• Analytical Science and Technology
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• v.14 no.3
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• pp.274-285
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• 2001

In this study, the thermal desorption-cryofocusing-gas chromatographic(TD-C-GC) method was developed for determination of volatile organic compounds(VOCs) in ambient air and was applied at the municipal solid waste landfill sites. On-column cryofocusing was possible only with a 100 ml dewars bottle in TD-C-GC method with a stainless steel column. However, high operating pressure was needed for purging VOCs from the absorbent trap, which was able to solve by pressure programming with a electric pressure controller. By using both pressure and temperature programming brought increasing of resolution power in on-column cryofocusing method, but the high pressure caused a leakage of sample tube with repeated use. A loop cryofocusing devise was also developed and compared with the direct on-column method. In loop cryofocusing method, VOCs were concentrated on a 0.8mm i.d. loop which is located between the injector and separation column by using liquid nitrogen. In order to purge VOCs from the absorbent trap, only 0.4 psi of pressure was need in the loop cryofocusing method. Dual detection system was applied for the analysis of VOCs; a FID was used for hydrocarbons and a FPD was used for sulfur-containing compounds. Qualitative analysis was done by on-column cryofocusing GC-MS system. Among the large number of VOCs, toluene was the most abundant. Hydrogen sulfide, dimethyl sulfide, carbon disulfide, dimethyl disulfide and methyl propyl disulfide were detected at landfill site by FPD.

• Analytical Science and Technology
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• v.25 no.2
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• pp.91-101
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• 2012

A list of volatile fatty acids (VFA) including propionic acid, butyric acid, isovaleric acid, valeric acid, etc. is well known for offensive odorants. The analysis of odorant VFA is a highly delicate task due to high reactivity and unstable recovery rate. At present, analytical methods of VFA are recommended to include alkali impregnation filter method and alkali absorption method by the malodor prevention law of the Korea Ministry of Environment (KMOE). In this review, a survey has been made to explore various approaches available for the analysis of VFA to include both official methods of the KMOE and others. In light of the unreliability of those established analytical methods, it is highly desirable to develop some substituting methods for VFA. Among such options, one may consider such option as sorbent tube (ST) sampling and cryogenic trapping-thermal desorption technique. Moreover, procedures used for standard preparation, sampling steps, and instrumental detection stage are also evaluated. Application of container sampling (like Tedlar bag) is however not recommendable due to significant (sorptive) loss in sampling and in storage stage. In the detection stage, the use of GC/MS is recommendable to replace GC/FID due to the presence of diverse interfering substances. Thus, it is essential to properly establish the basic quality assurance (QA) for VFA analysis in air.

• Proceedings of the Korean Radioactive Waste Society Conference
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• 2004.06a
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• pp.418-418
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• 2004

풀, 토양 또는 지하수와 같은 환경시료 중에 포함된 미량 우라늄을 분석하기 위하여 핵분열 트랙 기입법을 이용하였다. 시료 전처리 방법으로 지하수 시료는 질산 산성으로 만든 후, 토양시료는 질산과 불산을 이용하여 용액화 하였으며, 풀 시료는 전기로를 이용하여 회화한 후, 질산과 불산을 이용하여 용액화 하였다. 이 환경시료 전처리용액들을 각각 0.1mL를 0.9mL Collodion 분산용액에 섞은 후, 우라늄 표준용액과 함께 플라스틱 판($6{\times}6\textrm{cm}^2$) 위에 10$\mu\textrm{\ell}$씩 점적, 건고 시키고 핵분열 트랙기입법을 이용하여 우라늄 농도를 분석하였다. 핵분열 트랙기입법을 위한 중성자조사는 한국원자력연구소 하나로 연구용원자로(열중성자 선속: $2.7{\times}10^{13}n/\textrm{cm}^2{\cdot}sec^{-1}$)에서 10분간 하였으며, 6.25M NaOH 용액($60^{\circ}C$)을 이용하여 10분간 화학 에칭 하였다. 고체트랙검출기 표면에 생성된 핵분열 트랙들은 광학현미경과 image analyzer system을 이용하여 관찰하고 계수하였다. 시료와 같이 점적한 우라늄 표준용액을 이용하여 우라늄 농도에 대한 단위면적당 트랙 수의 상관관계를 구하였으며, 이를 이용하여 시료 내 우라늄 농도를 결정하였다. 본 실험의 결과에 대한 검증을 위하여 동일 시료용액을 분리관을 이용한 전처리 과정을 거친 후 ICP-MS를 이용하여 분석하였다. 우라늄의 선택적 분리를 위하여 U-TEVA 추출크로마토그래피 분리관을 이용하였다. 본 연구의 핵분열 트랙기입법을 이용하여 환경시료를 분석하는 방법은 일반적인 분광법을 이용할 경우, 문제가 되는 방해 원소의 분리를 위한 전처리 과정이 불필요한 장점을 가지고 있으며, 1ng 정도의 미량 우라늄을 분석할 수 있었고, ICP-MS 결과와 20% 오차 이내에서 일치하였다.

• Analytical Science and Technology
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• v.15 no.1
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• pp.7-14
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• 2002

Laser ablation ion trap mass spectrometry (LAITMS) was developed for the analysis of metal and ceramic samples. For this study, XeCl excimer laser (308 nm) was used for ablating the samples and ITMS was used as a detector. Samples were introduced from outside of a ring electrode and this way of sample introduction was very effective for solid samples when laser ablation was employed. Helium gas was used as a buffer gas, and its effect on sensitivity and some parameters (buffer gas pressure, ion storage time, and cut-off RF voltage) were studied. The optimized conditions were $1{\times}10^{-4}$ Torr of buffer gas pressure, 100 ms of ion storage time and $1150V_{p-p}$ of cut-off RF voltage. From that results, copper (Cu) and molybdenum (Mo) metals were tested with LAITMS and the mass spectra of these pure metals were compared with the natural abundance of isotope ratio. We also examined ceramic samples ($Al_2O_3$, $ZrO_2$) and represented the result of elemental analysis.

