma-enhanced chemical vacuum deposition (PECVD) and inductively coupled plasma chemical vapour deposition (ICP-CVD) methods The influence of processing temperature, radio-frequency power, treatment duration and other parameters on interface properties and degree of surface passivation were studied. It was found that passivation could be improved by post-deposition treatment using both ICP-CVD and PECVD, but PECVD treatment is more efficient for the improvement on passivation quality, whereas the minority carrier lifetime increased from 1.65 × 10-4 to 2.25 × 10-4 and 3.35 × 10-4 s after the hydrogen plasma treatment by ICP-CVD and PECVD, respectively. In addition to the improvement of carrier lifetimes at low temperatures, low RF powers and short processing times, both techniques are efficient in band gap adjustment at sophisticated interfaces.

Preparation of hair for measurement of elements by inductively coupled plasma-mass spectrometry (ICP-MS).

PubMed

Puchyr, R F; Bass, D A; Gajewski, R; Calvin, M; Marquardt, W; Urek, K; Druyan, M E; Quig, D

1998-06-01

The preparation of hair for the determination of elements is a critical component of the analysis procedure. Open-beaker, closed-vessel microwave, and flowthrough microwave digestion are methods that have been used for sample preparation and are discussed. A new digestion method for use with inductively coupled plasma-mass spectrometry (ICP-MS) has been developed. The method uses 0.2 g of hair and 3 mL of concentrated nitric acid in an atmospheric pressure-low-temperature microwave digestion (APLTMD) system. This preparation method is useful in handling a large numbers of samples per day and may be adapted to hair sample weights ranging from 0.08 to 0.3 g. After digestion, samples are analyzed by ICP-MS to determine the concentration of Li, Be, B, Na, Mg, Al, P, S, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ge, As, Se, Rb, Sr, Zr, Mo, Pd, Ag, Cd, Sn, Sb, I, Cs, Ba, Pt, Au, Hg, Tl, Pb, Bi, Th, and U. Benefits of the APLTMD include reduced contamination and sample handling, and increased precision, reliability, and sample throughput.

In-house validation of a method for determination of silver nanoparticles in chicken meat based on asymmetric flow field-flow fractionation and inductively coupled plasma mass spectrometric detection.

PubMed

Loeschner, Katrin; Navratilova, Jana; Grombe, Ringo; Linsinger, Thomas P J; Købler, Carsten; Mølhave, Kristian; Larsen, Erik H

2015-08-15

Nanomaterials are increasingly used in food production and packaging, and validated methods for detection of nanoparticles (NPs) in foodstuffs need to be developed both for regulatory purposes and product development. Asymmetric flow field-flow fractionation with inductively coupled plasma mass spectrometric detection (AF(4)-ICP-MS) was applied for quantitative analysis of silver nanoparticles (AgNPs) in a chicken meat matrix following enzymatic sample preparation. For the first time an analytical validation of nanoparticle detection in a food matrix by AF(4)-ICP-MS has been carried out and the results showed repeatable and intermediately reproducible determination of AgNP mass fraction and size. The findings demonstrated the potential of AF(4)-ICP-MS for quantitative analysis of NPs in complex food matrices for use in food monitoring and control. The accurate determination of AgNP size distribution remained challenging due to the lack of certified size standards. Copyright © 2015 Elsevier Ltd. All rights reserved.

[Determination of iodine and its species in plant samples using ion chromatography-inductively coupled plasma mass spectrometry].

PubMed

Lin, Li; Chen, Guang; Chen, Yuhong

2011-07-01

A method was established for the determination of iodine and its species in plant samples using ion chromatography-inductively coupled plasma mass spectrometry (IC-ICP/ MS). Alkaline extraction and IC-ICP/MS were applied as the sample pre-treatment method and the detection technique respectively, for iodate and iodide determination. Moreover, high-temperature pyrolysis absorption was adopted as the pre-treatment method for total iodine analysis, which finally converted all the iodine species into iodide and measured the iodide by IC-ICP/MS. The recoveries of iodine for alkaline extraction and high-temperature pyrolysis absorption were 89.6%-97.5% and 95.2%-111.2%, respectively. The results were satisfactory. The detection limit of iodine was 0.010 mg/kg. The iodine and its speciation contents in several kinds of plant samples such as seaweeds, kelp, cabbage, tea leaf and spinach were investigated. It was shown that the iodine in seaweeds mainly existed as organic iodine; while the ones in kelp, cabbage, tea leaf and spinach mainly existed as inorganic iodine.

Ultra-Sensitive Elemental Analysis Using Plasmas 4.Application of Inductively Coupled Plasma Mass Spectrometry to the Study of Environmental Radioactivity

NASA Astrophysics Data System (ADS)

Yoshida, Satoshi

Applications of inductively coupled plasma mass spectrometry (ICP-MS) to the determination of long-lived radionuclides in environmental samples were summarized. In order to predict the long-term behavior of the radionuclides, related stable elements were also determined. Compared with radioactivity measurements, the ICP-MS method has advantages in terms of its simple analytical procedures, prompt measurement time, and capability of determining the isotope ratio such as240Pu/239Pu, which can not be separated by radiation. Concentration of U and Th in Japanese surface soils were determined in order to determine the background level of the natural radionuclides. The 235U/238U ratio was successfully used to detect the release of enriched U from reconversion facilities to the environment and to understand the source term. The 240Pu/239Pu ratios in environmental samples varied widely depending on the Pu sources. Applications of ICP-MS to the measurement of I and Tc isotopes were also described. The ratio between radiocesium and stable Cs is useful for judging the equilibrium of deposited radiocesium in a forest ecosystem.

Use of Electrodeposition for Sample Preparation and Rejection Rate Prediction for Assay of Electroformed Ultra High Purity Copper for 232Th and 238U Prior to Inductively Coupled Plasma Mass Spectrometry (ICP/MS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoppe, Eric W.; Aalseth, Craig E.; Brodzinski, Ronald L.

The search for neutrinoless double beta decay in 76Ge has driven the need for ultra-low background Ge detectors shielded by electroformed copper of ultra-high radiopurity (<0.1µBq/kg). Although electrodeposition processes are almost sophisticated enough to produce copper of this purity, to date there are no methods sensitive enough to assay it. Inductively-coupled plasma mass spectrometry (ICP/MS) can detect thorium and uranium at femtogram levels, but in the past, this assay has been hindered by high copper concentrations in the sample. Electrodeposition of copper samples removes copper from the solution while selectively concentrating thorium and uranium contaminants to be assayed by ICP/MS.more » Spiking 232Th and 238U into the plating bath simulates low purity copper and allows for the calculation of the electrochemical rejection rate of thorium and uranium in the electroplating system. This rejection value will help to model plating bath chemistry.« less

Ion Chromatography as an Alternative to Standard Methods for Analysis of Macro-nutrients in Mehlich 1 Extracts of Unfertilized Forest Soils

Treesearch

Joseph B. Fischer; James H. Miller

2004-01-01

This study evaluates ion chromatography (IC) as an alternative to atomic absorption (AA) and inductively-coupled plasma spectromctry (ICP) for analysis of potassium (K), magnesium (Mg), and calcium (Ca), and and as an alternative to antimonylmolybdate colorimetry and ICP for analysis of phosphorus (P) macro-nutrients in Mehlich 1 extracts. Soils typical of pine forests...

Spectral emission from the alkali inductively-coupled plasma: Theory and experiment

NASA Astrophysics Data System (ADS)

Bazurto, R.; Huang, M.; Camparo, J.

2018-04-01

The weakly-ionized, alkali inductively-coupled plasma (ICP) has a long history as the light source for optical pumping. Today, its most significant application is perhaps in the rubidium atomic frequency standard (RAFS), arguably the workhorse of atomic timekeeping in space, where it is crucial to the RAFS' functioning and performance (and routinely referred to as the RAFS' "rf-discharge lamp"). In particular, the photon flux from the lamp determines the signal-to-noise ratio of the device, and variations in ICP brightness define the long-term frequency stability of the atomic clock as a consequence of the ac-Stark shift (i.e., the light-shift). Given the importance of Rb atomic clocks to diverse satellite navigation systems (e.g., GPS, Galileo, BeiDou) - and thereby the importance of alkali ICPs to these systems - it is somewhat surprising to find that the physical processes occurring within the discharge are not well understood. As a consequence, researchers do not understand how to improve the spectral emission from the lamp except at a trial-and-error level, nor do they fully understand the nonlinear mechanisms that result in ICP light instability. Here, we take a first step in developing an intuitive, semi-quantitative model of the alkali rf-discharge lamp, and we perform a series of experiments to validate the theory's predictions.

The separation of 99Tc from low and medium-level radioactive wastes and its determination by inductively coupled plasma mass spectrometry.

PubMed

Hepiegne, P; Dall'ava, D; Clement, R; Degros, J P

1995-06-01

A chemical separation method has been developed for the determination of (99)Tc in various types of radioactive wastes. Such a method includes (i) fusion with NaOH, (ii) extraction in a column containing methyltrioctylammonium chloride, (iii) extraction by solvent with N-benzoyl-N-phenylhydroxylamine and, (iv) measurement by inductively-coupled plasma mass spectrometry (ICP-MS). From the performance standpoint, the recovery of (99)Tc, using (99m)Tc as a yield tracer, is higher than 70%. This analytical method, as developed, ensures effective decontamination with respect to the radionuclides, insofar the decontamination factors are greater than 10(+5), whenever the residual activity may be measured. Taking into account a 3sigma counting error, the detection limit obtained with the ICP-MS technique is 1.9 mBq/ml; the method enabling hence to detect activities as low as 0.3 Bq/g, with analysed samples of 0.2 g and a radiochemical yield of 70%. Studies have been dedicated to the (99)Tc measurement, using the electrothermal vaporization ICP-MS technique, which lowers the detection limit by a factor 10, with the standard solution (0.3 pg/ml), compared with the previous ICP-MS technique.

Absolute measurements and certified reference material for iron isotopes using multiple-collector inductively coupled mass spectrometry.

PubMed

Zhou, Tao; Zhao, Motian; Wang, Jun; Lu, Hai

2008-01-01

Two enriched isotopes, 99.94 at.% 56Fe and 99.90 at.% 54Fe, were blended under gravimetric control to prepare ten synthetic isotope samples whose 56Fe isotope abundances ranged from 95% to 20%. For multiple-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) measurements typical polyatomic interferences were removed by using Ar and H2 as collision gas and operating the MC-ICP-MS system in soft mode. Thus high-precision measurements of the Fe isotope abundance ratios were accomplished. Based on the measurement of the synthetic isotope abundance ratios by MC-ICP-MS, the correction factor for mass discrimination was calculated and the results were in agreement with results from IRMM014. The precision of all ten correction factors was 0.044%, indicating a good linearity of the MC-ICP-MS method for different isotope abundance ratio values. An isotopic reference material was certified under the same conditions as the instrument was calibrated. The uncertainties of ten correction factors K were calculated and the final extended uncertainties of the isotopic certified Fe reference material were 5.8363(37) at.% 54Fe, 91.7621(51) at.% 56Fe, 2.1219(23) at.% 57Fe, and 0.2797(32) at.% 58Fe.

Direct determination of cadmium in foods by solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry using a tungsten coil trap

NASA Astrophysics Data System (ADS)

Zhang, Ying; Mao, Xuefei; Liu, Jixin; Wang, Min; Qian, Yongzhong; Gao, Chengling; Qi, Yuehan

2016-04-01

In this work, a solid sampling device consisting of a tungsten coil trap, porous carbon vaporizer and on-line ashing furnace of a Ni-Cr coil was interfaced with inductively coupled plasma mass spectrometry (ICP-MS). A modified double gas circuit system was employed that was composed of carrier and supplemental gas lines controlled by separate gas mass flow controllers. For Cd determination in food samples using the assembled solid sampling ICP-MS, the optimal ashing and vaporization conditions, flow rate of the argon-hydrogen (Ar/H2) (v:v = 24:1) carrier gas and supplemental gas, and minimum sampling mass were investigated. Under the optimized conditions, the limit of quantification was 0.5 pg and the relative standard deviation was within a 10.0% error range (n = 10). Furthermore, the mean spiked recoveries for various food samples were 99.4%-105.9% (n = 6). The Cd concentrations measured by the proposed method were all within the certified values of the reference materials or were not significantly different (P > 0.05) from those of the microwave digestion ICP-MS method, demonstrating the good accuracy and precision of the solid sampling ICP-MS method for Cd determination in food samples.

Evaluation of elemental profiling methods, including laser-induced breakdown spectroscopy (LIBS), for the differentiation of Cannabis plant material grown in different nutrient solutions.

PubMed

El-Deftar, Moteaa M; Robertson, James; Foster, Simon; Lennard, Chris

2015-06-01

Laser-induced breakdown spectroscopy (LIBS) is an emerging atomic emission based solid sampling technique that has many potential forensic applications. In this study, the analytical performance of LIBS, as well as that of inductively coupled plasma mass spectrometry (ICP-MS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and X-ray microfluorescence (μXRF), was evaluated for the ability to conduct elemental analyses on Cannabis plant material, with a specific investigation of the possible links between hydroponic nutrients and elemental profiles from associated plant material. No such study has been previously published in the literature. Good correlation among the four techniques was observed when the concentrations or peak areas of the elements of interest were monitored. For Cannabis samples collected at the same growth time, the elemental profiles could be related to the use of particular commercial nutrients. In addition, the study demonstrated that ICP-MS, LA-ICP-MS and LIBS are suitable techniques for the comparison of Cannabis samples from different sources, with high discriminating powers being achieved. On the other hand, μXRF method was not suitable for the discrimination of Cannabis samples originating from different growth nutrients. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Differentiating the Bishop ash bed and related tephra layers by elemental-based similarity coefficients of volcanic glass shards using solution inductively coupled plasma-mass spectrometry (S-ICP-MS)

USGS Publications Warehouse

Knott, J.R.; Sarna-Wojcicki, A. M.; Montanez, I.P.; Wan, E.

2007-01-01

Volcanic glass samples from the same volcanic center (intra-source) often have a similar major-element composition. Thus, it can be difficult to distinguish between individual tephra layers, particularly when using similarity coefficients calculated from electron microprobe major-element measurements. Minor/trace element concentrations in glass can be determined by solution inductively coupled plasma mass spectrometry (S-ICP-MS), but have not been shown as suitable for use in large tephrochronologic databases. Here, we present minor/trace-element concentrations measured by S-ICP-MS and compare these data by similarity coefficients, the method commonly used in large databases. Trial samples from the Bishop Tuff, the upper and lower tuffs of Glass Mountain and the tuffs of Mesquite Spring suites from eastern California, USA, which have an indistinguishable major-element composition, were analyzed using S-ICP-MS. The resulting minor/trace element similarity coefficients clearly separated the suites of tephra layers and, in most cases, individual tephra layers within each suite. Comparisons with previous instrumental neutron activation analysis (INAA) elemental measurements were marginally successful. This is important step toward quantitative correlation in large tephrochronologic databases to achieve definitive identification of volcanic glass samples and for high-resolution age determinations. ?? 2007 Elsevier Ltd and INQUA.

Determination of glyphosate and phosphate in water by ion chromatography--inductively coupled plasma mass spectrometry detection.

PubMed

Guo, Zhong-Xian; Cai, Qiantao; Yang, Zhaoguang

2005-12-30

Quantitative determination of trace glyphosate and phosphate in waters was achieved by coupling ion chromatography (IC) separation with inductively coupled plasma mass spectrometry (ICP-MS) detection. The separation of glyphosate and phosphate on a polymer anion-exchange column (Dionex IonPac AS16, 4.0 mm x 250 mm) was obtained by eluting them with 20 mM citric acid at 0.50 mL min(-1), and the analytes were detected directly and selectively by ICP-MS at m/z = 31. Parameters affecting their chromatographic behaviors and ICP-MS characteristics were systematically examined. Based on a 500-microL sample injection volume, the detection limits were 0.7 microgL(-1) for both glyphosate and phosphate, and the calibrations were linear up to 400 microgL(-1). Polyphosphates, aminomethylphosphonic acid (the major metabolite of glyphosate), non-polar and other polar phosphorus-containing pesticides showed different chromatographic behaviors from the analytes of interest and therefore did not interference. The determination was also interference free from the matrix anions (nitrate, nitrite, sulphate, chloride, etc.) and metallic ions. The analysis of certified reference material, drinking water, reservoir water and Newater yielded satisfactory results with spiked recoveries of 97.1-107.0% and relative standard deviations of < or = 7.4% (n = 3). Compared to other reported methods for glyphosate and phosphate, the developed IC-ICP-MS method is sensitive and simple, and does not require any chemical derivatization, sample preconcentration and mobile phase conductivity suppression.

