• Analytical Science and Technology
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• v.15 no.5
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• pp.475-481
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• 2002

The determination of phthalates and adipate in natural mineral water and its container is described. Phthalates and adipate were extracted from natural mineral water by liquid-liquid extraction with methylene chloride, concentrated and then injected in GC-MS (SIM). Phthalates and adipate from 1) PET, cap, label and glue were extracted in Soxhlet with 50 mL of carbon tetrachloride, purified with silicagel and detected with GC-MS (SIM). Peak shapes and quantitation of phthalates and adipate were excellent, with linear calibration curves over a range of $0.1{\sim}10{\mu}g/L$ in water sample ($r^2$ > 0.996) and over a range of $1{\sim}1,000{\mu}g/Kg$ in solid samples ($r^2$>0.994). The detection limits of analytes were $0.002{\sim}0.010{\mu}g/L$ in water and $0.01{\sim}0.02{\mu}g/Kg$ in solid samples. Five kinds of natural mineral water samples, two PETs, two labels, two caps and two glues were quantified by the described procedure. As a results, the concentrations of total phthalates in natural mineral water ranged from ND ~ 1.2 ng/mL. Otherwise, the concentrations of total phthalate extracted from PET ranged from 0.55 ~ 1.2 mg/Kg. We found that the accurate determination of phthalte and adipate in natural mineral water and container must be considered blank correction and the removal of label and glue in PET sample.

• Journal of Food Hygiene and Safety
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• v.24 no.4
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• pp.332-337
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• 2009

Most propionic acid is added to food (especially breads) as preservatives and its form is sodium or calcium salt. Most countries admitted propionic acid as food preservatives but a tolerance limit is somewhat different according to countries. Recoveries of the official method for propionates reported as 50.0~60.0%. Accordingly new rapid determination method for propionates was developed using formic acid added sodium chloride (5 g) and ether (formic acid : ether = 1 : 2) as the extraction solvent to improve the official method with the complex processes. Propionate was dissolved from the samples with formic acid omitting steam distillation and ion exchange procedure. Then propionate in formic acid was extracted with ether and sodium chloride again. A $1\;{\mu}l$ aliquot of the filtrate of ether was analyzed by gas chromatograph. Recoveries from sample A and B fortified with propionic acid sodium salt were 85.0 % and 90.0 %, respectively.

• Journal of the Korean Chemical Society
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• v.27 no.4
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• pp.279-286
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• 1983

An apparatus was made for the electrodeposition of alpha emitting actinide nuclides, $^{207}Bi$ and $^{210}Po$. The electrodeposition was made on a polished stainless steel plate cathode. The anode was made of platinum wire and to stir the solution. With the ammonium chloride as electrolyte initial pH = 4, chloride concentration = 0.6M and solution volume = 15ml, a current of 1.5 ampere(current density = 0.59A/$cm^2$) was flowed for 100 minutes for the quantitative recovery of electrodeposition and on average recovery of 98.3% was obtained within ${\pm}$0.7% uncertainty. Alpha spectrometry of the electrodeposited sample showed alpha peaks from $^{210}Po, ^{234}U$ and $^{239}Pu$ having energy resolution (FWHM) of 18.3, 21.8 and 36.0 keV respectively. The electrodeposition and alpha spectrometry for a natural uranium sample of domestic origin gave $^{238}U : ^{234}U = 1 : 6.1{\times}10^{-5}$ and for a neutron-irradiated uranium sample did $^{238}U : ^{239}Pu : ^{241}Am = 100 : 0.0263 : 5.20{times}10^{-5}$. The result of $^{238}U$ determination in the irradiated sample by electrodeposition-alpha spectrometry was in accord within ${\pm}1.6%$ of relative error with the results of solid fluorimetry and mass spectrometry. For $^{239}Pu$ the result of electrodeposition-alpha spectrometry was in accord within ${\pm}$4.0% of relative error with the results of anion exchange separation and the thenoyltrifluoroacetone(TTA) extraction both followed by alpha spectrometries.

• Journal of Conservation Science
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• v.31 no.2
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• pp.95-104
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• 2015

Excavated archaeological cast iron objects in improper storage are quickly corroded and disintegrated into block and powder finally. Hence desalination treatment which is a way of removing internal corrosive factors, especially chloride ion, is an important process. But desalination is often omitted or objects are dehydrated by alcohol because the destruction of objects could occur during desalting. Although current desalting methods mostly use an aqueous alkali solution, $OH^-$ ions of water could accelerate corrosion and broaden internal cracks cause of high surface tension. Therefore this study experimented desalting using ethyl alcohol, which is low surface tension, to investigate an effect of desalination. As a result, desalting using ethyl alcohol showed the similar or more effective results of desalting using water. In addition, as aspects of desalting safety, ethyl alcohol desalting method was smaller destruction of objects and extraction of Fe from the objects than the aqueous alkali solution. However, this study explored the possibility of desalting methods using organic solvent in fieldwork, so the results would provide basic date for making the safe and effective desalting method for archaeological cast iron objects through further experiments.

