• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.18 no.2_spc
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• pp.227-235
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• 2020

In this study, we discussed the limitations of gross alpha measurements for the characterization of radioactive wastes produced in nuclear facilities through experimental tests and Monte Carlo N-particle transport simulations. The determination of gross alpha is essential for the disposal of radioactive waste produced in nuclear facilities in Korea. The measurements of gross alpha are easy to perform and yield rapid analytical results, but it cannot be used for quantitative analysis. The error of counting efficiency for gross alpha with various masses of the deposit on planchets using KCl and ²⁴¹Am was determined. The relative deviation of the counting efficiency in samples having the same mass was 20%. Uranium was extracted from the soil through acid leaching and extraction chromatography, and the concentration of U determined by inductively coupled plasma-mass spectrometry (ICP-MS) was compared with the results for gross alpha. The gross alpha was underestimated by 50% compared to the U concentration by ICP-MS. The counting efficiency depended on the energy from the alpha emitters, which differed by up to three times in determination of the counting efficiency depending on the kinds of alpha radionuclides of interest. Therefore, the gross alpha is not compatible with the sum of radioactivity for each alpha emitter and is suitable as a screening method.

• Journal of Korean Society of Environmental Engineers
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• v.31 no.9
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• pp.825-830
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• 2009

Pharmaceutical compounds enter the water environment through the diverse pathways. Because their concentration in the water environment was frequently detected in the level of ppt to ppb, the monitoring system should be optimized as much as possible for finding appropriate management policies and technical solutions. One Factor At a Time (OFAT) approach approximating the response with a single variable has been preferred for the optimization of LC-MS/MS operational conditions. However, it is common that variables in analytical instruments are interdependent. Therefore, the best condition could be found by using the statistical optimization method changing multiple variables at a time. In this research, response surface analysis (RSA) was applied to the LC-MS/MS analysis of emerging antibiotic compound, sulfamethoxazole, for the best sensitivity. In the screening test, fragmentation energy and collision voltage were selected as independent variables. They were changed simultaneously for the statistical optimization and a polynomial equation was fit to the data set. The correlation coefficient, $R^2$ valuerepresented 0.9947 and the error between the predicted and observed value showed only 3.41% at the random condition, fragmentation energy of 60 and collision voltage of 17 eV. Therefore, it was concluded that the model derived by RSA successfully predict the response. The optimal conditions identified by the model were fragmentation energy of 116.6 and collision voltage of 10.9 eV. This RSA can be extensively utilized for optimizing conditions of solid-phase extraction and liquid chromatography.

• Korean Journal of Environmental Agriculture
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• v.18 no.2
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• pp.135-139
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• 1999

A new effective and economic method was developed, removing interferences such as chlorophyll and lipid from leaves with small amounts of reagents and solvents in order to analyse PAHs(Polycyclic Aromatic Hydrocarbons). The extract from a soxhlet containing $4{\sim}5g$ of leaves and 100ml of dichlormethane and refluxed for 20 hrs was concentrated and eluted with 60ml of a hexane:dichloromethane (1:1) mixture through a column of 9mm wide inner diameter and 130mm long, packed from the bottom with 2.5g of $Al_2O_3$, 1.5g of $SiO_2$and 2g of anhydrous $Na_2SO_4$. The eluent was concentrated and loaded on a GPC column of 20mm wide inner diameter and 280mm long, packed with 12g of Bio-beads. The column was washed with 37ml of the hexane:dichloromethane(1:1) mixture. Another 43ml of the mixture was eluted as a PAH fraction and collected. This eluent was concentrated under gentle nitrogen to $50{\mu}l$ and analysed using GC-MS. The recoveries, obtained by comparing with the amounts of the internal standards of deuterated PAHs were $43.3{\sim}107.5%$(RSD $2.2{\sim}9.5%$).