Analysis of high-purity germanium dioxide by ETV-ICP-AES with preliminary concentration of trace elements.

PubMed

Medvedev, Nickolay S; Shaverina, Anastasiya V; Tsygankova, Alphiya R; Saprykin, Anatoly I

2016-08-01

The paper presents a combined technique of germanium dioxide analysis by inductively coupled plasma atomic emission spectrometry (ICP-AES) with preconcentration of trace elements by distilling off matrix and electrothermal (ETV) introduction of the trace elements concentrate into the ICP. Evaluation of metrological characteristics of the developed technique of high-purity germanium dioxide analysis was performed. The limits of detection (LODs) for 25 trace elements ranged from 0.05 to 20ng/g. The accuracy of proposed technique is confirmed by "added-found" («or spiking») experiment and comparing the results of ETV-ICP-AES and ICP-AES analysis of high purity germanium dioxide samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Analysis of metal-laden water via portable X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Pearson, Delaina; Weindorf, David C.; Chakraborty, Somsubhra; Li, Bin; Koch, Jaco; Van Deventer, Piet; de Wet, Jandre; Kusi, Nana Yaw

2018-06-01

A rapid method for in-situ elemental composition analysis of metal-laden water would be indispensable for studying polluted water. Current analytical lab methods to determine water quality include flame atomic absorption spectrometry (FAAS), atomic absorption spectrophotometry (AAS), electrothermal atomic absorption spectrometry (EAAS), and inductively coupled plasma (ICP) spectroscopy. However only two field methods, colorimetry and absorptiometry, exist for elemental analysis of water. Portable X-ray fluorescence (PXRF) spectrometry is an effective method for elemental analysis of soil, sediment, and other matrices. However, the accuracy of PXRF is known to be affected while scanning moisture-laden soil samples. This study sought to statistically establish PXRF's predictive ability for various elements in water at different concentrations relative to inductively coupled plasma atomic emission spectroscopy (ICP-AES). A total of 390 metal-laden water samples collected from leaching columns of mine tailings in South Africa were analyzed via PXRF and ICP-AES. The PXRF showed differential effectiveness in elemental quantification. For the collected water samples, the best relationships between ICP and PXRF elemental data were obtained for K and Cu (R2 = 0.92). However, when scanning ICP calibration solutions with elements in isolation, PXRF results indicated near perfect agreement; Ca, K, Fe, Cu and Pb produced an R2 of 0.99 while Zn and Mn produced an R2 of 1.00. The utilization of multiple PXRF (stacked) beams produced stronger correlation to ICP relative to the use of a single beam in isolation. The results of this study demonstrated the PXRF's ability to satisfactorily predict the composition of metal-laden water as reported by ICP for several elements. Additionally this study indicated the need for a "Water Mode" calibration for the PXRF and demonstrates the potential of PXRF for future study of polluted or contaminated waters.

Review of inductively coupled plasmas: Nano-applications and bistable hysteresis physics

NASA Astrophysics Data System (ADS)

Lee, Hyo-Chang

2018-03-01

Many different gas discharges and plasmas exhibit bistable states under a given set of conditions, and the history-dependent hysteresis that is manifested by intensive quantities of the system upon variation of an external parameter has been observed in inductively coupled plasmas (ICPs). When the external parameters (such as discharge powers) increase, the plasma density increases suddenly from a low- to high-density mode, whereas decreasing the power maintains the plasma in a relatively high-density mode, resulting in significant hysteresis. To date, a comprehensive description of plasma hysteresis and a physical understanding of the main mechanism underlying their bistability remain elusive, despite many experimental observations of plasma bistability conducted under radio-frequency ICP excitation. This fundamental understanding of mode transitions and hysteresis is essential and highly important in various applied fields owing to the widespread use of ICPs, such as semiconductor/display/solar-cell processing (etching, deposition, and ashing), wireless light lamp, nanostructure fabrication, nuclear-fusion operation, spacecraft propulsion, gas reformation, and the removal of hazardous gases and materials. If, in such applications, plasma undergoes a mode transition and hysteresis occurs in response to external perturbations, the process result will be strongly affected. Due to these reasons, this paper comprehensively reviews both the current knowledge in the context of the various applied fields and the global understanding of the bistability and hysteresis physics in the ICPs. At first, the basic understanding of the ICP is given. After that, applications of ICPs to various applied fields of nano/environmental/energy-science are introduced. Finally, the mode transition and hysteresis in ICPs are studied in detail. This study will show the fundamental understanding of hysteresis physics in plasmas and give open possibilities for applications to various applied fields to find novel control knob and optimizing processing conditions.

Starter for inductively coupled plasma tube

DOEpatents

Hull, Donald E.; Bieniewski, Thomas M.

1988-01-01

A starter assembly is provided for use with an inductively coupled plasma (ICP) tube to reliably initate a plasma at internal pressures above about 30 microns. A conductive probe is inserted within the inductor coil about the tube and insulated from the tube shield assembly. A capacitive circuit is arranged for momentarily connecting a high voltage radio-frequency generator to the probe while simultaneously energizing the coil. When the plasma is initiated the probe is disconnected from the generator and electrically connected to the shield assembly for operation.

Iron-Isotopic Fractionation Studies Using Multiple Collector Inductively Coupled Plasma Mass Spectrometry

NASA Technical Reports Server (NTRS)

Anbar, A. D.; Zhang, C.; Barling, J.; Roe, J. E.; Nealson, K. H.

1999-01-01

The importance of Fe biogeochemistry has stimulated interest in Fe isotope fractionation. Recent studies using thermal ionization mass spectrometry (TIMS) and a "double spike" demonstrate the existence of biogenic Fe isotope effects. Here, we assess the utility of multiple-collector inductively-coupled plasma mass spectrometry(MC-ICP-MS) with a desolvating sample introduction system for Fe isotope studies, and present data on Fe biominerals produced by a thermophilic bacterium. Additional information is contained in the original extended abstract.

Corrosion Behavior Of Potential Structural Materials For Use In Nitrate Salts Based Solar Thermal Power Plants

NASA Astrophysics Data System (ADS)

Summers, Kodi

The increasing global demand for electricity is straining current resources of fossil fuels and placing increased pressure on the environment. The implementation of alternative sources of energy is paramount to satisfying global electricity demand while reducing reliance on fossil fuels and lessen the impact on the environment. Concentrated solar power (CSP) plants have the ability to harness solar energy at an efficiency not yet achieved by other technologies designed to convert solar energy to electricity. The problem of intermittency in power production seen with other renewable technologies can be virtually eliminated with the use of molten salt as a heat transfer fluid in CSP plants. Commercial and economic success of CSP plants requires operating at maximum efficiency and capacity which requires high temperature and material reliability. This study investigates the corrosion behavior of structural alloys and electrochemical testing in molten nitrate salts at three temperatures common to CSP plants. Corrosion behavior was evaluated using gravimetric and inductively-coupled plasma optical emission spectroscopy (ICP-OES) analysis. Surface morphology was studied using scanning electron microscopy. Surface oxide structure and chemistry was characterized using X-ray diffraction, Raman spectroscopy, energy dispersive spectroscopy, and X-ray photoelectron spectroscopy. Electrochemical behavior of candidate structural alloys Alloy 4130, austenitic stainless steel 316, and super-austenitic Incoloy 800H was evaluated using potentiodynamic polarization characteristics. It was observed that electrochemical evaluation of these candidate materials correlates well with the corrosion behavior observed from gravimetric and ICP-OES analysis. This study identifies that all three alloys exhibited acceptable corrosion in 300°C molten salt while elevated salt temperatures require the more corrosion resistant alloys, stainless steel 316 and 800H. Characterization of the sample surfaces revealed the presence of spinels at lower temperatures, while Fe2O3 was the dominant iron oxide at higher temperatures for each alloy. It is recommended that accelerated corrosion testing be investigated further to evaluate alloys in other molten salt systems considered for utilization in concentrated solar power plants.

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

PubMed

Low, Fiona; Zhang, Lian

2012-11-15

In this paper, microwave digestion conditions have been optimised to achieve complete recoveries for the ash-forming inorganic elements in coal and coal combustion fly ash, during the analysis by inductively coupled plasma optical emission spectroscopy (ICP-OES). The elements analysed include six major (Al, Ca, Fe, K, Mg and Na) and twelve trace (As, Ba, Be, Co, Cr, Cu, Li, Mn, Ni, Pb, Sr and V). Seven reference samples have been tested, including two standard coal references, SRM1632c and SARM19, their corresponding high-temperature ashes (HTAs), and three coal fly ash references, SRM1633c, SRM2690 and BCR38. The recoveries of individual elements in these samples have been examined intensively, as a function of the amount of hydrofluoric acid (HF, 0-2.0 ml), microwave power (900 W vs. 1200 W) and sample mass (0.05 g vs. 0.1 g). As have been confirmed, the recoveries of these individual elements varied significantly with the microwave digestion condition, elemental type and sample property. For the coal references and their HTAs, the use of HF can be ruled out for most of the elements, except K associated with feldspar, Pb and V. In particular, the recovery of Pb in coal is highly sample-specific and thus unpredictable. The majority of elements in fly ash references require the use of 0.1-0.2 ml HF for a complete recovery. Al in fly ash is the only exceptional element which gave incomplete recoveries throughout, suggesting the use of a complementary technique for its quantification. As has proven to be the only element inconsequential of sample type and digestion conditions, achieving complete recoveries for all cases. On the power parameter, using a higher power such as 1200 W is critical, which has proved to be an ultimatum for the recovery of certain elements, especially in fly ash. Halving sample mass from 0.1 g to 0.05 g was also found to be insignificant. Copyright © 2012 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2007-02-01

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

Quantification of Al2O3 nanoparticles in human cell lines applying inductively coupled plasma mass spectrometry (neb-ICP-MS, LA-ICP-MS) and flow cytometry-based methods

NASA Astrophysics Data System (ADS)

Böhme, Steffi; Stärk, Hans-Joachim; Meißner, Tobias; Springer, Armin; Reemtsma, Thorsten; Kühnel, Dana; Busch, Wibke

2014-09-01

In order to quantify and compare the uptake of aluminum oxide nanoparticles of three different sizes into two human cell lines (skin keratinocytes (HaCaT) and lung epithelial cells (A549)), three analytical methods were applied: digestion followed by nebulization inductively coupled plasma mass spectrometry (neb-ICP-MS), direct laser ablation ICP-MS (LA-ICP-MS), and flow cytometry. Light and electron microscopy revealed an accumulation and agglomeration of all particle types within the cell cytoplasm, whereas no particles were detected in the cell nuclei. The internalized Al2O3 particles exerted no toxicity in the two cell lines after 24 h of exposure. The smallest particles with a primary particle size ( x BET) of 14 nm (Alu1) showed the lowest sedimentation velocity within the cell culture media, but were calculated to have settled completely after 20 h. Alu2 ( x BET = 111 nm) and Alu3 ( x BET = 750 nm) were calculated to reach the cell surface after 7 h and 3 min, respectively. The internal concentrations determined with the different methods lay in a comparable range of 2-8 µg Al2O3/cm2 cell layer, indicating the suitability of all methods to quantify the nanoparticle uptake. Nevertheless, particle size limitations of analytical methods using optical devices were demonstrated for LA-ICP-MS and flow cytometry. Furthermore, the consideration and comparison of particle properties as parameters for particle internalization revealed the particle size and the exposure concentration as determining factors for particle uptake.

New approach to the determination phosphorothioate oligonucleotides by ultra high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry.

PubMed

Studzińska, Sylwia; Mounicou, Sandra; Szpunar, Joanna; Łobiński, Ryszard; Buszewski, Bogusław

2015-01-15

This text presents a novel method for the separation and detection of phosphorothioate oligonucleotides with the use of ion pair ultra high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry The research showed that hexafluoroisopropanol/triethylamine based mobile phases may be successfully used when liquid chromatography is coupled with such elemental detection. However, the concentration of both HFIP and TEA influences the final result. The lower concentration of HFIP, the lower the background in ICP-MS and the greater the sensitivity. The method applied for the analysis of serum samples was based on high resolution inductively coupled plasma mass spectrometry. Utilization of this method allows determination of fifty times lower quantity of phosphorothioate oligonucleotides than in the case of quadrupole mass analyzer. Monitoring of (31)P may be used to quantify these compounds at the level of 80 μg L(-1), while simultaneous determination of sulfur is very useful for qualitative analysis. Moreover, the results presented in this paper demonstrate the practical applicability of coupling LC with ICP-MS in determining phosphorothioate oligonucleotides and their metabolites in serum within 7 min with a very good sensitivity. The method was linear in the concentration range between 0.2 and 3 mg L(-1). The limit of detection was in the range of 0.07 and 0.13 mg L(-1). Accuracy varied with concentration, but was in the range of 3%. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of depleted uranium in urine via isotope ratio measurements using large-bore direct injection high efficiency nebulizer-inductively coupled plasma mass spectrometry.

PubMed

Westphal, Craig S; McLean, John A; Hakspiel, Shelly J; Jackson, William E; McClain, David E; Montaser, Akbar

2004-09-01

Inductively coupled plasma mass spectrometry (ICP-MS), coupled with a large-bore direct injection high efficiency nebulizer (LB-DIHEN), was utilized to determine the concentration and isotopic ratio of uranium in 11 samples of synthetic urine spiked with varying concentrations and ratios of uranium isotopes. Total U concentrations and (235)U/(238)U isotopic ratios ranged from 0.1 to 10 microg/L and 0.0011 and 0.00725, respectively. The results are compared with data from other laboratories that used either alpha-spectrometry or quadrupole-based ICP-MS with a conventional nebulizer-spray chamber arrangement. Severe matrix effects due to the high total dissolved solid content of the samples resulted in a 60 to 80% loss of signal intensity, but were compensated for by using (233)U as an internal standard. Accurate results were obtained with LB-DIHEN-ICP-MS, allowing for the positive identification of depleted uranium based on the (235)U/(238)U ratio. Precision for the (235)U/(238)U ratio is typically better than 5% and 15% for ICP-MS and alpha-spectrometry, respectively, determined over the concentrations and ratios investigated in this study, with the LB-DIHEN-ICP-MS system providing the most accurate results. Short-term precision (6 min) for the individual (235)U and (238)U isotopes in synthetic urine is better than 2% (N = 7), compared to approximately 5% for conventional nebulizer-spray chamber arrangements and >10% for alpha-spectrometry. The significance of these measurements is discussed for uranium exposure assessment of Persian Gulf War veterans affected by depleted uranium ammunitions.

Evaluation of a tunable bandpass reaction cell inductively coupled plasma mass spectrometer for the determination of selenium in serum and urine

NASA Astrophysics Data System (ADS)

Nixon, David E.; Neubauer, Kenneth R.; Eckdahl, Steven J.; Butz, John A.; Burritt, Mary F.

2003-01-01

A Dynamic Reaction Cell™ inductively coupled plasma mass spectrometer (DRC-ICP-MS) was evaluated for the determination of selenium in serum and urine. Reaction cell conditions were evaluated for the suppression of Ar 2+ dimer at m/ z 78 and 80 using methane as the reaction gas. A diluent containing 10% ethanol, 1% nitric acid, 0.5% Triton X-100 with gallium and yttrium internal standards was used to dilute urine and serum samples. Instrument response calibration was achieved by using aqueous acidic standards spiked into a urine matrix. Slopes for aqueous inorganic selenium, seleno- DL-cystine, seleno- DL-methionine and trimethylselenonium iodide spiked into urine and serum matrices were nearly identical. In general, reagent blank readings and detection limits were significantly lower in the DRC mode (reaction cell pressurized) than the standard mode (cell vented). Average results for the analysis of National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1598 bovine serum (attained over 13 days) are: 43.8±3.6 μg Se/l. Reference concentration is 43.6±3.6 μg Se/l. For NIST SRM 2670 Normal Urine the DRC-ICP-MS results are 30.7±4.6 μg Se/l with a certified concentration of 30±8 μg Se/l. For NIST SRM 2670 Elevated Urine the DRC-ICP-MS results are 463±35 μg Se/l with a certified concentration of 460±30 μg Se/l. The DRC-ICP-MS results for selenium determinations in urine and serum survey samples from the Institut National de Sante Publique du Quebec were compared with the reference concentrations and results produced by conventional ICP-MS. While conventional ICP-MS gave acceptable results for survey samples, DRC-ICP-MS gave excellent results for both urine and sera. Closer correlation was observed for DRC-ICP-MS results with target concentrations than with conventional ICP-MS.

