• Title/Summary/Keyword: 미량 화학

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Determination of Iron in Seawater by Adsorptive Stripping Voltammetry (흡착 벗김 전압전류법에 의한 해수중 미량 철의 정량)

  • Czae, Myung-Zoon;Kim, Kyung;Kwon, Young-Soon
    • Journal of the Korean Chemical Society
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    • v.39 no.3
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    • pp.186-190
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    • 1995
  • A simple procedure, readily available at low cost with a sensitivity sufficient to determine trace levels of iron in seawater is proposed, which utilizes adsorptive accumulation of the iron/catechol complex on the mercury drop electrode in a borate medium of pH 8.0. Optimal conditions include a solution concentration of 2 mM catechol, 2.5 mM borate and a pH of 8.0, an accumulation potential of - 0.25 V is applied for 1∼3 min, and the potential scan is in the differential pulse mode. The limit of detection is 1.5 nM Fe using a preconcentration time of 3 min. The interference from copper can be eliminated and baseline slope is greatly improved, because its peak is well separated from that of iron in the proposed medium.

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A Study on Air Emission Spectra Observed by Using Electrothermal-Hollow Cathode Glow Discharge Spectrometry (Et-HCGDS) (Electrothermal-Hollow Cathode Glow Discharge Spectrometry(Et-HCGDS)를 이용하여 살펴본 Air Emission에 관한 연구)

  • Lee, Sang Chun;Shin, Jung-Sook;Kang, Mi-Ra
    • Journal of the Korean Chemical Society
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    • v.39 no.5
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    • pp.399-407
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    • 1995
  • Electrothermal-Hollow Cathode Glow Discharge Spectrometry (Et-HCGDS) has been constructed in our laboratory for in-situ monitoring of traceble amounts of rare earth elements and actinides. Et-HCGDS is the portable glow discharge system that can perform the trace analysis of elements. The main structural design of Et-HCGDS was based upon the electrothermal heating and glow discharge techniques. More details on Et-HCGDS are available elsewhere. In this study, air was used as a flow gas for the glow discharge system. As a result, the emission spectra of air were collected and the assignment of air emission lines was performed with helps of pure nitrogen and oxygen emission spectra and previously published results. We found that the emission lines of air plasma were mainly due to nitrogen molecules. This paper includes the complete assignments of the air emission lines observed by using Et-HCGDS. Also, this study will be an useful reference for spectrochemical anaysis including air analysis.

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Determination of Bio-Accumulated Trace Mercury by Anodic Stripping Square Wave Voltammetry at Glassy Carbon Electrode (유리질 탄소전극에서 양극벗김 네모파 전압-전류법에 의한 생체내 미량 수은의 정량)

  • Kim, Il Kwang;Chun, Hyun Ja;Jeong, Seung Il;Beck, Seung Hwa;Han, Wan Soo
    • Journal of the Korean Chemical Society
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    • v.45 no.4
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    • pp.298-303
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    • 2001
  • The trace-level mercury in bio-materials has been determinated by the anodic stripping square wave voltammetry (ASSWV)-technique at glassy carbon electrode. Prior to the analysis, the bio-materials were digested with $HNO_3/H_2SO_4$ mixture and KMnO4 was added to complete an oxidation process of the mixture. The detection limit of the mercury varied greatly with deposition time, deposition potential, pH and stirring rate. When the deposition was carried out for 240 sec on 400 rpm stirring at -1.0 volts vs. Ag/AgCl, the detection limit was below 0.5 ppb ($2.5{\times}10^{-9}M$). The accumulated mercury was high in the kidney and liver, and low in the brain according to the determination of mercury accumulation for a white rat by this method.

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Simultaneous Determination of Traces of Platinum and Rhodium by Differential Pulse Polarograpy (펄스 차이 폴라로그래피법에 의한 미량 백금과 로듐의 동시 정량)

  • Czae, Myoung-Zoon;Lee, Chul;Hong, Tae-Kee;Kwon, Young-Soon;Hong, Mi-Jeong
    • Journal of the Korean Chemical Society
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    • v.39 no.1
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    • pp.35-39
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    • 1995
  • Simultaneous measurements of trace platinum and rhodium, based on catalytic reduction of protons by the adsorbed Pt-formazone and Rh-formaldehyde complexes formed in formaldehyde-hydrazine-sulfuric acid medium, were demonstrated. The conditions for the measurements of Pt and Rh both present at trace levels (>10-10 M) were 0.004% (w/v) formaldehyde-0.0012% (w/v) hydrazine-0.75 M sulfuric acid. In this medium method detection limits are 7.3${\times}$10-11 M Pt and 3.2${\times}$10-11 M Rh. And dynamic ranges are 5${\times}$10-10~6${\times}$10-8 M and 1${\times}$10-10∼2${\times}$10-8 M for platinum and rhodium respectively. In the linear dynamic ranges, Rh and Ir interfere platinum in the presence of only 10 and 100 times that of Pt respectively. There are no interferences from other platinum group metal ions for rhodium even in the presence of a 500-fold excess of Ir(IV), a hundredfold excess of platinum.

