• 한국방사성폐기물학회:학술대회논문집
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• 한국방사성폐기물학회 2004년도 학술논문집
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• pp.158-166
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• 2004

원자력 발전소에서 발생하는 방사성 폐기물인 이온교환수지, 제올라이트, 활성탄 및 슬러지에 포함된 핵종 분석을 위한 최적의 산분해 조건을 확립하였다. 방사성 폐기물의 분해에는 혼합산을 이용한 밀폐형 극초단파 산분해법을 사용하였으며, 제안한 방법에 따른 산분해 후의 용액은 맑고 색이 없는 투명한 상태임을 확인할 수 있었다. 또한, 산분해 과정을 거친 각각의 용액 시료는 ICP-AES와 AAS를 사용하여 분석하였고, 모의 방사성 폐기물에 첨가한 5종의 금속 원소들은 94% 이상의 높은 회수율을 보여주었다. 화학적 특성을 고려하여 제안된 산분해 조건은 핵종 분석을 위한 효과적인 전처리 방법으로써, 향후 원전의 유형별 방사성 폐기물에 대해 보편적으로 적용될 수 있을 것으로 판단된다.

• 방사성폐기물학회지
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• 제2권4호
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• pp.231-238
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• 2004

원자력 발전소에서 발생하는 고체 방사성 폐기물인 이온교환수지, 제올라이트, 활성탄 및 슬러지 에 포함된 성분 원소 분석을 위한 산분해 조건을 확립하였다. 방사성 폐기물의 분해 에는 흔합산을 이용한 밀폐형 극초단파 산분해법을 사용하였으며, 제안한 방법에 따른 산분해 후의 용액은 맑고 색이 없는 투명한 상태임을 확인할 수 있었다. 또한, 산분해 과정을 거친 각각의 용액 시료는 ICP-AES와 AAS를 사용하여 분석하였고, 모의 방사성 폐기물에 첨가한 5종의 금속 원소들은 $94{\%}$ 이상의 높은 회수율을 보여주었다. 화학적 특성을 고려하여 제안된 산분해 조건에 의해 용액화된 중${\cdot}$저준위 방사성 폐기물의 성분 원소 분석은 최적의 유리화 기술 개발을 위한 기초 자료로 유용하게 사용될 수 있을 것으로 판단된다.

• 공업화학
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• 제10권4호
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• pp.568-575
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• 1999

백금족 금소과 규산염을 포함하는 자동차 폐촉매 내의 백금족 금속과 주요 성분들을 ICP-AES로 동시에 분석하기 위한 두 종류의 전처리 방법이 비교되었다. HF, $HNO_3$, HCl, $HClO_4$, $H_2O_2$, 및 $H_3BO_3$ 등의 혼합산의 다양한 조합을 사용하여 열판(hot plate) 용해법과 밀폐용기를 사용하는 극초단파(microwave) 가압-가열법을 비교 검토하였다. 전통적인 열판 용해법보다 밀폐용기를 사용한 극초단파 가압-가열법이 화수율, 분석시간 및 사용하는 양 등의 측면에서 상대적으로 우수한 결과를 나타내었고, 0.25 g의 폐촉매 시료에 대하여 HF 2 mL, $HNO_3$2 mL, 그리고 HCl 6 mL를 사용하여 200 psi(13.79 bar), $180^{\circ}C$ 조건에서 1시간 동안 가열한 후, 5% (w/v) $H_3BO_3$ 16 mL를 사용하여 20 psi(1.38 bar), $100^{\circ}C$ 조건에서 10분간 가열한 다음, 왕수 10 mL로 열판에서 두 번 반복하여 처리하는 것이 백금족 금속의 회수율 측면에서 가장 좋은 결과를 가져왔고(XRF 분석 대비 85~110%), 이 방법은 2% 이내의 상대 표준 편차를 보임으로써, 자동차 폐촉매의 일상적인 분석기법으로서의 충분한 가능성을 보였다.

