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A direct sampling with organic solvent extracts for simultaneous multi-element determination implemented with inductively coupled plasma atomic emission spectrometry (ICP-AES) associated with a flow injection liquid-liquid extraction (FI-LLE) sample preconcentration method was studied. The "robustness" of the plasma discharge with tributyl phosphate (TBP) loading was diagnosed by using the Mg II 279.55 nm and Mg I 285.21 nm lines intensity ratio. A FI-LLE preconcentration system for rare earth elements (REEs)-nitrate-TBP was established by using a laboratory-designed phase separator. For these elements, an average sensitivity enhancement factor of 64 was obtained with respect to ICP-AES sampling with aqueous solutions. The precision of the method was characterized by a relative standard deviation (%RSD) of 1.8 - 5.2%. A throughput of 27 samples per hour can be achieved with an organic solvent consumption of less than 200 microl per determination. Good results were obtained for the analysis of standard reference materials.
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PMID:Determination of rare earth elements in geological samples by inductively coupled plasma atomic emission spectrometry with flow injection liquid-liquid extraction. 1469 26

Silver compounds are used in pharmaceutical and ayurvedic medicines. A method is proposed for the extraction separation of silver from Cu, Cd, Zn, Ni, Pt (IV) and Au (III) from nitrate solution using triphenylphosphine sulphide as an extractant. The recovery of silver is tested both volumetrically and/or by ICP-AES technique.
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PMID:Extraction and separation of silver using triphenylphosphine sulphide. 1504 40

Recent regulation in Japan requires more sensitive trace analysis methods for the determination of arsenic and selenium and their oxidation states As(III) and (V), Se(IV) and (VI). The hydride generation (HG) technique is usually used in combination with AAS and ICP-AES to increase sensitivity. However, hydrochloric acid is mostly used to acidify the sample solution in HG. Isobaric interferences due to chlorine-related species cause mass spectral problems when the same solution is used for the determination of these elements by ICP-MS. In this study, different oxidation states of As and Se were determined by coupling ion chromatography (IC) to an ICP-AES instrument. An HG technique was used to introduce test samples into the ICP. Nitric acid was employed to acidify the samples for HG. The concentrations of acid and base were kept as low as possible to reduce contamination. The formation of As and Se hydrides could be achieved without HCl, if the concentrations of acid and alkaline solutions were optimized. However, HCl was necessary for additional reduction of Se(VI) to Se(IV).
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PMID:Determination of different oxidation states of arsenic and selenium by inductively coupled plasma-atomic emission spectrometry with ion chromatography. 1504 2

New column leaching experiments were designed and used as an alternative rapid screening approach to element mobility assessment. In these experiments, field-moist material was treated with an extracting solution to assess the effects of acidification on element mobility in mine tailings. The main advantage of this version of column leaching experiments with partitioned segments is that they give quick information on current element mobility in conditions closely simulating field conditions to compare with common unrepresentative air-dried, sieved samples used for column leaching experiments. Layers from the tailings dump material were sampled and packed into columns. The design of columns allows extracting leachates from each layer. The extracting solutions used were natural (pH 6.8) and acidified (pH 4.2) rainwater. Metals and anions were determined in the leachates. The concentrations of metals (Ca, Mg, Fe, Mn, Al, Cr, Ni, Co, Zn, and Cu) in sample leachates were determined using ICP OES. The most important anions (NO3-, Cl-, and SO4(2)-) were determined using the closed system izotacophoresis ITP analyser. The chemical analytical data from tailings leaching and physico-chemical data from field measurements (including pH, conductivity, redox potential, temperature) were used for chemometric evaluation of element mobility. Principal factor analysis (PFA) was used to evaluate ions mobility from different layers of tailings dump arising from varied pH and redox conditions. It was found that the results from the partitioned column leaching illustrate much better complex processes of metals mobility from tailings dump than the total column. The chemometric data analysis (PFA) proofed the differences in the various layers leachability that are arising from physico-chemical processes due to chemical composition of tailings dump deposit.
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PMID:Ion mobility based on column leaching of South African gold tailings dam with chemometric evaluation. 1510 78

The possibility of screening the mercury(II) content in real environmental samples based on inhibition of the activity of dissolved invertase has been examined. The extent of inhibition was measured with an amperometric glucose biosensor with glucose oxidase immobilized on a membrane. Data concerning the stability and reproducibility of measurements are provided. The effects of heavy metals on the inhibition of invertase, together with that of common anions such as chloride, nitrate and sulfate are reported. The determination of mercury using this procedure has been carried out in samples of natural and waste water samples of various origins already analyzed by ICP-AES, by spiking ppb levels of mercury(II). Differences in the inhibiting effect of the samples and in the recoveries were found and are discussed.
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PMID:Limitations in the analytical use of invertase inhibition for the screening of trace mercury content in environmental samples. 1522 7