Determination of glyphosate and AMPA in surface and waste water using high-performance ion chromatography coupled to inductively coupled plasma dynamic reaction cell mass spectrometry (HPIC-ICP-DRC-MS).

PubMed

Popp, Maximilian; Hann, Stephan; Mentler, Axel; Fuerhacker, Maria; Stingeder, Gerhard; Koellensperger, Gunda

2008-05-01

A novel method employing high-performance cation chromatography in combination with inductively coupled plasma dynamic reaction cell mass spectrometry (ICP-DRC-MS) for the simultaneous determination of the herbicide glyphosate (N-phosphonomethylglycine) and its main metabolite aminomethyl phosphonic acid (AMPA) is presented. P was measured as (31)P(16)O(+) using oxygen as reaction gas. For monitoring the stringent target value of 0.1 μg L(-1) for glyphosate, applicable for drinking and surface water within the EU, a two-step enrichment procedure employing Chelex 100 and AG1-X8 resins was applied prior to HPIC-ICP-MS analysis. The presented approach was validated for surface water, revealing concentrations of 0.67 μg L(-1) glyphosate and 2.8 μg L(-1) AMPA in selected Austrian river water samples. Moreover, investigations at three waste water-treatment plants showed that elimination of the compounds at the present concentration levels was not straightforward. On the contrary, all investigated plant effluents showed significant amounts of both compounds. Concentration levels ranged from 0.5-2 μg L(-1) and 4-14 μg L(-1) for glyphosate and AMPA, respectively.

Evaluation of a direct injection nebulizer interface for flow injection analysis and high performance liquid chromatography with inductively coupled plasma-atomic emission spectroscopic detection

DOE Office of Scientific and Technical Information (OSTI.GOV)

LaFreniere, K.E.

A direct injection nebulizer (DIN) was designed, developed and evaluated to determine its potential utilization as an effective interface for flow injection analysis (FIA) and high performance liquid chromatography (HPLC) coupled with inductively coupled plasma-atomic emission spectroscopic detection. The analytical figures of merit for the DIN when used as an interface for FIA-ICP-AES were found to be comparable to or better than those obtained with conventional pneumatic nebulization in terms of limits of detection (LODs), reproducibility, linearity, and interelement effects. In the HPLC mode, the LODDs were found to be comparable to those obtained by continuous-flow sample introduction into themore » ICP, or inferior by up to only a factor of four. Stable plasma operation was maintained for the DIN sample introduction of a variety of pure organic solvents, including acetonitrile, methanol, methyl-isobutylketone, and pyridine. The HPLC-DIN-ICP-AES facility was specifically applied for the speciation of inorganic and organo-metallic species contained in synthetic mixtures, vanilla extracts and a variety of energy-related materials, such as shale oil process water, coal extracts, shale oil, crude oil, and an SRC II. Suggestions for future research are also considered.« less

Application of CE-ICP-MS and CE-ESI-MS/MS for identification of Zn-binding ligands in Goji berries extracts.

PubMed

Ruzik, Lena; Kwiatkowski, Piotr

2018-06-01

The identification of groups of ligands binding metals is a crucial issue for the better understanding of their bioaccessibility. In the current study, we have intended an approach for identification of Zn-binding ligands based on using capillary electrophoresis combined with inductively coupled plasma mass spectrometry (CE-ICP-MS) and tandem electrospray ionization mass spectrometry (CE-ESI-MS/MS). The approach, which featured the use of the coupling of capillary electrophoresis with inductively coupled plasma mass spectrometry allows to separate and observe zinc ions present in complexes with respect to their size and charge and to identify nine compounds with zinc isotopic profile. CE-ICP-MS provides us with information about presence of zinc species and elemental information about zinc distribution. CE-ESI-MS/MS provide us with information about the most favorable Zn binding ligands: amino acids, flavonols, stilbenoids, fenolic acids and carotenoids. The presented work is the continuation of previous studies based on using LC-ESI-MS/MS, though, now we presented a new solutions with the possibility of changing detectors without changing the separation techniques, what is important without re-optimizing the method. The new presented method allows to identify the zinc-binding ligands in shorter time. Copyright © 2018 Elsevier B.V. All rights reserved.

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

PubMed

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

2015-08-30

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

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

PubMed

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

2017-12-15

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

Ultrasound-assisted extraction for total sulphur measurement in mine tailings.

PubMed

Khan, Adnan Hossain; Shang, Julie Q; Alam, Raquibul

2012-10-15

A sample preparation method for percentage recovery of total sulphur (%S) in reactive mine tailings based on ultrasound-assisted digestion (USAD) and inductively coupled plasma-optical emission spectroscopy (ICP-OES) was developed. The influence of various methodological factors was screened by employing a two-level and three-factor (2(3)) full factorial design and using KZK-1, a sericite schist certified reference material (CRM), to find the optimal combination of studied factors and %S. Factors such as the sonication time, temperature and acid combination were studied, with the best result identified as 20 min of sonication, 80°C temperature and 1 ml of HNO(3):1 ml of HCl, which can achieve 100% recovery for the selected CRM. Subsequently a fraction of the 2(3) full factorial design was applied to mine tailings. The percentage relative standard deviation (%RSD) for the ultrasound method is less than 3.0% for CRM and less than 6% for the mine tailings. The investigated method was verified by X-ray diffraction analysis. The USAD method compared favorably with existing methods such as hot plate assisted digestion method, X-ray fluorescence and LECO™-CNS method. Copyright © 2012 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-08-01

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

Substitution of strontium and boron into hydroxyapatite crystals: Effect on physicochemical properties and biocompatibility with human Wharton-Jelly stem cells.

PubMed

Kolmas, Joanna; Velard, Frédéric; Jaguszewska, Aneta; Lemaire, Flora; Kerdjoudj, Halima; Gangloff, Sophie C; Kaflak, Agnieszka

2017-10-01

Hydroxyapatite (HA) enriched with strontium and boron ions was synthesized using two different methods: the precipitation method (Sr,B-HAw) and the dry method (Sr,B-HAd). Additionally, for the sake of comparison, the "pure" unsubstituted HA was prepared together with HAs substituted only with one type of a foreign ion. The obtained materials were subjected to physicochemical analysis with the use of various analytical methods, such as powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), inductively coupled plasma optical emission spectroscopy (ICP-OES), Fourier transform infrared spectroscopy (FT-IR) and solid-state proton nuclear magnetic resonance ( 1 H ssNMR). All the obtained materials were also biologically tested for their potential cytotoxicity. The obtained materials (Sr,B-HAw and Sr,B-HAd) were homogeneous and respectively showed nano- and microcrystal apatitic structures. The simultaneous introduction of Sr 2+ and BO 3 3- ions turned out to be more effective in respect of the dry method. Of importance, doped materials obtained using both synthesis routes have been demonstrated to be biocompatible, opening the way for medical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Zincon-modified activated carbon for solid-phase extraction and preconcentration of trace lead and chromium from environmental samples.

PubMed

Li, Zhenhua; Chang, Xijun; Hu, Zheng; Huang, Xinping; Zou, Xiaojun; Wu, Qiong; Nie, Rong

2009-07-15

A new method that utilizes zincon-modified activated carbon (AC-ZCN) as a solid-phase extractant has been developed for simultaneous preconcentration of trace Cr(III) and Pb(II) prior to the measurement by inductively coupled plasma optical emission spectrometry (ICP-OES). The separation/preconcentration conditions of analytes were investigated, including effects of pH, the shaking time, the sample flow rate and volume, the elution condition and the interfering ions. At pH 4, the maximum adsorption capacity of Cr(III) and Pb(II) onto the AC-ZCN were 17.9 and 26.7 mg g(-1), respectively. The adsorbed metal ions were quantitatively eluted by 1 mL of 0.1 mol L(-1) HCl. Common coexisting ions did not interfere with the separation. According to the definition of IUPAC, the detection limits (3 sigma) of this method for Cr(III) and Pb(II) were 0.91 and 0.65 ng mL(-1), respectively. The relative standard deviation under optimum condition is less than 3.5% (n=8). The method has been applied for the determination of Cr(III) and Pb(II) in biological materials and water samples with satisfactory results.

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

NASA Astrophysics Data System (ADS)

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

2010-02-01

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

Reductive spectrophotometry of divalent tin sensitization on soda lime glass

NASA Astrophysics Data System (ADS)

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

2016-07-01

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

Fabrication and Characterization of Electrospun PCL-MgO-Keratin-Based Composite Nanofibers for Biomedical Applications

PubMed Central

Boakye, Maame A. D.; Rijal, Nava P.; Adhikari, Udhab; Bhattarai, Narayan

2015-01-01

Polymeric nanofibers are of great interest in biomedical applications, such as tissue engineering, drug delivery and wound healing, due to their ability to mimic and restore the function of natural extracellular matrix (ECM) found in tissues. Electrospinning has been heavily used to fabricate nanofibers because of its reliability and effectiveness. In our research, we fabricated poly(ε-caprolactone)-(PCL), magnesium oxide-(MgO) and keratin (K)-based composite nanofibers by electrospinning a blend solution of PCL, MgO and/or K. The electrospun nanofibers were analyzed by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), mechanical tensile testing and inductively-coupled plasma optical emission spectroscopy (ICP-OES). Nanofibers with diameters in the range of 0.2–2.2 µm were produced by using different ratios of PCL/MgO and PCL-K/MgO. These fibers showed a uniform morphology with suitable mechanical properties; ultimate tensile strength up to 3 MPa and Young’s modulus 10 MPa. The structural integrity of nanofiber mats was retained in aqueous and phosphate buffer saline (PBS) medium. This study provides a new composite material with structural and material properties suitable for potential application in tissue engineering. PMID:28793426

Jujube honey from China: physicochemical characteristics and mineral contents.

PubMed

Zhou, Juan; Suo, Zhirong; Zhao, Pinpin; Cheng, Ni; Gao, Hui; Zhao, Jing; Cao, Wei

2013-03-01

We investigated and compared the physicochemical properties (moisture, color, ash, pH, electrical conductivity, free acidity, lactonic acidity, total acidity, fructose, glucose, sucrose, diastase activity, and HMF) and mineral contents (Al, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, As, Cd, Pb, and Zn), as well as total proline and total protein contents of 23 jujube honey samples collected from different regions of China. The mineral content was determined by inductively coupled plasma-optical emission spectrometry (ICP-OES). The physicochemical values were in the range of approved limits (conforming to EU legislation) in all 23 samples. The physicochemical properties of jujube honey showed significant variations among samples. The mean pH value of the jujube honeys was 6.71. The most abundant minerals were potassium, calcium, sodium, and magnesium, ranging between 1081.4 and 2642.9, 97.1 and 194.2, 7.79 and 127.8, and 10.36 and 24.67 mg/kg, respectively, and potassium made up 71% of the total mineral content. This study demonstrated remarkable variation in physicochemical parameters and mineral contents of jujube honey, mainly depending on its geographic source. © 2013 Institute of Food Technologists®

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

PubMed

Zakaria, Airin; Ho, Yu Bin

2015-10-01

This study aimed to determine the heavy metals (lead, cadmium, and chromium) concentration in lipsticks of different price categories sold in the Malaysian market and evaluate the potential health risks due to daily ingestion of heavy metals in lipsticks. A total of 374 questionnaires were distributed to the female staff in a public university in Malaysia in order to obtain information such as brand and price of the lipsticks, body weight, and frequency and duration of wearing lipstick. This information was important for the calculation of hazard quotient (HQ) in health risk assessment. The samples were extracted using a microwave digester and analyzed using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The concentrations of lead, cadmium, and chromium in lipsticks ranged from 0.77 to 15.44 mg kg(-1), 0.06-0.33 mg kg(-1), and 0.48-2.50 mg kg(-1), respectively. There was a significant difference of lead content in the lipsticks of different price categories. There was no significant non-carcinogenic health risk due to the exposure of these heavy metals through lipstick consumption for the prolonged exposure of 35 years (HQ < 1). Copyright © 2015 Elsevier Inc. All rights reserved.

Simultaneous quantification of 17 trace elements in blood by dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) equipped with a high-efficiency sample introduction system.

PubMed

D'Ilio, S; Violante, N; Di Gregorio, M; Senofonte, O; Petrucci, F

2006-10-10

A quadrupole inductively coupled plasma mass spectrometer (Q-ICP-MS) equipped with a dynamic reaction cell (DRC) and coupled with a desolvating nebulization system (APEX-IR) was employed to determine 17 elements (Al, As, Ba, Cd, Co, Cr, Li, Mn, Mo, Ni, Pb, Sb, Se, Sn, Sr, V, and Zr) in blood samples. Ammonia (for Al, Cr, Mn, and V) and O2 (for As and Se) were used as reacting gases. Selection of the best flow rate of the gases and optimization of the quadrupole dynamic bandpass tuning parameter (RPq) were carried out, using digested blood diluted 1+9 with deionized water and spiked with 1 microg L(-1) of Al, Cr, Mn, V and 5 microgL(-1) of As and Se. Detection limits were determined in digested blood using the 3sigma criterion. The desolvating system allowed a sufficient sensitivity to be achieved to determine elements at levels of ng L(-1) without detriment of signal stability. The accuracy of the method was tested with the whole blood certified reference material (CRM), certified for Al, As, Cd, Co, Cr, Mn, Mo, Ni, Pb, Sb, Se, and V, and with indicative values for Ba, Li, Sn, Sr, and Zr. The addition calibration approach was chosen for analysis. In order to confirm the DRC data, samples were also analyzed by means of sector field inductively coupled plasma mass spectrometry (SF-ICP-MS), operating in medium (m/Deltam=4000) and high (m/Deltam=10,000) resolution mode and achieving a good agreement between the two techniques.

A comparison of laser ablation-inductively coupled plasma-mass spectrometry and high-resolution continuum source graphite furnace molecular absorption spectrometry for the direct determination of bromine in polymers

NASA Astrophysics Data System (ADS)

de Gois, Jefferson S.; Van Malderen, Stijn J. M.; Cadorim, Heloisa R.; Welz, Bernhard; Vanhaecke, Frank

2017-06-01

This work describes the development and comparison of two methods for the direct determination of Br in polymer samples via solid sampling, one using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and the other using high-resolution continuum source graphite furnace molecular absorption spectrometry with direct solid sample analysis (HR-CS SS-GF MAS). The methods were optimized and their accuracy was evaluated by comparing the results obtained for 6 polymeric certified reference materials (CRMs) with the corresponding certified values. For Br determination with LA-ICP-MS, the 79Br+ signal could be monitored interference-free. For Br determination via HR-CS SS-GF MAS, the CaBr molecule was monitored at 625.315 nm with integration of the central pixel ± 1. Bromine quantification by LA-ICP-MS was performed via external calibration against a single CRM while using the 12C+ signal as an internal standard. With HR-CS SS-GF MAS, Br quantification could be accomplished using external calibration against aqueous standard solutions. Except for one LA-ICP-MS result, the concentrations obtained with both techniques were in agreement with the certified values within the experimental uncertainty as evidenced using a t-test (95% confidence level). The limit of quantification was determined to be 100 μg g- 1 Br for LA-ICP-MS and 10 μg g- 1 Br for HR-CS SS-GF MAS.

A provenance study of iron archaeological artefacts by Inductively Coupled Plasma-Mass Spectrometry multi-elemental analysis

NASA Astrophysics Data System (ADS)

Desaulty, Anne-Marie; Mariet, Clarisse; Dillmann, Philippe; Joron, Jean Louis; Fluzin, Philippe

2008-11-01

Raw materials and wastes (i.e. ore, slag and laitier) from ironmaking archaeological sites have been analyzed in order to understand the behavior of the trace elements in the ancient ironmaking processes and to find the significant-most elements to characterize an iron making region. The ICP-MS (Inductively Coupled Plasma Mass Spectrometry) appears to be an excellent technique for this type of studies. The comparison between the ICP-MS results obtained with the Standard Addition method and the INAA (Instrumental Neutron Activation Analyses) results proved that Sc, Co, (Ni), Rb, Cs, Ba, La, Ce, Sm, Eu, Yb, Hf, Th, U contents in the ores, slag and laitiers, and Co and Ni contents in the cast iron can be successfully determined by ICP-MS after wet acid digestion (low detection limits, good sensitivity and precision). By using significant trace element pairs (Yb/Ce, Ce/Th, La/Sc, U/Th, Nb/Y) present in the ores, laitiers and slag, it is possible to discriminate different French ironmaking regions as the Pays de Bray, Lorraine and Pays d'Ouche. These results open the way to further studies on the provenance of iron objects. The comparison between the ICP-MS results obtained with the Standard Calibration Curves method and the INAA results shows that matrices rich in iron, affect the ICP-MS analyses by suppressing the analytes signal. Further studies are necessary to improve understanding matrix effects.

