• 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.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.54 no.4
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• pp.346-350
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• 2009

The cultivated radish (Raphanus sativus L.) is a major vegetable crop in the world wide and fast-growing species that grows inhabitats of six continents. It is very important to determine hybrid seed purity in the production of hybrid Brassica vegetable seeds to avoid unacceptable contamination with self-inbred (sib) seeds. The use of random amplified polymorphic DNA (RAPD) markers for evaluating seed purity in $F_2$-hybrid radish cultivars demonstrated. One hundred eighty seeds from the F1 male and female harvest were subsequently screened for seed purity using 13 primers. The 13 primers result in 17 cultivar-specific bands and 23 variable RAPD bands scored for cultivar. RAPD analysis of hybrid seeds from the harvest revealed 128 seeds tested except underdevelopment and decayed seeds were sibs. Especially, $F_2$ hybrids of radish, OPC13, OPD20 were presented clear hybrid bands. It maintains higher than average level of genetic diversity compared with their correspondent parents. RAPD amplification of DNA extracted from germinated individuals from the female harvest reveal that 10 of 208 seeds tested were self-inbred (4.8%). RAPD analysis of hybrid seeds from the male harvest revealed 7 of the 208 seeds tested were sibs (3.4%). The RAPD may lead to a better insight in to the hybrid seed purity.

• Proceedings of the Materials Research Society of Korea Conference
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• 2007.11a
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• pp.82.2-82.2
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• 2007

• Analytical Science and Technology
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• v.35 no.5
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• pp.205-211
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• 2022

Deuterium (D) is an isotope with one more neutron number than hydrogen (H). Heavy elements rarely change their chemical properties with little effect even if the number of neutrons increases, but low-mass elements change their vibration energy, diffusion rate, and reaction rate because the effect cannot be ignored, which is called an isotope effect. Recently, in the semiconductor and display industries, there is a trend to replace hydrogen gas (H₂) with deuterium gas (D₂) in order to improve process stability and product quality by using the isotope effect. In addition, as the demand for D₂ in industries increases, domestic gas producers are making efforts to produce and supply D₂ on their own. In the case of high purity D₂, most of them are produced by electrolysis of heavy water (D₂O), and among D₂, hydrogen deuteride (HD) molecules are present as isotope impurities. Therefore, in order to maximize the isotope effect of hydrogen in the electronic industry, HD, which is an isotope impurity of D₂ used in the process, should be small amount. To this end, purity analysis of D₂ for industrial processing is essential. In this study, HD quantitative analysis of D₂ for high purity D₂ purity analysis was established and hydrogen isotope RM (Reference material) was developed. Since hydrogen isotopes are difficult to analyze with general gas analysis instrument, they were analyzed using a high-precision mass spectrometer (Gas/MS, Finnigan MAT271). High purity HD gas was injected into Gas/MS, sensitivity was determined by a signal according to pressure, and HD concentrations in two bottles of D₂ were quantified using the corresponding sensitivity. The amount fraction of HD in each D₂ was (4518 ± 275) μmol/mol, (2282 ± 144) μmol/mol. D₂, which quantifies HD amount using the developed quantitative analysis method, will be manufactured with hydrogen isotope RM and distributed for quality management and maintenance of electronic industries and gas producers in the future.

• Journal of the Korean Magnetic Resonance Society
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• v.24 no.1
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• pp.30-37
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• 2020

Quantitative nuclear magnetic resonance (qNMR) has been gaining attention as a purity assessment method. In particular, qNMR is recognized as the primary method to realize the Internal System of Units (SI) in organic analysis. The capability of quantitative analysis is recognized as the beginning of NMR development. NMR signals are proportional to the number of nuclei and qNMR has been used in various fields, such as metabolomics and food and pharmaceutical analysis. However, careful sample preparation and thorough optimization of measurement parameters are required to obtain accurate and reliable results. In this review, quantitative methods used in qNMR are discussed, and the important factors to be considered also introduced. The recent development of qNMR techniques including combination with chromatography and, multidimensional NMR are also presented.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.27 no.1
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• pp.57-63
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• 2017