• Korean Journal of Environmental Agriculture
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• v.13 no.2
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• pp.199-208
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• 1994

Analytical methods for the determination of the derivatives of the herbicide (${\pm}$)-2-(4-chloro-2-methylphenoxy)propionic acid (MCPP) by capillary column gas chromatography with mass spectrometer (GC-MS) and electron-capture detection (GC-ECD) were studied. A successful procedure was introduced for the ester preparation using $H_2SO_4$, as the catalyst and the alcohol 2,2,2-trichloroethanol (TCE) or 2,2,2-trifluoroethanol (TFE). The identificaiton and elucidation of MCPP by GC-MS spectrometry following the esterification with diazomethane, $BF_3$/methanol, $H_2SO_4$/methanol, TCE, TFE, or pentafluorobenzyl bromide (PFB) were carried out. A comparison of the response-sensitivities among those MCPP esters was made with GC-ECD. Although the methylation product of MCPP was confirmed by GC-MS, its low sensitivity to the ECD limited the detection of MCPP. TCE, TFE, and PFB derivatization methods resulted in a high rate of MCPP esterifications and very sensitive ECD molecular responses. Based on efficiency, convenience, worker safety, and least sample contamination, TFE esterificaiton was considered as the superior method for MCPP analysis to the other methods of derivatization. An accurate method is described for quantifying MCPP in soil leachates by GC-ECD at very low concentrations without the requirement of a complicated clean-up process. As a result, MCPP residues at concentrations of less than $0.1{\mu}g$ in 100ml soil leachate were detected.

• The Korean Journal of Pesticide Science
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• v.4 no.1
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• pp.1-10
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• 2000

The purpose of this study is to establish the assessment techniques of hazardous chemicals by the development of analytical method of biological samples. In this study, we have developed an extraction method of nine pesticides used for rice paddy that resulted in high recovery from the spiked human urine by the liquid-liquid extraction with diethyl ether at pH 7.0. Calibration curve obtained from each pesticide standard using by gas chromatography/mass spectrometry/selected ion monitoring has shown good linearity and detection limits were the range of $0.4{\sim}2.0$ ng/mL in urine. As a biological monitoring, urine samples of local farmers exposed directly to nine pesticides in the field were collected and analyzed by GC/MS. Of the tested pesticides, metabolites of phenthoate assumed were identified by GC/MS analysis. No parent compound was detected.

• The Korean Journal of Pesticide Science
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• v.18 no.4
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• pp.321-329
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• 2014

This experiment was conducted to establish an analytical method for residues of amisulbrom, as recently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops using HPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was diluted with 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice sample, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, amisulbrom was successfully separated from sample co-extractives and sensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of amisulbrom was 0.04 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue. The proposed method was sensitive, reproducible and easy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.

• Korean Journal of Food Science and Technology
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• v.43 no.5
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• pp.532-536
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• 2011

The internal standard method using ion chromatography combined with tandem mass spectrometry (IC-MS/MS) for quantifying perchlorate in different types of food was established. Because the presence of ions and other biomolecules in matrices usually interrupts accurate determination of perchlorate, it is necessary to develop efficient, reproducible method to determine perchlorate concentrations in food. In this study, the internal standard method was compared with the external standard method to determine perchlorate concentrations in standard samples. The obtained method detection limit (MDL) for perchlorate was 0.005 ${\mu}g/L$ for bottled water, 0.12 ${\mu}g/L$ for milk, 0.27 ${\mu}g/kg$ for rice, 0.16 ${\mu}g/kg$ for vegetables, and 0.07 ${\mu}g/kg$ for seaweed, respectively. The limit of quantitation (LOQ) was calculated by multiplying the MDL by 7. The recoveries of perchlorate from food samples spiked with perchlorate ranged from 98 to 105% and their percent relative standard deviation (%RSD) levels were <20%. This method was successfully applied for the quantitative determination of perchlorate in various kinds of food.

• Applied Biological Chemistry
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• v.20 no.2
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• pp.236-241
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• 1977

Analytical method of carbofuran (2,3-dihydro-2, 2-dimethyl-7-benzofuranyl methyl carbamate) residues and its persistence in rice seeds, rice seedlings, rice plants and soils were studied by gas-liquid chromatographic analysis using electron capture detector. 1. The effective column material for clean-up is Florisil (5% $H_2O$)+Alumina (4% $H_2O$)+absorbent mixture with rinsing the first 300l of eluants to remove impurities in the column materials. 2. The method of applying an gelatin encapsulated carbofuran to the root zone of rice plant is the longest persistence in its residues. 3. By seed treatment, no carbofuran residues were detected in rice seeds and seedlings. 4. The amounts of carbofuran residues in rice seedlings is in proportion to the soaking time of rice seedlings in carbofuran solution rather than the concentration of the chemical. 5. Applying carbofuran by root zone has the higher and the loger residual effect than broadcast. 6. Persistence of carbofuran in the high clay content soil is longer than in the low clay content soil. 7. No carbofuran residue was detected in rough rice at havesting time.

