• Title/Summary/Keyword: 분석법

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High-Performance Liquid Chromatographic Determination of Phenothrin and Silafluofen Residues in Crops with Mass Spectrometric Confirmation (고성능 액체크로마토그래피와 질량분석법을 이용한 농산물 중 Phenothrin 및 Silafuofen의 정밀 잔류분석법 개발)

  • Lee, Young-Deuk;Oh, Jae-Ho;Jang, Sang-Won
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.389-400
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    • 2011
  • A high-performance liquid chromatographic (HPLC) method was developed to determine residues of phenothrin and silafluofen, known as synthetic pyrethroids, in agricultural commodities. Insecticide residues were extracted with acetone from representative samples of four crops which comprised rice, apple, pepper and cabbage. The extract was purified serially by liquid-liquid partition and Florisil column chromatography. For rice and pepper samples, acetonitrile/n-hexane partition was additionally adopted to remove nonpolar interferences. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate two phenothrin isomers and silafluofen from sample co-extractives. Intact parent compounds were sensitively detected by ultraviolet absorption at 226 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine phenothrin and silafluofen residues at 0.02 and 0.01 mg/kg, respectively. Mean recoveries of phenothrin and silafluofen from four crop samples fortified at three levels in triplicate were in the range of 82.4~109.8% and 83.7~109.8%, respectively. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types and spiking levels. A selected-ion monitoring (SIM) LC/mass spectrometry (MS) with electrospray ionization was provided to confirm the suspected residue of phenothrin, even though no sufficient ionization of silafluofen was obtained. Both phenothrin and silafluofen could be successfully confirmed by gas chromatography/MS SIM with electron impact at 70 eV. The proposed method is sensitive, repeatable and rapid enough to apply to officially routine inspection of agricultural products.

Headspace-GC-MS에 의한 토양 중 MTBE와 BTEX의 동시분석법에 관한 연구

  • Sin Ho-Sang;An Hye-Sin;Ryu Sang-Hui;Kim Tae-Seung
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2005.04a
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    • pp.31-35
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    • 2005
  • 본 연구는 토양에 휘발유 첨가제인 MTBE와 휘발유의 주성분인 BTEX를 headspace 법에 의해 동시 분석하는 방법이다. 인산으로 pH를 2로 조절한 후 NaCl로 포화시킨 용액 5ml를 헤드스페이스 바이알에 보존제로 넣은 후 토양시료 약 2g을 이 용액에 침지시켜 시료 채취한 다음 헤드스페이스 장치에 넣고 $80^{\circ}C$에서 40분 가온하여 상부 기상의 일정량을 취해 GC-MS (SIM)으로 분석하였다. 본 분석법에 의한 검출한계는 methyl-tert-butyl ether(MTBE)와 benzene, toluene, ethylbenzene, o,m,p-xylene(BTEX)이 각각 0.1, 0.1, 0.1, 0.2, 0.1, 0.2 ng/g이었고, 직선성은 0.995이상이었으며, 재현성도 10%내외의 정밀한 값을 보였다. 실제 시료를 분석한 결과, MTBE가 3-6,993 ng/g의 농도분포를 보였고 total BTEX는 1 ng/g으로 검출되었다. 이 방법은 빠르고 정밀 정확한 분석법으로 공정시험법으로 활용가치가 높다.

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A Study the Relationship between Tutoring Experience and the Achievement in Major Subjects using R (분석도구 R을 활용한 튜터링 학습 경험과 전공교과 성취도 간의 관계 연구)

