• Bulletin of the Korean Chemical Society
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• 제26권3호
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• pp.440-446
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• 2005

A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

• 분석과학
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• 제35권6호
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• pp.249-255
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• 2022

본 연구에서는 기체 크로마토그래피-불꽃이온화검출기(GC-FID)를 이용한 고순도 질소의 새로운 순도분석법을 개발하였다. 고순도 질소에 존재할 수 있는 불순물인 일산화탄소(CO), 이산화탄소(CO₂), 및 메탄(CH₄)에 대한 3 µmol/mol 수준의 인증표준물질(Certified reference material, CRM)을 중량법을 이용하여 제조하였고, 이를 순도분석에 활용하였다. 개발된 순도분석법에서는 운반가스로 초고순도 질소와 순도분석 대상 질소를 사용하여, 제조된 인증표준물질의 기체 크로마토그래피에서 얻어지는 크로마토그램의 면적 값 차이를 비교함으로써 순도분석 대상 질소의 불순물을 정량 분석하였다. 순도분석 대상 질소로는 액체질소 및 제조사가 각기 다른 3곳의 고순도 질소를 사용하였다. 또한, 개발된 순도분석법의 유효성을 평가하기 위하여 순도분석 대상 질소 내 불순물의 물질량 분율을 기존 순도분석법과 비교하였다. 두 가지 순도분석법을 이용하였을 때 대상 질소 내 불순물의 물질량 분율이 불확도 (k = 2) 내에서 서로 일치함을 확인함으로써, 개발된 순도분석법이 유효함을 확인하였다.

• 분석과학
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• 제30권5호
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• pp.226-233
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• 2017

In general, quantitative chemical analysis in various areas including food, the environment, in vitro diagnostics, etc., requires traceability in order to increase the reliability of the measurements. Measurement traceability is a property of an unbroken chain of comparisons relating an instrument's measurements to SI units. Purity analysis is the first process for establishing traceability to SI units in chemical measurements. The purpose of this study is to develop and validate a method of purity assignment for establishing the traceability of $17{\beta}$-estradiol measurements in an in vitro diagnostics field. The establishment of this method is very important as it can be applied to the development of CRM and to the analysis of the purity of other hormones. The method of assignment of the purity of $17{\beta}$-estradiol was developed using the mass balance method and was validated through participation in an International comparison. In the mass balance method, impurities are categorized into four classes as follows: total related structure impurities, water, residual organic solvents, and nonvolatiles/inorganics. In this study, total related structure impurities were characterized by a gas chromatography-flame ionization detector (GC-FID) and a high-performance liquid chromatography-ultraviolet (HPLC-UV) detector, water content was determined by a Karl-Fisher coulometer, and total residual solvents and nonvolatiles/inorganics were checked simultaneously by thermogravimetric analysis (TGA). The purity of the $17{\beta}$-estradiol was 985.6 mg/g and the expanded uncertainty was 2.1 mg/g at 95% confidence. The developed method can be applied to the development of certified reference materials, which play a critical role in traceability.

• 분석과학
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• 제22권4호
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• pp.293-301
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• 2009

휴대용 형광 분석기의 개발을 위한 사전 기초연구로서 bench-top ED-XRF 및 휴대용 XRF를 이용하여 토양 시료 중의 Cr, As, Se, Hg, Pb, Cd 등 6종의 유해금속 성분들을 비교 분석하였다. 유해금속 원소를 0~1500 mg/kg 농도 범위로 오염시킨 토양 인증표준물질을 구입하여 XRF 분석의 중요 인자인 X-선 튜브 전압 및 측정 시간 등에 따른 최적 분석조건을 확립하고, 각각의 유해 중금속에 대한 검량선을 작성하였다. 유해금속 원소가 포함된 토양 인증표준물질 외에 7종의 다른 토양 시료 중의 유해금속 원소에 대해서도 empirical 법 및 fundamental parameter 법으로 정량분석하고 그 결과를 비교 분석하였다.

• Journal of Genetic Medicine
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• 제12권2호
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• pp.79-84
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• 2015

Purpose: We developed and validated a fetal trisomy detection method for use as a noninvasive prenatal test (NIPT) including a Clinical Laboratory Improvement Amendments (CLIA)-certified bioinformatics pipeline on a cloud-based computing system using both Illumina and Life Technology sequencing platforms for 221 Korean clinical samples. We determined the necessary proportions of the fetal fraction in the cell-free DNA (cfDNA) sample for NIPT of trisomies 13, 18, and 21 through a limit of quantification (LOQ) test. Materials and Methods: Next-generation sequencing libraries from 221 clinical samples and three positive controls were generated using Illumina and Life Technology chemistries. Sequencing results were uploaded to a cloud and mapped on the human reference genome (GRCh37/hg19) using bioinformatics tools. Based on Z-scores calculated by normalization of the mapped read counts, final aneuploidy reports were automatically generated for fetal aneuploidy determination. Results: We identified in total 29 aneuploid samples, and additional analytical methods performed to confirm the results showed that one of these was a false-positive. The LOQ test showed that the proportion of fetal fraction in the cfDNA sample would affect the interpretation of the aneuploidy results. Conclusion: Noninvasive chromosome examination (NICE), a CLIA-certified NIPT with a cloud-based bioinformatics platform, showed unambiguous success in fetus aneuploidy detection.