High Resolution Studies of the Origins of Polyatomic Ions in Inductively Coupled Plasma-Mass Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ferguson, Jill Wisnewski

2006-01-01

The inductively coupled plasma (ICP) is an atmospheric pressure ionization source. Traditionally, the plasma is sampled via a sampler cone. A supersonic jet develops behind the sampler, and this region is pumped down to a pressure of approximately one Torr. A skimmer cone is located inside this zone of silence to transmit ions into the mass spectrometer. The position of the sampler and skimmer cones relative to the initial radiation and normal analytical zones of the plasma is key to optimizing the useful analytical signal [1]. The ICP both atomizes and ionizes the sample. Polyatomic ions form through ion-molecule interactionsmore » either in the ICP or during ion extraction [l]. Common polyatomic ions that inhibit analysis include metal oxides (MO +), adducts with argon, the gas most commonly used to make up the plasma, and hydride species. While high resolution devices can separate many analytes from common interferences, this is done at great cost in ion transmission efficiency--a loss of 99% when using high versus low resolution on the same instrument [2]. Simple quadrupole devices, which make up the bulk of ICP-MS instruments in existence, do not present this option. Therefore, if the source of polyatomic interferences can be determined and then manipulated, this could potentially improve the figures of merit on all ICP-MS devices, not just the high resolution devices often utilized to study polyatomic interferences.« less

Fourier Transform Infrared (FT-IR) and Laser Ablation Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS) Imaging of Cerebral Ischemia: Combined Analysis of Rat Brain Thin Cuts Toward Improved Tissue Classification.

PubMed

Balbekova, Anna; Lohninger, Hans; van Tilborg, Geralda A F; Dijkhuizen, Rick M; Bonta, Maximilian; Limbeck, Andreas; Lendl, Bernhard; Al-Saad, Khalid A; Ali, Mohamed; Celikic, Minja; Ofner, Johannes

2018-02-01

Microspectroscopic techniques are widely used to complement histological studies. Due to recent developments in the field of chemical imaging, combined chemical analysis has become attractive. This technique facilitates a deepened analysis compared to single techniques or side-by-side analysis. In this study, rat brains harvested one week after induction of photothrombotic stroke were investigated. Adjacent thin cuts from rats' brains were imaged using Fourier transform infrared (FT-IR) microspectroscopy and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The LA-ICP-MS data were normalized using an internal standard (a thin gold layer). The acquired hyperspectral data cubes were fused and subjected to multivariate analysis. Brain regions affected by stroke as well as unaffected gray and white matter were identified and classified using a model based on either partial least squares discriminant analysis (PLS-DA) or random decision forest (RDF) algorithms. The RDF algorithm demonstrated the best results for classification. Improved classification was observed in the case of fused data in comparison to individual data sets (either FT-IR or LA-ICP-MS). Variable importance analysis demonstrated that both molecular and elemental content contribute to the improved RDF classification. Univariate spectral analysis identified biochemical properties of the assigned tissue types. Classification of multisensor hyperspectral data sets using an RDF algorithm allows access to a novel and in-depth understanding of biochemical processes and solid chemical allocation of different brain regions.

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

PubMed

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

2010-02-05

A method for determination of Co, Cr, Cu, Fe, Mn, Ni, Ti, V and Zn in coal fly ash samples using ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) is proposed. The digestion procedure consisted in the sonication of the previously dried sample with hydrofluoric acid and aqua regia at 80 degrees C for 30 min, elimination of fluorides by heating until dryness for about 1h and dissolution of the residue with nitric acid solution. A classical digestion method, used as comparative method, consisted in the addition of HCl, HNO(3) and HF to 1 g of sample, and heating on a hot plate until dryness for about 6h. The proposed method presents several advantages: it requires lower amounts of sample and reagents, and it is faster. It is also advantageous when compared to the published methods, which also use ultrasound-assisted digestion procedure: lower detection limits for Co, Cu, Ni, V and Zn, and it does not require shaking during the digestion. The detection limits (microg g(-1)) for Co, Cr, Cu, Fe, Mn, Ni, Ti, V and Zn were 0.06, 0.37, 1.0, 25, 0.93, 0.45, 4.0, 1.7 and 4.3, respectively. The results were in good agreement with those obtained by the classical method and reference values. The exception was Cr, which presented low recoveries in classical and proposed methods (83 and 87%, respectively). Also, the concentration for Cu obtained by the proposed method was significantly different from the reference value, in spite of the good recovery (91+/-1%). Copyright 2009 Elsevier B.V. All rights reserved.

Boron detection from blood samples by ICP-AES and ICP-MS during boron neutron capture therapy.

PubMed

Linko, S; Revitzer, H; Zilliacus, R; Kortesniemi, M; Kouri, M; Savolainen, S

2008-01-01

The concept of boron neutron capture therapy (BNCT) involves infusion of a (10)B containing tracer into the patient's bloodstream followed by local neutron irradiation(s). Accurate estimation of the blood boron level for the treatment field before irradiation is required. Boron concentration can be quantified by inductively coupled plasma atomic emission spectrometry (ICP-AES), mass spectrometry (ICP-MS), spectrofluorometric and direct current atomic emission spectrometry (DCP-AES) or by prompt gamma photon detection methods. The blood boron concentrations were analysed and compared using ICP-AES and ICP-MS to ensure congruency of the results if the analysis had to be changed during the treatment, e.g. for technical reasons. The effect of wet-ashing on the results was studied in addition. The mean of all samples analysed with ICP-MS was 5.8 % lower than with ICP-AES coupled to wet-ashing (R (2) = 0.88). Without wet-ashing, the mean of all samples analysed with ICP-MS was 9.1 % higher than with ICP-AES (R (2) = 0.99). Boron concentration analysed from whole blood samples with ICP-AES correlated well with the values of ICP-MS with wet-ashing of the sample matrix, which is generally considered the reference method. When using these methods in parallel at certain intervals during the treatments, reliability of the blood boron concentration values remains satisfactory, taking into account the required accuracy of dose determination in the irradiation of cancer patients.

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF METALS FROM SOIL, DUST, AIR FILTER, AND SURFACE AND DERMAL SAMPLES FOR AA (GRAPHITE FURNACE OR FLAME) OR ICP-AES ANALYSIS (BCO-L-3.1)

EPA Science Inventory

The purpose of this SOP is to describe the acid digestion of soil, house dust, air filter, and surface or dermal wipe samples for analysis using inductively coupled plasma atomic emissions spectrometry (ICP-AES) and/or graphite furnace atomic absorption spectrometry (GFAAS) or fl...

NETL Research Technology

ScienceCinema

None

2018-01-16

NETL is committed to providing its researchers with the latest scientific equipment. This video highlights three technologies: the Beowulf Cluster supercomputer, the OASIS Surface Analytical and Imaging System, and the gas chromatograph-inductively coupled plasma-mass spectrometer, or GC-ICP-MS.

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

USGS Publications Warehouse

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

1984-01-01

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

Applying of Factor Analyses for Determination of Trace Elements Distribution in Water from River Vardar and Its Tributaries, Macedonia/Greece

PubMed Central

Popov, Stanko Ilić; Stafilov, Trajče; Šajn, Robert; Tănăselia, Claudiu; Bačeva, Katerina

2014-01-01

A systematic study was carried out to investigate the distribution of fifty-six elements in the water samples from river Vardar (Republic of Macedonia and Greece) and its major tributaries. The samples were collected from 27 sampling sites. Analyses were performed by mass spectrometry with inductively coupled plasma (ICP-MS) and atomic emission spectrometry with inductively coupled plasma (ICP-AES). Cluster and R mode factor analysis (FA) was used to identify and characterise element associations and four associations of elements were determined by the method of multivariate statistics. Three factors represent the associations of elements that occur in the river water naturally while Factor 3 represents an anthropogenic association of the elements (Cd, Ga, In, Pb, Re, Tl, Cu, and Zn) introduced in the river waters from the waste waters from the mining and metallurgical activities in the country. PMID:24587756

Applying of factor analyses for determination of trace elements distribution in water from Vardar and its tributaries, Macedonia/Greece.

PubMed

Popov, Stanko Ilić; Stafilov, Trajče; Sajn, Robert; Tănăselia, Claudiu; Bačeva, Katerina

2014-01-01

A systematic study was carried out to investigate the distribution of fifty-six elements in the water samples from river Vardar (Republic of Macedonia and Greece) and its major tributaries. The samples were collected from 27 sampling sites. Analyses were performed by mass spectrometry with inductively coupled plasma (ICP-MS) and atomic emission spectrometry with inductively coupled plasma (ICP-AES). Cluster and R mode factor analysis (FA) was used to identify and characterise element associations and four associations of elements were determined by the method of multivariate statistics. Three factors represent the associations of elements that occur in the river water naturally while Factor 3 represents an anthropogenic association of the elements (Cd, Ga, In, Pb, Re, Tl, Cu, and Zn) introduced in the river waters from the waste waters from the mining and metallurgical activities in the country.

Use of laser ablation-inductively coupled plasma-time of flight-mass spectrometry to identify the elemental composition of vanilla and determine the geographic origin by discriminant function analysis.

PubMed

Hondrogiannis, Ellen M; Ehrlinger, Erin; Poplaski, Alyssa; Lisle, Meredith

2013-11-27

A total of 11 elements found in 25 vanilla samples from Uganda, Madagascar, Indonesia, and Papua New Guinea were measured by laser ablation-inductively coupled plasma-time-of-flight-mass spectrometry (LA-ICP-TOF-MS) for the purpose of collecting data that could be used to discriminate among the origins. Pellets were prepared of the samples, and elemental concentrations were obtained on the basis of external calibration curves created using five National Institute of Standards and Technology (NIST) standards and one Chinese standard with (13)C internal standardization. These curves were validated using NIST 1573a (tomato leaves) as a check standard. Discriminant analysis was used to successfully classify the vanilla samples by their origin. Our method illustrates the feasibility of using LA-ICP-TOF-MS with an external calibration curve for high-throughput screening of spice screening analysis.

Rapid determination of 237Np in soil samples by multi-collector inductively-coupled plasma mass spectrometry and gamma spectrometry.

PubMed

Yi, Xiaowei; Shi, Yanmei; Xu, Jiang; He, Xiaobing; Zhang, Haitao; Lin, Jianfeng

A radiochemical procedure is developed for the determination of 237 Np in soil with multi-collector inductively-coupled plasma mass spectrometry (MC-ICP-MS) and gamma-spectrometry. 239 Np (milked from 243 Am) was used as an isotopic tracer for chemical yield determination. The neptunium in the soil is separated by thenoyl-trifluoracetone extraction from 1 M HNO 3 solution after reducing Np to Np(IV) with ferrous sulfamate, and then purified with Dowex 1 × 2 anion exchange resin. 239 Np in the resulting solution is measured with gamma-spectrometry for chemical yield determination while the 237 Np is measured with MC-ICP-MS. Measurement results for soil samples are presented together with those for two reference samples. By comparing the determined value with the reference value of the 237 Np activity concentration, the feasibility of the procedure was validated.

Simulation of a large size inductively coupled plasma generator and comparison with experimental data

NASA Astrophysics Data System (ADS)

Lei, Fan; Li, Xiaoping; Liu, Yanming; Liu, Donglin; Yang, Min; Yu, Yuanyuan

2018-01-01

A two-dimensional axisymmetric inductively coupled plasma (ICP) model with its implementation in the COMSOL (Multi-physics simulation software) platform is described. Specifically, a large size ICP generator filled with argon is simulated in this study. Distributions of the number density and temperature of electrons are obtained for various input power and pressure settings and compared. In addition, the electron trajectory distribution is obtained in simulation. Finally, using experimental data, the results from simulations are compared to assess the veracity of the two-dimensional fluid model. The purpose of this comparison is to validate the veracity of the simulation model. An approximate agreement was found (variation tendency is the same). The main reasons for the numerical magnitude discrepancies are the assumption of a Maxwellian distribution and a Druyvesteyn distribution for the electron energy and the lack of cross sections of collision frequencies and reaction rates for argon plasma.

A study of increasing radical density and etch rate using remote plasma generator system

NASA Astrophysics Data System (ADS)

Lee, Jaewon; Kim, Kyunghyun; Cho, Sung-Won; Chung, Chin-Wook

2013-09-01

To improve radical density without changing electron temperature, remote plasma generator (RPG) is applied. Multistep dissociation of the polyatomic molecule was performed using RPG system. RPG is installed to inductively coupled type processing reactor; electrons, positive ions, radicals and polyatomic molecule generated in RPG and they diffused to processing reactor. The processing reactor dissociates the polyatomic molecules with inductively coupled power. The polyatomic molecules are dissociated by the processing reactor that is operated by inductively coupled power. Therefore, the multistep dissociation system generates more radicals than single-step system. The RPG was composed with two cylinder type inductively coupled plasma (ICP) using 400 kHz RF power and nitrogen gas. The processing reactor composed with two turn antenna with 13.56 MHz RF power. Plasma density, electron temperature and radical density were measured with electrical probe and optical methods.

Application of laser ablation multicollector inductively coupled plasma mass spectrometry for the measurement of calcium and lead isotope ratios in packaging for discriminatory purposes.

PubMed

Santamaria-Fernandez, Rebeca; Wolff, Jean-Claude

2010-07-30

The potential of high-precision calcium and lead isotope ratio measurements using laser ablation coupled to multicollector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS) to aid distinction between four genuine and five counterfeit pharmaceutical packaging samples and further classification of counterfeit packaging samples has been evaluated. We highlight the lack of reference materials for LA-MC-ICP-MS isotope ratio measurements in solids. In this case the problem is minimised by using National Institute of Standards and Technology Standard Reference Material (NIST SRM) 915a calcium carbonate (as solid pellets) and NIST SRM610 glass disc for sample bracketing external standardisation. In addition, a new reference material, NIST SRM915b calcium carbonate, has been characterised in-house for Ca isotope ratios and is used as a reference sample. Significant differences have been found between genuine and counterfeit samples; the method allows detection of counterfeits and aids further classification of packaging samples. Typical expanded uncertainties for measured-corrected Ca isotope ratio values ((43)Ca/(44)Ca and (42)Ca/(44)Ca) were found to be below 0.06% (k = 2, 95% confidence) and below 0.2% for measured-corrected Pb isotope ratios ((207)Pb/(206)Pb and (208)Pb/(206)Pb). This is the first time that Ca isotope ratios have been measured in packaging materials using LA coupled to a multicollector (MC)-ICP-MS instrument. The use of LA-MC-ICP-MS for direct measurement of Ca and Pb isotopic variations in cardboard/ink in packaging has definitive potential to aid counterfeit detection and classification. Copyright 2010 John Wiley & Sons, Ltd.

Method optimization and quality assurance in speciation analysis using high performance liquid chromatography with detection by inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Larsen, Erik H.

1998-02-01

Achievement of optimum selectivity, sensitivity and robustness in speciation analysis using high performance liquid chromatography (HPLC) with inductively coupled mass spectrometry (ICP-MS) detection requires that each instrumental component is selected and optimized with a view to the ideal operating characteristics of the entire hyphenated system. An isocratic HPLC system, which employs an aqueous mobile phase with organic buffer constituents, is well suited for introduction into the ICP-MS because of the stability of the detector response and high degree of analyte sensitivity attained. Anion and cation exchange HPLC systems, which meet these requirements, were used for the seperation of selenium and arsenic species in crude extracts of biological samples. Furthermore, the signal-to-noise ratios obtained for these incompletely ionized elements in the argon ICP were further enhanced by a factor of four by continously introducing carbon as methanol via the mobile phase into the ICP. Sources of error in the HPLC system (column overload), in the sample introduction system (memory by organic solvents) and in the ICP-MS (spectroscopic interferences) and their prevention are also discussed. The optimized anion and cation exchange HPLC-ICP-MS systems were used for arsenic speciation in contaminated ground water and in an in-house shrimp reference sample. For the purpose of verification, HPLC coupled with tandem mass spectrometry with electrospray ionization was additionally used for arsenic speciation in the shrimp sample. With this analytical technique the HPLC retention time in combination with mass analysis of the molecular ions and their collision-induced fragments provide almost conclusive evidence of the identity of the analyte species. The speciation methods are validated by establishing a mass balance of the analytes in each fraction of the extraction procedure, by recovery of spikes and by employing and comparing independent techniques. The urgent need for reference materials certified for elemental species is stressed.

