• Title/Summary/Keyword: Instrumental Analysis Method

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Development of Analytical Method for Cymoxanil in Agricultural Commodities using HPLC/UVD (HPLC/UVD를 이용한 농산물 중 cymoxanil의 개별 분석법 확립)

  • Kim, Ji-Yoon;Kim, Hea-Na;Kim, Ja-Young;Kim, Jong Geol;Ham, Hun-Ju;Lee, Young-Deuk;Hur, Jang-Hyun
    • The Korean Journal of Pesticide Science
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    • v.18 no.2
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    • pp.69-78
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    • 2014
  • In the present study, we developed an official individual analytical method for cymoxanil using HPLC/UVD, respectively in different representative crops. Individual analytical methods for these pesticides are not included in the Korea food code. The samples were extracted with acetonitrile, concentrated and partitioned with dichloromethane and saturated sodium chloride solution. For cymoxanil, extracts were concentrated and clean-up through silica gel column chromatography with dicloromethane/acetone (60/40 v/v) and subjected to instrumental analysis. The limit of detection (LOD) for cymoxanil were 0.1 ng and 1 ng respectively and limit of quantitation (LOQ) were 0.02 mg/kg. Recoveries for cymoxail ranged from 79.6~107.6% respectively, at fortification level of 0.02 mg/kg (LOQ), 0.2 mg/kg (10 LOQ) and 1.0 mg/kg (50 LOQ) and the coefficient of variation (CV) was less than 10%, regardless of sample types. These results were further confirmed with LC/MS. The proposed simultaneous analysis method is reproducible and sensitive enough to determine the residues of cymoxanil in the agricultural commodities. According to the validation data and performance characteristics and high sample throughput, the proposed method is suitable for routine application.

Comparison of Liquid Chromatography-Mass/Mass Spectrometry (MS) and Gas Chromatography-MS for Quantitative Analysis of Indole-3-acetic acid and Indole-3-butyric acid from the Concentrated Liquid Fertilizer (Liquid Chromatography-Mass/Mass Spectrometry (MS)와 Gas Chromatography-MS를 이용한 농축 액상 비료제품 중 Indole-3-acetic acid 및 Indole-3-butyric acid 정량분석능 비교)

  • Kim, Jin Hyo;Park, Jong Min;Choi, Geun-Hyoung;Park, Yun-Ki;Im, Geon-Jae;Kim, Doo-Ho;Kwon, Oh-Kyung
    • Journal of Applied Biological Chemistry
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    • v.56 no.1
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    • pp.53-57
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    • 2013
  • In here, we investigated the quantitative analysis method of indole-3-acetic acid (IAA) and indole-3-butyric acid (IBA) with liquid chromatography-mass/mass spectrometry (LC-MS/MS) or gas chromatography-MS. Two ways of clean-up process were investigated for LC-MS/MS instrumental analysis of IAA, but both a simple dilution and hydrophile-lipophile balance (HLB) solid phase extraction (SPE) were not met the optimal recovery rates for quantitative analysis. On the other hand, the clean-up method for GC-MS was finally optimized through HLB-SPE from 250-folds diluted sample and methylation with trimethylsilyl chloride in methanol for 4 h. The limit of detection for methyl ester of IAA and IBA were both 1.4 mg/L, and recovery rates showed 93-107% from the concentrated liquid fertilizer.

A review of analytical method for volatile fatty acids as designated offensive odorants in Korea (악취성 유기지방산 성분의 분석기술)

  • Ahn, Ji-Won;Kim, Yong-Hyun;Kim, Ki-Hyun;Song, Hee-Nam
    • 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.

Determination of individual sugars in different varieties of persian grape using Near Infrared spectroscopy

  • Kargosha, Kazem;Azad, Jila;Lary, Abas Motamed
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1527-1527
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    • 2001
  • Glucose, fructose and sucrose being the main sugars that can be found in natural fruit juice. Many instrumental methods, such as GC, LC, electrochemical or spectrometric methods provide information about both the total content of sugars and the specific concentration of each carbohydrate[1]. The simplicity of sample handling and measurement in the near IR(NIR) wavelength region, which allows the use of long pathlength, optical glass cells and optical fibers, makes NIR a good alternative for sugar determination [2]. In the present study, six varieties of persian grapes were harvested at intervals through august to october and analysed for sugars by NIR. The results were processed by principal component regression (PCR) and partial least squares (PLS) analysis. Sample juice was prepared by squeezing through gauze from crashed grape. This solution was treated by zinc ferrocyanide prior to analysis in order to eliminate colored compounds and all optically active nonsugar substances. For glucose and fructose the most characteristic wavelengths were 1456nm corresponding to the first harmonic O-H stretching and the second at 2062nm corresponding to O-H stretching and deformation; secondary characteristic combination bands were also seen at 2265 nm (O-H and C-C stretching) and at 2240 nm (C-H and C-C stretching). However these spectra were taken over a wavelength range from 1100-2500nm at room temperature of 25-$30^{\circ}C$. To test the accuracy of the described procedure, samples of six varieties of grape were analysed by the proposed NIR and a standard method[2]. Good agreement were found between these two sets of the results. To perform the recovery studies , samples of grape juices previously analysed by the proposed method, were spiked with known amounts of each individual sugars and then analysed again. Relative standard deviations varied from 1.4 to 1.8% for six independent measurements of individual and total sugar concentration. In the analysis of real and synthetic samples, precise and accurate results were obtained , providing accuracy errors lower than 1.9% in all cases. Average recoveries of ${97}{\pm}{4%}$ for total sugar and between ${95}{\pm}{5%}$ and ${99}{\pm}{2%}$ for sing1e sugars demonstrate the applicability of the methodology developed to the direct analysis of grape Juice.

