• 공업화학
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• 제7권6호
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• pp.1204-1208
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• 1996

파라자일렌(p-xylene)을 산화반응시켜 테레프탈산(terephthatic acid)을 제조하는 과정 중에 발생하는 주요 유기불순물을 효과적으로 분석하는 방법을 수립하였다. 이 제조공정 중에 발생하는 유기불순물은 매우 다양하나, 여기에서는 주로 benzoic acid, p-toluic acid, p-tolualdehyde, 4-carboxybenzaldehyde, phthalic acid, isophthalic acid, trimellitic acid와 4-hydroxymethyl benzoic acid 등의 유기불순물을 분석하는데 촛점을 맞추었다. 이 유기물들은 공정 중의 모액이나 고체상태의 테레프탈산 입자에 존재하는데, 이들을 동시에 분석하기 위해 99% bis(trimethylsilyl)trifluoroacetamide와 1% trimethylchlorosilane의 내부표준용액과 pyridine의 혼합용액내에서 trimethylsilylation으로 시료를 전처리하고 gas chromatography를 이용하여 분석한 결과 상기한 유기물이 모두 성공적으로 분리되어 50분 이내에 정량분석할 수 있었다.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2004년도 춘계학술대회 논문집 방전 플라즈마 유기절연재료 초전도 자성체연구회
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• pp.133-137
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• 2004

In this paper, we investigated impurities content, absorption properties, and thermal properties showing by changing the content of carbon black which is semiconductive materials for underground power transmission. Specimens were made of sheet form with the three of existing resins and the nine of specimens for measurement. Impurities content of specimens and absorption properties were measured by ICP-AES (Inductively Coupled Plasma Atomic Emission Spectrometer) and Karl Fisher. And high temperature, heat degradation initiation temperature, and heat weight loss were measured by TGA (Thermogravimetric Analysis). The dimension of measurement temperature was 0$[^{\circ}]$ to 800$[^{\circ}]$, and rising temperature was 10$[^{\circ}/min]$. Impurities content was highly measured according to increasing the content of carbon black from this experimental result also absorption amount was increased according to these properties. Specially, impurities content values of the A1 and A2 of existing resins were measured more than 4000[ppm]. Heat degradation initiation temperature from the TGA results was decreased according to increasing the content of carbon black. All over, heat stabilities were EEA>EBA>pEVA. That is, heat stabilities of EVA containing the weak VA(vinyl acetate) against heat was measured the lowest.

• 한국표면공학회지
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• 제57권2호
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• pp.92-97
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• 2024

The LiBr aqueous solution, which is the absorption liquid of absorption refrigerator, must be replaced periodically because the concentration of impurities such as Cu²⁺, Fe²⁺, Ca²⁺, etc., increases due to corrosion of the tubes as the period of use increases, and the refrigeration efficiency decreases significantly. In order to reuse the waste absorption liquid, flocculation-precipitation method is mainly applied to precipitate the impurities, which requires hundreds of times the concentration of impurities and generates additional waste. In this study, a process for removing Cu ion impurities from cyclone electrolyzer by electrolytic reduction is presented in a small-scale facility without additional waste. It was confirmed that Cu ion impurities can be removed down to 1 ppm by electrolytic reduction process, and to further improve the removal rate, the mass transfer rate was increased by using a cyclone electrolyzer. The removal rate of Cu ions increased with the increase of flow rate and current density, and it was confirmed that Cu was removed at a rate of 1.48 ppm/h under the condition of 330 mL/sec and 2.5 mA/cm².

