• Analytical Science and Technology
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• v.32 no.4
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• pp.121-130
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• 2019

Alumina is one of the most important ceramic materials because of its useful physical and chemical properties. Recently, high-purity alumina has been used in various industrial fields. This leads to increasing demand for reliable elemental analysis of impurities in alumina samples. However, the chemical inertness of alumina makes the sample preparation for conventional elemental analysis a tremendously difficult task. Herein, we demonstrated the feasibility of laser ablation for effective sampling of alumina powder. Laser ablation performs sampling rapidly without any chemical reagents and also allows simultaneous optical emission spectroscopy and mass spectrometry analyses. For six alumina samples including certified reference materials and commercial products, laser-induced breakdown spectroscopy (LIBS) and laser-ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS) analyses were performed simultaneously based on a common laser ablation sampling. LIBS was found to be useful to quantify alkali and alkaline earth metals with limits-of-detection (LODs) around 1 ppm. LA-ICP-MS could quantify transition metals such as Ti, Cu, Zn, and Zr with LODs in the range from a few tens to hundreds ppb.

• Analytical Science and Technology
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• v.35 no.6
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• pp.249-255
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• 2022

In this study, a new method for the analysis of high-purity nitrogen was developed. A gas chromatography-flame ionization detector (GC-FID) was used for purity analysis. Certified reference materials (CRMs) at a level of 3 µmol/mol of carbon monoxide (CO), carbon dioxide (CO₂), and methane (CH₄), which may exist in high-purity nitrogen, were prepared using the gravimetric method, and these CRMs were used for purity analysis. In this new method, ultra-high-purity and high-purity nitrogen were used as carrier gases. The impurities in high-purity nitrogen were quantitatively analyzed by comparing the differences in the area values of the GC chromatograms of the prepared CRMs. We purchased liquid nitrogen and three bottles of nitrogen gas, which were produced by three different manufacturers, using high-purity nitrogen. Furthermore, to validate the developed purity analysis method, the fraction of impurities in high-purity nitrogen was compared with the results of the typical purity analysis method. The comparison results were consistent within the expanded uncertainties (k = 2).

• Analytical Science and Technology
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• v.30 no.5
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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.

• Analytical Science and Technology
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• v.22 no.4
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• pp.293-301
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• 2009

As a basic research for development of the domestic field-portable XRF spectrometer, we discussed the analytical results of bench-top ED-XRF and field-portable XRF method for polluted heavy metals such as Cr, As, Se, Hg, Pb, Cd in soil samples. To obtain the best performance of the XRF spectrometer, the instrumental parameters of X-ray tube-voltage and measurement time were optimized for 6 heavy-metal elements in soil using certified reference material. The quantitative analysis of Cr, As, Se, Hg, Pb, Cd concentration in certified reference materials and soil samples were compared by empirical method and fundamental parameter method.

• Journal of Genetic Medicine
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• v.12 no.2
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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.

• Journal of the Korean Vacuum Society
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• v.7 no.3
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• pp.176-186
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• 1998

Pure Pt, Co and their alloy thin films with three different compositions (Pt66-Co34, Pt40-Co60 and Pt18-Co82) were deposited on Si(100) wafers and proposed as a set of certified reference materials (CRM) for the quantification and standardization of surface compositional analysis. The compositions of the binary alloy thin films were controlled by in-situ XPS analyses and the certified compositions of the films have been determined by ICP-AES and RBS analyses after thin film growth. Through comparison of the compositions determined by in-situ XPS with those by ICP, relatively accurate compositions could be obtained with a matrix effect correction. Standard deviations of XPS and AES round robin tests with the Pt-Co alloy thin films were large up to about 4%. On the other hand, the average compositions of the Pt-Co alloy thin films by two methods were in a good agreement within 1%. The formation of a Pt rich surface layer by ion beam sputtering indicates that the surface modification by preferential sputtering must be understood for a better compositional analysis.

• Analytical Science and Technology
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• v.21 no.1
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• pp.14-19
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• 2008

Among the many odor materials, aldehyde has bad influences not only on human nose, but also on human health. Aldehyde has a strong odor at infinitesimal level, such as down to ppt concentration. Also aldehydes are highly reactive and have poor stability. Therefore, manufacture of standard gases, analysis of aldehydes are very difficult compare to other air pollution analysis. Aldehyde CRM containing 4 different aldehydes at $10{\mu}mol/mol$ (ppm) is developed by using gravimetry method according to ISO 6142 guide. The standard gases were reproduced again, and examined its reproducibility of preparation by GC-FID. The developed aldehyde CRM's certified value showed a relative expanded uncertainties of 2.11 % (95 % of confidence level, k=2).

• Food Science and Biotechnology
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• v.18 no.5
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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.

• Analytical Science and Technology
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• v.24 no.6
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• pp.443-450
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• 2011

Quantitative analytical condition for nickel in ceramic, metal and plastic materials using complexation and solvent extraction followed by inductively coupled plasma-atomic emission spectrometry (ICP-AES) and atomic absorption spectrophotometry (AAS) was studied. Ceramic, metal and plastic samples were dissolved by acid digestion. Nickel was determined by ICP-AES and AAS after extraction of Ni $(DMG)_2$ in $CHCl_3$. Recovery efficiency of nickel was satisfactory, and most of matrix elements causing interference could be effectively eliminated by the separation. Nickel in the certified reference materials (BAM-376 and PACS-2) were quantitatively determined without influence of sample matrix.

• Journal of the Korean Society for Heat Treatment
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• v.13 no.1
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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.