• Analytical Science and Technology
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• v.13 no.5
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• pp.636-645
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• 2000

A method is described for the determination of organotins in water samples by GC/MS. Optimized derivatization methods for ethylation and hydrogenation of organotins were surveyed according to various reaction conditions such as time, pH and concentration of reagents. The organotins were extracted with n-hexane in presence of 0.1% tropolone and hydrogenated with sodium borohydride. Extraction recoveries of organotins with hydrogenation were in the range of 61-112%. After ethylation, organotins in water samples were extracted by liquid-liquid extraction (LLE) and solid-phase extraction (SPE). Using LLE, extraction recoveries were in the range of 74-113%. The recoveries ranged from 61-97% in the case of SPE with styrene-divinylbenzene copolymers. Method detection limits of hydrogenated and ethylated organotins ranged from 0.05 to 0.5 ng/ml and from 0.02 to 0.05 ng/ml, respectively.

• The Journal of the Acoustical Society of Korea
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• v.16 no.1
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• pp.39-46
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• 1997

In this paper, the PA(PhotoAcoustic) signals excited in metals by Xef, KrF excimer laser pulse were detected by a PZT transducer, and its transforming machanism and directivity patterns were analysed. The laser energy density in irradiation spot divides the PA trasnsorming machanism to be classified into thermoelastic and plasma regime, and the transforming machanisms in two regimes are different from each other. Based on theoretical model, it is predicted that shear wave is greater than longitudinal in the thermoelastic regime and longitudinal is greater than shear wave by reaction force in plasma regime. These predictions were verified through experiments by using of the XeF excimer pulsed laser of 480nm center-wavelength and the KrF excimer pulsed laser of 248nm. Also, for its directivity pattern, an arrival angle of the maximum longitudinal energy was around $60^{\circ}$ and maximum shear energy was around $30^{\circ}$ in the thermoelastic regime, and an arrival angle of maximum longitudinal energy was shown on nomal to the surface and maximum shear energy was represented in about $30^{\circ}$ in plasma regime.

• Journal of Radiation Protection and Research
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• v.36 no.3
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• pp.160-167
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• 2011

This study conducts cross-comparison through verification of treatment planning of using beam spoiler and bolus, according to the dose variation of different tumor bed and metastatic lymph node cancers, against ionization and optically stimulated luminescence detectors(OSLDs), in head and neck radiotherapy. Verification of treatment planning examined the feasibility of inserting detectors through simulated solid dry water slabs under identical irradiated conditions from treatment planning system to measure beam spoiler and 0.5, 1 cm bolus. In addition, two detectors were cross-compared for verification of treatment planning accuracy and reliability within ${\pm}$2%. The study found that, given a beam spoiler thickness of 0.5 cm and beam spoiler-to-skin distance of 10 cm subjected to optimal dose distribution given for metastatic lymph node cancers, the bolus low-level skin dose was less, and the tumor bed dose reduced slightly. Additionally, two detectors were cross-compared for accuracy within ${\pm}$1%. Accordingly, The use of beam spoiler was determined that reduces skin side effects and can deliver an optimal dose distribution for tumor, and to apply to future clinical studies should be performed.

• Food Science and Preservation
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• v.16 no.2
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• pp.246-252
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• 2009

Diacylglycerol(DAG) was produced by enzymatic esterification of glyceryl mono-oleate(GMO) and conjugated linoleic acid(CLA) in a stirred-batch type reactor. The reaction was catalyzed by lipozyme RMIM(an immobilized lipase from Rizomucor miehei). DAG was isolated by a short-path distillation process and decolorized. DAG oil was composed of 87.3% DAG, 11.4% triacylglycerol(TAG), and 1.5% monoacylglycerol(MAG)(all w/w). Major fatty acids in DAG oil were oleic acid(54%), CLA(31.1%), and linoleic acid(7%). DAG oil iodine,and acid values were 108.8, 2.57, and 1, respectively. The DAG oil solid fat index(SFI) and thermograms were obtained using differential scanning calorimetry.

• Journal of Navigation and Port Research
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• v.33 no.1
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• pp.57-63
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• 2009

In order to effectively isolate the marine wastes with an effluent standard, the pretreatment process is required to isolate solid materials from the liquid-solid mixed wastes. The more effective the pretreatment becomes, the more processing capacity of posttreatment will be improved and process facilities will be downsized. In this paper, we suggested the vibrating reverse-slant screen, investigated the optimal vibration frequency and vibrator installation angle for the separation of the liquid solid mixed wastes. Several experiments for separation efficiency were conducted under the condition of various vibration frequency($35{\sim}60Hz$, 5Hz interval) and vibrator angle($0^{\circ}$, $30^{\circ}$, $45^{\circ}$, $90^{\circ}$) considering the crack of screen. The screen inclination angle is set up the gradient as $3^{\circ}{\sim}5^{\circ}$ through the preliminary experiments. Also, we made two types of screen(respectively rectangle and square screen). The separation device has shown the optimum efficiency at vibrator angle $0^{\circ}$ and vibration frequency 60Hz, and has no relation with the shape of screen. And the proposed technology is verified by comparing with quantity of suspended solids before and after filtration.

• 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.