• 분석과학
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• 제15권5호
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• pp.433-438
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• 2002

국제원자력기구로부터 제공받은 2종 (V-50, P-50)의 인공적으로 준비된 여과지상의 도시분진시료중의 미량원소를 중성자방사화분석법을 사용하여 비파괴 분석하였다. 중성자방사화분석의 품질관리를 위해 미국표준기술원의 인증표준물질 (Urban Particulate Matter, NIST SRM1648)이 사용되었으며 여과지상의 분진시료에서는 약 20종의 원소를 분석하였다. 측정결과는 실험실간 비교 및 숙련도 평가를 위하여 중성자방사화분석법, 하전입자유도 X-선 방출분광법, 유도결합플라즈마 질량분석법 등을 이용한 세계 40개국, 49개 실험실의 분석값들과 함께 통계처리 되었다. 통계 처리한 결과, 본 실험실의 분석값들의 Z-score가 ${\pm}2$ 이내에 들어오는 결과를 얻었으며, 숙련도 시험도 분석된 모든 원소의 정확도와 정밀도가 기준에 통과되는 신뢰성 있는 결과를 얻어 현재 수행하고 있는 대기분진시료들의 분석품질관리가 적합함을 입증하였다.

• 분석과학
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• 제11권5호
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• pp.1057-1064
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• 1998

• 한국산업보건학회지
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• 제31권1호
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• pp.22-30
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• 2021

Objectives: The objectives of this study were to develop a quality control protocol of inorganic acids using ion chromatograph and to evaluate analytical proficiency of the legally designated agencies. Methods: This study prepared inorganic acid samples by injecting three anion certified solutions (chloride, nitrate, and sulfate) on the quartz filters. To investigate the storage stability and concentration consistency of the samples, 240 samples for each anion were tested at weeks 0, 2, 4, 8, 12, and 16 while storing at 4℃ and 25℃. To evaluate analytical proficiency, two separate testings were administrated for six skilled analysts and 46 analysts affiliated with legally designated agencies. Results: Average recoveries of the three ions after 16 weeks of storage were fairly high (over 95%). In addition, average recoveries (chloride = 97%, nitrate = 96%, and sulfate = 103%) after 16 weeks of storage at low temperate were relatively higher than those (94%, 93%, and 98%) at room temperature. The coefficients of variation (CV) for the three ions were less than 5% except for the sulfate sample at 5.56 ㎍ (CV = 12.4%). The average ratios of the concentration values analyzed by the legally designated agencies to the injected concentrations were close to 1. However, their CVs were relatively greater (chloride ≤ 49%, nitrate ≤ 14%, and sulfate ≤ 28%), which implies a need for quality control. Conclusions: The quality control protocol used in this study for the three inorganic acids can be utilized in the quality control for ion chromatography.

• Mass Spectrometry Letters
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• 제9권1호
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• pp.30-36
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• 2018

A quantitation method for free amino acids in human serum was developed using a stepwise-dilution method and a bimodal cation exchange (CEX)/hydrophilic interaction liquid chromatography (HILIC)-tandem mass spectrometry system equipped with an electrospray ionization source (ESI/MS/MS). This method, which was validated using quality control samples, was optimized for enhanced selectivity and sensitivity. Dithiothreitol (DTT) was used as a reducing agent to prevent the oxidation of a serum sample ($50{\mu}L$), which was then subjected to stepwise dilution using 3, 30, and 90 volumes of acetonitrile containing 0.1% formic acid. Chromatographic separation was performed on an Imtakt Intrada Amino Acid column ($50mm{\times}3mm$, $3{\mu}m$) in mixed mode packed with CEX and HILIC ligands embedded in the stationary phase. Underivatized free amino acids were eluted and separated within 10 min. As a result of the validation, the precision and accuracy for the inter- and intraday assays were determined as 2.11-11.51% and 92.82-109.40%, respectively. The lowest limit of quantification (LLOQ) was $0.5-4.0{\mu}g/mL$ and the matrix effect was 80.22-115.93%. The proposed method was successfully applied to the quantitative analysis of free amino acids in human serum.

• Nuclear Engineering and Technology
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• 제49권3호
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• pp.562-568
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• 2017

Background: The chemical characterization of metallic alloys and oxides is conventionally carried out by wet chemical analytical methods and/or instrumental methods. Instrumental neutron activation analysis (INAA) is capable of analyzing samples nondestructively. As a part of a chemical quality control exercise, Zircaloys 2 and 4, nimonic alloy, and zirconium oxide samples were analyzed by two INAA methods. The samples of alloys and oxides were also analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES) and direct current Arc OES methods, respectively, for quality assurance purposes. The samples are important in various fields including nuclear technology. Methods: Samples were neutron irradiated using nuclear reactors, and the radioactive assay was carried out using high-resolution gamma-ray spectrometry. Major to trace mass fractions were determined using both relative and internal monostandard (IM) NAA methods as well as OES methods. Results: In the case of alloys, compositional analyses as well as concentrations of some trace elements were determined, whereas in the case of zirconium oxides, six trace elements were determined. For method validation, British Chemical Standard (BCS)-certified reference material 310/1 (a nimonic alloy) was analyzed using both relative INAA and IM-NAA methods. Conclusion: The results showed that IM-NAA and relative INAA methods can be used for nondestructive chemical quality control of alloys and oxide samples.

