• Title/Summary/Keyword: methods:analytical

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Development of Multi-sample Loading Device for TEM Characterization of Hydroxyapatite Nanopowder

  • Lee, Jong-Moon;Kim, Jung-Kyun;Jeong, Jong-Man;Kim, Jin-Gyu;Lee, Eunji;Kim, Youn-Joong
    • Bulletin of the Korean Chemical Society
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    • v.34 no.3
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    • pp.788-792
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    • 2013
  • A shortcoming of using transmission electron microscopy (TEM) for structural analysis via electron diffraction is the relatively large error of the measurements as compared to X-ray diffraction. To reduce these errors, various internal standard methods from earlier studies have been widely used. We developed a new device to facilitate the application of internal standard methods in preparation of TEM grids used for nanopowder analysis. Through the application of a partial mask on the TEM grid, both the internal standards and the research materials can be loaded on the same grid. Through this process, we conducted a TEM analysis that compared synthetic hydroxyapatite (HAp) nanopowder to bone apatite from a bovine femur. We determined that the accuracy of the d-spacing measurements of the HAp and bone powders could be improved to better than 1% after statistical treatments of the experimental data. By applying a quarter mask, we loaded four different nanoparticles on a single TEM grid, with one section designated for the internal standard.

A Study on the Research of Analytical Method for 1,4-Dioxane in Water (1,4-Dioxane의 분석방법 연구)

  • Park, Sun-Ku;Kim, Tae-Ho;Rim, Yeon-taek;Myung, Nho-Il
    • Journal of Korean Society on Water Environment
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    • v.21 no.6
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    • pp.549-563
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    • 2005
  • The study was carried out to develop and standardize the analytical method of 1,4-dioxane in water. The National Institute of Environmental Research in Korea has monitored for 1,4-dioxane in water since 1998 and it has been detected in environmental water occasionally. But the environmental pollution and analytical method in water is not well known over the world. The trace analytical method at low-${\mu}/L$ level is prerequisite in order to evaluate the residue of 1,4-dioxane in water. Evaluation of the method was demonstrated by comparing and analyzing with liquid-liquid extraction, solid-phase extraction and purge & trap technique. As a result of experiment by standard solutions and raw samples, the precision and accuracy for three methods were obtained within error rate of about 10%. Therefore, three methods were standardized as official monitoring method in Korea. Also, a convenient and simple liquid-liquid extraction method for the analysis of 1,4-dioxane in water was developed by combined with gas chromatography/mass spectrometry and applied to the water samples in Korea

Analysis of the Behavior of Bolt Jointed Wood Connections by Applying Semi-Rigid Theory

  • Kim, Gwang-Chul;Lee, Jun-Jae
    • Journal of the Korean Wood Science and Technology
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    • v.28 no.4
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    • pp.72-82
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    • 2000
  • Attempts were made to analyze the behavior of single and multiple-bolted connections through theoretical methods such as European yield theory, empirical approaching method, and semi-rigid theory instead of many experimental methods that have been actually inefficient and non-economical. In the case of a single-bolted connection, if accurate characteristic values of a material could be guaranteed, it would be more convenient and economical to perform the behavior analysis using a model based on the semi-rigid theory, instead of the existing complex yield model, or the empirical formula which produces errors, giving different results from the actual ones. If the variables of equation determining the load and deformation could be appropriately controlled, the analytical method in conjunction with a semi-rigid theory could be effectively applied to obtain the desirably predicted value, considering that the appropriate solution could be derived through a simpler equation using a less difficult method compared to the existing yield model. It is concluded that analytical method with semi-rigid theory can be used in the behavior analysis of bolted connection because our developed method showed excellent analysis ability of behavior until number of bolt is two. Although our analytical method has the disadvantage that the number of bolt is limited to two, it is concluded that it has the advantage than numerical method which complicated and time-consuming.