• 한국진공학회지
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• 제7권3호
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• pp.176-186
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• 1998

Si 기판 위에 3종의 Pt-Co 합금박막 (Pt66-Co34, Pt40-Co60, Pt18-Co82)과 순수한 Pt, Co 박막 시료를 제작하여 표면 조성분석의 정량화 및 표준화를 위한 표준시료로 제안하 였다. in-istu X-ray photoelectron spectroscopy(XPS)분석에 의해 증착된 이원 합금박막의 조성이 정확히 조절되었으며, 합금박막의 실제 조성은 유도결합플라즈마-원자방출분광법 (inductively coupled plasma-atomic emission spectroscopy: ICP-AES)과 러더퍼드 후방산 란분광법(Ruthford back-scattering spectrometry: RBS)에 의해 결정되었다. in-situ XPS 결과와 ICP에 의한 조성을 비교한 결과 매질 효과를 고려하면 비교적 정확한 조성을 구할 수 있음이 확인되었다. 이 시료를 이용한 XPS와 Auger electron spectroscopy(AES)에 의한 국내 공동분석 결과는 약4%내외의 큰 편차를 보이고 있지만, 평균 조성 값은 약1%의 오차 범위 내에서 두 방법에 의한 결과가 서로 잘 일치하였다. 이온빔 스퍼터링에 의해 Pt조성이 증가된 표면층이 형성되어 정확한 조성분석을 위해서는 선택스퍼터링에 의한 표면 변형을 정량적으로 함을 알았다.

• 분석과학
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• 제21권1호
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• pp.14-19
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• 2008

많은 악취물질 중에 알데하이드는 인간의 호흡기 자극을 유발할 뿐만 아니라 인간의 건강에 상당히 안좋은 영향을 미친다. 알데하이드류의 악취물질은 일반 대기오염물질과 달리 ppt 수준의 매우 극미량에서 악취를 발생하는 성분이 많아 매우 극미량의 측정기술의 필요하다. 또한 대부분 반응성이 크고 안정성이 낮아 표준가스 제조 및 분석이 매우 어려워 정확한 측정이 어렵다. $10{\mu}mol/mol$ 수준의 농도로 제조된 4성분 알데하이드 CRM(MK0731)은 ISO 6142에 의한 중량법으로 제조하였다. $10{\mu}mol/mol$ 알데하이드 표준가스 실린더를 반복 제조하여 각각 GC-FID로 제조의 균질성을 조사하였고, 개발된 알데하이드류 CRM 인증값의 상대 확장불확도는 2.11 %(95%의 신뢰수준, k=2)로 조사되었다.

• Food Science and Biotechnology
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• 제18권5호
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• pp.1118-1123
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• 2009

Event-specific real-time polymerase chain reaction (PCR) detection method for genetically modified (GM) maize MIR604 was developed based on integration junction sequences between the host plant genome and the integrated transgene. In this study, 2 primer pairs and probes were designed for specific amplification of 100 and 111 bp DNA fragments from the zSSIIb gene (the maize endogenous reference gene) and MIR604. The quantitative method was validated using 3 certified reference materials (CRMs) with levels of 0.1, 1, and 10% MIR604. The method was also assayed with 14 different plants and other GM maize. No amplification signal was observed in real-time PCR assays with any of the species tested other than MIR604 maize. As a result, the bias from the true value and the relative deviation for MIR604 was within the range from 0 to 9%. Precision, expressed as relative standard deviation (RSD), varied from 2.7 to 10% for MIR604. Limits of detections (LODs) of qualitative and quantitative methods were all 0.1%. These results indicated that the event-specific quantitative PCR detection system for MIR604 is accurate and useful.

• 분석과학
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• 제24권6호
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• pp.443-450
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• 2011

ICP-AES와 AAS를 이용하여 세라믹, 금속 및 플라스틱 소재에 함유된 니켈을 정량하기 위한 조건을 연구하였다. 니켈 정량을 위해 산분해하여 조제된 시험 용액을 직접 ICP-AES 또는 AAS로 분석할 때 철이나 크로뮴 등의 원소가 방해하므로, 니켈을 dimethylglyoxime으로 착화시키고 $CHCl_3$로 추출하여 방해원소로부터 분리한 후 $CHCl_3$을 제거하고 염산으로 용해하여 측정하였다. 니켈에 대한 측정 회수율이 우수하였고, 방해를 일으키는 매질원소를 효율적으로 제거할 수 있어 본 방법은 인증표준물질(BAM-376 및 PACS-2)에 대한 용매추출시험에서 matrix의 영향을 받지 않고 니겔을 정량할 수 있었다.

• 열처리공학회지
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• 제13권1호
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• pp.10-15
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• 2000

Evaluation of long term stability of the Brinell standard hardness tester was carried out to secure its application as a national standard in Brinell hardness. Accuracy and repeatability in load application were tested through evaluating errors in hardness measurement of certified reference blocks. All of those requirements in KS as well as ISO specifications were satisfied by this standard hardness tester. In addition to this, long term stability test of automatic indentation measurement system was carried out. The scattering range was almost the same with its error range. To figure out an optimum test condition for better repeatability and long term stability, the effect of load variation, load application speed and time have been studied using orthogonal array experimental plan. It was found that the best combination is $30{\mu}m/s$ of load application speed and 25 seconds of load application time.