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

PubMed

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

2017-03-01

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

Determination of heavy metals by ICP-OES and F-AAS after preconcentration with 2,2'-bipyridyl and erythrosine.

PubMed

Feist, Barbara; Mikula, Barbara; Pytlakowska, Katarzyna; Puzio, Bozena; Buhl, Franciszek

2008-04-15

The applicability of 2,2'-bipyridyl and erythrosine co-precipitation method for the separation and preconcentration of some heavy metals, such as Cd, Co, Cu, Ni, Pb and Zn in actual samples for their determination by ICP-OES and F-AAS was studied. Experimental conditions influencing the recovery of the investigated metals, such as pH, molar ratio of 2,2'-bipyridyl to erythrosine, the effect of time on co-precipitation were optimized. The analytical characteristics of the method (e.g. limit of detection, sensitivity, linear range and preconcentration factor) were obtained. The limits of detection LOD (ng mL(-1)) of the ICP-OES (F-AAS) method were: Cd: 4.0 (7.75), Co: 3.1 (57.2), Cu: 18 (10.3), Ni 21.3 (32.8), Pb: 35.9 (29.2) and Zn: 10.2 (6.90). The recovery of all the elements tested was more than 93%. The influence of inorganic matrix was examined. The proposed method was applied to determination of Cd, Co, Cu, Ni, Pb and Zn in vegetables and certified reference material (NCS ZC85006 Tomato).

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

PubMed

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

2015-01-01

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

Single-cell analysis by ICP-MS/MS as a fast tool for cellular bioavailability studies of arsenite.

PubMed

Meyer, S; López-Serrano, A; Mitze, H; Jakubowski, N; Schwerdtle, T

2018-01-24

Single-cell inductively coupled plasma mass spectrometry (SC-ICP-MS) has become a powerful and fast tool to evaluate the elemental composition at a single-cell level. In this study, the cellular bioavailability of arsenite (incubation of 25 and 50 μM for 0-48 h) has been successfully assessed by SC-ICP-MS/MS for the first time directly after re-suspending the cells in water. This procedure avoids the normally arising cell membrane permeabilization caused by cell fixation methods (e.g. methanol fixation). The reliability and feasibility of this SC-ICP-MS/MS approach with a limit of detection of 0.35 fg per cell was validated by conventional bulk ICP-MS/MS analysis after cell digestion and parallel measurement of sulfur and phosphorus.

Applications of inductively coupled plasma-mass spectrometry in environmental radiochemistry

USGS Publications Warehouse

Grain, J.S.

1996-01-01

The state of the art in ICP-MS is now such that there are few discernible differences between radiochemical and mass spectrometric determinations of longlived radionuclides. Indeed, ICP-MS may provide better (more sensitive) data for many radionuclides, depending upon how one wishes to define "long-lived." In lowlevel determinations, sample preparation remains an important part of the analytical procedure, even with ICP-MS, but the speed and isotopic selectivity of the mass spectrometer appear to offer distinct procedural advantages over radiochemical techniques. Therefore, "radioanalytical" ICP-MS applications should continue to grow, especially in the area of radiation protection, but further research (on efficient sample introduction, for example) and method development may be required to get ICP-MS "off the ground" in the geochemical research areas that have traditionally been supported by radiochemistry.

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

NASA Astrophysics Data System (ADS)

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

Heavy metal contamination exists in aqueous wastes and sludge of many industrial discharges and domestic wastewater, among other sources. Determination of metals in the wastewater and sludge requires sample pre-treatment prior to analysis because of certain challenges such as the complexity of the physical state of the sample, which may lead to wrong readings in the measurement. This is particularly the case with low analyte concentration to be detected by the instrument. The purpose of this work was to assess and validate the different sample preparation methods namely, hot plate and microwave-assisted digestion procedures for extraction of metal ions in wastewater and sludge samples prior to their inductively coupled plasma optical emission spectrometric (ICP-OES) determination. For the extraction of As, Al, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Zn, three acid mixtures, that is, HNO3/H2O2, HNO3/HClO4/H2O2 and aqua regia + H2O2, were evaluated. Influent wastewater spiked with the SRM (CWW-TM-B) was used for the optimization of acid mixtures affecting the extraction procedure. After sample digestion, the filtration capabilities of cellulose-acetate filter paper and the acrodisc syringe filter with the pore size of 0.45 μm were compared. In terms of performance, acrodisc syringe filter in terms of the improved recoveries obtained, was found to be the best filtration method compared to the filter paper. Based on the analytical results obtained, microwave-assisted digestion (MAD) using aqua regia + H2O2 mixture was found to be the most suitable method for extraction of heavy metals and major elements in all the sample matrices. Therefore, MAD using aqua regia + H2O2 mixture was used for further investigations. The precision of the developed MAD method expressed in terms of relative standard deviations (% RSD) for different metals was found to be <5%. The limits of detection (LOD) and limits of quantification (LOQ) ranged from 0.12% to 2.18 μg L-1 and 0.61% to 3.43 μg L-1, respectively. The accuracy of the developed method (MAD using aqua regia + H2O2) was verified by analyzing two SRMs (CWW-TM-A and CWW-TM-B) and the obtained results were in agreement with certified values with recoveries ranging from 80% to 104% for CWW-TM-A and 84% to 102% for CWW-TM-B. The accuracy of the developed method was verified also by the recovery test in the spiked sludge samples. The accuracy and spike recovery test for different metal ions were in the range 80-104% and 92-106%, respectively. The developed method was applied for extraction of the As, Al, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Zn in environmental samples, namely wastewater and sludge.

Tissue gadolinium deposition in hepatorenally impaired rats exposed to Gd-EOB-DTPA: evaluation with inductively coupled plasma mass spectrometry (ICP-MS).

PubMed

Sato, Tomohiro; Tamada, Tsutomu; Watanabe, Shigeru; Nishimura, Hirotake; Kanki, Akihiko; Noda, Yasufumi; Higaki, Atsushi; Yamamoto, Akira; Ito, Katsuyoshi

2015-06-01

This study was undertaken to quantify tissue gadolinium (Gd) deposition in hepatorenally impaired rats exposed to gadolinium ethoxybenzyl diethylenetriamine pentaacetic acid (Gd-EOB-DTPA) by means of inductively coupled plasma mass spectrometry (ICP-MS) and to compare differences in Gd distribution among major organs as possible triggers for nephrogenic systemic fibrosis. Five hepatorenally impaired rats (5/6-nephrectomized, with carbon-tetrachloride-induced liver fibrosis) were injected with Gd-EOB-DTPA. Histological assessment was conducted and Gd content of the skin, liver, kidneys, lungs, heart, spleen, diaphragm, and femoral muscle was measured by inductively coupled plasma mass spectrometry (ICP-MS) at 7 days after last injection. In addition, five renally impaired rats were injected with Gd-EOB-DTPA and the degree of tissue Gd deposition was compared with that in the hepatorenally impaired rats. ICP-MS analysis revealed significantly higher Gd deposition in the kidneys, spleen, and liver (p = 0.009-0.047) in the hepatorenally impaired group (42.6 ± 20.1, 17.2 ± 6.1, 8.4 ± 3.2 μg/g, respectively) than in the renally impaired group (17.2 ± 7.7, 5.4 ± 2.1, 2.8 ± 0.7 μg/g, respectively); no significant difference was found for other organs. In the hepatorenally impaired group, Gd was predominantly deposited in the kidneys, followed by the spleen, liver, lungs, skin, heart, diaphragm, and femoral muscle. Histopathological investigation revealed hepatic fibrosis in the hepatorenally impaired group. Compared with renally impaired rats, tissue Gd deposition in hepatorenally impaired rats exposed to Gd-EOB-DTPA was significantly increased in the kidneys, spleen, and liver, probably due to the impairment of the dual excretion pathways of the urinary and biliary systems.

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF METALS FROM SOIL, DUST, AIR FILTER, AND SURFACE AND DERMAL WIPE SAMPLES FOR AA (GRAPHITE FURNACE OR FLAME) OR ICP-AES ANALYSIS (BCO-L-3.1)

EPA Science Inventory

The purpose of this SOP is to describe the acid digestion of soil, house dust, air filter, and surface or dermal wipe samples for analysis using inductively coupled plasma atomic emissions spectrometry (ICP-AES) and/or graphite furnace atomic absorption spectrometry (GFAAS) or fl...

Determination of aluminium in groundwater samples by GF-AAS, ICP-AES, ICP-MS and modelling of inorganic aluminium complexes.

PubMed

Frankowski, Marcin; Zioła-Frankowska, Anetta; Kurzyca, Iwona; Novotný, Karel; Vaculovič, Tomas; Kanický, Viktor; Siepak, Marcin; Siepak, Jerzy

2011-11-01

The paper presents the results of aluminium determinations in ground water samples of the Miocene aquifer from the area of the city of Poznań (Poland). The determined aluminium content amounted from <0.0001 to 752.7 μg L(-1). The aluminium determinations were performed using three analytical techniques: graphite furnace atomic absorption spectrometry (GF-AAS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The results of aluminium determinations in groundwater samples for particular analytical techniques were compared. The results were used to identify the ascent of ground water from the Mesozoic aquifer to the Miocene aquifer in the area of the fault graben. Using the Mineql+ program, the modelling of the occurrence of aluminium and the following aluminium complexes: hydroxy, with fluorides and sulphates was performed. The paper presents the results of aluminium determinations in ground water using different analytical techniques as well as the chemical modelling in the Mineql+ program, which was performed for the first time and which enabled the identification of aluminium complexes in the investigated samples. The study confirms the occurrence of aluminium hydroxy complexes and aluminium fluoride complexes in the analysed groundwater samples. Despite the dominance of sulphates and organic matter in the sample, major participation of the complexes with these ligands was not stated based on the modelling.

Uncertainty Measurement for Trace Element Analysis of Uranium and Plutonium Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gallimore, David L.

2012-06-13

The measurement uncertainty estimatino associated with trace element analysis of impurities in U and Pu was evaluated using the Guide to the Expression of Uncertainty Measurement (GUM). I this evalution the uncertainty sources were identified and standard uncertainties for the components were categorized as either Type A or B. The combined standard uncertainty was calculated and a coverage factor k = 2 was applied to obtain the expanded uncertainty, U. The ICP-AES and ICP-MS methods used were deveoped for the multi-element analysis of U and Pu samples. A typical analytical run consists of standards, process blanks, samples, matrix spiked samples,more » post digestion spiked samples and independent calibration verification standards. The uncertainty estimation was performed on U and Pu samples that have been analyzed previously as part of the U and Pu Sample Exchange Programs. Control chart results and data from the U and Pu metal exchange programs were combined with the GUM into a concentration dependent estimate of the expanded uncertainty. Comparison of trace element uncertainties obtained using this model was compared to those obtained for trace element results as part of the Exchange programs. This process was completed for all trace elements that were determined to be above the detection limit for the U and Pu samples.« less

Analysis of Inorganic Nanoparticles by Single-particle Inductively Coupled Plasma Time-of-Flight Mass Spectrometry.

PubMed

Hendriks, Lyndsey; Gundlach-Graham, Alexander; Günther, Detlef

2018-04-25

Due to the rapid development of nanotechnologies, engineered nanomaterials (ENMs) and nanoparticles (ENPs) are becoming a part of everyday life: nanotechnologies are quickly migrating from laboratory benches to store shelves and industrial processes. As the use of ENPs continues to expand, their release into the environment is unavoidable; however, understanding the mechanisms and degree of ENP release is only possible through direct detection of these nanospecies in relevant matrices and at realistic concentrations. Key analytical requirements for quantitative detection of ENPs include high sensitivity to detect small particles at low total mass concentrations and the need to separate signals of ENPs from a background of dissolved elemental species and natural nanoparticles (NNPs). To this end, an emerging method called single-particle inductively coupled plasma mass spectrometry (sp-ICPMS) has demonstrated great potential for the characterization of inorganic nanoparticles (NPs) at environmentally relevant concentrations. Here, we comment on the capabilities of modern sp-ICPMS analysis with particular focus on the measurement possibilities offered by ICP-time-of-flight mass spectrometry (ICP-TOFMS). ICP-TOFMS delivers complete elemental mass spectra for individual NPs, which allows for high-throughput, untargeted quantitative analysis of dispersed NPs in natural matrices. Moreover, the multi-element detection capabilities of ICP-TOFMS enable new NP-analysis strategies, including online calibration via microdroplets for accurate NP mass quantification and matrix compensation.

Measurements of natural uranium concentration and isotopic composition with permil-level precision by inductively coupled plasma-quadrupole mass spectrometry

NASA Astrophysics Data System (ADS)

Shen, Chuan-Chou; Lin, Huei-Ting; Chu, Mei-Fei; Yu, Ein-Fen; Wang, Xianfeng; Dorale, Jeffrey A.

2006-09-01

A new analytical technique using inductively coupled plasma-quadrupole mass spectrometry (ICP-QMS) has been developed that produces permil-level precision in the measurement of uranium concentration ([U]) and isotopic composition (δ234U) in natural materials. A 233U-236U double spike method was used to correct for mass fractionation during analysis. To correct for ratio drifting, samples were bracketed by uranium standard measurements. A sensitivity of 6-7 × 108 cps/ppm was generated with a sample solution uptake rate of 30 μL/min. With a measurement time of 15-20 min, standards of 30-ng uranium produced a within-run precision better than 3‰ (±2 R.S.D.) for δ234U and better than 2‰ for [U]. Replicate measurements made on standards show that a between-run reproducibility of 3.5‰ for δ234U and 2‰ for [U] can be achieved. ICP-QMS data of δ234U and [U] in seawater, coral, and speleothem materials are consistent with the data measured by other ICP-MS and TIMS techniques. Advantages of the ICP-QMS method include low cost, easy maintenance, simple instrumental operation, and few sample preparation steps. Sample size requirements are small, such as 10-14 mg of coral material. The results demonstrate that this technique can be applied to natural samples with various matrices.

Metal characterization of white hawthorn organs and infusions.

PubMed

Juranović Cindrić, Iva; Zeiner, Michaela; Konanov, Darija Mihajlov; Stingeder, Gerhard

2015-02-18

Hawthorn is one of the most commonly used European and North American phytopharmaceuticals. Because there is no information on metals in seeds, and only rare data for leaves and flowers, the aim of the present study was elemental analysis of the white hawthorn (Crataegus monogyna) by inductively coupled plasma emission spectrometry (ICP-AES) or inductively coupled plasma mass spectrometry (ICP-MS) after digestion in a microwave-assisted system. The limits of detection are below 2 μg/g for ICP-AES and 0.5 μg/g for ICP-MS. Hawthorn leaves and flowers contain essential elements at concentrations (mean values, RSD 2-8%) in mg/g of Ca, 1-4; K, 4-5; Mg, 1-2; and Na, <0.2); and at μg/g levels of Ba, 1-10; Co, <0.16; Cr, <1.4; Cu, 0.6-7; Fe, 1-37; Li, <0.5; Mn, 1-13; Mo, <0.17; Ni, <0.6; Sr, 0.2-2; and Zn, 1-31. Toxic elements were found in low quantities: As (<0.04), Cd (0.04-0.1), and Pb (0.1-2). Up to 10% of the metals is extracted into the infusions. The analyzed plant parts and infusions contain essential elements justifying its use as a medicinal plant, whereas the low quantities of harmful elements will not pose any risk to humans when consumed.

Strontium isotope ratios (87Sr/86Sr) of tooth enamel: a comparison of solution and laser ablation multicollector inductively coupled plasma mass spectrometry methods.