  • Lee, Hyung-Mook
    • Proceedings of the Korean Society of Computer Information Conference
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    • 2017.07a
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    • pp.354-355
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    • 2017
  • 분석도구 R은 대용량 데이터의 고급 분석과 통계 계산을 위한 스크립트 언어로 빅데이터의 자료 분석에 다양하게 활용되고 있다. 대학의 학습 활동 측면에서의 튜터링 학습법은 학습 능력이 우수한 선배 또는 동료인 튜터와 학습 받고자하는 튜티가 1:1 또는 1:N의 관계를 이루고 학습 활동을 진행해 나가는 과정이다. 지난 연구에서는 튜터링 학습법에 참여한 학생들의 학업 성취도가 튜터링 학습법에 참여하지 않은 일반 학생들의 학업 성취도 보다 얼마나 높은지 정량적 값을 도출했었다. 본 연구에서는 튜터링 학습법에 참여했던 학생들의 튜터링 참여 과목 이외 다른 전공과목의 성적 성취도를 분석도구 R을 이용하여 분석해 봄으로써 튜터링 학습법 참여 경험이 튜터링을 실시하지 않은 다른 전공과목의 학업 성취도에 영향을 미치고 있는지 분석하였다.

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Analysis of Odorous Sulfur compounds in Air by Solid Phase Microextraction (대기중의 악취성 황화물분석을 위한 SPME 분석법)

  • 허귀석;김대원;윤영경;정용순
    • Proceedings of the Korea Air Pollution Research Association Conference
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    • 2000.11a
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    • pp.343-344
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    • 2000
  • 대기중의 황화합물 분석은 현행 우리나라 악취공정시험법에 고시되어 있으나 복잡한 농축장치를 필요로하고 조작법이 복잡하고 시간이 많이 소요된다. 특히 황화합물은 주요 악취물질로서 대기오염을 일으키고 있으며, 극미량에서(ppb) 악취를 발생시키는 악취물질임에도 불구하고 분석방법 및 정확도에 많은 문제점을 갖고 있다. 본 연구에서는 황화물 시료농축이 간단하며, 직접 주입, 분석할 수 있는 SPME(Solid-phase microextraction)을 이용하여 황화물을 신속하게 분석할 수 있는 분석법을 개발하고 저 하였다. 분석방법에 대한 분석재현성, 분석한계를 조사하였으며, 이 분석방법이 대기중 황화물분석 방법으로 활용될 수 있도록 분석법을 확립하고자 하였다. (중략)

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Simplified Procedure of Amylose Analysis by Rapid Flow Autoanalyzer RFA-300 (자동분석기 RFA-300 이용한 아밀로스 분석법)

  • Choi, Hae-Chune;Son, Yong-Hee;Cho, Soo-Yeon
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.38 no.1
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    • pp.66-71
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    • 1993
  • Several trials and errors were repeated to develop a simplified recipe of amylose analysis using a Rapid Flow Autoanalyzer(Alpkem, RFA-300). The amylose content of rice samples analyzed by the Rapid Flow Autoanalyzer were compared with those of Williams’ and Juliano’s assay. The results by the simplified recipe of RFA amylose analysis were highly correlated with those by Williams’ and Juliano’s method(r=0.95$^{**}$-0.97$^{**}$). The relative amylose content of defatted rice starch was higher than those of non-defatted rice flour, showing very close correlations between those analyzed by three method.

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Forensic Classification of Latent Fingerprints Applying Laser-induced Plasma Spectroscopy Combined with Chemometric Methods (케모메트릭 방법과 결합된 레이저 유도 플라즈마 분광법을 적용한 유류 지문의 법의학적 분류 연구)

  • Yang, Jun-Ho;Yoh, Jai-Ick
    • Korean Journal of Optics and Photonics
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    • v.31 no.3
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    • pp.125-133
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    • 2020
  • An innovative method for separating overlapping latent fingerprints, using laser-induced plasma spectroscopy (LIPS) combined with multivariate analysis, is reported in the current study. LIPS provides the capabilities of real-time analysis and high-speed scanning, as well as data regarding the chemical components of overlapping fingerprints. These spectra provide valuable chemical information for the forensic classification and reconstruction of overlapping latent fingerprints, by applying appropriate multivariate analysis. This study utilizes principal-component analysis (PCA) and partial-least-squares (PLS) techniques for the basis classification of four types of fingerprints from the LIPS spectra. The proposed method is successfully demonstrated through a classification example of four distinct latent fingerprints, using discrimination such as soft independent modeling of class analogy (SIMCA) and partial-least-squares discriminant analysis (PLS-DA). This demonstration develops an accuracy of more than 85% and is proven to be sufficiently robust. In addition, by laser-scanning analysis at a spatial interval of 125 ㎛, the overlapping fingerprints were separated as two-dimensional forms.