• 분석과학
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• 제35권3호
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• pp.93-115
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• 2022

의약품의 제조, 유통, 보관 과정에서 발생할 수 있는 잠재적 불순물은 의약품의 품질과 안전에 영향을 미치며 반응성이 높은 불순물의 경우 인체에 대한 발암성(변이원성)을 나타내기도 한다. 이를 위해 국제의약품규제조화위원회(International Conference on Harmonisation, ICH)에서는 "잠재적 발암 위해를 제한하기 위한 의약품 중 DNA 반응성(변이원성) 불순물의 평가 및 관리"에 대한 내용을 담은 M7(R1) 가이드라인을 제공하여 채택을 권고하였다. 하지만 가이드라인에서도 잠재적 불순물에 대한 분류, 섭취 허용량, 관리방안 등과 대표적인 불순물 14 종에 대한 가이드라인 적용을 소개하는데 그치고 있어 제약회사와 규제 당국에서 실제 관리를 위한 의약품 중 잠재적 불순물의 분석에 어려움을 겪고 있다. 이에 따라 본 총설에서는 비의도적 변이원성 불순물의 정의와 ICH M7(R1) 가이드라인에 소개된 내용을 간략하게 살펴보는 한편 현재까지 보고된 주요 잠재적 불순물의 분석 동향을 살펴보고자 한다. 이를 통해 식약처를 비롯한 감독 기관과 제약회사 등에서 의약품 중 잠재적 불순물 관리에 조금이나마 도움이 되고자 한다.

• 농약과학회지
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• 제8권2호
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• pp.129-136
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• 2004

생장조절제 Atonic 원제 중 부성분의 함량과 화학구조를 구명하기 위하여 diethyl ether와 dichloromethane 분배액을 각각 GC-FID와 GC-MSD로 분석하여 5종 부성분의 화학구조를 구명하였다. 주성분인 Atonic의 함량은 약 84%이었으며, 부성분의 함량은 $0.24\sim10.74%$이었다. 확인된 부성분은 2-methoxy-phenol (guaiacol, m/z 124), 2-chloro-6-methoxyphenol 또는 4-chloro-6-methoxyphenol (m/z 158), 1,2-dimethoxy-4-nitrobenzene (m/z 183), 그리고 2,6-bis(1,1-dimethylethyl)-4-methylphenol (m/z 220)이었으며, 국내에서 규제중인 6종의 유해성분은 포함되지 않은 것으로 판단되었다.

• 한국물환경학회지
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• 제20권5호
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• pp.432-436
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• 2004

The principle and methodology of risk assessment was applied to establish the quality standard of potential impurities of drinking water treatment chemicals. The impurities(arsenic, lead, cadmium, chromium, mercury, etc.) are regulated as the contained quantity of chemicals in Korea while they are regulated as the quality standard with the idea of 10% of the national safety drinking water standard in U.S.A(NSF) and Japan(JWWA). According to risk assessment of the current standard implemented in Korea, the excess cancer risk of arsenic and lead were determined in around $10^{-5}$ and the hazard quotient(HQ) of cadmium and chromium were below $10^{-2}$, respectively. And the standard concentration of the impurities are regulated as much as 2%~6% of the national drinking water quality standard. The values are more enforced rather than the standards in U.S.A(NSF) and Japan(JWWA) regulating the concentration of impurities the 10% of the national drinking water quality standard. We conclude that the impurities standard of drinking water treatment chemicals should be reconsidered comprehensively concerning the national safety drinking water quality standard and risk assessment.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2004년도 하계학술대회 논문집 Vol.5 No.1
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• pp.489-494
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• 2004

In this paper, we investigated impurities content and thermal properties showing by changing the content of carbon black which is semiconductive materials for underground power transmission. Specimens were made of sheet form with the three of existing resins and the nine of specimens for measurement. Impurities content of specimens was measured by ICP-AES(Inductively Coupled Plasma Atomic Emission Spectrometer), and density of specimens were measured by density meter. And then heat capacity(${\Delta}H$) and melting temperature(Tm), specific heat(Cp) were measured by DSC(Differential Scanning Calorimetry). The dimension of measurement temperature was $0[^{\circ}C]\;to\;200[^{\circ}C]$, and rising temperature was $4[^{\circ}C/min]$. Impurities content was highly measured according to increasing the content of carbon black from this experimental result also density was increased according to these properties. Specially, impurities content values of the A1 and A2 of existing resins were measured more than 4000[ppm]. Heat capacity, melting temperature, and specific heat from the DSC results were simultaneously decreased according to increasing the content of carbon black. Because metallic impurities of carbon black having Fe, Co, Mn, A1 and Zn are rapidly passed kinetic energy increasing the number of times breaking during the unit time with the near particles according to increasing vibration of particles by the applied heat energy.

