• Title/Summary/Keyword: 전처리법

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Development of humic acid extraction method in soil and sediment using ultrasonic for 14C dating (초음파를 이용한 14C 연대측정 토양시료의 부식산 추출법 개발)

  • Park, Jiyoun;Hong, Wan;Park, Junghun
    • Analytical Science and Technology
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    • v.22 no.2
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    • pp.136-140
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    • 2009
  • To improve the carbon recovery yield of chemical pretreatment in soil and sediment for $^{14}C$ age dating using AMS (Accelerator Mass Spectrometry), we have developed ultrasonic method in chemical pretreatment to replace with stirring method which has been generally used in each step of humic acid extraction for soil and sediment samples. Extraction conditions such as ultrasonic power, temperature and reaction time have been optimized. Six times higher carbon recovery yield could be obtained from low carbon content samples using ultrasonic method. We also compared the dating results by AMS obtained using ultrasonic method with the ages of samples treated by the stirring method. It was found that this new method could be applied to the pretreatment process of low carbon content samples for AMS age dating without effects on the dated ages, and with highly improved carbon recovery yields.

Comparison of Pretreatment Methods for Determination of 55Fe and 63Ni Activity in Nuclear Wastes Sample (원자력 시설 해체 폐기물 내 55Fe 와 63Ni 방사능 분석을 위한 전처리 방법 비교 연구)

  • Lee, Hoon;Lim, Jong-Myoung;Ji, Young-Yong;Jung, Kun-Ho;Kang, Mun-Ja;Choi, Geun-Sik;Lee, Jin-Hong
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.13 no.2
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    • pp.113-122
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    • 2015
  • 55Fe and 63Ni are key factors in deciding the proper handling of the decommissioning of radioactive waste from nuclear facilities. For determining beta emitting radionuclides, the dismantled waste samples should be completely decomposed and separated from the sample matrix. This study reports the comparison results of the recovering efficiencies of Iron and Nickel with wet digestion methods that use various acids and alkali-fusion methods. Various matrices of NIST SRMs (1646a, 1944, 8704, 2709a, and 1633c), the recovering efficiencies of using alkali-fusion methods ranged from 95.3 to 98.3% for Iron, and from 86.6 to 88.1% for Nickel within about 2% of relative standard deviation. On the other hand, those using one of the three wet digestion methods ranged from 77.9 to 105.3% for Iron and from 40.1 to 78.5% for Nickel with over 10% of relative standard deviation. Therefore, one may draw the conclusion that the analytical results derived from Iron and Nickel using alkali-fusion methods are fairly reliable due to the recovering efficiencies observed.

Determination of Formaldehyde in Cosmetics Using a Convenient DNPH Derivatization Procedure Followed by HPLC Analysis (간편한 DNPH 유도체화 HPLC 분석법을 이용한 화장품 중 포름알데하이드 분석)

  • Choi, Jongkeun
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.42 no.1
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    • pp.65-73
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    • 2016
  • Korea Food and Drug Administration (KFDA) has officially announced 2,4-dinitrophenylhydrazine (DNPH) derivatization - high performance liquid chromatography (HPLC) methods for analysis of formaldehyde. This study was conducted to develop a convenient derivatization method for cosmetics by improving complex pre-treatment procedures included in KFDA method. To simplify pre-treatment procedures of KFDA method, reaction conditions including pH, time and temperature were optimized. This pre-treatment method does not require complicate pre-treatment steps of KFDA method such as pH adjustment of test solution with acetate buffer (pH 5.0), solvent-solvent partitioning with dichloromethane and concentrating procedure with vacuum evaporator. Formaldehyde-dinitrophenylhydrazone (formaldehyde-DNP) product produced by derivatization reaction was separated and quantified with a reversed-phase HPLC, which was slightly modified with KFDA method. The linearity test showed good results with 0.9999 of correlation coefficient ($r^2$) in the range of 2 ~ 40 ppm of standard solutions. In this method, limit of detection (LOD) and limit of quantitation (LOQ) values for formaldehyde were 0.2 ppm and 0.5 ppm, respectively. In addition, recovery test demonstrated that the method was also accurate and reproducible. Therefore, the proposed method can be applicable to rapid analysis of formaldehyde in cosmetics.