PubMed

Copeland, Sandi R; Sponheimer, Matt; le Roux, Petrus J; Grimes, Vaughan; Lee-Thorp, Julia A; de Ruiter, Darryl J; Richards, Michael P

2008-10-01

Strontium isotope ratios (87Sr/86Sr) in tooth enamel provide a means to investigate migration and landscape use in humans and other animals. Established methods for measuring (87)Sr/(86)Sr in teeth use bulk sampling (5-20 mg) and labor-intensive elemental purification procedures before analysis by either thermal ionization mass spectrometry (TIMS) or multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS). Another method for measuring 87Sr/86Sr is laser ablation MC-ICP-MS, but concerns have been expressed about its accuracy for measuring tooth enamel. In this study we test the precision and accuracy of the technique by analyzing 30 modern rodent teeth from the Sterkfontein Valley, South Africa by laser ablation MC-ICP-MS and solution MC-ICP-MS. The results show a mean difference in 87Sr/86Sr measured by laser ablation and by solution of 0.0003 +/- 0.0002. This degree of precision is well within the margin necessary for investigating the potential geographic origins of humans or animals in many areas of the world. Because laser ablation is faster, less expensive, and less destructive than bulk sampling solution methods, it opens the possibility for conducting 87Sr/86Sr analyses of intra-tooth samples and small and/or rare specimens such as micromammal and fossil teeth.

Separation techniques for the clean-up of radioactive mixed waste for ICP-AES/ICP-MS analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Swafford, A.M.; Keller, J.M.

1993-03-17

Two separation techniques were investigated for the clean-up of typical radioactive mixed waste samples requiring elemental analysis by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) or Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). These measurements frequently involve regulatory or compliance criteria which include the determination of elements on the EPA Target Analyte List (TAL). These samples usually consist of both an aqueous phase and a solid phase which is mostly an inorganic sludge. Frequently, samples taken from the waste tanks contain high levels of uranium and thorium which can cause spectral interferences in ICP-AES or ICP-MS analysis. The removal of these interferences ismore » necessary to determine the presence of the EPA TAL elements in the sample. Two clean-up methods were studied on simulated aqueous waste samples containing the EPA TAL elements. The first method studied was a classical procedure based upon liquid-liquid extraction using tri-n- octylphosphine oxide (TOPO) dissolved in cyclohexane. The second method investigated was based on more recently developed techniques using extraction chromatography; specifically the use of a commercially available Eichrom TRU[center dot]Spec[trademark] column. Literature on these two methods indicates the efficient removal of uranium and thorium from properly prepared samples and provides considerable qualitative information on the extraction behavior of many other elements. However, there is a lack of quantitative data on the extraction behavior of elements on the EPA Target Analyte List. Experimental studies on these two methods consisted of determining whether any of the analytes were extracted by these methods and the recoveries obtained. Both methods produced similar results; the EPA target analytes were only slightly or not extracted. Advantages and disadvantages of each method were evaluated and found to be comparable.« less

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

PubMed

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

2006-01-23

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

Determination of mercury compounds in fish by microwave-assisted extraction and liquid chromatography-vapor generation-inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Chiou, Chwei-Sheng; Jiang, Shiuh-Jen; Kumar Danadurai, K. Suresh

2001-07-01

A method employing a vapor generation system and LC combined with inductively coupled plasma mass spectrometry (LC-ICP-MS) is presented for the determination of mercury in biological tissues. An open vessel microwave digestion system was used to extract the mercury compounds from the sample matrix. The efficiency of the mobile phase, a mixture of L-cysteine and 2-mercaptoethanol, was evaluated for LC separation of inorganic mercury [Hg(II)], methylmercury (methyl-Hg) and ethylmercury (ethyl-Hg). The sensitivity, detection limits and repeatability of the liquid chromatography (LC) ICP-MS system with a vapor generator were comparable to, or better than, that of an LC-ICP-MS system with conventional pneumatic nebulization, or other sample introduction techniques. The experimental detection limits for various mercury species were in the range of 0.05-0.09 ng ml -1 Hg, based on peak height. The proposed method was successfully applied to the determination of mercury compounds in a swordfish sample purchased from the local market. The accuracy of the method was evaluated by analyzing a marine biological certified reference material (DORM-2, NRCC).

Results of an interlaboratory method performance study for the size determination and quantification of silver nanoparticles in chicken meat by single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS).

PubMed

Weigel, Stefan; Peters, Ruud; Loeschner, Katrin; Grombe, Ringo; Linsinger, Thomas P J

2017-08-01

Single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS) promises fast and selective determination of nanoparticle size and number concentrations. While several studies on practical applications have been published, data on formal, especially interlaboratory validation of sp-ICP-MS, is sparse. An international interlaboratory study was organized to determine repeatability and reproducibility of the determination of the median particle size and particle number concentration of Ag nanoparticles (AgNPs) in chicken meat. Ten laboratories from the European Union, the USA, and Canada determined particle size and particle number concentration of two chicken meat homogenates spiked with polyvinylpyrrolidone (PVP)-stabilized AgNPs. For the determination of the median particle diameter, repeatability standard deviations of 2 and 5% were determined, and reproducibility standard deviations were 15 and 25%, respectively. The equivalent median diameter itself was approximately 60% larger than the diameter of the particles in the spiking solution. Determination of the particle number concentration was significantly less precise, with repeatability standard deviations of 7 and 18% and reproducibility standard deviations of 70 and 90%.

High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles

NASA Astrophysics Data System (ADS)

Duyck, Christiane Béatrice; Saint'Pierre, Tatiana Dillenburg; Miekeley, Norbert; da Fonseca, Teresa Cristina Oliveira; Szatmari, Peter

2011-05-01

A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 μg L - 1 and 8 μg L - 1 . The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract.

Analysis of metal-binding proteins separated by non-denaturating gel electrophoresis using matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS).

PubMed

Becker, J Susanne; Mounicou, Sandra; Zoriy, Miroslav V; Becker, J Sabine; Lobinski, Ryszard

2008-09-15

Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) have become established as very efficient and sensitive biopolymer and elemental mass spectrometric techniques for studying metal-binding proteins (metalloproteins) in life sciences. Protein complexes present in rat tissues (liver and kidney) were separated in their native state in the first dimension by blue native gel electrophoresis (BN-PAGE). Essential and toxic metals, such as zinc, copper, iron, nickel, chromium, cadmium and lead, were detected by scanning the gel bands using quadrupole LA-ICP-MS with and without collision cell as a microanalytical technique. Several proteins were identified by using MALDI-TOF-MS together with a database search. For example, on one protein band cut from the BN-PAGE gel and digested with the enzyme trypsin, two different proteins - protein FAM44B and cathepsin B precursor - were identified. By combining biomolecular and elemental mass spectrometry, it was possible to characterize and identify selected metal-binding rat liver and kidney tissue proteins.

Direct determination of lead in biological samples by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) after furnace-fusion in the sample cuvette-tungsten boat furnace.

PubMed

Okamoto, Y

2000-06-01

The newly conceived electrothermal vaporization (ETV) system using a tungsten boat furnace (TBF) sample cuvette was designed for the direct analysis of solid samples with detection by inductively coupled plasma mass spectrometry (ICP-MS). Into this small sample cuvette, a solid mixture of the biological samples and diammonium hydrogenphosphate powder as a fusion flux was placed and situated on a TBF. Tetramethylammonium hydroxide solution was added to the mixture. After the on-furnace digestion had been completed, the analyte in the cuvette was vaporized and introduced into the ICP mass spectrometer. The solid samples were analyzed by using a calibration curve prepared from the aqueous standard solutions. The detection limit was estimated to be 5.1 pg of lead, which corresponds to 10.2 ng g(-1) of lead in solid samples when a prepared sample amount of 1.0 mg was applied. The relative standard deviation for 8 replicate measurements obtained with 100 pg of lead was calculated to be 6.5%. The analytical results for various biological samples are described.

Determination of tin isotope ratios in cassiterite by femtosecond laser ablation multicollector inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Schulze, Marie; Ziegerick, Marco; Horn, Ingo; Weyer, Stefan; Vogt, Carla

2017-04-01

In comparison to isotope analysis of dissolved samples femtosecond laser ablation multicollector inductively coupled plasma mass spectrometry (fs-LA-MC-ICP-MS) enables precise isotope ratio analyses consuming much less sample material and with a minimum effort in sample preparation. This is especially important for the investigation of valuable historical objects for which visual traces of sampling are unwanted. The present study provides a basis for tin isotope ratio measurements using LA-MC-ICP-MS technique. For this, in house isotope standards had to be defined. Investigations on interferences and matrix effects illustrate that beside Sb only high Te contents (with values above those to be expected in cassiterite) result in a significant shift of the measured tin isotope ratios. This effect can partly be corrected for using natural isotope abundances. However, a natural isotope fractionation of Te cannot be excluded. Tin beads reduced from cassiterite were analysed by laser ablation and after dissolution. It was shown that tin isotope ratios can be determined accurately by using fs-LA-MC-ICP-MS. Furthermore the homogeneity of tin isotope ratios in cassiterite was proven.

Slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Cd and Pb in plastics.

PubMed

Li, Po-Chien; Jiang, Shiuh-Jen

2006-07-01

Ultrasonic slurry sampling electrothermal vaporization dynamic reaction cell inductively coupled plasma mass spectrometry (USS-ETV-DRC-ICP-MS) for the determination of Cr, Cd and Pb in several plastic samples, using NH4NO3 as the modifier, is described. The influences of the instrumental operating conditions and the slurry preparation technique on the ion signals are investigated. A reduction in the intensity of the background at signals corresponding to chromium masses (arising from matrix elements) was achieved by using NH3 as the reaction cell gas in the DRC. The method was applied to determine Cr, Cd and Pb in two polystyrene (PS) samples and a polyvinyl chloride (PVC) sample using two different calibration methods, namely standard addition and isotope dilution. The results were in good agreement with those for digested samples analyzed by ultrasonic nebulization DRC-ICP-MS. The precision between sample replicates was better than 17% with the USS-ETV-DRC-ICP-MS method. The method detection limits, estimated from standard addition curves, were about 6-9, 1-2 and 8-11 ng g(-1) for Cr, Cd and Pb, respectively, in the original plastic samples.

Starter for inductively coupled plasma tube

DOEpatents

Hull, D.E.; Bieniewski, T.M.

1988-08-23

A starter assembly is provided for use with an inductively coupled plasma (ICP) tube to reliably initiate a plasma at internal pressures above about 30 microns. A conductive probe is inserted within the inductor coil about the tube and insulated from the tube shield assembly. A capacitive circuit is arranged for momentarily connecting a high voltage radio-frequency generator to the probe while simultaneously energizing the coil. When the plasma is initiated the probe is disconnected from the generator and electrically connected to the shield assembly for operation. 1 fig.

Inductive Electron Heating Revisited

NASA Astrophysics Data System (ADS)

Tuszewski, M.

1996-11-01

Inductively Coupled Plasmas (ICPs) have been studied for over a century. Recently, ICPs have been rediscovered by the multi-billion dollar semiconductor industry as an important class of high-density, low-pressure plasma sources suitable for the manufacture of next-generation integrated circuits. Present low-pressure ICP development is among the most active areas of plasma research. However, this development remains largely empirical, a prohibitively expensive approach for upcoming 300-mm diameter wafers. Hence, there is an urgent need for basic ICP plasma physics research, including experimental characterization and predictive numerical modeling. Inductive radio frequency (rf) power absorption is fundamental to the ICP electron heating and the resulting plasma transport but remains poorly understood. For example, recent experimental measurements and supporting fluid calculationsfootnote M. Tuszewski, Phys. Rev. Lett. 77 in press (1996) on a commercial deposition tool prototype show that the induced rf magnetic fields in the source can cause an order of magnitude reduction in plasma conductivity and in electron heating power density. In some cases, the rf fields penetrate through the entire volume of the ICP discharges while existing models that neglect the induced rf magnetic fields predict rf absorption in a thin skin layer near the plasma surface. The rf magnetic fields also cause more subtle changes in the plasma density and in the electron temperature spatial distributions. These data will be presented and the role of basic research in the applied world of semiconductor manufacturing will be discussed. ^*This research was conducted under the auspices of the U.S. DOE, supported by funds provided by the University of California for discretionary research by Los Alamos National Laboratory.

Comparison of ion chromatographic methods based on conductivity detection, post-column-reaction and on-line-coupling IC-ICP-MS for the determination of bromate.

PubMed

Schminke, G; Seubert, A

2000-02-01

An established method for the determination of the disinfection by-product bromate is ion chromatography (IC). This paper presents a comparison of three IC methods based on either conductivity detection (IC-CD), a post-column-reaction (IC-PCR-VIS) or the on-line-coupling with inductively coupled plasma mass spectrometry (IC-ICP-MS). Main characteristics of the methods such as method detection limits (MDL), time of analysis and sample pretreatment are compared and applicability for routine analysis is critically discussed. The most sensitive and rugged method is IC-ICP-MS, followed by IC-PCR-VIS. The photometric detection is subject to a minor interference in real world samples, presumably caused by carbonate. The lowest sensitivity is shown by the IC-CD method as slowest method compared, which, in addition, requires a sample pretreatment. The highest amount of information is delivered by IC-PCR-VIS, which allows the simultaneous determination of the seven standard anions and bromate.

Fast Determination of Toxic Arsenic Species in Food Samples Using Narrow-bore High-Performance Liquid-Chromatography Inductively Coupled Plasma Mass Spectrometry.

PubMed

Terol, Amanda; Marcinkowska, Monika; Ardini, Francisco; Grotti, Marco

2016-01-01

A new method for the speciation analysis of arsenic in food using narrow-bore high-performance liquid-chromatography inductively coupled plasma mass spectrometry (HPLC-ICP-MS) has been developed. Fast separation of arsenite, arsenate, monomethylarsonic acid and dimethylarsinic acid was carried out in 7 min using an anion-exchange narrow-bore Nucleosil 100 SB column and 12 mM ammonium dihydrogen phosphate of pH 5.2 as the mobile phase, at a flow rate of 0.3 mL min(-1). A PFA-ST micronebulizer jointed to a cyclonic spray chamber was used for HPLC-ICP-MS coupling. Compared with standard-bore HPLC-ICP-MS, the new method has provided higher sensitivity, reduced mobile-phase consumption, a lower matrix plasma load and a shorter analysis time. The achieved instrumental limits of detection were in the 0.3 - 0.4 ng As mL(-1) range, and the precision was better than 3%. The arsenic compounds were efficiently (>80%) extracted from various food samples using a 1:5 methanol/water solution, with additional ultrasonic treatment for rice products. The applicability of this method was demonstrated by the analysis of several samples, such as seafood (fish, mussels, shrimps, edible algae) and rice-based products (Jasmine and Arborio rice, spaghetti, flour, crackers), including three certified reference materials.

Stream-sediment samples reanalyzed for major, rare earth, and trace elements from ten 1:250,000-scale quadrangles, south-central Alaska, 2007-08

USGS Publications Warehouse

Bailey, Elizabeth A.; Shew, Nora B.; Labay, Keith A.; Schmidt, Jeanine M.; O'Leary, Richard M.; Detra, David E.

2010-01-01

During the 1960s through the 1980s, the U.S. Geological Survey (USGS) conducted reconnaissance geochemical surveys of the drainage basins throughout most of the Anchorage, Bering Glacier, Big Delta, Gulkana, Healy, McCarthy, Mount Hayes, Nabesna, Talkeetna Mountains, and Valdez 1:250,000-scale quadrangles in Alaska as part of the Alaska Mineral Resource Assessment Program (AMRAP). These geochemical surveys provide data necessary to assess the potential for undiscovered mineral resources on public and other lands, and provide data that may be used to determine regional-scale element baselines. This report provides new data for 366 of the previously collected stream-sediment samples. These samples were selected for reanalysis because recently developed analytical methods can detect additional elements of interest and have lower detection limits than the methods used when these samples were originally analyzed. These samples were all analyzed for arsenic by hydride generation atomic absorption spectrometry (HGAAS), for gold, palladium, and platinum by inductively coupled plasma-mass spectrometry after lead button fire assay separation (FA/ICP-MS), and for a suite of 55 major, rare earth, and trace elements by inductively coupled plasma-atomic emission spectrometry and inductively coupled plasma-mass spectrometry (ICP-AES-MS) after sodium peroxide sinter at 450 degrees Celsius.

Evaluation of a direct injection nebulizer interface for flow injection analysis and high performance liquid chromatography with inductively coupled plasma-atomic emission spectroscopic detection

DOE Office of Scientific and Technical Information (OSTI.GOV)

LaFreniere, K.E.

