• Title/Summary/Keyword: 3-D Analytical Method

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Development of Analytical Methods of Spinosad in Agricultural Commodities by HPLC with UV Detector and Monitoring (HPLC-UVD를 이용한 농산물 중 스피노사드 분석법 개선 및 잔류실태 조사)

  • Kim, Hee-Yun;Choi, Sun-Hee;Chung, So-Young;Choi, Hee-Ju;Kim, Yong-Hoon;Cho, Min-Ja;Seo, Eun-Chae;Han, Kyoung-Jin;Choi, Jae-Chun;Park, Hee-Ok;Ha, Sang-Chul;Shin, Il-Shik;Eom, Ji-Yoon
    • Korean Journal of Food Science and Technology
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    • v.43 no.2
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    • pp.125-133
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    • 2011
  • The purpose of this study was to develop a methodology to detect spinosad which are difficult to analyze by multi-component simultaneous analysis of pesticide residues. We monitored spinosad due to the paucity of related information. The spinosad was determined using HPLC with UV detector at 250 nm. Correlation coefficient ($r^2$) for standard curve of spinosad A and D at standard concentration of 0.1-5.0 mg/kg were 0.999, respectively. Limit of quantitation (LOQ) of HPLC analysis was 0.005 mg/kg while limit of detection (LOD) was 0.001 mg/kg. Recovery experiments were conducted on five representative agricultural products to validate the analytical method. The recovery of proposed methods ranged from 74.9% to 104.0% and relative standard deviations were less than 10%. Spinosad residues were investigated in 16 commodities collected from 22 provinces. In this study, residues on all samples were not detected.

Improvement of an Simultaneous Determination for Clenbuterol and Ractopamine in Livestock Products using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 clenbuterol과 ractopamine의 동시 분석법 개선)

  • Cho, Yoon-Jae;Chae, Young-Sik;Kim, Jae-Young;Kim, Hyung-Soo;Kang, Ilhyun;Do, Jung-Ah;Oh, Jae-Ho;Kwon, Kisung;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.45 no.1
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    • pp.25-33
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    • 2013
  • Clenbuterol and ractopamine, which are ${\beta}$-agonists, have been misused as a growth promoting agent in meat producing animals. Clenbuterol was banned for veterinary drug in Korea because of its problems regarding safety. Due to their adverse effects, such as cardiovascular and central nervous diseases on human health proper control and monitoring should be conducted. The existing analytical method of clenbuterol and ractopamine in the Food code was improved through our present study. The bovine muscle samples were subjected to enzymatic hydrolysis, extracted with ethyl acetate and defatted by hexane-methanol partitioning. A molecular imprinted polymer (MIP) solid phase extraction cartridge was used for clean-up and LC-MS/MS was operated in positive multiple reaction monitoring (MRM). Clenbuterol-$d_9$ and ractopamine-$d_3$ were used as an internal standard. The renewed method was validated according to the CODEX guideline. The limits of quantitation for clenbuterol and ractopamine were 0.2 and 0.5 ${\mu}g/kg$, respectively. The mean recoveries ranged in 104.2-113.5% for clenbuterol and in 107.6-118.1% for ractopamine. The improved method was able to save both time and expenses.

A Novel Volumetric Method for Quantitation of Titanium Dioxide in Cosmetics (용량분석법을 이용한 화장품 중 티타늄옥사이드의 정량)

  • Kim, Young-So;Kim, Boo-Min;Park, Sang-Chul;Jeong, Hye-Jin;Chang, Ih-Seop
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.31 no.4 s.54
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    • pp.289-293
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    • 2005
  • Nowadays there are many sun protection cosmetics including organic or inorganic UV filter as an active ingredient. Chemically stable inorganic sunsEreen agents, usually metal oxides, we widely employed in high SPF products. Titanium dioxide is one of the most frequently used inorganic UV filters. It has been used as pigments for a long period of cosmetic history. With the development of micronization techniques, it becomes possible to incorporate titanium dioxide in sunscreen formulations without whitening effect and it becomes an important research topic. However, there are very few works related to quantitations of titanium dioxide in sunscreen products. In this research, we analyzed amounts of titanium dioxide in sunscreen cosmetics by adapting redof titration, reduction of Ti(IV) to Ti(III) and reoxidation to Ti(IV). After calcification of other organic ingredients of cosmetics, titanium dioxide is dissolved by hot sulfuric acid. The dissolved Ti(IV) is reduced to the Ti(III) by adding aluminum metals. The reduced Ti(III) is titrated against a standard oxidizing agent, Fe(III) (ammonium iron(III) sulfate), with potassium thiocyanate as an indicator In order to test accuracy and applicability of the proposed method, we analyzed the amounts of titanium dioxide in four types of sunscreen cosmetics, such as cream, make-up base, foundation and powder, after adding known amounts of titanium dioxide $(1{\sim}25w/w%)$. The percent recoveries of the titanium dioxide in four types of formulations were in the range between 96 and 105%. We also analyzed 7 commercial cosmetic products labeled titanium dioxide as an ingredient and compared the results with those of obtained from ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry), one of the most powerful atomic analysis techniques. The results showed that the titrated amounts were well coincided with the analyzed amounts of titanium dioxide by ICP-AES. Although instrumental analytical methods, ICP-MS (Inductively Coupled Plasma-Mass Spectrometry) and ICP-AES, are the best for the analysis of titanium, it is hard to adopt because of their high prices for small cosmetic companies. It was found that the volumetric method presented here gat e quantitative and reliable results with routine lab-wares and chemicals.