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A Study on the Analysis of the Error in Photometric Stereo Method Caused by the General-purpose Lighting Environment (測光立體視法에서 범용조명원에 기인한 오차 해석에 관한 연구)

  • Kim, Tae-Eun;Chang, Tae-Gyu;Choi, Jong-Soo
    • Journal of the Korean Institute of Telematics and Electronics B
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    • v.31B no.11
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    • pp.53-62
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    • 1994
  • This paper presents a new approach of analyzing errors resulting from nonideal general-purpose lighting environment when the Photometric Stereo Method (PSM) is applied to estimate the surface-orientation of a three-dimensional object. The approach introduces the explicit modeling of the lighting environment including a circular-disk type irradiance object plane and the direct simulation of the error distribution with the model. The light source is modeled as a point source that has a certain amount of beam angle, and the luminance distribution on the irradiance plane is modeled as a Gaussian function with different deviation values. A simulation algorithm is devised to estimate the light source orientation computing the average luminance intensities obtained from the irradiance object planes positioned in three different orientations. The effect of the nonideal lighting model is directly reflected in such simulation, because of the analogy between the PSM and the proposed algorithm. With an instrumental tool designed to provide arbitrary orientations of the object plane at the origin of the coordinate system, experiment can be performed in a systematic way for the error analysis and compensation. Simulations are performed to find out the error distribution by widely varying the light model and the orientation set of the object plane. The simulation results are compared with those of the experiment performed in the same way as the simulation. It is confirmed from the experiment that a fair amount of errors is due to the erroneous effect of the general-purpose lighting environment.

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Analysis Method of N-Nitrosamines in Human Urine by LC-MS/MS System (LC-MS/MS 시스템을 이용한 소변 중 N-니트로사민류 분석법 확립)

  • Park, Na-Youn;Jung, Woong;Kho, Younglim
    • Journal of the Korean Chemical Society
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    • v.61 no.2
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    • pp.51-56
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    • 2017
  • N-nitrosamines are the nitroso compounds which are produced by nitrosation reactions of the secondary amine and nitrite under acidic conditions. Approximately 300 species of N-nitrosamine have been tested for carcinogenicity in laboratory experiments, with 90% of them demonstrated carcinogenic effects different animal species, including higher primates. In 1978, IARC classified NDMA and NDEA as Group 2A, and NDPA, NDBA, NPIP, NPYR and NMOR as Group 2B. In this study, we established pretreatment and analytical method for N-nitrosamines (NDMA, NDEA, NMEA, NDPA, NDBA, NPIP, NPYR and NMOR) in human urine for biological monitoring of N-nitrosamines. The analytes were extracted using solid phase extraction (SPE), then quantitative analysis was performed by LC-(APCI)-MS/MS. The accuracies of the established method were between 85.8~108.7% and precisions were lower than 20%. The limit of detection (LOD) were between 0.0002 (NDBA) and 0.0793 (NDMA) ng/ml. The linearity obtained was satisfying for the 8 N-nitrosamines, with a coefficient of determination ($r^2$) higher than 0.999. The mean concentrations of N-nitrosamines in the urine were 2.645 mg/g creatinine for NDMA, 0.067 mg/g creatinine for NDEA, 0.009 mg/g creatinine for NMEA, 0.011 mg/g creatinine for NDBA, 0.271 mg/g creatinine for NPIP and 0.413 mg/g creatinine for NPYR. NDPA and NMOR were not detected. It can be used as a instrumental methodology for evaluation and risk assessment of human exposure to N-nitrosamines for the further research.