High-purity ${\beta}-SiC$ powders for SiC single-crystal growth were synthesized by direct carbonization. The use of high-purity raw materials to improve the quality of a SiC single crystal is important. To grow SiC single crystals by the PVT method, both the particle size and the packing density of the SiC powder are crucial factors that determine the sublimation rate. In this study, we tried to produce high-purity ${\beta}-SiC$ powder with large particle sizes and containing low silicon by introducing a milling step during the direct carbonization process. Controlled heating improved the purity of the ${\beta}-SiC$ powders to more than 99 % and increased the particle size to as much as ${\sim}100{\mu}m$. The ${\beta}-SiC$ powders were characterized by SEM, XRD, PSA, and chemical analysis to assess their purity. Then, we conducted single-crystal growth experiments, and the grown 4H-SiC crystals showed high structural perfection with a FWHM of about 25-48 arcsec.

• Natural Product Sciences
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• v.25 no.3
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• pp.222-227
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• 2019

Quantitative nuclear magnetic resonance (qNMR) is a well-established method adopted by international pharmacopoeia for quantitative and purity analyses. Emodin is a type of anthraquinone, well known as the main active component of Fabaceae, Polygonaceae and Rhamnaceae. Purity analysis of emodin is usually performed by using the high-performance liquid chromatography (HPLC)-UV method. However, it cannot detect impurities such as salts, volatile matter, and trace elements. Using the qNMR method, it is possible to determine the compound content as well as the nature of the impurities. Several experimental parameters were optimized for the quantification, such as relaxation delay, spectral width, number of scans, temperature, pulse width, and acquisition time. The method was validated, and the results of the qNMR method were compared with those obtained by the HPLC and mass balance analysis methods. The qNMR method is specific, rapid, simple, and therefore, a valuable and reliable method for the purity analysis of emodin.

• Analytical Science and Technology
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• v.33 no.2
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• pp.68-75
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• 2020

We have developed 10 μmol/mol nitrogen and oxygen certified reference materials (CRMs) in helium, as a SI-traceable gas standard for a quantifying of impurities in pure gases for the first time in Korea. The standard gas mixtures of nitrogen and oxygen were prepared in 5000 μmol/mol and sequentially were diluted to 250 μmol/mol and 10 μmol/mol according to the gravimetric preparation. In each dilution step, two cylinders of CRMs were prepared. The verification of internal consistency among the prepared gas mixtures was performed by using GC-TCD. The amount fractions and those expanded uncertainties (k = 2) of nitrogen and oxygen in the standard gas mixtures were (10.12 ± 0.08) μmol/mol and (10.18 ± 0.08) μmol/mol for nitrogen, and (9.88 ± 0.06) μmol/mol and (9.94 ± 0.06) μmol/mol for oxygen, respectively. We have conducted a purity assessment of two commercial helium gases using developed CRMs. As the results of the purity assessment, nitrogen and oxygen were detected by (1.66 ± 0.03) μmol/mol and (0.31 ± 0.02) μmol/mol, respectively, as the impurities in one of the pure helium.

• Korean Journal of Metals and Materials
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• v.50 no.12
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• pp.907-911
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• 2012

High purity silicon can be obtained from Al-Si alloys by a combination of solvent refining and centrifugation. Silicon purification by crystallization of silicon from an Al-Si alloy melt was carried out using 2N and 4N purity aluminum and 2N purity silicon as raw materials. The effect of the purity of raw materials on the final silicon ingot purity by centrifugation was investigated for an Al-50 wt% Si alloy. Alloys were melted using an electrical resistance furnace, and then poured into a centrifuging apparatus. A silicon lump like foam was obtained after centrifugation and was leached by an acid in order to get pure silicon flakes. Then silicon flakes were melted to make a silicon ingot using an induction furnace. The purities of the silicon flakes and silicon ingot were enhanced significantly compared to those of the raw materials of silicon and aluminum. The silicon ingot made of 4N aluminum and 2N silicon showed the lowest impurities.