Solidification of Molten Salt Waste by Gel-Route Pre-treatment (겔화 전처리법을 이용한 폐용융염의 고형화)

  • Park Hwan Seo;Kim In Tae;Kim Hwan Young;Ryu Seung Kon;Kim Joon Hyung
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.3 no.1
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    • pp.57-65
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    • 2005
  • This study suggested a new method for the solidification of molten salt waste generated from the electro-metallurgical process in the spent fuel treatment. Using binary material system, sodium silicate and phosphoric acid, metal chlorides were converted into metal phosphate in the micro-reaction module formed by SiO$_{2} particles. The volatile element in the reaction module would little vaporized below 1100$^{circ}$C After the gel product was mixed with borosilicate glass powder and thermally treated at 1000$^{circ}$C, li exists as Li$_{3}$PO$_4$ separated from glass phase and, Cs and Sr would be incorporated into an amorphous phase from XRD analysis. In case of the addition of ZrCl$_{4}$ to the binary system, the gel products were transformed into NZP structure considered as an prospective ceramic waste form after heat-treatment above 700 $^{circ}$C. From these results, the gel-route pretreatment can be considered as an effective approach to the solidincation of molten salt waste by the confirmed process or waste form and this also would be an alternative method on the ANL method using zeolites in USA by the confirmation of its chemical durability as an future work.

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Method development for quantitative analysis of naturally occurring radioactive nuclides in building materials (실내 건축자재 중 천연방사성핵종의 정량분석법 연구)

  • Lim, Jong-Myoung;Lee, Hoon;Kim, Chang-Jong;Jang, Mee;Park, Ji-Young;Chung, Kun Ho
    • Analytical Science and Technology
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    • v.30 no.5
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    • pp.252-261
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    • 2017
  • Naturally occurring radioactive materials (NORMs) increase radiation exposure to the public as these materials are concentrated through artificial manufacturing processes by human activities. This study focuses on the development of a method for the quantitative analysis of $^{232}Th$, $^{235}U$, and $^{238}U$ in building materials. The accuracy and precision of inductively coupled plasma mass spectrometry (ICP-MS) for determination of digestion processes was evaluated for certified reference materials (CRMs) digested using various mixed acid (e.g., aqua regia, hydrofluoric acid, and perchloric acid) digestions and a $LiBO_2$ fusion method. The method validation results reveal that a $LiBO_2$ fusion and $Fe(OH)_3$ co-precipitation should be applied as the optimal sample digestion process for the quantitative analysis of radionuclides in building materials. The radioactivity of $^{232}Th$, $^{235}U$, and $^{238}U$ in a total of 51 building material (e.g., board, brick, cement, paint, tile, and wall paper) samples was quantitatively analyzed using an established process. Finally, the values of $^{238}U$ and $^{232}Th$ radioactivity were comprehensively compared with those from the indirect method using ${\gamma}$-spectrometry.

DEPENDENCE OF WEIGHTING PARAMETER IN PRECONDITIONING METHOD FOR SOLVING LOW MACH NUMBER FLOW (낮은 Mach수유동 해석을 위한 Preconditioning 가중계수의 의존성)

  • An, Y.J.;Shin, B.R.
    • Journal of computational fluids engineering
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    • v.15 no.2
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    • pp.55-61
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    • 2010
  • A dependence of weighting parameter in preconditioning method for solving low Mach number flow with incompressible flow nature is investigated. The present preconditioning method employs a finite-difference method applied Roe‘s flux difference splitting approximation with the MUSCL-TVD scheme and 4th-order Runge-Kutta method in curvilinear coordinates. From the computational results of benchmark flows through a 2-D backward-facing step duct it is confirmed that there exists a suitable value of the weighting parameter for accurate and stable computation. A useful method to determine the weighting parameter is introduced. With this method, high accuracy and stable computational results were obtained for the flow with low Mach number in the range of Mach number less than 0.3.

Pretreatment Method Development of PCDD/Fs in Sediment Using ASE and SPMDs (ASE와 SPMDs를 이용한 퇴적물중 PCDD/Fs의 전처리법 개발)

  • Chun, Man-Young
    • Environmental Analysis Health and Toxicology
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    • v.22 no.1 s.56
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    • pp.49-55
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    • 2007
  • Three kind of ASE (Accelerated Solvent Extraction) and SPMDs (Semi-Permeable Membrane Devices) combined methods (ASE-SPMDs, ASE-accelerated SPMDs and SPMDs without extraction) and general Soxhlet-GPC were compared each other for the analysis of PCDD/FS in sediment. The average recovery rate of three types ASE and SPMDs combined methods (108.1%) were higher than that of the Soxhlet-GPC (79.5%) for three samples in each method using surrogate internal standards. The average coefficient of variation (10%, $2.1{\sim}25.2%$) for each congener of PCDD/Fs shows the reasonable results. Total PCDD/Fs concentrations after SPMDs without extraction were quite low, but those after ASE-SPMDs and ASE-accelerated SPMDs methods were close to the Soxhlet-GPC. Thus, the ASE-SPMDs and ASE-accelerated SPMDs methods are considered as the excellent pre-treatments method because they need less solvent and time without quality degradation.

