• Applied Chemistry for Engineering
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• v.10 no.4
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• pp.568-575
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• 1999

Two different digestion procedures for the simultaneous determination of major and platinum-group element(PGE) in spent automobile catalysts containing PGE and silicates by inductively coupled plasma atomic emission spectrometry(ICP-AES) are compared. Combinations of mixed aids using HF, $HNO_3$, HCl, $HClO_4$, $H_2O_2$, and $H_3BO_3$ are utilized for the hot plate dissolution method and the closed-vessel microwave digestion method, The latter method has been shown to be relatively superior in terms of recovery, analysis time, and amount of aqua regia (3 parts HCl + part $HNO_3$ required to dissolve PGE in comparison with conventional open vessel hot-plate dissolution. The best results were drawn from the following conditions: In closed Teflon PFA vessels under microwave heating with temperature/pressure regulation, a 0.25 g portion of sample was digested in 2 mL of HF, 2 mL of $HNO_3$ and 6mL of HCl under the pressure of 200 psi(13.79 bar) at $180^{\circ}C$ for 1hr, followed by a second digestion stage with 16 mL of 5%(w/v) boric acid under the pressure of 20 psi(1.38 bar) at $100^{\circ}C$ for 10 min. After the microwave heating, the sample was post-treated with 10 mL of aqua regia twice by hot-plate heating. This condition gives the PGE recovery within 85~110% and the relative standard deviations within 2%. The method developed can therefore be regarded as an alternative method for routine analysis of spent automobile catalysts.

• Journal of Korean Society of Environmental Engineers
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• v.36 no.11
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• pp.764-770
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• 2014

This study assessed analysis of N-nitrosamines by separation, identification, and quantification using a gas chromatography (GC) mass spectrometer (MS) with electron impact (EI) mode. Samples were pretreated by a automated solid phase extraction (SPE) and a nitrogen concentration technique to detect low concentration ranges. The analysis results by EI-GC/MS (SIM) and EI-GC/MS/MS (MRM) on standard samples with no pretreatment exhibited similar results. On the other hand, the analysis of pretreated samples at low concentrations (i.e. ng/L levels) were not reliable with a EI-GC/MS due to the interferences from impurity peaks. The method detection limits of eight (8) N-nitrosamines by EI-GC/MS/MS analysis ranged from 0.76 to 2.09 ng/L, and the limits of quantification ranged from 2.41 to 6.65 ng/L. The precision and accuracy of the method were evaluated using spiked samples at concentrations of 10, 20 and 100 ng/L. The precision were 1.2~13.6%, and the accuracy were 80.4~121.8%. The $R^2$ of the calibration curves were greater than 0.999. The recovery rates for various environmental samples were evaluated with a surrogate material (NDPA-$d_{14}$) and ranged 86.2~122.3%. Thus, this method can be used to determine low (ng/L) levels of N-nitrosamines in water samples.

• Analytical Science and Technology
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• v.28 no.3
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• pp.228-235
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• 2015

The efficiency and applicability of the solid phase extraction disk method in a ²²⁶Ra analysis were examined by the gamma ray spectrometer (GRS) method using a Marinelli beaker and the liquid scintillation counter (LSC) method for groundwater. The recovered ²²⁶Ra, which was filtered by the solid phase extraction disk, was analyzed using gamma ray spectrometer The disks, which were pretreated for caulking the daughter nuclide, were sealed with polyethylene film. Distilled water was used for the blank value of the ²²⁶Ra activity. The recovery values of ²¹⁴Bi and ²¹⁴Pb in the solid phase extraction disk, which used ²²⁶Ra standard material, were 80% (295.21 Kev) and 104% (351.92 Kev), respectively, which were higher than 75% determined by the LSC. The injection of nitrogen gas into the measuring chamber reduced the interference values by about 10%. The detection limits of the ²²⁶Ra activity in a blank sample of 5 L were 0.17~0.40 pCi/L after 80,000 seconds of measuring time. The relationship of the ²²⁶Ra activity in the solid phase extraction disk method and in the LSC method in seven groundwater samples showed a correlation coefficient value 0.987, which implies the applicability of the solid phase extraction disk method. The results showed that ²²⁶Ra activity in groundwater using the solid phase extraction disk method has the following benefits: simple pretreatment, time saving, high recovery values, a low detection limit, and so on. Compared with the LSC method and the GRS method using the Marinelli beaker for the ²²⁶Ra analysis, the solid phase extraction disk method could be useful in groundwater samples with low levels of activities of radionuclides because the method is not restricted by the volume of the sample.

• Applied Biological Chemistry
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• v.10
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• pp.1-13
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• 1968

