• Title/Summary/Keyword: 한계검정

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Study on analysis of PAHs in consumer products (공산품 함유 PAHs 분석법에 관한 연구)

  • Song, Moon Hwan;Cho, Young Dal;Choe, Eun Kyung
    • Analytical Science and Technology
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    • v.27 no.4
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    • pp.201-212
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    • 2014
  • Polycyclic aromatic hydrocarbons (PAHs) that are carcinogenic and persistent will be restricted in consumer products from December 27, 2015 by EU REACH regulation. Pretreatment using Soxhlet extraction and quantitative analysis by GC-MS were studied to develop the method for analyzing 18 PAHs in consumer products as well as to detect the amounts and the kinds of PAHs in consumer products such as grips of a bag and a hammer, a cable and a plastic sandal. Linearity and precisions were evaluated by analyses of the standard PAH solutions ranging from 0.3125 mg/L to 5.00 mg of each of 18 PAHs. Linearity of resulting standard curves for all 18 PAHs were obtained with $R^2$ above 0.999. Precisions of the retention times and the peak areas were found to be 0.00%~0.05% and 1.16%~3.69% of relative standard deviations, respectively. The recoveries for spiked samples were all around 95%~105% after Soxhlet extration using three different solvents such as dichloromethane, hexane and toluene. The limits of quantitation for 18 PAHs in solutions and polymer samples by GC-MS were evaluated to be 0.327 mg/L (Benzo[ghi]perylene)~0.464 mg/L (Acenaphthylene) and 1.635 mg/kg (Benzo[ghi]perylene)~2.32 mg/kg (Acenaphthylene) based upon dilution factor of 5, respectively. Under the developed analytical method, only trace amounts of phenanthrene were detected in three samples while 15 kinds of PAHs including phenanthrene were detected in a grip of hammer with concentrations of maximum 83.4 mg/kg of Phenanthrene and minimum 8.5 mg/kg of Acenaphthylene. Further studies are needed to decrease the quantitation limit and to check the feasibility of decreasing Soxhlet time as well as to demonstrate cases that the clean up is required.

Optimal design of a nonparametric Shewhart-Lepage control chart (비모수적 Shewhart-Lepage 관리도의 최적 설계)

  • Lee, Sungmin;Lee, Jaeheon
    • Journal of the Korean Data and Information Science Society
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    • v.28 no.2
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    • pp.339-348
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    • 2017
  • One of the major issues of statistical process control for variables data is monitoring both the mean and the standard deviation. The traditional approach to monitor these parameters is to simultaneously use two seperate control charts. However there have been some works on developing a single chart using a single plotting statistic for joint monitoring, and it is claimed that they are simpler and may be more appealing than the traditonal one from a practical point of view. When using these control charts for variables data, estimating in-control parameters and checking the normality assumption are the very important step. Nonparametric Shewhart-Lepage chart, proposed by Mukherjee and Chakraborti (2012), is an attractive option, because this chart uses only a single control statistic, and does not require the in-control parameters and the underlying continuous distribution. In this paper, we introduce the Shewhart-Lepage chart, and propose the design procedure to find the optimal diagnosis limits when the location and the scale parameters change simultaneously. We also compare the efficiency of the proposed method with that of Mukherjee and Chakraborti (2012).

Analytical Method Validation of Quercetin in Changnyeong Onion Extract as a Functional Ingredient for Functional Health Food (건강기능식품 기능성원료로서 창녕양파추출액의 지표성분 Quercetin 분석법)

  • Jeon, Seon-Young;Jeong, Eun-Jeong;Baek, Jeong-Hwa;Cha, Yong-Jun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.40 no.4
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    • pp.565-569
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    • 2011
  • Validation of quercetin as a marker compound in the standardization of Changnyeong onion extract developed for functional health food was attempted by analytical method. The specificity was satisfied with retention time and photo diode array (PDA) spectrum by analysis of quercetin using HPLC and comparison with standard compound. It showed a high linearity in the calibration curve as coefficient of correlation ($R^2$) of 0.9986, and the limit of detection (LOD) and limit of quantitation (LOQ) were 0.2 mg/L and 0.5 mg/L, respectively. Recovery rate test with quercetin concentration of 0.05, 0.075 and 0.1 mg/mL was revealed in the high range of 82.36~95.26%, 82.70~98.24% and 87.91~95.11%, respectively. The intra-day and inter-day precision in quercetin for Changnyeong onion extracts was 0.10~3.28% and 0.96~5.79%, respectively. Therefore, application of quercetin was validated in analytical method as a marker compound in Changnyeong onion extracts.