• 농약과학회지
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• 제15권4호
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• pp.529-544
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• 2011

분석표준화 관련 국제기관인 ISO, CIPAC 등은 농약제품 시험기관에 대한 정도관리(QC), 숙련도 시험 및 분석법 검증을 수행하기 위한 요구조건을 지침서로 제시하고 있다. 일반적으로, 숙련도 시험은 시험기관의 분석능력 평가를 위하여 시험기관간 비교시험을 바탕으로 시험기관의 수행능력과 기술능력 정도를 판단할 수 있다. 분석법 검증 절차는 정도관리(QC)에서 중요한 단계 중 하나로 특이성, 선택성, 직선성 등의 항목들이 포함되며, 대부분의 국제기관이 농약제품 중 주요성분에 대한 정량분석법에서 재현성, 정확성 및 정밀성 등을 요구하고 있다. 본 연구에서는 농약 이화학시험 분석기관의 시험연구과정 및 결과에 대한 신뢰성을 높이기 위해 국내 외 정도관리에 관한 지침서를 비교 검토하여 국제적으로 표준화된 지침서에 적합한 구체적이고, 효율적인 농약 이화학시험 분석기관의 농약분석법 검증절차 및 시험기관 정도관리 체계(안)를 제안하고자 한다.

• Journal of Ginseng Research
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• 제37권4호
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• pp.475-482
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• 2013

The main active components of Panax ginseng are ginsenosides. Ginsenoside Rb1 and Rg1 are accepted as marker substances for quality control worldwide. The analytical methods currently used to detect these two compounds unfairly penalize steamed and dried (red) P. ginseng preparations, because it has a lower content of those ginsenosides than white ginseng. To manufacture red ginseng products from fresh ginseng, the ginseng roots are exposed to high temperatures for many hours. This heating process converts the naturally occurring ginsenoside Rb1 and Rg1 into artifact ginsenosides such as ginsenoside Rg3, Rg5, Rh1, and Rh2, among others. This study highlights the absurdity of the current analytical practice by investigating the time-dependent changes in the crude saponin and the major natural and artifact ginsenosides contents during simmering. The results lead us to recommend (20S)- and (20R)-ginsenoside Rg3 as new reference materials to complement the current P. ginseng preparation reference materials ginsenoside Rb1 and Rg1. An attempt has also been made to establish validated qualitative and quantitative analytical procedures for these four compounds that meet International Conference of Harmonization (ICH) guidelines for specificity, linearity, range, accuracy, precision, detection limit, quantitation limit, robustness and system suitability. Based on these results, we suggest a validated analytical procedure which conforms to ICH guidelines and equally values the contents of ginsenosides in white and red ginseng preparations.

• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2001년도 NIR-2001
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• pp.1081-1081
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• 2001

The constant need for quality improvement and production rationalization in the chemical and related industries has led to the increasing replacement of conservative control procedures by more specific and environmentally compatible analytical techniques. In this respect, vibrational spectroscopy has developed over the last yews - in combination with new instrumental accessories and statistical evaluation procedures - to one of the most important analytical tools for industrial chemical quality control and process monitoring in a wide field of applications. In the present communication this potential is demonstrated in order to further support the implementation of mid-infrared (MIR), near-infrared (NIR) and Raman spectroscopy Primarily as industrial on-line tools. To this end the data of selected feasibility studies will be discussed in terms of the individual strengths of the different techniques for the respective application.

• 분석과학
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• 제24권6호
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• pp.414-420
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• 2011

본 연구에서는 알파선, 베타선 및 감마선 방출 핵종에 대한 검출기를 선정하여, 방사성 시료의 핵종분석을 위한 방사선 측정 시스템을 연구하고 구성하였다. 그리고 알파, 베타 및 감마 측정 시스템에 대한 검출효율을 교정하였다. 방사선 검출기에 대한 안정도를 확보하기 위해 품질관리 프로그램이 확립되었다. 또한 분석결과에 대한 신뢰도를 확보하기 위해 시료유형에 따른 최소검출방사능을 구하였다.

• 품질경영학회지
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• 제12권2호
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• pp.15-24
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• 1984

Since W.A. Shewhart (1931) developed the quality control method using the control chart, many theoretical and empirical works about such an analytical method have been done. However there are two major methods relating to the control chart analysis; the conventional 3 sigma control method and the warning limit method which has been suggested as a modification of the former. The conventional 3 sigma method requires to take a remedial action only when a quality characteristic is beyond the control limit (3 sigma). However, once a quality characteristic is over the control limit, searching and repairing an assignable cause requires time consuming job and high costs. Therefore if we set the warning limit between the central line and the control limit, we will be able to take remedial measures before too late. In spite of its advantage, much attention has not been paid to use the control chart with warning limit in Korean industries. The main object of this study is to examine improvement of quality and productivity when the control chart with warning limit is used.