Determination of Color Value (L, a, b) in Green Tea Using Near-Infrared Reflectance Spectroscopy (근적외 분광분석법을 이용한 녹차의 색도 분석)

  • Lee, Min-Seuk;Choung, Myoung-Gun
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.53 no.spc
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    • pp.108-114
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    • 2008
  • Near infrared spectroscopy (NIRS) is a rapid and accurate analytical method for determining the composition of agricultural products and feeds. The applicability of near infrared reflectance spectroscopic method was tested to determine the color value (L, a, b) of green tea. A total of 162 green tea calibration samples and 82 validation samples were used for NIRS equation development and validation, respectively. In the developed NIRS equation for analysis of the color value (L, a, b), the most accurate equation for L value was obtained at 2, 8, 6, 1 (2nd derivative, 8 nm gap, 6 points smoothing, and 1pointsecond smoothing), and for a, and b value were obtained at 1, 4, 4, 1 (1st derivative, 4 nm gap, 4points smoothing, and 1 point second smoothing) math treatment condition with SNVD (Standard Normal Variate and Detrend) scatter correction method and entire spectrum ($400{\sim}2,500\;nm$) by using MPLS (Modified Partial Least Squares) regression. Validation results of these NIRS equations showed very low bias (L: 0.005%, a: 0.003%, b: -0.013%) and standard error of prediction (SEP, L: 0.361%, a: 0.141%, b: 0.306%) as well as high coefficient of determination ($R^2$, L: 0.905, a: 0.986, b: 0.931). Therefore, these NIRS equations can be applicable and reliable for determination of color value (L, a, b) of green tea, and NIRS method could be used as a mass screening technique for breeding programs and quality control in the green tea industry.

On the Evaluation of Physical Distribution Service in Ports (항만물류서비스의 평가에 관하여)

    • Journal of Korean Port Research
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    • v.10 no.2
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    • pp.17-29
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    • 1996
  • It is required to consider pricing and non-pricing factors and external economy in order to achieve the objects of physical distribution system in a port. Recently, among the three factors, much attention has been paid to non-pricing factor in the system. Although physical distribution service in a port(PDSP)has been frequently mentioned in documents and literature related to port and shipping studies, few study on it has not been systematically and scientifically made due to the following problems; $\circ$ there are not proper criteria to evaluate level and quality of PDSP and as a result it is difficult to set up a unified standard for doing so. $\circ$ algorithms to evaluate problems with complex and ambiguous attributes and multiple levels in PDSP are not available. This thesis aims to establish a paradigm to evaluate PDSP and to abvance existing decision making methods to deal with complex and ambiguous problems in PDSP. To tackle the first purpose, extensive and thorough literature survey was carried out on general physical distribution service, which is a corner stone to handle PDSp. In addition, through interviews and questionnaire to the expert, it have extracted 82 factors of physical distribution service in a port. They have been classified into 6 groups by KJ method and each group defined by the expert's advice as follows; a. Potentiality b. Exactness c. safety d. Speediness e. Convenience f. Linkage Prior to the service evaluation, many kinds of its attributes must be identified on the basis of rational decision owing to complexity and ambiguity inherent in PDSP. An analytical hierarchy process (AHP) is a method to evaluate them but it is not applicable to PDSP that have property of non-additivity and overlapped attributes. Therefore, probablility measure can not be used to evaluate PDSP but fuzzy measure is required. Hierarchical fuzzy integral method, which is merged AHP with fuzzy measure, is also not effective method to evaluate attributes because it has vary complicated way to calculate fuzzy measure identification coefficient of attributes. A new evaluation algorithm has been introduced to solve problems with multi-attribute and multi-level hierarchy, which is called hierarchy fuzzy process(HFP).Analysis on ambiguous aspects of PDSP under study which is not easy to be defined is prerequisite to evaluate it. HFP is different from algorithm existed in that it clarified the relationship between fuzzy measure and probability measure adopted in AHP and that it directly calculates the family of fuzzy measure from overlapping coefficient and probability measure to treat and evaluate ambiguous and complex aspects of PDSP. A new evaluation algorithm HFP was applied to evaluate level of physical distribution service in the biggest twenty container port in the world. The ranks of the ports are as follows; 1. Rotterdam Port, 2. Hamburg Port, 3. Singapore Port, 4. Seattle Port, 5. Yokohama Port, 6. Long beach Port, 7. Oakland Port, 8. Tokyo Port, 9. Hongkong Port, 10. Kobe Port, 11. Los Angeles Port, 12. New york Port, 13. Antwerp Port, 14. Felixstowe Port, 15. Bremerhaven Port, 16. Le'Havre Port, 17. Kaoshung Port, 18. Killung Port, 19. Bangkok Port, 20. Pusan Port