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An Investigation on the Extraction and Quantitation of a Hexavalent Chromium in Acrylonitrile Butadiene Styrene Copolymer (ABS) and Printed Circuit Board (PCB) by Ion Chromatography Coupled with Inductively Coupled Plasma Atomic Emission Spectrometry

  • Nam, Sang-Ho;Kim, Yu-Na
    • Bulletin of the Korean Chemical Society
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    • v.33 no.6
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    • pp.1967-1971
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    • 2012
  • A hexavalent chromium (Cr (VI)) is one of the hazardous substances regulated by the RoHS. The determination of Cr (VI) in various polymers and printed circuit board (PCB) has been very important. In this study, the three different analytical methods were investigated for the determination of a hexavalent chromium in Acrylonitrile Butadiene Styrene copolymer (ABS) and PCB. The results by three analytical methods were obtained and compared. An analytical method by UV-Visible spectrometer has been generally used for the determination of Cr (VI) in a sample, but a hexavalent chromium should complex with diphenylcarbazide for the detection in the method. The complexation did make an adverse effect on the quantitative analysis of Cr (VI) in ABS. The analytical method using diphenylcarbazide was also not applicable to printed circuit board (PCB) because PCB contained lots of irons. The irons interfered with the analysis of hexavalent chromium because those also could complex with diphenylcarbazide. In this study, hexavalent chromiums in PCB have been separated by ion chromatography (IC), then directly and selectively detected by inductively coupled plasma atomic emission spectrometry (ICP-AES). The quantity of Cr (VI) in PCB was 0.1 mg/kg.

Optimized Design of Dioxin Analysis for Water Sample

  • Choi, Jaewon;Lee, Jaehee;Kim, Kyoungsim;Kim, Sunheong;Bae, Kyunghee
    • Journal of Korean Society on Water Environment
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    • v.21 no.3
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    • pp.219-229
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    • 2005
  • The analytical methods for dioxins in water sample from wastewater to tap water were reviewed. For extraction method, liquid-liquid extraction (LLE) has been widely used, however, this process needs too much time and man power. New approach including solid phase extraction (SPE) is now applicable to large volume of water sample with high extraction efficiency. Column clean up in classical analytical methods were very complex and time consuming procedures during decade. Modifications were tried to decrease solvent and reagents volume. Moreover, use of column connection method has been demonstrated in the environmental matrices. Instrumental configurations also have been improved, in which GC/MS/MS with large volume injection approach can analyze picogram levels. Absolute sensitivities of HRMS increased compared to old versions of double focusing sector type mass spectrometers. Based on these analytical evolutions during last 10 years, we tried to optimize the analytical method for dioxins in water sample from sample extraction to instrumental analysis.

Development of primary reference gas mixtures of 18 volatile organic compounds in hazardous air pollutants (5 nmol/mol level) and their analytical methods

  • Kang, Ji Hwan;Kim, Yong Doo;Lee, Jinhong;Lee, Sangil
    • Analytical Science and Technology
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    • v.34 no.5
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    • pp.202-211
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    • 2021
  • Volatile organic compounds (VOCs) in hazardous air pollutants (HAPs) have been regulated by the Air Pollution Control Act (1978) and their atmospheric concentrations have been monitored in 39 monitor sites in Korea. However, measurement standards of volatile organic compounds (VOCs) in HAPs at ambient levels have not been established in Korea. Primary reference gas mixtures (measurement standards) at ambient levels are required for accurately monitoring atmospheric VOCs in HAPs and managing their emissions. In this study, primary reference gas mixtures (PRMs) at 5 nmol/mol were developed in order to establish primary national standards of VOCs in HAPs at ambient levels. Primary reference gas mixtures (PRMs) were prepared in pressurized aluminum cylinders with special internal surface treatment using gravimetric method. Analytical methods using gas chromatography-flame ionization detector (GC-FID) coupled with a cryogenic preconcentrator were also developed to verify the consistency of gravimetrically prepared HAP VOCs PRMs. Three different columns installed in the GC-FID were evaluated and compared for the retention times and separation of eighteen target components in a chromatogram. Results show that the HAP VOCs PRMs at 5 nmol/mol were consistent within a relative expanded uncertainty (k=2) of less than 3 % except acrylonitrile (less than 6 %) and the 18 VOCs were stable for 1 year within their associated uncertainties.