Phytin is a salt(mainly calcium and magnesium) of phytic acid and its purity and molecular formula can be determined by assaying the contents of phosporus, calcium and magnesium in phytin. In order to devise a new method for the quantitative analysis of the three elements in phytin, the chelatometric method was developed as follows: 1) As the pretreatment for phytin analysis, it was ashfied st $550{\sim}600^{\circ}C$ in the presence of concentrated nitric acid. This dry process is more accurate than the wet process. 2) Phosphorus, calcium and megnesium were analyzed by the conventional and the new method described here, for the phytin sample decomposed by the dry process. The ashfied phytin solution in hydrochloric acid was partitioned into cation and anion fractions by means of a ration exchange resin. A portion of the ration fraction was adjusted to pH 7.0, followed by readjustment to pH 10 and titrated with standard EDTA solution using the BT [Eriochrome black T] indicator to obtain the combined value of calcium and magnesium. Another portion of the ration fraction was made to pH 7.0, and a small volume of standard EDTA solution was added to it. pH was adjusted to $12{\sim}13$ with 8 N KOH and it was titrate by a standard EDTA solution in the presence of N-N[2-Hydroxy-1-(2-hydroxy-4-sulfo-1-naphytate)-3-naphthoic acid] diluted powder indicator in order to obtain the calcium content. Magnesium content was calculated from the difference between the two values. From the anion fraction the magnesium ammonium phosphate precipitate was obtained. The precipitate was dissolved in hydrochloric acid, and a standard EDTA solution was added to it. The solution was adjusted to pH 7.0 and then readjusted to pH 10.0 by a buffer solution and titrated with a standard magnesium sulfate solution in the presence of BT indicator to obtain the phosphorus content. The analytical data for phosphorus, calcium and magnesium were 98.9%, 97.1% and 99.1% respectively, in reference to the theoretical values for the formula $C_6H_6O_{24}P_6Mg_4CaNa_2{\cdot}5H_2O$. Statical analysis indicated a good coincidence of the theoretical and experimental values. On the other hand, the observed values for the three elements by the conventional method were 92.4%, 86.8% and 93.8%, respectively, revealing a remarkable difference from the theoretical. 3) When sodium phytate was admixed with starch and subjected to the analysis of phosphorus, calcium and magnesium by the chelatometric method, their recovery was almost 100% 4) In order to confirm the accuracy of this method, phytic acid was reacted with calcium chloride and magnesium chloride in the molar ratio of phytic: calcium chloride: magnesium chloride=1 : 5 : 20 to obtain sodium phytate containing one calcium atom and four magnesium atoms per molecule of sodium phytate. The analytical data for phosporus, calcium and magnesium were coincident with those as determine d by the aforementioned method. The new method employing the dry process, ion exchange resin and chelatometric assay of phosphorus, calcium and magnesium is considered accurate and rapid for the determination of phytin.

• Clinical and Experimental Pediatrics
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• v.48 no.2
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• pp.191-196
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• 2005

Purpose : Short stature is one of the characteristic features of Turner syndrome. We investigated the factors affecting final adult height(FAH) in patients with Turner syndrome. Methods : The study group was comprised of 60 patients who were diagnosed with Turner syndrome by chromosomal study and clinical phenotypes and attained FAH. Data were obtained from retrospective review of the medical records. We analyzed the factors influencing FAH in growth hormone(GH) treated and GH untreated groups. Results : Sixty patients were enrolled; 48 patients received GH treatment, and 12 patients did not. Mean duration of GH treatment was 35.8 months(range 4 to 120 months), and mean dosage of GH was $0.8{\pm}0.2IU/kg/wk$ in GH treated group. Mean growth velocity was $5.6{\pm}2.0cm/yr$, which was significantly higher than that during pretreatment period. In the GH treated group, mean chronological age, bone age, mean height, and height standard deviation(SD) score at GH treatment were $12.2{\pm}2.7yr$ $10.3{\pm}2.5yr$ $127.5{\pm}10.1cm$ and $-3.1{\pm}1.1$, respectively. In the GH treated group, the mean FAH and SD score of FAH were $146.9{\pm}5.8cm$ and $-2.7{\pm}1.2$, respectively, which showed significant differences compared with those of the GH untreated group. Analyzing the factors affecting FAH in GH-treated patients, only the SD score of height at the time of treatment was significantly related to FAH. Conclusion : GH treatment leads to an increment in FAH in patients with Turner syndrome. Average FAH gain was as much as 5.8 cm. SD score of height at the time of GH treatment was the only factor influencing FAH.

• Economic and Environmental Geology
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• v.55 no.6
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• pp.727-736
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• 2022

Ice wedges are subsurface ice mass structures that formed mainly by freezing precipitation with airborne dust and surrounding soil particles flowed through the active layer into the cracks growing by repeating thermal contractions in the deeper permafrost layer over time. These ice masses characteristically contain high concentrations of solutes and solids. Because of their unique properties and distribution, the possibility of harnessing ice wedges as an alternative archive for reconstructing paleoclimate and paleoenvironment has been recently suggested despite limited studies. It is imperative to preserve the physicochemical properties of the ice wedge (e.g., solute concentration, mineral particles) without any potential alteration to use it as a proxy for reconstructing the paleo-information. Thawing the ice wedge samples is prerequisite for the assessment of their physicochemical properties, during which the paleo-information could be unintentionally altered by any methodological artifact. This study examined the effect of thawing conditions and procedures on the physicochemical properties of solutes and solid particles in ice wedge samples collected from Cyuie, East Siberia. Four different thawing conditions with varying temperatures (4 and 23℃) and oxygen exposures (oxic and anoxic) for the ice wedge sample treatment were examined. Ice wedge samples thawed at 4℃ under anoxic conditions, wherein biological activity and oxidation were kept to a minimum, were set as the standard thawing conditions to which the effects of temperature and oxygen were compared. The results indicate that temperature and oxygen exposure have negligible effects on the physicochemical characteristics of the solid particles. However, the chemical features of the solution (e.g., pH, electric conductivity, alkalinity, and concentration of major cations and trace elements) at 4℃ under oxic conditions were considerably altered, compared to those measured under the standard thawing conditions. This study shows that the thawing condition of ice wedge samples can affect their chemical features and thereby the geochemical information therein for the reconstruction of the paleoclimate and/or paleoenvironment.