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Tetrakis(pentafluorophenyl)indium(Ⅲ) 음이온 착물의 합성과 특성
최철호,Choi, Zel Ho 대한화학회 1999 대한화학회지 Vol.43 No.1
In($C_6F_5)_3{\cdot}D(D=CH_3CN$, O($C_2H_5)_2$)와 ($CH_3)_3SiC_6F_5$/CsF, $C_6F_5$MgBr 또는 Cd($C_6F_5)_2$을 반응시켜 [In($C_6F_5)_4$]- 음이온 화합물을 합성하였으나, 이들 indium(III) 음이온 화합물들은 온도에 민감하고 습기에 대해 불안정하다. 안정한 indium(III) 음이온 착물은 PNPCl(PNP=bis(triphenylphosphino)ammonium)과의 양이온 치환반응시켜 얻었으며, 관 크로마토 그래피를 이용하여 분리 정제하였다. 합성된 화합물의 특성은 핵자기 공명 분석법, 적외선 분광분석법, 분자량 측정, DTA/TG 그리고 원소분석법을 이용하여 조사하였다. The anionic complexes, [ln($C_6F_5)_4$]-, which are thermal and moisture sensitive, have been prepared by the reaction of In($C_6F_5)_3{\cdot}D(D=CH_3CN$, O($C_2H_5)_2$) with the system ($CH_3)_3SiC_6F_5$/CsF, $C_6F_5$MgBr or Cd($C_6F_5)_2$. The stable anionic indium(III) complexes are obtained through cation exchange with PNPCI ([PNP]= bis(triphenylphosphino)ammonium). The pure substance is obtained by column chromatography. These new anionic complexes are unambiguously identifed by NMR-spectroscopy, IR spectroscopy, molecular weight, DTA/TG and elemental analysis.
Indium(III) 화합물의 Acetonitrile 과 DMAP 착물의 합성 및 특성
최철호,Choi, Zel Ho 대한화학회 1998 대한화학회지 Vol.42 No.2
Indium(III) trihalides (halogen=Cl, Br)와 bis(pentafluorophenyl)cadmiumd을 acetonitrile에서 반응시켜 acetonitrile이 배위된 tris(pentafluorophenyl)indium을 합성하였으며 원소분석, 핵자기 공명과 질량분석 스펙트럼을 이용하여 특성을 조사하였다. 그 결과 acetonitrile과 배위한 tris(pentafluorophenyl)indium는 pentafluorophenylindium화합물과 acetonitrile이 1:1로 배위된다는 것을 알 수 있었다. 또한 In$(C_6F_5)_3{\cdot} CH_3CN$과 DMAP(dimethylaminopyridine)를 dichloro methane 용매에서 리간드를 치환반응시켜 In$In(C_6F_5)_3{\cdot}DMAP$를 합성하였다. 리간드들의 치환은 acetonitrile보다 주개 성질이 강한 DMAP가 acetonitrile의 자리에 배위하는 것으로 생각된다. Tris(pentafluorophenyl)indium acetonitrile complexes have been prepared from the reaction of Indium trihalides (halogen=Cl, Br) and bis(pentafluorophenyl)cadmium in acetonitrile, and characterized by elementary analysis, $^13C{^1H}-,\; ^1H-\;and\; ^{19}F-NMR$ spectroscopy and mass spectrometry. The Indium (III) compounds were formed stable 1:1 adducts with acetonitrile. $In(C_6F_5)_3{\cdot}DMAP$ has been prepared from the ligand exchange reaction of In$(C_6F_5)_3 {\cdot} CH_3CN$ with DMAP in $CH_2Cl_2 {\cdot} DMAP$ has higher donating character and replaced the $CH_3CN$ through the ligand transfer reaction.