Determination of trace bromate in various water samples by direct-injection ion chromatography and UV/Visible detection using post-column reaction with triiodide

  • Kim, Jungrae;Sul, Hyewon;Song, Jung-Min;Kim, Geon-Yoon;Kang, Chang-Hee
    • Analytical Science and Technology
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    • v.33 no.1
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    • pp.42-48
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    • 2020
  • Bromate is a disinfection by-product generated mainly from the oxidation of bromide during the ozonation and disinfection process in order to remove pathogenic microorganism of drinking water, and classified as a possible human carcinogen by International Agency for Research of Cancer (IARC) and World Health Organization (WHO). For the purpose of determining the trace level concentration of bromate, several sensitive techniques are applied mostly based on suppressed conductivity detection and UV/Visible detection after postcolumn reaction (PCR). In this study, the suppressed conductivity detection method and the PCR-UV/Visible detection method through the triiodide reaction were compared to analyze the trace bromate in water samples and estimated for the availability of these analytical methods. In addtion, the state-of-the-art techniques was applied for the determination of trace level bromate in various water matrices, i.e., soft drinking water, hard drinking water, mineral water, swimming pool water, and raw water. In comparison of two analytical methods, it was found that the conductivity detection had the suitable advantage to simultaneously analyze bromate and inorganic anions, however, the bromate might not be precisely quantified due to the matrix effect especially by chloride ion. On the other hand, the trace bromate was analyzed effectively by the method of PCR-UV/Visible detection through triiodide reaction to satisfactorily minimize the matrix interference of chloride ion in various water samples, showing the good linearity and reproducibility. Furthermore, the method detection limit (MDL) and recovery were 0.161 ㎍/L and 101.0-108.1 %, respectively, with a better availability compared to conductivity detection.

Safety Critical I&C Component Inventory Management Method for Nuclear Power Plant using Linear Data Analysis Technic

  • Jung, Jae Cheon;Kim, Haek Yun
    • Journal of the Korean Society of Systems Engineering
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    • v.16 no.1
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    • pp.84-97
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    • 2020
  • This paper aims to develop an optimized inventory management method for safety critical Instrument and Control (I&C) components. In this regard, the paper focuses on estimating the consumption rate of I&C components using demand forecasting methods. The target component for this paper is the Foxboro SPEC-200 controller. This component was chosen because it has highest consumption rate among the safety critical I&C components in Korean OPR-1000 NPPs. Three analytical methods were chosen in order to develop the demand forecasting methods; Poisson, Generalized Linear Model (GLM) and Bootstrapping. The results show that the GLM gives better accuracy than the other analytical methods. This is because the GLM considers the maintenance level of the component by discriminating between corrective and preventive.

Development of Evaluation Softwares for Job Hazard Analysis (유해요인조사용 평가 소프트웨어 개발)

  • Jeong, Byung-Yong;Lee, Jong-Hyup;Kim, Kuk
    • Journal of the Ergonomics Society of Korea
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    • v.24 no.4
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    • pp.79-83
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    • 2005
  • Efforts to identify jobs or tasks having known risk factors for work-related musculoskeletal disorder can provide the groundwork for changes aimed at risk reduction. An effective identification method is the ergonomic job hazard analysis which breaks a job into its various elements or actions, describes them, measures and quantifies the ergonomics risk factors. Some analytical methods including OWAS, RULA, REBA, and NLE have been used as tools in quantifying the risk factors. But these traditional methods using worksheet or paper are difficult to explain to participants for performing the job hazard analysis in the field, and take a long time. We develop some software tools to implement the analytical methods using EXCEL programs or computer program. These tools developed in this study are faster and easier to perform the ergonomic job analysis than the traditional methods using worksheet.

Comparison of Analytical Methods for Volatile Flavor Compounds in Leaf of Perilla frutescens

  • Kim, Kwan-Su;Ryu, Su-Noh;Song, Ji-Sook;Bang, Jin-Ki;Lee, Bong-Ho
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.44 no.2
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    • pp.154-158
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    • 1999
  • Volatile flavor compounds from perilla leaves were extracted and analyzed with different methods, head-space analysis (HS), simultaneous steam distillation and extraction (SDE) , and solvent extraction (SE), and to compare their efficiencies for quick analysis. Over 30 volatile compounds were isolated and 28 compounds were identified by GC/MSD. Major compound was perillaketone showing the compositions of which were 92% in SDE method, 86% in headspace analysis, and 62% in solvent extraction method. For quick evaluation of leaf flavor in perilla, it was desirable because the headspace analysis method had a shorter analyzing time and smaller sample amount than the other methods.

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