A direct injection nebulizer (DIN) was designed, developed, and evaluated to determine its potential utilization as an effective interface for flow injection analysis (FIA) and high performance liquid chromatography (HPLC) coupled with inductively coupled plasma-atomic emission spectroscopic detection. The analytical figures of merit for the DIN when used as an interface for FIA-ICP-AES were found to be comparable to or better than those obtained with conventional pneumatic nebulization in terms of limits of detection (LODs), reproducibility, linearity, and interelement effects. Stable plasma operation was maintained for the DIN sample introduction of a variety of pure organic solvents, including acetonitrile, methanol,more » methylisobutylketone, and pyridine. The HPLC-DIN-ICP-AES facility was specifically applied for the speciation of inorganic and organometallic species contained in synthetic mixtures, vanilla extracts, and a variety of energy-related materials, such as shale oil process water, coal extracts, shale oil, crude oil, and an SRC II. Suggestions for future research are also considered. 227 refs., 44 figs., 15 tabs.« less

Integral electrical characteristics and local plasma parameters of a RF ion thruster

DOE Office of Scientific and Technical Information (OSTI.GOV)

Masherov, P. E.; Riaby, V. A., E-mail: riaby2001@yahoo.com; Godyak, V. A.

2016-02-15

Comprehensive diagnostics has been carried out for a RF ion thruster based on inductively coupled plasma (ICP) source with an external flat antenna coil enhanced by ferrite core. The ICP was confined within a cylindrical chamber with low aspect ratio to minimize plasma loss to the chamber wall. Integral diagnostics of the ICP electrical parameters (RF power balance and coil current) allowed for evaluation of the antenna coils, matching networks, and eddy current loss and the true RF power deposited to plasma. Spatially resolved electron energy distribution functions, plasma density, electron temperatures, and plasma potentials were measured with movable Langmuirmore » probes.« less

Precise and traceable carbon isotope ratio measurements by multicollector ICP-MS: what next?

PubMed

Santamaria-Fernandez, Rebeca

2010-06-01

This article reviews recent developments in the use of multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) to provide high-precision carbon isotope ratio measurements. MC-ICP-MS could become an alternative method to isotope ratio mass spectrometry (IRMS) for rapid carbon isotope ratio determinations in organic compounds and characterisation and certification of isotopic reference materials. In this overview, the advantages, drawbacks and potential of the method for future applications are critically discussed. Furthermore, suggestions for future improvements in terms of precision and sensitivity are made. No doubt, this is an exciting analytical challenge and, as such, hurdles will need to be cleared.

Characterization of Diamond-like Carbon (DLC) films deposited by RF ICP PECVD method

NASA Astrophysics Data System (ADS)

Oleszkiewicz, Waldemar; Kijaszek, Wojciech; Gryglewicz, Jacek; Zakrzewski, Adrian; Gajewski, Krzysztof; Kopiec, Daniel; Kamyczek, Paulina; Popko, Ewa; Tłaczała, Marek

2013-07-01

The work presents the results of a research carried out with Plasmalab Plus 100 system, manufactured by Oxford Instruments Company. The system was configured for deposition of diamond-like carbon films by ICP PECVD method. The deposition processes were carried out in CH4 or CH4/H2 atmosphere and the state of the plasma was investigated by the OES method. The RF plasma was capacitively coupled by 13.56 MHz generator with supporting ICP generator (13.56 Mhz). The deposition processes were conducted in constant value of RF generator's power and resultant value of the DC Bias. The power values of RF generator was set at 70 W and the power values of ICP generator was set at 300 W. In this work we focus on the influence of DLC film's thickness on optical, electrical and structural properties of the deposited DLC films. The quality of deposited DLC layers was examined by the Raman spectroscopy, AFM microscopy and spectroscopic ellipsometry. In the investigated DLC films the calculated sp3 content was ranging from 60 % to 70 %. The films were characterized by the refractive index ranging from 2.03 to 2.1 and extinction coefficient ranging from 0.09 to 0.12.

Inductively coupled plasma mass spectrometry for stable isotope metabolic tracer studies of living systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Luong, Elise

1999-05-10

This dissertation focuses on the development of methods for stable isotope metabolic tracer studies in living systems using inductively coupled plasma single and dual quadrupole mass spectrometers. Sub-nanogram per gram levels of molybdenum (Mo) from human blood plasma are isolated by the use of anion exchange alumina microcolumns. Million-fold more concentrated spectral and matrix interferences such as sodium, chloride, sulfate, phosphate, etc. in the blood constituents are removed from the analyte. The recovery of Mo from the alumina column is 82 ± 5% (n = 5). Isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS) is utilized for the quantitative ultra-tracemore » concentration determination of Mo in bovine and human blood samples. The average Mo concentration in reference bovine serum determined by this method is 10.2 ± 0.4 ng/g, while the certified value is 11.5 ± 1.1 ng/g (95% confidence interval). The Mo concentration of one pool of human blood plasma from two healthy male donors is 0.5 ± 0.1 ng/g. The inductively coupled plasma twin quadrupole mass spectrometer (ICP-TQMS) is used to measure the carbon isotope ratio from non-volatile organic compounds and bio-organic molecules to assess the ability as an alternative analytical method to gas chromatography combustion isotope ratio mass spectrometry (GC-combustion-IRMS). Trytophan, myoglobin, and β-cyclodextrin are chosen for the study, initial observation of spectral interference of 13C + with 12C 1H + comes from the incomplete dissociation of myoglobin and/or β-cyclodextrin.« less

Spatial mapping of mineralization with manganese-enhanced magnetic resonance imaging

USGS Publications Warehouse

Chesnick, I.E.; Centeno, J.A.; Todorov, T.I.; Koenig, A.E.; Potter, K.

2011-01-01

Paramagnetic manganese can be employed as a calcium surrogate to sensitize the magnetic resonance imaging (MRI) technique to the processing of calcium during the bone formation process. At low doses, after just 48h of exposure, osteoblasts take up sufficient quantities of manganese to cause marked reductions in the water proton T1 values compared with untreated cells. After just 24h of exposure, 25??M MnCl2 had no significant effect on cell viability. However, for mineralization studies 100??M MnCl2 was used to avoid issues of manganese depletion in calvarial organ cultures and a post-treatment delay of 48h was implemented to ensure that manganese ions taken up by osteoblasts is deposited as mineral. All specimens were identified by their days in vitro (DIV). Using inductively coupled plasma optical emission spectroscopy (ICP-OES), we confirmed that Mn-treated calvariae continued to deposit mineral in culture and that the mineral composition was similar to that of age-matched controls. Notably there was a significant decrease in the manganese content of DIV18 compared with DIV11 specimens, possibly relating to less manganese sequestration as a result of mineral maturation. More importantly, quantitative T1 maps of Mn-treated calvariae showed localized reductions in T1 values over the calvarial surface, indicative of local variations in the surface manganese content. This result was verified with laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). We also found that ??R1 values, calculated by subtracting the relaxation rate of Mn-treated specimens from the relaxation rate of age-matched controls, were proportional to the surface manganese content and thus mineralizing activity. From this analysis, we established that mineralization of DIV4 and DIV11 specimens occurred in all tissue zones, but was reduced for DIV18 specimens because of mineral maturation with less manganese sequestration. In DIV25 specimens, active mineralization was observed for the expanding superficial surface and ??R1 values were increased due to the mineralization of small, previously unmineralized areas. Our findings support the use of manganese-enhanced MRI (MEMRI) to study well-orchestrated mineralizing events that occur during embryonic development. In conclusion, MEMRI is more sensitive to the study of mineralization than traditional imaging approaches. ?? 2011.

Chemostratigraphy of glaciomarine sediments in the Sarah Formation, northwest Saudi Arabia

NASA Astrophysics Data System (ADS)

Craigie, Neil W.; Rees, Andrew J.

2016-05-01

The Sarah Formation of northern Saudi Arabia mainly consists of glacial 'outwash' sediments deposited by turbidite channels and fans. Prior to undertaking chemostratigraphy, the results of seismic interpretation revealed the Sarah Formation to be mainly deposited in a NW-SE trending turbidite system in the study area, comprising channels with associated fans. These are succeeded by fluvio marine sediments at the top of the Sarah Formation. In the absence of good biostratigraphic control, chemostratigraphy was found to be one of the few techniques that could be employed to produce a high resolution correlation scheme for four study wells. Geochemical data were acquired for 50 elements in 550 core samples by ICP-OES (Inductively Coupled Plasma - Optical Emission Spectrometry) and ICP-MS (Inductively Coupled Plasma - Mass Spectrometry) but only the 'key' ratios Zr/Nb, Nb/Ti, Nb/Cr, Rb/K and Th/Cr were employed for chemostratigraphic purposes as they show significant trends that enable correlative boundaries to be identified and a hierarchical scheme to be proposed. Variations in these parameters are largely related to changes in source/provenance. In order to avoid geochemical variations relating to changes in grain size/lithology, separate schemes were proposed for the sandstone and mudrock samples. The sandstone scheme consists of a hierarchical order of three zones, seven subzones and five divisions, while the mudrock scheme is less detailed, comprising three zones and seven subzones. A 'finalised' scheme, based on a combination of the two aforementioned ones, was found to be more useful than employing the correlation proposed for individual lithologies. One of the main conclusions of the study was that the basal chemozones (general term used to describe any chemostratigraphic zone, subzone or division) were identified in wells B and C but were missing from A and D. It is thought that the areas around the two latter wells represented topographically 'high' areas during the deposition of the lowermost part of the Sarah Formation, hence the reason that these chemozones may be missing as a result of erosion/non-deposition. Conversely, chemozone C3-2a, occurring towards the top of the Sarah Formation turbidites, is correlative between all four wells. The turbidites are succeeded by the marginal marine sediments of chemozones M3-1 and C3-2bb at the top of the Sarah Formation.

Spatial mapping of mineralization with manganese-enhanced magnetic resonance imaging☆☆☆

PubMed Central

Chesnick, Ingrid E.; Centeno, Jose A.; Todorov, Todor I.; Koenig, Alan E.; Potter, Kimberlee

2011-01-01

Paramagnetic manganese can be employed as a calcium surrogate to sensitize the magnetic resonance imaging (MRI) technique to the processing of calcium during the bone formation process. At low doses, after just 48 h of exposure, osteoblasts take up sufficient quantities of manganese to cause marked reductions in the water proton T1 values compared with untreated cells. After just 24 h of exposure, 25 μM MnCl2 had no significant effect on cell viability. However, for mineralization studies 100 μM MnCl2 was used to avoid issues of manganese depletion in calvarial organ cultures and a post-treatment delay of 48 h was implemented to ensure that manganese ions taken up by osteoblasts is deposited as mineral. All specimens were identified by their days in vitro (DIV). Using inductively coupled plasma optical emission spectroscopy (ICP-OES), we confirmed that Mn-treated calvariae continued to deposit mineral in culture and that the mineral composition was similar to that of age-matched controls. Notably there was a significant decrease in the manganese content of DIV18 compared with DIV11 specimens, possibly relating to less manganese sequestration as a result of mineral maturation. More importantly, quantitative T1 maps of Mn-treated calvariae showed localized reductions in T1 values over the calvarial surface, indicative of local variations in the surface manganese content. This result was verified with laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). We also found that ΔR1 values, calculated by subtracting the relaxation rate of Mn-treated specimens from the relaxation rate of age-matched controls, were proportional to the surface manganese content and thus mineralizing activity. From this analysis, we established that mineralization of DIV4 and DIV11 specimens occurred in all tissue zones, but was reduced for DIV18 specimens because of mineral maturation with less manganese sequestration. In DIV25 specimens, active mineralization was observed for the expanding superficial surface and ΔR1 values were increased due to the mineralization of small, previously unmineralized areas. Our findings support the use of manganese-enhanced MRI (MEMRI) to study well-orchestrated mineralizing events that occur during embryonic development. In conclusion, MEMRI is more sensitive to the study of mineralization than traditional imaging approaches. PMID:21352960

Tissue gadolinium deposition in renally impaired rats exposed to different gadolinium-based MRI contrast agents: evaluation with inductively coupled plasma mass spectrometry (ICP-MS).

PubMed

Sato, Tomohiro; Ito, Katsuyoshi; Tamada, Tsutomu; Kanki, Akihiko; Watanabe, Shigeru; Nishimura, Hirotake; Tanimoto, Daigo; Higashi, Hiroki; Yamamoto, Akira

2013-10-01

To quantify tissue gadolinium (Gd) deposition in renally impaired rats exposed to Gd-EOB-DTPA and other Gd-based MRI contrast agents by means of inductively coupled plasma mass spectrometry (ICP-MS), and to compare the differences in distribution among major organs as possible triggers for nephrogenic systemic fibrosis (NSF). A total of 15 renally impaired rats were injected with Gd-EOB-DTPA, Gd-DTPA-BMA and Gd-HP-DO3A. Gd contents of skin, liver, kidney, lung, heart, spleen, diaphragm and femoral muscle were measured by inductively coupled plasma mass spectrometry (ICP-MS). Histological assessment was also conducted. Tissue Gd deposition in all organs was significantly higher (P=0.005~0.009) in the Gd-DTPA-BMA group than in the Gd-HP-DO3A and Gd-EOB-DTPA groups. In the Gd-DTPA-BMA group, Gd was predominantly deposited in kidney (1306±605.7μg/g), followed by skin, liver, lung, spleen, femoral muscle, diaphragm and heart. Comparing Gd-HP-DO3A and Gd-EOB-DTPA groups, Gd depositions in the kidney, liver and lung were significantly lower (P=0.009~0.011) in the Gd-EOB-DTPA group than in the Gd-HP-DO3A group although no significant differences were seen for any other organs. Gd-EOB-DTPA is a stable and safe Gd-based contrast agent (GBCA) showing lower Gd deposition in major organs in renally impaired rats, compared with other GBCAs. This fact suggests that the risk of NSF onset would be low in the use of Gd-EOB-DTPA. Copyright © 2013 Elsevier Inc. All rights reserved.

Étude comparative des techniques d'analyse par fluorescence X à dispersion d'énergie (ED-XRF) et à dispersion de longueur d'onde (WD-XRF), et par spectrométrie d'émission atomique à source plasma couplée par induction (ICP-AES)

NASA Astrophysics Data System (ADS)

Rahmani, A.; Benyaïch, F.; Bounakhla, M.; Bilal, E.; Moutte, J.; Gruffat, J. J.; Zahry, F.

2004-11-01

Dans ce travail, nous présentons une étude comparative des techniques d'analyse par fluorescence X à dispersion d'énergie (ED-XRF) et à dispersion de longueur d'onde (WD-XRF), et par spectrométrie d'émission atomique à source plasma couplée par induction (ICP-AES). Les résultats de la calibration des spectromètres à dispersion d'énergie, à excitation par sources radioactives (55Fe, 109Cd et 241Am) et à excitation secondaire (cible secondaire Mo et Cu) du Centre National pour l'Energie, les Sciences et les Techniques Nucléaires (CNESTEN, Rabat, Maroc) sur des échantillons étalons de références de l'Agence International de l'Energie Atomique (AIEA) et du Community Bureau of Référence (BCR) ont été comparés aux résultats d'analyse des mêmes échantillons étalons par la spectrométrie X à dispersion de longueur d'onde (WD-XRF) et par spectrométrie d'émission atomique à source plasma couplé par induction (ICP-AES) au département GENERIC du centre SPIN à l'Ecole des Mines de Saint-Etienne (France). Les trois techniques d'analyse utilisées donnent des résultats comparables pour le dosage des éléments majeurs, alors que pour les traces on note des déviations importantes à cause des effets de matrice qui sont difficiles à corriger dans le cas de la fluorescence X.

Comparative study of atomic fluorescence spectroscopy and inductively coupled plasma mass spectrometry for mercury and arsenic multispeciation.

PubMed

Gómez-Ariza, José Luis; Lorenzo, Fernando; García-Barrera, Tamara

2005-05-01

Mercury and arsenic are two elements of undoubted importance owing to their toxic character. Although speciation of these elements has been developed separately, in this work for the first time the speciation of As and Hg using two atomic fluorescence detectors in a sequential ensemble is presented. A coupling based on the combination of high-performance liquid chromatography (where mercury and arsenic species are separated) and two atomic fluorescence detectors in series, with several online treatments, including photooxidation (UV) and hydride generation, has allowed the determination of mercury and arsenic compounds simultaneously. The detection limits for this device were 16, 3, 17, 12 and 8 ng mL(-1) for As(III), monomethylarsinic acid, As(V), Hg2+ and methylmercury, respectively. This coupling was compared with an analogous one based on inductively coupled plasma-mass spectrometry (ICP-MS) detection, with detection limits of 0.7, 0.5, 0.8, 0.9 and 1.1 ng mL(-1), respectively. Multispeciation based on ICP-MS exhibits better sensitivity than the coupling based on tandem atomic fluorescence, but this second device is a very robust system and exhibits obvious advantages related to the low cost of acquisition and maintenance, as well as easy handling, which makes it a suitable system for routine laboratories.

