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The comparison of sample extraction procedures for the determination of cations in soil by IC and ICP-AES

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Stanišić S., Ignjatović L., Manojlović D., Dojčinović B.
Open Chemistry
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2011
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vol. 9
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issue 3
481-491
EN
This paper presents the extraction of cations from a soil sample, type ranker on serpentinite, in deionized water, by use of three different extraction techniques. The first extraction technique included the use of a rotary mixer, the second technique involved the use of a microwave digestion system with different extraction temperatures, and the third technique employed an ultrasonic bath with different extraction times. Ion chromatography was used for determining the concentration of Li, Na, K, Ca, Mg and ammonium ions in soil extracts with subsequent determination of concentrations for all cations, except for ammonium ion extraction, conducted by Inductively Coupled Plasma-Atomic Emission Spectrometry. The results of cation extractions showed that microwave assisted extraction was most efficient for the Li, Na, K, Ca, Mg, Co, Mn, Ni, Pb and ammonium ions. Use of a rotary mixer for extraction was most efficient for Cd and Zn ions, while use of ultrasound bath was most efficient for Cr, Cu, Fe and Al ions. Several times higher amount of cations extracted by the most efficient, compared to the second best technique, under optimal conditions, were noticed in the case of: Ca, Mg, Co, Mn, Fe, Al, and Zn ions.
2
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Ion chromatographic method for the determination of cations of group IA and IIA in water samples, pharmaceuticals and energy drinks by non-suppressed conductometric detection

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Zachariadis G., Lyratzi A., Stratis J.
Open Chemistry
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2011
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vol. 9
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issue 5
941-947
EN
An efficient ion chromatographic (IC) method was developed for the simultaneous quantitative determination of Li+, Na+, NH4+, K+, Cs+, Ca2+, Mg2+, Sr2+, Ba2+ and Be2+ in energy drinks, pharmaceutical and drinking water samples by non-suppressed conductometric detection. The separation of ten cations including ammonium was achieved using a cation-exchange column and low conductivity mobile phase. The mobile phase consisted of tartaric acid, dipicolinic acid and boric acid. The separation of the cations was completed in less than 18 min, with a flow rate of 1.2 mL min−1. The separation was not affected by the existence of cations Co2+, Cr3+, Cd2+, Cu2+, Bi3+, Ag+, Fe3+ and Zn2+ in concentrations up to 20 mg L−1. Using an injection volume of 20 μL the obtained detection limits were 0.003 mg L−1, 0.02 mg L−1, 0.01 mg L−1, 0.01 mg L−1, 0.10 mg L−1, 0.01 mg L−1, 0.02 mg L−1, 0.02 mg L−1, 0.003 mg L−1 and 0.1 mg L−1, for Li+, Na+, NH4+, K+, Cs+, Ca2+, Mg2+, Sr2+, Be2+ and Ba2+ respectively. The intra-day repeatability (RSD%, n=5) ranged from 1.1% to 4.8%, and the inter-day (n=5) between 1.8% and 5.4% respectively. The method was applied to the analysis of various bottled and tap water, pharmaceutical preparations and energy drinks commercially available. [...]
3
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High-throughput powder X-ray diffraction, IR-spectroscopy and ion chromatography analysis of urinary stones: A comparative study

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Yusenko E., Yusenko K., Korolkov I., Shubin A., Kapsargin F., Efremov A., Yusenko M.
Open Chemistry
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2013
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vol. 11
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issue 12
2107-2119
EN
The instrumental qualitative analysis of urinary stones is a critical step in clinical practice and urological research. A powder X-ray diffraction, IR-spectroscopy and ion chromatography have been applied for the qualitative analysis of 20 urinary stones. Suggestions for a sample preparation and an optimal measurement strategy were formulated. The main difficulties for the powder X-ray diffraction qualitative analysis are a limiting amount of the sample and a preferential orientation of crystals, both issues should be minimized by the special sample preparation. Urinary stones samples have been clustered into four groups using different sets of numerical input data (cation and anion content, phase composition). At the same time a high-throughput multivariate clustering has been applied for powder X-ray diffraction and IR-spectroscopy data. The multivariate whole-profile approach can be used as a tool for a high-throughput time reducing technique for clinical practice, when a quick and stable classification of samples is required. All three sets of the data can be automatically separated into three clusters: oxalate-reach, oxalate-pure and non-oxalate samples. Uricite-pure and uricite-rich samples can be easily clustered. [...]
4
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Spatial variations in the distribution of trace ionic impurities in the water-steam cycle in a thermal power plant based on a multivariate statistical approach

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Živojinović D., Rajaković-Ognjanović V., Onjia A., Rajaković L.
Open Chemistry
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2013
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vol. 11
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issue 9
1456-1470
EN
Abstract In this study, a multivariate statistical approach was used to identify the key variables responsible for process water quality in a power plant. The ion species that could cause corrosion in one of the major thermal power plants (TPP) in Serbia were monitored. A suppressed ion chromatographic (IC) method for the determination of the target anions and cations at trace levels was applied. In addition, some metals important for corrosion, i.e., copper and iron, were also analysed by the graphite furnace atomic absorption spectrophotometric (GFAAS) method. The control parameters, i.e., pH, dissolved oxygen and silica, were measured on-line. The analysis of a series of representative samples from the TPP Nikola Tesla, collected in different plant operation modes, was performed. Every day laboratory and on-line analysis provides a large number of data in relation to the quality of water in the water-steam cycle (WSC) which should be evaluated and processed. The goal of this investigation was to apply multivariate statistical techniques and choose the most applicable technique for this case. Factor analysis (FA), especially principal component analysis (PCA) and cluster analysis (CA) were investigated. These methods were applied for the evaluation of the spatial/temporal variations of process water and for the estimation of 13 quality parameters which were monitored at 11 locations in the WSC in different working conditions during a twelve month period. It was concluded that PCA was the most useful method for identifying functional relations between the elements. After data reduction, four main factors controlling the variability were identified. Hierarchical cluster analysis (HCA) was applied for sample differentiation according to the sample location and working mode of the TPP. On the basis of this research, the new design of an optimal monitoring strategy for future analysis was proposed with a reduced number of measured parameters and with reduced frequency of their measurements. Graphical abstract [...]
5
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A preliminary study on the effect of mineralization parameters on determination of metals in Viscum album species

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Blicharska E., Komsta Ł., Kocjan R., Gumieniczek A., Robak A.
Open Chemistry
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2010
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vol. 8
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issue 2
264-268
EN
An increasing interest in determination of various macro- and microelements in medicinal plants has been observed. The majority of studies are carried out using one mineralization method without any optimization. The present study demonstrates that changes in mineralization parameters can significantly affect the recovery of the elements determined. In the study, the dried plant material was mineralized in 12 ways and iron (Fe), copper (Cu), zinc (Zn), nickel (Ni) and manganese (Mn) levels were determined. The samples were mineralized in the dry or open microwave mode as well as 10 closed microwave modes. The influence of acid amounts, irradiation power and time, addition of hydrogen peroxide and perfluoric acid was examined. All parameters were shown to be critical - good efficiency was observed with larger amounts of acid. The determined content varied significantly in the same sample and were in the ranges (ug g−1): 46–136 (Fe), 1.4–11.8 (Cu), 4.0–11.3 (Ni), 15.4–53.8 (Zn) and 9.5–67.6 (Mn). Increased irradiation resulted in the loss of copper and zinc and better recovery of nickel. The results demonstrate that such determinations should include the mineralization optimization step. [...]
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