Development and Validation of Analytical Method for Decursin in Aerial Parts of Angelica gigas Nakai Extract (참당귀 지상부 추출물의 지표성분 decursin의 분석법 개발 및 검증)

  • Kim, Hee-Yeon;Lee, Ki-Yeon;Kim, Tae-Hee;Park, A-Reum;Noh, Hee-Sun;Kim, Si-Chang;Ahn, Mun-Seob
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.52-57
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    • 2019
  • Method development and validation of decursin for the standardization of Angelica gigas Nakai as a functional ingredient and health food were accomplished. The quantitative determination method of decursin as a marker compound of aerial parts of Angelica gigas Nakai extract (AAGE) was optimized by HPLC analysis using a C18 column ($3{\times}150mm$, $3{\mu}m$) with 0.1% TFA in water and acetonitrile as the mobile phase at a flow rate of 0.5 mL/min and detection wavelength of 330 nm. The HPLC/PDA method was applied successfully to quantification of the marker compound in AAGE after validation of the method with linearity, accuracy, and precision. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.9994 and the limit of detection and limit of quantitation were $0.011{\mu}g/mL$ and $0.033{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 1.10% and 1.13%, respectively. Recovery of decursin at 0.5, 1, 5 and $10{\mu}g/mL$ were 92.38 ~ 104.11%. These results suggest that the developed HPLC method is very useful for the determination of marker compound in AAGE to develop a health functional material.

Effects of thickness and background on the masking ability of high-trasnlucent zirconias (고투명도 지르코니아의 두께 및 하부 배경에 따른 색조 차단 효과)

  • Kim, Young-Gon;Jung, Ji-Hye;Kong, Hyun-Jun;Kim, Yu-Lee
    • Journal of Dental Rehabilitation and Applied Science
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    • v.37 no.4
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    • pp.199-208
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    • 2021
  • Purpose: The purpose of this study was to compare and evaluate the masking ability of three types of high translucent zirconia according to the various thicknesses and backgrounds. Materials and Methods: Using three types of high-translucency zirconia (Ceramill zolid fx white, Ceramill zolid ht+ white, Ceramill zolid ht+ preshade A2), 10 cylindrical specimens were fabricated in 10mm diameter and each with four thicknesses (0.6 mm, 1.0 mm, 1.5 mm, 2.0 mm), respectively by CAD/CAM method. The background was 10 mm in diameter and 10 mm in thickness. A1, A2, A3 flowable resin backgrounds, blue-colored core resin background, and Ni-Cr alloy background were prepared, and black, white backgrounds provided by the spectrophotometer manufacturer (x-rite, Koblach, Austria) were used. zirconia specimens and the background specimen were stacked to measure L, a*, b* with Spectrophotometer (Color i5, x-rite, Koblach, Austria) and the ΔE value with the other background is calculated. The Calculated mean ΔE values were compared based on perceptibility threshold 1.0 and acceptability threshold 3.7. Nonparametric tests such as Kruskal-Wallis test were performed to verify statistical significance (α = 0.05). Results: There was a significant difference in the mean ΔE value according to the zirconia type, background and thickness change (P = 0.000). Conclusion: According to the results of this study, the pre-colored high-translucent zirconia can obtain the desired zirconia shade when it is restored on teeth, composite resins, and abutments except for the blue resin core.

Cadmium Extraction from Solutions by Solid-Phase and its Trace Determination (고상에서 용액으로 부터 카드뮴 추출과 잔유물 측정)

  • Ashrafi, F.;Attaran, A.M.;Kermani, N. Memar
    • Journal of the Korean Chemical Society
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    • v.52 no.2
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    • pp.133-139
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    • 2008
  • A new sensitive and selective spectrophotometric method for determination of trace amounts of cadmium using a polyvinyl chloride membrane containing bis-(2-ethylhexyl)phthalate as a solid phase extraction medium was investigated. Bis-(2-ethylhexyl)phthalate has used as a plasticizer. Cd(II) in an aqueous solution was trapped on the membrane in the form of colorful Cd (II)-I- - MG complexes (which MG is malachite green) and the cadmium complex was concentrated in the membrane. The absorbance of the green membrane was measured at 629 nm using a spectrophotometer, and then, the concentration of the cadmium was calculated using a calibration curve, which expressed the relationship between the Cd(II) concentration and the membrane absorbance after coloring for 25 min. The calibration curve was linear in the range of 10-760 μgL-1 cadmium in the test solution. The detection limit based on the 3Sbl criterion was 1.8199 μgL-1 and the relative standard deviations (RSD) were less than 4 % (n=5). The proposed method has been successfully applied to the determination of trace amounts of cadmium in the Tadjan River water sample (Sari-Iran), and the mean value of 28.7 μgL-1 was obtained.