• Journal of the Korean Chemical Society
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• v.8 no.3
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• pp.113-120
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• 1964

The critical examination of the spectrophotometric method for determining microgram quantities of phosphate by the n-butyl acetate extraction as molybdophosphoric acid and subsequent development of the molybdenum blue has been made. In this procedure from 2 to 8 ${\mu}g$. of phosphate-phosphorus can be determined under optimum conditions. The final concentration of ammonium molybdate and the final acidity of perchloric acid for the formation of heteropoly acid are suitable to be ranges of 0.5 to 1.1% and 0. 5 to 1. 1 N respectively, and subsequently extracted with 10 ml. of n-butyl acetate. The extract is developed to molybdenum blue with 5.0 ml. of 1. 3% stannous chloride in 1N hydrochloric acid. The color is stable for at least one hour in the use of perchloric acid for the condensation. In order to determination of submicrogram amounts of phosphate, the sensitivity of the molybdenum blue method is hardly sufficient, a sensitive and stable molybdenum(V)-thiocyanate complex method has been investigated. By the procedure less than 1.2 ${\mu}g$. of phosphate-phosphorus can be determined with an accuracy of less than 5% the relative error. The molybdenum(Ⅵ) extracted by the above procedure is reduced to molybdenum(V) in the extract directly with a solution of 4 to 10% of stannous chloride, 0.5 to 1.5 mM of copper, and 0.1 to 0.9 N of perchloric acid as final concentration in 4.3 to 6.3 N of hydrochloric acid or 9.0 to 13.0 N of sulfuric acid by heating for one minute in boiling water, after cooling, the molybdenum(V)-thiocyanate complex color is developed by adding 6.0 M ammonium thiocyanate solution making the final concentration to be in a range of 0.4 to 0.9 M. This procedure the very sensitive, reliable, and stable can be applied to determining submicrogram amounts of phosphate in natural waters with a precision of 1.6 ${\times}\;10^{-2}$ the standard deviation as absorbance.

• Journal of the Korean Vacuum Society
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• v.18 no.3
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• pp.236-243
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• 2009

Proton Engineering Frontier Project (PEFP) has supplied the metal ions to users by using an installed metal ion implanter of 120 keV. At present a feasibility study is being performed for a cobalt ion implantation. For a cobalt ion extraction we studied to sustain the high temperature($648^{\circ}C$) for metal ions vaporization from a cobalt chloride powder by using an alumina crucible in the ion source. The temperature condition of the crucible was satisfied with the plasma generation at the arc current of 120V and EHC power of 250W. The extracted beam current of $Co^+$ ions was dependent on the arc current in the plasma. The maximum beam current was $100{\mu}A$ at 0.18A of the arc current. The 3 peak currents of the extracted ions such as $Co^+$, $CoCl^+$ and $Cl^+$ were obtained by adjusting a mass analyzing magnet and the $Co^+$ ion beam peak current fraction as around 70% in the sum of the peak currents. The fluence of the implanted cobalt ions at the $10{\mu}A$ of the beam current and 90 minutes of the implantation time into an aluminum sample as measured around $1.74{\times}10^{17}#/cm^2$ by a quantitative analysis method of RBS (Rutherford Backscattering Spectrometry).

• Food Science and Preservation
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• v.22 no.6
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• pp.859-866
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• 2015

The purpose of this study was to develop a supplemental healthy food that can help prevent high blood pressure-related diseases caused due to the excessive consumption of sodium in salt. This was achieved by using ion-displacement techniques to produce mineral salt with lower sodium content by using fermented brown rice by-products rich in minerals. Mineral salt containing 2019.2 mg/100 g of potassium, 678.5 mg/100 g of magnesium, 48.7 mg/100 g of calcium, and 19.5 mg/100 g of sodium was obtained by fermenting brown rice by-products to create a culture medium for the mineral salt. Mineral salt containing 1769.7 mg/100 g of potassium, 573.6 mg/100 g of magnesium, 35.3 mg/100 g of calcium, and 19.5 mg/100 g of sodium was obtained by filtering and refining the by-product extract of fermented brown rice. The results showed that when the stream velocity of the instrument used for electrolysis was 200 mL/min and the current and the concentration of the reactive liquid in the purified water chamber were higher, the effect of electrolysis was greater. Ion hot water extraction of the fermented brown rice by-products improved by up to 95% and was collected as purified water within 90 min of the reaction time. Chloride ions with pH 7.4 were produced by mixing sodium hydroxide in a purified saline water chamber with electro-analyzed water. The salt produced in this study contained low sodium, 5.7~30%, as compared to 40% sodium content of the normal salt.