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Modeling of Elastodynamic Problems in Finite Solid Media (유한 고체내 탄성동역학 문제의 모델링)

  • Cho, Youn-Ho
    • Journal of the Korean Society for Nondestructive Testing
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    • v.20 no.2
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    • pp.138-149
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    • 2000
  • Various modeling techniques for ultrasonic wave propagation and scattering problems in finite solid media are presented. Elastodynamic boundary value problems in inhomogeneous multi-layered plate-like structures are set up for modal analysis of guided wave propagation and numerically solved to obtain dispersion curves which show propagation characteristics of guided waves. As a powerful modeling tool to overcome such numerical difficulties in wave scattering problems as the geometrical complexity and mode conversion, the Boundary Element Method(BEM) is introduced and is combined with the normal mode expansion technique to develop the hybrid BEM, an efficient technique for modeling multi mode conversion of guided wave scattering problems. Time dependent wave forms are obtained through the inverse Fourier transformation of the numerical solutions in the frequency domain. 3D BEM program development is underway to model more practical ultrasonic wave signals. Some encouraging numerical results have recently been obtained in comparison with the analytical solutions for wave propagation in a bar subjected to time harmonic longitudinal excitation. It is expected that the presented modeling techniques for elastic wave propagation and scattering can be applied to establish quantitative nondestructive evaluation techniques in various ways.

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Avoidance of Internal Resonances in Hemispherical Resonator Assemblies from Fused Quartz Connected by Indium Solder

  • Sarapuloff, Sergii A.;Rhee, Huinam;Park, Sang-Jin
    • Proceedings of the Korean Society for Noise and Vibration Engineering Conference
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    • 2013.04a
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    • pp.835-841
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    • 2013
  • Modern solid-state gyroscopes (HRG) with hemispherical resonators from high-purity quartz glass and special surface superfinishing and ultrathin gold coating become the best instruments for precise-grade inertial reference units (IRU) targeting long-term space missions. Designing of these sensors could be a notable contribution into development of Korea as a space nation. In participial, 40mm diameter thin-shell resonator from high-purity fused quartz, fabricated as a single-piece with its supporting stem has been designed, machined, etched, tuned, tested, and delivered by STM Co. (ATS of Ukraine) several years ago; an extremely-high Q-factor (upto 10~20 millions) has been shown. Understanding of the best way how to match such a unique sensor with inner glass assembly of the gyro means how to use the high potential in a maximal extent; and this has become the urgent task. Inner quartz glass assembly has a very thin indium (In) layer soldered the resonator and its silica base (case), but effects of internal resonances between operational modal pair of the shell-cup and its side (parasitic) modes can notable degrade the potential of the sensor as a whole, instead of so low level of resonator's intrinsic losses. Unfortunately, there are special combinations of dimensions of the parts (so-called, "resonant sizes"), when intensive losses of energy occurs. The authors proposed to use the length of stem's fixture as an additional design parameter to avoid such cases. So-called, a cyclic scheme of finite element method (FEM) and ANSYS software were employed to estimate different combinations of gyro assembly parameters. This variant has no mismatches of numerical origin due to FEM's discrete mesh. The optimum length and dangerous "resonant lengths" have been found. The special attention has been paid to analyses of 3D effects in a cup-stem transient zone, including determination of a difference between the positions of geometrical Pole of the resonant hemisphere and of its "dynamical Pole", i.e., its real zone of oscillation node. Boundary effects between the shell (cup) and 3D short "beams" (inner and outer stems) have been ranged. The results of the numerical experiments have been compared with the classic model of a quasi-hemispherical shell band with inextensional midsurface, and the solution using Rayleigh's functions of the $1^{st}$ and $2^{nd}$ kinds. To guarantee the truth of the recommended sizes to a designer of the real device, the analytical and FEM results have been compared with experimental data for a party of real resonators. The consistency of the results obtained by different means has been shown with errors less than 5%. The results notably differ from the data published earlier by different researchers.