• 분석과학
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• 제37권1호
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• pp.25-38
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• 2024

The study aimed to investigate a novel approach by utilizing liquid chromatography (LC) and liquid chromatography-mass spectrometry (LC-MS) to separate, identify and characterize very nominal quantities of degradation products (DPs) of balsalazide along with its process related impurities without isolation from their reaction mixtures. The impurities along with balsalazide were resolved on spherisorb ODS2 (250×4.6 mm, 5.0 ㎛) column at room temperature using 0.2 M sodium acetate solution at pH 4.5 and methanol in the ratio of 55:45 (v/v) as mobile phase pumped isocratically at 1.0 mL/min as mobile phase and UV detection at 255 nm. The method shows sensitive detection limit of 0.003 ㎍/mL, 0.015 ㎍/mL and 0.009 ㎍/mL respectively for impurity 1, 2 and 3 with calibration curve liner in the range of 50-300 ㎍/mL for balsalazide and 0.05-0.30 for its impurities. The balsalazide pure compound was subjected to stress studies and a total of four degradation products (DPs) were formed during the stress study and all the DPs were characterized with the help of their fragmentation pattern and the masses obtained upon LC-MS/MS. The DPs were identified as 3-({4-[(E)-(4-hydroxyphenyl) diazenyl]benzoyl}amino)propanoic acid (DP 1), 4-[(E)-(4-hydroxyphenyl)diazenyl] benzamide (DP 2), 5-[(E)-(4-carbamoylphenyl)diazenyl]-2-hydroxybenzoic acid (DP 3) and 3-({4-[(E)-phenyldiazenyl]benzoyl}amino)propanoic acid (DP 4). Based on findings, it was concluded that, the proposed method was successfully applicable for routine analysis of balsalazide and its process related impurities in pure drug and formulations and also applicable for identification of known and unknown impurities of balsalazide.

• 한국재료학회지
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• 제26권6호
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• pp.306-310
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• 2016

To produce 4N grade high-purity silica powder from natural ore, the mineralogical characteristics of natural silica ore were investigated and their effects on the purification process were revealed. The Chinese silica mineral ore used was composed of iron and aluminum as main impurities and calcium, magnesium, potassium, sodium, and titanium as trace impurities; these trace impurities generally exist as either single oxides or complex oxides. It was confirmed that liberation and acidic washing of the impurities were highly dependent on the particle size of the ground silica ore and on its mineralogical characteristics such as the distribution and phases of existing impurities. It is suggested that appropriate size reduction of silica ore should be realized for optimized purification according to the origin of the natural silica ore. A single step purification process, the mechano-chemical washing (MCW) process, was proposed and verified in comparison with the conventional multi step washing process.

• 한국분말재료학회지
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• 제10권5호
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• pp.344-347
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• 2003

Pure tantalum powder has been produced by combining Na as a reducing agent, $K_2$TaF$_{7}$ as feed material, KCl and KF as a diluent in a stainless steel (SUS) bomb, using the method of metallothermic reduction. And we examined various types of after-treatment that affect the high purification of powder. A significant amount of impurities contained in recovered powder was removed in various conditions of acid washing. In particular, 20% (HCl + HNO$_3$) was effective in removing heavy metal impurities such as Fe, Cr and Ni, 8% H$_2$SO$_4$ + 8% $Al_2$(SO$_4$)$_3$ in removing fluorides such as K and F from non-reactive feed material, and 2% $H_2O$$_2$ + 1 % HF in removing oxides that formed during reaction. Significant amounts of oxygen and part of light metal impurities could be removed through deoxidation and heat treatment process. On the other hand, because it is difficult to remove completely heavy metal impurities such as Fe, Cr, and Ni through acid washing or heat treatment process if their contents are too high, it is considered desirable to inhibit these impurities from being mixed during the reduction process as much as possible.