• 한국산업보건학회지
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• 제9권2호
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• pp.135-144
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• 1999

The purposes of this study were to survey types of pretreatment methods adopted by industrial hygiene laboratories in Korea for extracting heavy metals in welding fume samples and to compare performances of two pretreatment methods, the acid extraction and the microwave digestion, in extracting heavy metals contained in the real workplace samples from various welding jobs including arc, argon, and carbon dioxide. A total of 25 analytical chemists in the industrial hygiene laboratories participating the quality control program directed by the Korea Industrial Safety Corporation were interviewed by telephone. For the purpose of comparing performance of extracting heavy metals from real workplace samples, a total of 53 welders from 21 workplaces located in Anyang, Uiwang, and Kunpo areas were sampled from the period of March 22, 1999 to April 20, 1999. It was found that the most frequently adopted method for samples from the quality control program was the acid extraction method(40%) followed by the NIOSH 7300 method(36%). The NIOSH method, however, was the dominant method(36%) for samples from workplace followed by the acid extraction method(28%). In this study, two extraction methods, the acid extraction and the microwave digestion, were compared in terms of recovery rate, accuracy, and precision for both manganese and chromium. Both methods produced comparable results for the samples prepared for the quality control program. In contrast, concentrations of two heavy metals determined from real workplace samples pretreated with the microwave digestion method were statis tically significantly higher, manganese(166%) and chromium (200%), than those of utilizing the acid extraction method. These findings were consistent regardless of types of welding techniques used. The results of this study clearly show the importance of verifying the analytical performances of extraction methods for heavy metals not only for the samples from the quality control program but also from the real world samples collected from welding jobs.

• 분석과학
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• 제17권4호
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• pp.363-367
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• 2004

A simple and convenient digestion method was developed for the determination of heavy metal in polyurethane sample using only nitric acid in open system without heating. This digestion method had prevented loss of volatile elements of Hg and As and reduced the pretreatment time for the sample digestion. The detection limit is lowered over 10 times than that of microwave digestion method. Recoveries in polyurethane material were 108% for As, 96 ~ 99% for Hg, 102 ~ 103% for Cr, 98 ~ 102% for Pb, 86 ~ 90% for Cd, and 90 ~ 93% for Cu.

• 분석과학
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• 제33권4호
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• pp.186-196
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• 2020

A simple and rapid preconcentration method of actinide from seawater using Actinide resin was developed and tested with the seawater spiked with a known U and Th. The developed method of Actinide resin based on column chromatography is less time-consuming and requires less labor compared with a typical co-precipitation technique for preconcentration of actinides. U and Th, which are relatively weak-bonded with Actinide resin among actinides, were used to determine the optimum flow rate of seawater sample and evaluate the capacity of Actinide resin to concentrate actinides from seawater. A flow rate of 50 mL min^-1 was available with Actinide resin 2 mL (BV, bed volume). When 5 or 10 L of seawater containing U were loaded on Actinide resin (2 mL, BV) at 50 mL min^-1, the recovery of U was 93 % and 86 %, respectively. For extraction of actinides bound with Actinide resin, we compared three methods: solvent extraction, ashing-acid digestion, and ashing-microwave digestion. Ashing-microwave digestion method shows the best performance of which is the recovery of 100 % for U and 81 % for Th. For the preconcentration of actinides in 200 L of seawater, a typical coprecipitation method requires 2-3 days, but the developed method in this study is achieved the high recovery of actinides within 12 h.

• 대한화학회지
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• 제38권8호
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• pp.576-584
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• 1994

수중의 금속 산화물을 신속하고 간단하게 용해시킬 수 있는 연속흐름 마이크로파 용해장치를 개발하였다. 이로서 금속 산화물 입자를 용해시킴과 동시에 유도결합 플라즈마 분광기(ICP-AES)를 이용하여 ON-LINE으로 분석하는 완전 자동화 분석 장치의 개발이 가능토록 하였다. 연속흐름 마이크로파 용해장치는 개방형 튜브 장치와 억제형 튜브 장치로 구분하여 제작하고 최적화 시험을 수행하였다. 개방형 튜브 용해장치의 최적조건은 튜브길이가 30m, 마이크로파 출력 20%, 염산 농도 0.6N, 유속은 3.5ml/min였으며, 억제형 튜브 용해장치는 튜브 길이가 7.2m, 마이크로파 출력 30%, 염산 농도 0.6N, 유속은 3.1ml/min였다. 억제형 튜브 용해장치가 개방형 장치에 비하여 용해시간이 3배 정도 단축되었고 용해시킬 수 있는 시료의 농도 범위도 10배 정도 높았다. 제작된 용해장치의 정밀도는 베치식 용기 용해법과 거의 유사한 결과를 나타내어 Fe, Cu는 5% 정도의 상대 표준 편차값을 나타내었고, Zn,Co는 10%내외로 다소 높게 나타났다.