Missing Value Estimation and Sensor Fault Identification using Multivariate Statistical Analysis (다변량 통계 분석을 이용한 결측 데이터의 예측과 센서이상 확인)

  • Lee, Changkyu;Lee, In-Beum
    • Korean Chemical Engineering Research
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    • v.45 no.1
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    • pp.87-92
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    • 2007
  • Recently, developments of process monitoring system in order to detect and diagnose process abnormalities has got the spotlight in process systems engineering. Normal data obtained from processes provide available information of process characteristics to be used for modeling, monitoring, and control. Since modern chemical and environmental processes have high dimensionality, strong correlation, severe dynamics and nonlinearity, it is not easy to analyze a process through model-based approach. To overcome limitations of model-based approach, lots of system engineers and academic researchers have focused on statistical approach combined with multivariable analysis such as principal component analysis (PCA), partial least squares (PLS), and so on. Several multivariate analysis methods have been modified to apply it to a chemical process with specific characteristics such as dynamics, nonlinearity, and so on.This paper discusses about missing value estimation and sensor fault identification based on process variable reconstruction using dynamic PCA and canonical variate analysis.

Establishment of Analytical Method for Carpropamid in Agricultural Commodities using HPLC-DAD/MS (HPLC-DAD/MS를 이용한 농산물 중 살균제 Carpropamid의 정밀 잔류분석법 확립)

  • Lee, Hyeri;Choi, Hoon;Kim, Eunhye;Lee, Young Deuk;Kim, Jeong-Han
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.185-194
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    • 2015
  • This study was performed to establish a single residue analytical method for determining fungicide carpropamid residues in various agricultural commodities. Korean cabbage, apple, brown rice and green pepper were selected as representative crops. Samples were homogenized, extracted with acetone and purified by liquid-liquid partition and Florisil column chromatography. Carpropamid residues were analyzed at 220 nm with reversed phase HPLC equipped octylsilyl and octadecylsilyl column and confirmed using mass spectrometry. ILOQ (Instrumental limit of quantitation) of carpropamid was 2 ng and MLOQ (Method LOQ) was 0.02 mg/kg. Mean recoveries from four kinds of crop samples fortified at three levels (MLOQ, 10LOQ, 100LOQ) in triplicate were in the range of 84~112%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types.

Study on Internal Ballistic Performance Analysis for Single-chamber Dual-thrust Rocket Motors (단일연소관 이중추력 로켓모터의 내탄도성능 분석법 연구)

  • Kwon, Hyeokmin
    • Journal of the Korean Society of Propulsion Engineers
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    • v.24 no.4
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    • pp.1-11
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    • 2020
  • In this study, study on the internal ballistic analysis method for single-chamber dual-thrust rocket motors meeting a dual-thrust profile requirement by tailoring the grain burning area is presented. The analysis method, which can acquire variables required for the performance prediction, considering gradual change of burning rate correction factor and specific impulse in the transition phase, is proposed. Improvements compared to the analysis method in the previous study, which do not consider change in the transition phase, are verified through comparison between the newly proposed method and the method in the previous study. Internal ballistic variables are obtained for four different ground firing test conditions using the proposed method, and the performance prediction for each condition is conducted using these variables. These prediction results and the ground test data are in good agreement, so it is confirmed that the performance prediction of dual-thrust motors with same design geometries based on the proposed analysis method is available.