Determination of Brassinolide by HPLC equipped with Fluoresence Detector in Rice(Oriza sativa L.) (HPLC 형광분석법을 통한 벼에서 Brassinolide의 검정)

  • Kim, In-Seon;Lee, Kang-Bong;Suh, Yong-Tack;Morgan, E.D.;Shim, Jae-Han
    • Applied Biological Chemistry
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    • v.39 no.1
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    • pp.84-88
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    • 1996
  • To determine brassinolide in rice(Oriza sativa L.) using HPLC equipped with fluoresence detector, a highly sensitive fluorescence reagent. 1-cyanoisoindole-2-m-phenylboronic acid, was synthesized from the reaction of o-phthaldehyde, m-phenylboronic acid and KCN, then was reacted with brassinolide. The formation ratio of brassinolide boronate exhibited 90% up at the ratio of $20\;:\;1({\mu}g/{\mu}g)$ of 1-cyanoisoindole-2-m-phenylboronic acid and brassinolide respectively. The detection limit of brassinolide boronate with fluoresence detector was 0.16 ng. Brassinolide was detected in heading stage(biomass : 10 g) and panicle formation stage(biomass : 100 g) of the rice(Oryza sativa L.) with quantity of $0.8\;{\mu}g\;and\;0.2\;{\mu}g$respectively. However, brassinolide was not detected in blooming and elongation stage.

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Developing a Parametric Method for Testing the Significance of Gene Sets in Microarray Data Analysis (마이크로어레이 자료분석에서 모수적 방법을 이용한 유전자군의 유의성 검정)

  • Lee, Sun-Ho;Lee, Seung-Kyu;Lee, Kwang-Hyun
    • Communications for Statistical Applications and Methods
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    • v.16 no.3
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    • pp.397-408
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    • 2009
  • The development of microarray technology makes possible to analyse many thousands of genes simultaneously. While it is important to test each gene whether it shows changes in expression associated with a phenotype, human diseases are thought to occur through the interactions of multiple genes within a same functional cafe-gory. Recent research interests aims to directly test the behavior of sets of functionally related genes, instead of focusing on single genes. Gene set enrichment analysis(GSEA), significance analysis of microarray to gene-set analysis(SAM-GS) and parametric analysis of gene set enrichment(PAGE) have been applied widely as a tool for gene-set analyses. We describe their problems and propose an alternative method using a parametric analysis by adopting normal score transformation of gene expression values. Performance of the newly derived method is compared with previous methods on three real microarray datasets.

Characterization of the Variability of Summer Extreme Precipitation According to the Local Features (지역특성에 따른 여름철 극한강수 변화특성 분석)

  • Kim, Gwangseob;Kim, Jong Pil
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.31 no.2B
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    • pp.129-146
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    • 2011
  • Characterization the regional impact of the variability of summer extreme precipitation and the rain days over several thresholds (i.e. 10, 20, 30, 40, 50, 60, 70 and 80 mm/day) in South Korea was performed using daily precipitation data of 59 weather stations operated by Korean Meteorological Administration (KMA). To consider the local features of weather stations, we characterized the variability according to the difference of elevations, latitudes, longitudes, river basins, inland or shore area, and the ratio of urbanization. The results showed that the summer extreme precipitation is sensible to the geographical effect which is similar to that of the annual precipitation. Rain days over thresholds have increased during 1973-2009 while the annual rain days have decreased. This indicate that the concentration of precipitation in summer season will be intensified in the future. Increase of summer precipitation amount and number of extreme rain days is higher in inland area, urbanized area, and Han-River basin than that of shore area, unurbanized area, and the other river basins respectively.

Studies on Electrochemical Behavior of Some Light Lanthanide Ions in Nonaqueous Solution, Flow Injection Determination and Photochemical Characterization of Heavy Metal Ion Chelate Eight Coordinated Complexes. (Part 2) (비수용액에서 가벼운 란탄족 이온의 전기화학적 거동, 흐름 주입법에 의한 정량 및 중금속 이온의 킬레이트형 8-배위 착물의 광화학적 특성 연구 (제 2 보) : 계면활성제 존재하에서 Chromeazurol S를 사용하여 몇 가지 란탄이온의 흐름주입법에 의한 정량)

  • Gang, Sam U;Jang, Ju Hwan;Kim, Il Gwang;Han, Hong Seok;Jo, Gwang Hui
    • Journal of the Korean Chemical Society
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    • v.38 no.1
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    • pp.50-54
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    • 1994
  • Spectrophotometric determination of some light lanthanide ions by flow injection method is described. Chromeazurol S forms water soluble complex with lanthanide ions in the presence of DTAB. The absorption maximum of the complexes are from 650 nm to 655 nm and the molar absorptivities were ca. $1.8{\times}10^5\;L mol^{-1}cm^{-1}$ on Tris buffer (pH 10.5). The calibration curves for Nd(III), Eu(III) and Sm(III) obtained by FIA are over the range of 0.1 to 0.6 ppm and the correlation coefficient were ca. 0.9993. The detection limits (S/N) were from 10 ppb for Nd(III) and Eu(III) to 20 ppb for Sm(III). The relative standard deviations was ${\pm}$.2% for 0.4 ppm sample. The samples throughput was ca. $50\;cm^{-1}$.

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