구리를 함유한 탄소소재의 납 및 카드뮴 분석에 관한 연구
최철호,Choi, Zel-Ho 한국결정성장학회 2010 韓國結晶成長學會誌 Vol.20 No.6
용매추출과 ICP-AES를 이용하여 구리와 탄소가 주성분인 탄소소재에 함유된 납 및 카드뮴을 정량하기 위한 조건을 연구하였다. 구리성분은 납 및 카드뮴 정량에 방해를 하므로 potassium cyanide로 masking한 다음 dithizone을 가하여 납 및 카드뮴을 Pb- 또는 Cd-dithizone 착물을 형성한 다음 chloroform으로 추출하여 측정하였다. 납 및 카드뮴에 대한 측정 회수율이 우수하였고, 방해를 일으키는 매질원소를 효율적으로 제거할 수 있었다. 납 및 카드뮴 화합물이 첨가된 시험기준 물질에 대한 용매추출시험에서 matrix의 영향을 받지 않고 정량하였다. Quantitative analytical condition for lead and cadmium in copper contained carbon materials using solvent extraction followed by inductively coupled plasma-atomic emission spectrometry was studied. Copper contained carbon samples were dissolved by nitric acid-perchloric acid digestion. Lead and cadmium were determined after separation with KCN masked copper by an dithizone-chloroform solvent extraction. Recovery efficiency of analyte elements was satisfactory, and most of matrix elements causing interference could be effectively eliminated by the separation. Lead and cadmium were quantitatively determined without influence of sample matrix, by applying it procedure to artifact sample.
김선택(Sun Teak KIM),최기인(Ki In CHOI),이재인(Jae In LEE),임다혜(Da Hye LIM),최철호(Zel Ho CHOI),구상만(Sang Man KOO) 한국생태공학회 2014 한국생태공학회지 Vol.4 No.1
PVC is one of the common thermoplastic polymers well mixed up with other plasticizer, stabilizer, and additive agent. It is also a highly energy efficient material widely used in many industries related with vehicles, accessories, furniture, packaging, pipes, wallpaper, wire coating, and so on. Since it has been reported that VCM, the raw material of PVC, could be related with high of bio-carcinogenicity in human, however, the level of residual VCM not only in the polymer resins but also in the environment have been regulated in many countries. There are several testing methods for the determination of residual VCM in the polymer resins as well as environment samples, including those by ISO, ASTM, EPA, KS, and other governmental guidelines. However, it is still difficult to measure residual VCM because of its high vapor pressure. No suitable commercial reference material for VCM is another problem. To establish and develop more reliable test method for residual VCM, this paper introduces several typical standard methods for residual VCM testing in Korea and other countries.
GC/MS를 이용한 폴리스타이렌 소재의 PCBs 정량분석 방법 개발
이재인(Jae in LEE),최기인(Gi In CHOI),최철호(Zel Ho CHOI),조훈식(Hun Sik CHO),최인석(In seok CHOI),이태규(Tai Kyu LEE) 한국생태공학회 2012 한국생태공학회지 Vol.3 No.1
A study on the determination method of PCBs(polychlorinated Biphenyls) content in polystyrene(PS) materials by GC/MS was performed. The toluene was selected for the extraction of PCBs in plastics and the best extraction time was 4 hours. The artifact materials produced from polystyrene with 2,2’,3,4,4’,5,5’-heptachlorobiphenyl standard solution were examined by homogeniety test. PCBs in average concentration of 118 mg/kg were quantitatively determined for the artifact materials by applying our procedure in interlaboratory comparison test.
이재인(Jae In LEE),이태규(Tai Gyu LEE),최기인(Ki In CHOI),엄희정(Hui Jeong EOM),권덕준(Deok Jun KWEON),최철호(Zel Ho CHOI) 한국생태공학회 2012 한국생태공학회지 Vol.3 No.1
This study presents a method for the quantitative analysis of residual musk xylene in product samples. Toluene, acetonitrile, hexane, acetone, and methanol were tested for the solvent selection with artificial samples made from paper filter and glass filter. Musk xylene dissolves most often through soxhlet extraction of toluene over six hours. Both GC/MS and GC/ECD showed relative low detection limit for musk xylene. Based on the results of round robin test with seven laboratories, it seems valid the extraction and analysis method of musk xylene proposed in this study.