• Journal of Environmental Health Sciences
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• v.32 no.4 s.91
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• pp.359-372
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• 2006

In order to investigate the daily deposition characteristics of water-soluble inorganic components in airborne deposit on the Iksan, deposition samples were collected using a deposition gauge from October 16 to November 1, 2004. Deposition samples were collected using two different sampling gauges, a dry gauge and a wet gauge, respectively. To get wet the bottom of wet gauge during the sampling period, the volume of $30{\sim}50ml$ distilled ionized water was added in a wet gauge before the beginning of each deposition sampling. Deposition samples were collected twice a day and analyzed for inorganic water-soluble anions ($Cl^-,\;{NO_3}^-,\;{SO_4}^{2-}$) and cations (${NH_4}^+,\;Na^+,\;K^+,\;Mg^{2+},\;Ca^{2+}$) using ion chromatography. Qualify control and quality assurance of analytical data were checked by the data obtained from reinjection of standard solution, Dionex cross check standard solutions, and random several deposition samples, and measured data was estimated to be reliable. Considering the deposition sample volume, the sampling time, the surface area of sampling container, and the ion concentration measured, the daily deposition amounts for measured ions were calculated in $mg/m^2$. The total daily deposition amounts of all measured ions for dry and wet gauge were $7.5{\pm}2.8$ and $17.7{\pm}4.2mg/m^2$, respectively. A significant increase in deposition amount during rainfall days was observed for both wet gauge and dry gauge, having no difference of deposition amount between in wet gauge and in dry gauge. The mean deposition of all ions measured in this study were higher in wet gauge than in dry gauge because of the surface difference of the sampling container, especially for ${NH_4}^+\;and\;{SO_4}^{2-}$. The mean deposition amounts of ${NH_4}^+\;and\;{SO_4}^{2-}$ in wet gauge were found to be about 10 times and 3 times higher than those in dry gauge, while the rest of the chemical species were equal or a little higher in wet gauge than in dry gauge. Dominant species in dry gauge were ${NO_3}^-\;and\;Ca^{2+}$, accounting for 21% and 28% of the total ion deposition, whereas those in wet gauge were ${SO_4}^{2-}\;and\;{NH_4}^+$, accounting for 19% and 41% of the total ion deposition, respectively.

• Journal of Soil and Groundwater Environment
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• v.17 no.3
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• pp.1-9
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• 2012

According to the agreement on WTO/TBT, we are under the situation to adopt international standard (ISO standard) as a national standard if it exists. However, in case of environmental area, it is a domestic legal obligation to use Korean environmental standard method(KESM) for analyzing various contaminants. Therefore it is necessary to assess the comparability between KEM and ISO standard prior to apply ISO standard to soil conservation law in Korea. The main purpose of this study is to assess the comparability of both methods for analyzing heavy metals in soil. We looked over various aspects like pre-treatment, calibration curve range, detection wavelength, soil organic matter content and so on. Apparently, the procedure of both methods is almost same. However in details, both methods are different in stationary time before aqua-regia extraction using reflux system, calibration curve range for Cu, Pb, Ni and measuring wavelength for Pb. According to the results of comparison test, the results were significantly different when the different calibration range was used. In case that all the extracts independent of methods were reanalyzed with the same calibration range of each method, both methods showed statistically same results. Other conditions like different stationary time, measuring wavelength of AAS and soil organic matter content did not have any influence on the analytical result. Therefore, we suggest to extend the calibration curve range to 0~8 mg/L which is used in KS I ISO standard(Korean standard related with environment which is translation version of ISO standard without any technical change). In case of $Cr^{6+}$, the results showed no significant differences between two methods even though the pretreatment, instrumentation and other analysis conditions were different. In addition to UV/Visble spectrometry of KESM for soil contamination, we suggest to adopt ion chromatography of ISO 15192(US EPA method 7199) for analyzing $Cr^{6+}$ with the consideration of laboratory work efficiency.