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Development of Simultaneous Analytical Method of Veterinary Antibiotics in Manure using Liquid Chromatography Coupled with Tandem Mass Spectrometry (LC-MS/MS를 이용한 퇴비 및 액비 중 항생제 동시 분석법 개발)

  • Chung, Hyung Suk;Lee, Young Jun;Lee, Han Sol;Rahman, Md. Musfiqur;Kabir, Md. Humayun;Park, Byung-Jun;Kim, Jang-Eok;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.36 no.3
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    • pp.201-210
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    • 2017
  • BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.

Study on the production of porous CuO/MnO2 using the mix proportioning method and their properties (반응몰비에 따른 다공성 CuO/MnO2의 제조 및 특성 연구)

  • Kim, W.G.;Woo, D.S.;Cho, N.J.;Kim, Y.O.;Lee, H.S.
    • Analytical Science and Technology
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    • v.28 no.3
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    • pp.182-186
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    • 2015
  • In this study, the porous CuO/MnO2 catalyst was prepared through the co-precipitation process from an aqueous solution of potassium permanganate (KMnO4), manganese(II) acetate (Mn(CH3COO)2·4H2O) and copper(II) acetate (Cu(CH3COO)2·H2O). The phase change in MnO2 was analyzed according to the reaction molar ratio of KMnO4 to Mn(CH3COO)2. The reaction mole ratio of KMnO4 to Mn(CH3COO)2·4H2O was varied at 0.3:1, 0.6:1, and 1:1. The aqueous solution of Cu(CH3COO)2 was injected into a mixed solution of KMnO4 and Mn(CH3COO)2 to 10~75 wt% relative to MnO2. The Cu ion co-precipitates as CuO with MnO2 in a highly dispersed state on MnO2. The physicochemical property of the prepared CuO/MnO2 was analyzed by using the TGA, DSC, XRD, SEM, and BET. The different phase types of MnO2 were prepared according to the reaction mole ratio of KMnO4 to Mn(CH3COO)2·4H2O. The results confirmed that the porous CuO/MnO2 catalyst with γ-phase MnO2 was produced in the reaction mole ratio of KMnO4 to Mn(CH3COO)2 as 0.6:1 at room temperature.

Priority Analysis of Cause Factors of Safety Valve Failure Mode Using Analytical Hierarchy Process (AHP를 활용한 안전밸브(PSV) 고장모드의 Cause Factors 우선순위 분석)

  • Kim, Myung Chul;Lee, Mi Jeong;Lee, Dong Geon;Baek, Jong-Bae
    • Korean Chemical Engineering Research
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    • v.60 no.3
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    • pp.347-355
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    • 2022
  • The safety valve (PSV) is a safety device that automatically releases a spring when the pressure generated by various causes reaches the set pressure, and is restored to a normal state when the pressure falls below a certain level. Periodic inspection and monitoring of safety valves are essential so that they can operate normally in abnormal conditions such as pressure rise. However, as the current safety inspection is performed only at a set period, it is difficult to ensure the safety of normal operation. Therefore, evaluation items were developed by finding failure modes and causative factors of safety valves required for safety management. In addition, it is intended to provide decision-making information for securing safety by deriving the priority of items. To this end, a Delphi survey was conducted three times to derive evaluation factors that were judged to be important in relation to the Failure Mode Cause Factor (FMCFs) of the safety valve (PSV) targeting 15 experts. As a result, 6 failure modes of the safety valve and 22 evaluation factors of its sub-factors were selected. In order to analyze the priorities of the evaluation factors selected in this way, the hierarchical structure was schematized, and the hierarchical decision-making method (AHP) was applied to the priority calculation. As a result of the analysis, the failure mode priorities of FMCFs were 'Leakage' (0.226), 'Fail to open' (0.201), 'Fail to relieve req'd capacity' (0.152), 'Open above set pressure' (0.149), 'Spuriously' 'open' (0.146) and 'Stuck open' (0.127) were confirmed in the order. The lower priority of FMCFs is 'PSV component rupture' (0.109), 'Fail to PSV size calculation' (0.068), 'PSV Spring aging' (0.065), 'Erratic opening' (0.059), 'Damage caused by improper installation and handling' (0.058), 'Fail to spring' (0.053), etc. were checked in the order. It is expected that through efficient management of FMCFs that have been prioritized, it will be possible to identify vulnerabilities of safety valves and contribute to improving safety.