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

NASA Astrophysics Data System (ADS)

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

2014-05-01

Accurate, routine testing of nutrients in soil samples is critical to understanding soil potential fertility. There are different factors which must be taken into account selecting the best analytical technique for soil laboratory analysis. Several techniques can provide adequate detection range for same analytical subject. In similar cases the choise of technique will depend on factors such as sample throughput, required infrastructure, ease of use, used chemicals and need for gas supply and operating costs. Mehlich 3 extraction method is widely used for the determination of the plant available nutrient elements contents in agricultural soils. For determination of Ca, K, and Mg from soil extract depending of laboratory ICP and AAS techniques are used, also flame photometry for K in some laboratories. For the determination of extracted P is used ICP or Vis spectrometry. The excellent sensitivity and wide working range for all extracted elements make ICP a nearly ideal method, so long as the sample throughput is big enough to justify the initial capital outlay. Other advantage of ICP techniques is the multiplex character (simultaneous acquisition of all wavelengths). Depending on element the detection limits are in range 0.1 - 1000 μg/L. For smaller laboratories with low sample throughput requirements the use of AAS is more common. Flame AAS is a fast, relatively cheap and easy technique for analysis of elements. The disadvantages of the method is single element analysis and use of flammable gas, like C2H2 and oxidation gas N2O for some elements. Detection limits of elements for AAS lays from 1 to 1000 μg/L. MP-AES offers a unique alternative to both, AAS and ICP-OES techniques with its detection power, speed of analysis. MP-AES is quite new, simple and relatively inexpensive multielemental technique, which is use self-sustained atmospheric pressure microwave plasma (MP) using nitrogen gas generated by nitrogen generator. Therefore not needs for argon and flammable (C2H2) gases, cylinder handling and the running costs of equipment are low. Detection limits of elements for MP-AES lays between the AAS and ICP ones. The objective of this study was to compare the results of soil analysis using two multielemental analytical methods - ICP-OES and MP-AES. In the experiment, different soil types with various texture, content of organic matter and pH were used. For the study soil samples of Albeluvisols, Leptosols, Cambisols, Regosols and Histosols were used . The plant available nutrients were estimated by Mehlich 3 extraction. The ICP-OES analysis were provided in the Estonian Agricultural Research Centre and MP-AES analysis in department of Soil Science and Agrochemistry at Estonian University of Life Sciences. The detection limits and limits of quantification of Ca, K, Mg and P in extracts are calculated and reported.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gundlach-Graham, Alexander W.; Dennis, Elise; Ray, Steven J.

An inductively coupled plasma distance-of-flight mass spectrometer (ICP-DOFMS) has been coupled with laser-ablation (LA) sample introduction for the elemental analysis of solids. ICP-DOFMS is well suited for the analysis of laser-generated aerosols because it offers both high-speed mass analysis and simultaneous multi-elemental detection. Here, we evaluate the analytical performance of the LA-ICP-DOFMS instrument, equipped with a microchannel plate-based imaging detector, for the measurement of steady-state LA signals, as well as transient signals produced from single LA events. Steady-state detection limits are 1 mg g1, and absolute single-pulse LA detection limits are 200 fg for uranium; the system is shown capablemore » of performing time-resolved single-pulse LA analysis. By leveraging the benefits of simultaneous multi-elemental detection, we also attain a good shot-to-shot reproducibility of 6% relative standard deviation (RSD) and isotope-ratio precision of 0.3% RSD with a 10 s integration time.« less

Analysis and comparison of glass fragments by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and ICP-MS.

PubMed

Trejos, Tatiana; Montero, Shirly; Almirall, José R

2003-08-01

The discrimination potential of Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) is compared with previously reported solution ICP-MS methods using external calibration (EC) with internal standardization and a newly reported solution isotope dilution (ID) method for the analysis of two different glass populations. A total of 91 different glass samples were used for the comparison study; refractive index and elemental composition were measured by the techniques mentioned above. One set consisted of 45 headlamps taken from a variety of automobiles that represents a range of 20 years of manufacturing dates. A second set consisted of 46 automotive glasses (side windows, rear windows, and windshields) representing casework glass from different vehicle manufacturers over several years. The element menu for the LA-ICP-MS and EC-ICP-MS methods include Mg, Al, Ca, Mn, Ce, Ti, Zr, Sb, Ga, Ba, Rb, Sm, Sr, Hf, La, and Pb. The ID method was limited to the analysis of two isotopes each of Mg, Sr, Zr, Sb, Ba, Sm, Hf, and Pb. Laser ablation analyses were performed with a Q switched Nd:YAG, 266 nm, 6 mJ output energy laser. The laser was used in depth profile mode while sampling using a 50 microm spot size for 50 sec at 10 Hz (500 shots). The typical bias for the analysis of NIST 612 by LA-ICP-MS was less than 5% in all cases and typically better than 5% for most isotopes. The precision for the vast majority of the element menu was determined generally less than 10% for all the methods when NIST 612 was measured (40 microg x g(-1)). Method detection limits (MDL) for the EC and LA-ICP-MS methods were similar and generally reported as less than 1 microg x g(-1) for the analysis of NIST 612. While the solution sample introduction methods using EC and ID presented excellent sensitivity and precision, these methods have the disadvantages of destroying the sample, and also involve complex sample preparation. The laser ablation method was simpler, faster, and produced comparable discrimination to the EC-ICP-MS and ID-ICP-MS. LA-ICP-MS can offer an excellent alternative to solution analysis of glass in forensic casework samples.

STATISTICAL VALIDATION OF SULFATE QUANTIFICATION METHODS USED FOR ANALYSIS OF ACID MINE DRAINAGE

EPA Science Inventory

Turbidimetric method (TM), ion chromatography (IC) and inductively coupled plasma atomic emission spectrometry (ICP-AES) with and without acid digestion have been compared and validated for the determination of sulfate in mining wastewater. Analytical methods were chosen to compa...

Arsenic biotransformation and volatilization in transgenic rice

PubMed Central

Meng, Xiang-Yan; Qin, Jie; Wang, Li-Hong; Duan, Gui-Lan; Sun, Guo-Xin; Wu, Hui-Lan; Chu, Cheng-Cai; Ling, Hong-Qing; Rosen, Barry P.; Zhu, Yong-Guan

2011-01-01

Summary Biotransformation of arsenic includes oxidation, reduction, methylation and conversion to more complex organic arsenicals. Members of the class of arsenite [As(III)] S-adenosylmethyltransferase enzymes catalyze As(III) methylation to a variety of mono-, di- and trimethylated species, some of which are less toxic than As(III) itself. However, no methyltransferase gene has been identified in plants. Here, an arsM gene from the soil bacterium Rhodopseudomonas palustris was expressed in Japonica rice (Oryza sativa L.) cultivar Nipponbare, and the transgenic rice produced methylated arsenic species, which were measured by inductively coupled plasma mass spectrometry (ICP-MS) and high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS). Both monomethylarsenate [MAs(V)] and dimethylarsenate [DMAs(V)] were detected in the root and shoot of transgenic rice. After 12-d exposure to As(III), the transgenic rice gave off 10-fold more volatile arsenicals. The present study demonstrates that expression of an arsM gene in rice induces arsenic methylation and volatilization, providing a potential stratagem for phytoremediation theoretically. PMID:21517874

Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

NASA Astrophysics Data System (ADS)

Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A.; Landero-Figueroa, Julio

2014-10-01

The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV-VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag+) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg- 1 detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm.

Multielemental analysis of prehistoric animal teeth by laser-induced breakdown spectroscopy and laser ablation inductively coupled plasma mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Galiova, Michaela; Kaiser, Jozef; Fortes, Francisco J.

2010-05-01

Laser-induced breakdown spectroscopy (LIBS) and laser ablation (LA) inductively coupled plasma (ICP) mass spectrometry (MS) were utilized for microspatial analyses of a prehistoric bear (Ursus arctos) tooth dentine. The distribution of selected trace elements (Sr, Ba, Fe) was measured on a 26 mmx15 mm large and 3 mm thick transverse cross section of a canine tooth. The Na and Mg content together with the distribution of matrix elements (Ca, P) was also monitored within this area. The depth of the LIBS craters was measured with an optical profilometer. As shown, both LIBS and LA-ICP-MS can be successfully used for themore » fast, spatially resolved analysis of prehistoric teeth samples. In addition to microchemical analysis, the sample hardness was calculated using LIBS plasma ionic-to-atomic line intensity ratios of Mg (or Ca). To validate the sample hardness calculations, the hardness was also measured with a Vickers microhardness tester.« less

Silicon macroporous arrays with high aspect ratio prepared by ICP etching

NASA Astrophysics Data System (ADS)

Wang, Guozheng; Yang, Bingchen; Wang, Ji; Yang, Jikai; Duanmu, Qingduo

2018-02-01

This paper reports on a macroporous silicon arrays with high aspect ratio, the pores of which are of 162, 205, 252, 276μm depths with 6, 10, 15 and 20 μm diameters respectively, prepared by Multiplex Inductively Coupled Plasma (ICP) etching. It was shown that there are very differences in process of high aspect ratio microstructures between the deep pores, a closed structure, and deep trenches, a open structure. The morphology and the aspect ratio dependent etching were analyzed and discussed. The macroporous silicon etched by ICP process yield an uneven, re-entrant, notched and ripples surface within the pores. The main factors effecting on the RIE lag of HARP etching are the passivation cycle time, the pressure of reactive chamber, and the platen power of ICP system.

Application of high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for determination of chromium compounds in the air at the workplace.

PubMed

Stanislawska, Magdalena; Janasik, Beata; Wasowicz, Wojciech

2013-12-15

The toxicity and bioavailability of chromium species are highly dependable on the form or species, therefore determination of total chromium is insufficient for a complete toxicological evaluation and risk assessment. An analytical method for determination of soluble and insoluble Cr (III) and Cr (VI) compounds in welding fume at workplace air has been developed. The total chromium (Cr) was determined by using quadruple inductively coupled plasma mass spectrometry (ICP-MS) equipped with a dynamic reaction cell (DRC(®)). Soluble trivalent and hexavalent chromium compounds were determined by high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). A high-speed, reversed-phase CR C8 column (PerkinElmer, Inc., Shelton, CT, USA) was used for the speciation of soluble Cr (III) and soluble Cr (VI). The separation was accomplished by interaction of the chromium species with the different components of the mobile phase. Cr (III) formed a complex with EDTA, i.e. retained on the column, while Cr (VI) existed in the solutions as dichromate. Alkaline extraction (2% KOH and 3% Na2CO3) and anion exchange column (PRP-X100, PEEK, Hamilton) were used for the separation of the total Cr (VI). The results of the determination of Cr (VI) were confirmed by the analysis of the certified reference material BCR CRM 545 (Cr (VI) in welding dust). The results obtained for the certified material (40.2±0.6 g kg(-1)) and the values recorded in the examined samples (40.7±0.6 g kg(-1)) were highly consistent. This analytical method was applied for the determination of chromium in the samples in the workplace air collected onto glass (Whatman, Ø 37 mm) and membrane filters (Sartorius, 0.8 μm, Ø 37 mm). High performance liquid chromatography with inductively coupled plasma mass spectrometry is a remarkably powerful and versatile technique for determination of chromium species in welding fume at workplace air. Crown Copyright © 2013 Published by Elsevier B.V. All rights reserved.

Geochemical modelling and speciation studies of metal pollutants present in selected water systems in South Africa

NASA Astrophysics Data System (ADS)

Magu, M. M.; Govender, P. P.; Ngila, J. C.

2016-04-01

Metal pollutants in water poses great threats to living beings and hence requires to be monitored regularly to avoid loss of lives. Various analytical methods are available to monitor these pollutants in water and can be improved with time. Modelling of metal pollutants in any water system helps chemists, engineers and environmentalists to greatly understand the various chemical processes in such systems. Water samples were collected from waste water treatment plant and river from highlands close to its source all the way to the ocean as it passing through areas with high anthropogenic activities. Pre-concentration of pollutants in the samples was done through acid digestion and metal pollutants were analysed using inductively coupled plasma-optical emission spectra (ICP-OES) to determine the concentration levels. Metal concentrations ranged between 0.1356-0.4658 mg/L for Al; 0.0031-0.0050 mg/L for Co, 0.0019-0.0956 mg/L for Cr; 0.0028-0.3484 mg/L for Cu; 0.0489-0.3474 mg/L for Fe; 0.0033-0.0285 mg/L for Mn; 0.0056-0.0222 mg/L for Ni; 0.0265-0.4753 mg/L for Pb and 0.0052-0.5594 mg/L for Zn. Modelling work was performed using PHREEQC couple with Geochemist's workbench (GWB) to determine speciation dynamics and bioavailability of these pollutants. Modelling thus adds value to analytical methods and hence a better complementary tool to laboratory-based experimental studies.

Urinary iodine: comparison of a simple method for its determination in microplates with measurement by inductively-coupled plasma mass spectrometry

PubMed Central

Haap, Michael; Roth, Heinz Jürgen; Huber, Thomas; Dittmann, Helmut; Wahl, Richard

2017-01-01

The aim of our study was to develop and validate an inexpensive, rapid, easy to use quantitative method to determine urinary iodine without major procurement costs for equipment. The rationale behind introducing this method is the increasing demand for urinary iodine assessments. Our study included 103 patients (76 female, 27 male), age (arithmetic mean) 52 ± 17.3 years. Urinary iodine was determined in microplates by a modification of the Sandell-Kolthoff reaction. The results were compared with inductively-coupled plasma mass spectrometry (ICP-MS) for iodine, considered as reference method. Geometric mean of urinary iodine determined by the Sandell-Kolthoff reaction method was 62.69 μg/l (95% confidence interval 53.16–73.92) whereas by the ICP-MS method it was 65.53 μg/l (95% confidence interval 54.77–78.41). Passing-Bablok regression equations for both methods gave y = 3.374 + 0.873x (y: Sandell-Kolthoff method, x: ICP-MS). Spearman´s correlation coefficient was 0.981, indicating a very high degree of agreement between the two methods. Bland-Altman plots showed no significant systematic difference between the two methods. The modified Sandell-Kolthoff method using microtiter plate technique presented here is a simple, inexpensive semi-automated method to determine urinary iodine with very little toxic waste. Comparison with the ICP-MS-technique yielded a good agreement between the two methods. PMID:28045077

The potential of inductively coupled plasma mass spectrometry (ICP-MS) for the simultaneous determination of trace elements in whole blood, plasma and serum.

PubMed

Krachler, M; Irgolic, K J

1999-11-01

The advantages accruing to biochemical and clinical investigations from a method that allows the simultaneous quantification (RSD < or = 10%) of many elements in blood, plasma, and serum at concentrations equal to one-hundredth of the lower limits of the normal ranges are undeniable. The suitability of inductively coupled argon plasma low-resolution quadrupole mass spectrometry (ICP-MS), a simultaneous method with low detection limits, is evaluated for the quantification of inorganic constituents in whole blood, plasma, and serum with consideration of the dilution associated with the mineralization of the samples, of isobaric and polyatomic interferences and of normal ranges. Of the 3 bulk elements, the 3 major electrolytes, the 15 essential elements, the 8 toxic elements, the 4 therapeutic elements, and the 14 elements of potential interest (total of 47 elements) only 7 elements (Ca, Cu, K, Mg, Rb, Sr, Zn) can be simultaneously quantified under these rigorous conditions in serum and only 8 elements (additional element Pb) in whole blood. Quantification of elements in the Seronorm Standards "Whole Blood" and "Serum" showed, that this list of simultaneously determinable elements in these matrices is reasonable. Although this list is disappointingly short, the number of elements determinable simultaneously by ICP-MS is still larger than that by ICP-AES or GFAAS. Improved detectors, more efficient nebulizers, avoidance of interferences, better instrument design, and high-resolution mass spectrometers promise to increase the number of elements that can be determined simultaneously.