The trend of surface treatment and coating technology for metallic bipolar plates of PEMFC (PEMFC용 금속분리판의 고전도/내부식 표면처리 기술 개발 현황)

  • Han, Yeong-Hun;Jo, Chang-Wan;Bang, Min-Guk;Yun, Hyo-Seop;Lee, Min-Cheol;Jeong, Yeon-Su;Jeon, Yu-Taek
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2014.11a
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    • pp.32-33
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    • 2014
  • 수소자동차용 연료전지의 중요 핵심부품 중 하나인 금속분리판의 경우 표면 처리 및 코팅기법을 이용해 전기적 고전도 특성과 화학적 내부식 특성을 확보하는 것이 관건이다. 본 연구내용은 향후 상용화를 목적으로 지금까지 진행해 온 금속분리판을 위한 건식 진공 표면처리 및 코팅기술 개발 현황에 대한 것이다. 생산비용의 저가화와 대량생산 가능성을 고려하여 고속의 연속 전처리법 및 진공증착법을 기본 공정으로 선정하고, 고전도/내부식성 증착물질 선택에도 귀금속을 배제하는 등의 기본 전제와 연구 결과를 소개한다. 기 확보된 기술에 의한 접촉저항 및 내부식 특성은 미국 DOE의 2017년 목표치를 만족하는 결과를 보였다.

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Qualitative Analysis of Ignitable Liquid Residues in Extracts from Fire Debris Samples (유류화재증거물의 정성적 분석 기법 연구)

  • Han, Dong-Hun;Rhee, Sung-Ryong;Kim, Soo-Young
    • Fire Science and Engineering
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    • v.25 no.6
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    • pp.14-20
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    • 2011
  • It is very difficult for fire investigators to analyze the fire debris in fire scene to figure out the reason of fire. ASTM E 1618 method with Gas Chromatoghraphy-Mass Spectrometry was used to analyze the ignitable liquid residues in fire debris prepared in our laboratory. According to fire cases, sample handling procedure methods and fire debris store time, different total ion chromatograms were obtained. We wish the study will be helpful to fire investigators to figure out the reason of fire.

Evaluation of Chemical Pre-treatment for the Optimization of CO2 Fixatiom Using by Carbonation Reaction with Serpentine (이산화탄소 광물고정화 효율 증가를 위한 사문석의 화학적 전처리에 관한 연구)

  • Jang, Na Hyung;Shim, Hyun Min;Hua, Xu Li;Kim, Hyung Teak
    • Applied Chemistry for Engineering
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    • v.19 no.5
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    • pp.526-532
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    • 2008
  • The proposed $CO_2$ storage technology in the present study is a one-step sequestration process that stabilizes $CO_2$ in a reactor with Serpentine. The advantage of this technology is associated with its high stability of final product so that the entire system is recognized as permanent environment-friendly $CO_2$ removal method. Since the sequestration reaction mechanisms are generally understood that carbonation reaction proceeds with very slow rate, so that pretreatment method to increases reaction rate of $CO_2$ carbonation reaction should be developed. To increase the reactivity of Serpentine with $CO_2$, two different methods of pretreatment are carried out in the present investigation. One is heat-treatment, the other is chemical pretreatment. In this study, only chemical pretreatment is considered leaching method of magnesium from Serpentine using sulfuric acid at the various reaction temperatures, times, and acid concentrations. Experimental results illustrated that pretreatment by sulfuric acid increases surface area of serpentine from $11.1209m^2/g$ to $98.7903m^2/g$ and extracts magnesium compounds. Single variable experiment demonstrated the enhancements of magnesium extraction with increased reaction temperature and time. Amount of magnesium extraction is obtained by using the data of ICP-AES as maximum extraction condition of magnesium is 2 M acid solution, $75^{\circ}C$ and 1hr. After performing chemical pretreatment, carbonation yield increased from 23.24% to 46.30% of weight.