This paper proposes a practical method for estimating source attribution by using a three-step methodology. The main objective of this study is to explore the use of the three-step methodology for quantifying the source impacts of 24-h PM2.5 particles at an urban site in Seoul, Korea. 12-h PM2.5 samples were collected and analyzed for their elemental composition by ICP-AES/ICP-MS/AAS to generate the source composition profiles. In order to assess the daily average PM2.5 source impacts, 24-h PM2.5 and polycyclic aromatic hydrocarbons (PAH) ambient samples were simultaneously collected at the same site. The PM2.5 particle samples were then analyzed for trace elements. Ionic and carbonaceous species concentrations were measured by ICP-AES/ICP-MS/AAS, IC, and a selective thermal MnO2 oxidation method. The 12-h PM2.5 chemical data was used to estimate possible source signatures using the principal component analysis (PCA) and the absolute principal component scores method followed by the multiple linear regression analysis. The 24-h PM2.5 source categories were extracted with a combination of PM2.5 and some PAH chemical data using the PCA, and their quantitative source contributions were estimated by chemical mass balance (CMB) receptor model using the estimated source profiles and those in the literature. The results of PM2.5 source apportionment using the 12-h derived source composition profiles show that the CMB performance indices; chi2, R2, and percent of mass accounted for are 2.3%, 0.97%, and 100.7%, which are within the target range specified. According to the average PM2.5 source contribution estimate results, motor vehicle exhaust was the major contributor at the sampling site, contributing 26% on average of measured PM2.5 mass (41.8 microg m-3), followed by secondary sulfate (23%) and nitrate (16%), refuse incineration (15%), soil dust (13%), field burning (4%), oil combustion (2.7%), and marine aerosol (1.3%). It can be concluded that quantitative source attribution to PM2.5 in an urban area where source profiles have not been developed can be estimated using the proposed three-step methodology approach.
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PMID:Source contributions to fine particulate matter in an urban atmosphere. 1572 93

By using ICP-MS method, this paper determined the accumulation of La in mice liver after the mice being fed with La(NO3)3 water solution for thirty days, and through in vitro experiment, studied the effect of La(NO3)3 on the micronucleus rate of mice bone marrow cells and the cleavage action of La(NO3)3 on genome DNA to investigate the genetic toxicity of La. The results showed that when the treated concentration was 1000, 500, 300 and 50 microg x ml(-1), the amount of La in mice liver reached 1.46, 0.558, 0.529 and 0.083 microg x g(-1), respectively. Compared with control, the La amount in disposed groups' mice livers increased with increasing La(NO3)3 concentration in water (r = 0.980). T-test results showed that there existed significant differences in 1000, 500 and 300 microg x ml(-1) disposed groups when compared with the control (P < 0.05). The micronucleus rate of mice bone marrow cells increased with increasing La(NO3)3 concentration in water (r = 0.853). The in vitro experiments showed that La(NO3)3 could make DNA cleaved. It could be concluded that that La might be accumulated in organisms, and could induce the damage of genetic material in cells.
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PMID:[Accumulation of La(NO3)3 in mice liver and its genetic toxicity]. 1585 73

The main aim of the international UNECE monitoring program ICP Waters under the Convention of Long-range Transboundary Air Pollution (CLRTAP) is to assess, on a regional basis, the degree and geographical extent of the impact of atmospheric pollution, in particular acidification, on surface waters. Regional trends are calculated for 12 geographical regions in Europe and North America, comprising 189 surface waters sites. From 1990-2001 sulphate concentrations decreased in all but one of the investigated regions. Nitrate increased in only one region, and decreased in three North American regions. Improvements in alkalinity and pH are widely observed. Results from the ICP Waters programme clearly show widespread improvement in surface water acid-base chemistry, in response to emissions controls programs and decreasing acidic deposition. Limited site-specific biological data suggest that continued improvement in the chemical status of acid-sensitive lakes and streams will lead to biological recovery in the future.
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PMID:Regional scale evidence for improvements in surface water chemistry 1990-2001. 1594 47

Since years, ion exclusion chromatography (ICE) has been the standard method to separate strong acid analyte anions from concentrated weak acid matrices such as hydrofluoric acid (HF). In this work, the commercially available IonPac ICE-AS 1 column was used to separate trace levels of chloride, nitrate, sulfate and phosphate from HF solutions at 20% (w/w). The efficiency of the separation was studied in more detail using techniques such as ion chromatography (IC), inductively coupled plasma optical emission spectrometry (ICP-OES) and ICP-mass spectrometry (ICP-MS). For 20% (w/w) HF solutions and at a water carrier flow-rate of 0.50 ml/min, the cut window was set from 8.5 to 14.5 min. Under these conditions, analyte recoveries of better than 90% were obtained for chloride, nitrate and sulfate, but only about 75% for phosphate. The HF rejection efficiency was better than 99.9%. It was found that the ICP techniques, measuring total element levels and not species, yielded significantly higher recoveries for phosphorus and sulfur compared to IC. Evidence will be given that part of the added phosphorus (approximately 15% for an addition of 10 mg PO4/kg) is present as mono-fluorophosphoric acid (H2FPO3). In the case of sulfate, the difference between IC and ICP-MS could be attributed to an important matrix effect from the residual HF concentration.
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PMID:Trace anion determination in concentrated hydrofluoric acid solutions by two-dimensional ion chromatography I. Matrix elimination by ion-exclusion chromatography. 1610 49

Selenium (Se) is an essential trace element that is often deficient in the natural diets of domestic animal species. The measurement of Se in whole blood or liver is the most accurate way to assess Se status for diagnostic purposes. This study was conducted to compare hydride generation atomic absorption spectroscopy (HG-AAS) with inductively coupled plasma-mass spectrometry (ICP-MS) for the detection and quantification of Se in liver samples. Sample digestion was accomplished with magnesium nitrate and nitric acid for HG-AAS and ICP-MS, respectively. The ICP-MS detection was optimized for 82Se with yttrium used as the internal standard and resulted in a method detection limit of 0.12 microg/g. Selenium was quantified by both methods in 310 samples from a variety of species that were submitted to the Toxicology Laboratory at New Bolton Center (Kennett Square, PA) for routine diagnostic testing. Paired measurements for each sample were evaluated by a mean difference plot method. Limits of agreement were used to describe the maximum differences likely to occur between the 2 methods. Results suggest that under the specified conditions ICP-MS can be reliably used in place of AAS for quantitation of tissue Se at or below 2 microg/g to differentiate between adequate and deficient liver Se concentrations.
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PMID:Comparison of selenium determination in liver samples by atomic absorption spectroscopy and inductively coupled plasma-mass spectrometry. 1613 Sep 90


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