• Journal of the Korean GEO-environmental Society
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• v.11 no.5
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• pp.61-67
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• 2010

In this study, Solid-phase microextraction (SPME) with GC/FID was studied as a possible alternative to liquid-liquid extraction for the analysis of chlorinated solvents (PCE and TCE) and these by-products (cis-DCE, VC, and Ethylene). Experimental parameters affecting the SPME process (such as kind of fibers, adsorption time, desorption time, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. Experimental parameters such as CAR/PDMS, adsorption time of 20 min, desorption time of 5 min at $250^{\circ}C$, headspace volume of 50mL, sodium chloride (NaCl) concentration of 25% combined with magnetic stirring were selected in optimal experimental conditions for analysis of chlorinated solvents and these by-products. The general affinity of analytes to CAR/PDMS fiber was high in the order PCE>TCE>cis-DCE>VC>Ethylene. The linearity of $R^2$ for chlorinated solvents and these by-products was from 0.912 to 0.999 when analyte concentrations range from $10{\mu}g/L$ to $500{\mu}g/L$, respectively. The relative standard deviation (% RSD) were from 2.1% to 3.6% for concentration of $500{\mu}g/L$ (n=5), respectively. Finally, the limited of detection (LOD) observed in our study for chlorinated solvents and these by-products were from $0.5{\mu}g/L$ to $10{\mu}g/L$, respectively.

• Korean Journal of Environmental Agriculture
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• v.37 no.2
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• pp.117-124
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• 2018

BACKGROUND: Oxycarboxin(5,6-dihydro-2-methyl-N-phenyl-1,4-oxathiin-3-carboxamide-4,4-dioxide) as oxanthiin is a systemic fungicide commonly used for control of various pathogens in agronomic and horticultural crops. In an effort to develop an analytical method to trace the fungicide, a method using HPLC equipped with UVD/MS was studied. METHODS AND RESULTS: Oxycarboxin was extracted with acetone from hulled rice, soybean, Kimchi cabbage, green pepper, and apple samples. The extract was diluted with saline water, followed by liquid-liquid extraction with methylene chloride. Florisil column chromatography was employed for the purification of the extracts. Oxycarboxin was determined on a Zorbax SB-AQ $C_{18}$ column by HPLC with UVD. Accuracy of the proposed method was validated by the recovery tests from crop samples fortified with oxycarboxin at 3 levels per crop. CONCLUSION: Mean recoveries ranged from 78.3% to 96.1% in five representative agricultural commodities. The coefficients of variation were less than 10%, and limit of quantitation of oxycarboxin was 0.04 mg/kg. A confirmatory technique using LC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. The method was reproducible and sensitive to determine the residue of oxycarboxin in agricultural commodities.

• Journal of the Korean Society of Food Science and Nutrition
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• v.31 no.1
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• pp.21-25
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• 2002

The contribution of lipid to thermal flayer generation from glucose-protein reaction was accomplished by isolating flavor compounds from casein-glucose (CG)and casein-glucose-coin oil (CGL) which were stored for 2 and 4 weeks at 6$0^{\circ}C$ and then reacted at 16$0^{\circ}C$ for 1hr. The volatiles from the reactant mixtures were isolated by a solvent extraction method with methylene chloride and analyzed by gas chromatography and gas chromatography-mass spectrometry. Pyrazine, methylpyrazine, 2,5-dimethylpyrazine, 2-dimethylpyrazine ,2-ethy-5- methyIpyrazine and 2-acetylpyrrole originated from interaction of thermal degradation of casein and lipid oxidation were identified in the CGL samples. It was also found that 3-methyl-1-butanol, 2-cyclopene-1,4-diode, heptanal, nonanal, and 2-heptanone were derived from lipid source. Two additional fatty acids, heptanoic acid and octanoic acid were also identified in the CGL samples. 5-Hydroxymethyl-2-furfural, the most abundant volatile, was responsible for the formation of sugar degradation product. The results suggested that the presence of lipid in the samples had more effect on the contribution of volatile formation of glucose-protein thermal reaction than the absence of lipid in the samples.