Asymmetric Catalytic Activity of Mesoporous Mordenite containing Polymeric Chiral Salen Complexes in the Mesopore System (폴리머 키랄 살렌을 함유한 메조세공 모더나이트의 비대칭 촉매 활성)

  • Guo, Xiao-Feng;Kim, Yong-Suk;Kawthekar, Rahul B.;Kim, Geon-Joong
    • Applied Chemistry for Engineering
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    • v.20 no.3
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    • pp.279-284
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    • 2009
  • The formation of mesoporous pores in the microporous mordenite crystals was performed by controlled silica extraction on alkaline treatment. Inner tunable mesopore size could be controlled by changing the concentration of alkaline solution. The pore structure of mordenite zeolite was studied by instrumental analysis after alkaline-treatment. To obtain the cage type mesopores, Ti-coating on the ourside mordenite crystals before alkaline treatment was investigated to be the most effective. Polymeric chiral salen Co (III) complexes were successfully encapsulated in mesoporous mordenite zeolite by "ship-in-a-bottle" method. The heterogeneous catalyst could be applied in asymmetric ring opening of epichlorohydrine by water. It showed very excellent enantioselectivity with a high yield in the catalysis.

Dynamic response of functionally gradient austenitic-ferritic steel composite panels under thermo-mechanical loadings

  • Isavand, S.;Bodaghi, M.;Shakeri, M.;Mohandesi, J. Aghazadeh
    • Steel and Composite Structures
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    • v.18 no.1
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    • pp.1-28
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    • 2015
  • In this paper, the dynamic response of functionally gradient steel (FGS) composite cylindrical panels in steady-state thermal environments subjected to impulsive loads is investigated for the first time. FGSs composed of graded ferritic and austenitic regions together with bainite and martensite intermediate layers are analyzed. Thermo-mechanical material properties of FGS composites are predicted according to the microhardness profile of FGS composites and approximated with appropriate functions. Based on the three-dimensional theory of thermo-elasticity, the governing equations of motionare derived in spatial and time domains. These equations are solved using the hybrid Fourier series expansion-Galerkin finite element method-Newmark approach for simply supported boundary conditions. The present solution is then applied to the thermo-elastic dynamic analysis of cylindrical panels with three different arrangements of material compositions of FGSs including ${\alpha}{\beta}{\gamma}M{\gamma}$, ${\alpha}{\beta}{\gamma}{\beta}{\alpha}$ and ${\gamma}{\beta}{\alpha}{\beta}{\gamma}$ composites. Benchmark results on the displacement and stress time-histories of FGS cylindrical panels in thermal environments under various pulse loads are presented and discussed in detail. Due to the absence of similar results in the specialized literature, this paper is likely to fill a gap in the state of the art of this problem, and provide pertinent results that are instrumental in the design of FGS structures under time-dependent mechanical loadings.

Drone Detection with Chirp-Pulse Radar Based on Target Fluctuation Models

  • Kim, Byung-Kwan;Park, Junhyeong;Park, Seong-Jin;Kim, Tae-Wan;Jung, Dae-Hwan;Kim, Do-Hoon;Kim, Taihyung;Park, Seong-Ook
    • ETRI Journal
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    • v.40 no.2
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    • pp.188-196
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    • 2018
  • This paper presents a pulse radar system to detect drones based on a target fluctuation model, specifically the Swerling target model. Because drones are small atypical objects and are mainly composed of non-conducting materials, their radar cross-section value is low and fluctuating. Therefore, determining the target fluctuation model and applying a proper integration method are important. The proposed system is herein experimentally verified and the results are discussed. A prototype design of the pulse radar system is based on radar equations. It adopts three different pulse modes and a coherent pulse integration to ensure a high signal-to-noise ratio. Outdoor measurements are performed with a prototype radar system to detect Doppler frequencies from both the drone frame and blades. The results indicate that the drone frame and blades are detected within an instrumental maximum range. Additionally, the results show that the drone's frame and blades are close to the Swerling 3 and 4 target models, respectively. By the analysis of the Swerling target models, proper integration methods for detecting drones are verified and can thus contribute to increasing in detectability.

Safe Decomposition of the Vehicle Waste Battery Module and Development of Separation Process of Cathode Active Material from Aluminum Thin Film (자동차용 폐 리튬 이차전지 모듈의 안정적 해체와 알루미늄 박막으로부터 양극활물질의 분리공정 개발)

  • Kim, Younjung;Oh, In-Gyung;Hong, Yong Pyo;Ryoo, Keon Sang
    • Journal of the Korean Chemical Society
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    • v.63 no.6
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    • pp.440-445
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    • 2019
  • It has developed a method that can recover efficiently the reproducible resources from the vehicle waste lithium second battery module. Module cell consists of copper thin film, aluminum thin film and diaphragm made with polymer between these thin films. Cell was disassembled completely without any damage in glove box and through several steps. Preferentially, cathode active material was separated from aluminum thin film at heat treatment of 400 ℃. The retrieved cathode active material was then obtained as high purity after calcining at 800 ℃ to remove residual carbon. Based on this study, it was found that rare metals such as Co, Ni, Mn and Li made up of cathode active material could recover above 80% from aluminum thin film.