• Mass Spectrometry Letters
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• 제8권3호
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• pp.53-58
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• 2017

Glycated hemoglobin ($HbA_{1c}$) has been commonly used to screen and diagnose for patients with diabetes mellitus. Here the accelerated procedure of microwave-assisted sample treatment from acid hydrolysis to enzyme digestion followed by isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) was optimized and applied to measure $HbA_{1c}$ in an effort to speed up analysis time. First, two signature peptides of $HbA_{1c}$ and hemoglobin $A_0$ were certified with amino acid analysis by setting optimized acid hydrolysis conditions to $150^{\circ}C$, 1.5 h and $10{\mu}M$ sample concentration in 8 M hydrochloric acid. Consequently, the accurate certified peptides above were used as calibration standards to implement the proteolytic procedure with endoproteinase Glu-C at $37^{\circ}C$, 700 W for 6 h. Compared to the traditional method, the microwave heating not only shortened dramatically sample preparation time, but also afforded comparable recovery yields. The optimized protocol and analytical conditions in this study are suitable for a primary reference method of $HbA_{1c}$ quantification with full SI-traceability and other similar proteins in complex biological samples.

• Environmental Engineering Research
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• 제24권4호
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• pp.662-669
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• 2019

Anaerobic digestion is a popular sewage sludge (Ss) treatment method as it provides significant pollution control and energy recovery. However, the low C/N ratio and poor biodegradability of Ss necessitate pretreatment methods that improve solubilization under anaerobic conditions in addition to anaerobic co-digestion with other substrates to improve the process efficiency. In this study, three pretreatment methods, namely microwave irradiation, ultrasonication, and heat treatment, were investigated, and the corresponding improvement in methane production was assessed. Additionally, the simplex centroid design method was utilized to determine the optimum mixture ratio of food waste (Fw), livestock manure (Lm), and Ss for maximum methane yield. Microwave irradiation at 700 W for 6 min yielded the highest biodegradability (62.0%), solubilization efficiency (59.7%), and methane production (329 mL/g VS). The optimum mixture ratio following pretreatment was 61.3% pretreated Ss, 28.6% Fw, and 10.1% Lm. The optimum mixture ratio without pretreatment was 33.6% un-pretreated Ss, 46.0% Fw, and 20.4% Lm. These results indicate that the choice of pretreatment method plays an important role in efficient anaerobic digestion and can be applied in operational plants to enhance methane production. Co-digestion of Ss with Fw and Lm was also beneficial.

• 환경위생공학
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• 제16권1호
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• pp.91-101
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• 2001

In order to propose a optimum method increasing accuracy and reproducibility in analysis of urine lead levels, we compared matrix modifier addition method and microwave digestion method. The results were as follows ; 1. Where the concentration of $Pd(NO_3)_2$(matrix modifier) was $50mg/{\ell}$, and ashing temperature was $900^{\circ}C$, the results were optimum. In case of matrix modifier addition method, the average coefficient of variation (CV) of normal man was 24.1%, and lead worker was 7.9%. The average urine lead levels of standard were $10.42\mu{g}/{\ell}$ and $19.89\mu{g}/{\ell}$ , the accuracies compared to reference values were 97.0% and 92.6%, respectively. 2. Microwave digestion temperature($160~180^{\circ}C$), time(15~25min) and the ratio of urine/ashing acid(1:1~4:1) did not significantly affect lead absorbance and background absorbance. Therefore we set up a optimum analytical conditions as follows: temperature, $160^{\circ}C$; time, 15min; the ratio of urine/ashing acid, 4:1. after samples were digested by the above analytical conditions, lead absorbance and background absorbance was measured at $450^{\circ}C$ as ashing temperature. The average coefficient of variation (CV) of normal man was 12.4%, and lead worker was 6.2%. The average urine lead levels of standard urine were $10.66\mu{g}/{\ell}$ and $23.31\mu{g}/{\ell}$, the accuracies compared to reference values were 99.3% and 103.9%, respectively. From the results, we suggest that microwave digestion method is a more favorable method than matrix modifier addition method because of easiness to reduce organic matter, possibility to analysis at low temperature and accuracy.