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A New Analytical Method for the $Tb^{+3}$ and $Eu^{+3}$ Ions Using the Fluorescence Enhancement on the TLC Plate (TLC상에서의 형광증폭을 이용한 $Tb^{+3}$$Eu^{+3}$ 이온의 미량분석에 관한 연구)

  • Jeong, Hyuk;Lee, Gee-Yeoun;An, Seong-Hee;Kim, Hai-Dong;Lee, Won;Shin, Dae-Ho
    • Journal of the Korean Chemical Society
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    • v.39 no.1
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    • pp.40-46
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    • 1995
  • A new analytical luminescence method for the Tb+3 and Eu+3 ions was studied using the fluorescence enhancement of the ions on the TLC plate. Compared to the specific emission intensities of the ions in aqueous or ethanol solution, if spotted on the TLC plate, the line intensities were extremely enhanced. There was additional enhancement effect of the lines from the ions on the TLC plate, if treated with ο-phenanthroline. Based on the luminescence enhancement, the detection limit of the ions was lowered more than 6 order of magnitude compared to the luminescence method using solution samples. The energy-transfer mechanism was also explained for the theoretical back ground of the luminescence enhancement.

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Study on the Separation and Determination of Pure Rare Earth Oxides by Anion Exchange Resin (음이온 교환수지에 의한 고순도 희토류산화물의 분리 및 정량에 관한 연구)

  • Cha, Gi Won;Ham, Yun Beom
    • Journal of the Korean Chemical Society
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    • v.34 no.6
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    • pp.606-615
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    • 1990
  • The purity of CeO$_2$, Sm$_2$O$^{3+}$ and La2O$^{3+}$ have been determinated by separating the impurity of rare earth-elements in those oxides with anion exchange resin and measuring the absorbance of the separated element with MTB. 1 ml of the mixture solution containing each 1 mg/ml of Y$^{3+}$, Yb$^{3+}$, Eu$^{3+}$, Sm$^{3+}$, Nd$^{3+}$, Pr$^{3+}$, Ce$^{4+}$and La$^{3+}$ is loaded in top layer of anion exchange resin column, Amberlite CG400 and separated with the mixture solution of the various concentration of methyl alcohol and nitric acid as an eluent. Using the result, the impure rare earth elements in pure CeO$_2$, Sm$_2$O$^{3+}$ and La$_2$O$^{3+}$ are determinated.

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Geochemistry of the Major and Trace Elements in a Soil Profile of the Hyangdeung Area, Gwangju City, Korea (광주광역시 향등지역의 토양단면에서 주성분원소 및 미량성분원소의 지화학적 특성)

  • Shin, In-Hyun;Ahn, Kun-Sang;Kang, Jong-Hyun
    • Journal of the Korean earth science society
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    • v.26 no.8
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    • pp.800-808
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    • 2005
  • Elemental mobility during the weathering of granite in the Gwangju Hyangdeung area was investigated using ICP-MS analysis. It appeared that Al, Fe, Ti, K were lost from the profile, whereas Si, Ca, Na Mg, P and Mn were immobile during chemical weathering. In less weathered soil, large enrichment of K and Ti were found relative to Al, whereas other elements such as Si, Ca, Na, Mg and P are deplete. Fe content is constant throughout the weathered profiles. Amounts of Rb, Sr, Y, Cs, Pb, Th and U increased toward the surface. Nb, and Co have accumulated in the deepest parts of the weathered soil profile. These results agree with similar published studies. In addition, the analytical data shows that Ba and Ga increased, while Cu, Zn, Cr and Ni were relatively constant in this area. REE tend to increase in most samples, while LREEs, relative to Al, were enriched in the lower and upper saprolite. HREEs were enriched in the lower and upper saprolite.

Determination of Trace Amount of Germanium in Rocks and Sediments by Hydride Vapor Generation-ICP-AES (수소화합물 발생법-유도결합플라스마 원자방출 분광기를 이용한 암석및 퇴적물중 미량의 게르마늄 분석)

  • Shin, Hyung Seon;Choi, Man Sik;Kim, Kang Jin
    • Journal of the Korean Chemical Society
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    • v.41 no.8
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    • pp.399-405
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    • 1997
  • We examined the determination of trace amount of germanium in rocks and sediments by hydride vapor generation-ICP-AES. Germanium is formed volatile compounds with various types of acid reagents, but volatilizing of germanium was decreased in the presence of $H_3PO_4$. Sediments and rocks can be dissolved by mixed acids of $HF-HNO_3-H_3PO_4$ without volatilizing loss of germanium in open digestion system and it was possible to determine germanium by hydride generation-ICP-AES without further sample treatment. Detection limit of Ge is reached to 0.08 ppb under the condition of 5M $H_3PO_4$ and 1% $NaBH_4$ as a supporting acid and a reducing reagent, respectively. The measured values by hydride generation-ICP-AES agreed well with the reference values of SRMs as well as the values determined by solution nebulization-ICP-MS.

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Micro-Determination of D-Amino Acids in Milk by using Column Switching System (Column-Switching System을 이용한 우유속의 D-아미노산의 미량정량)

  • Lee, Sun Haing;Kim, Kyoung Hee;Lee, Young Cheol;Kim, Sang Tae
    • Journal of the Korean Chemical Society
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    • v.39 no.4
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    • pp.257-265
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    • 1995
  • Free amino acids were isolated from milk and their absolute amounts were determined by reversed phase high performance liquid chromatography after derivatization with dansyl chloride. The determination of D- and L-amino acids was based on achiral separation on a C18 column. It was found that milk contained totally 41.00 mg DL-amino acids in 100 mL milk. The level of D-amino acids to L-amino acids was determined by a column-switching system combining an achiral reversed phase separation and chiral chelate additive. The chiral separation was carried out with addition of the chiral Cu(N-benzyl-L-proline)2 chelate to the mobile phase in reversed phase liquid chromatography. It was found that the determination of 16 different amino acids is feasible in the milk sample with a C18 column separation and 12 D-amino acids out of the 16 amino acids can be determined via the column-switching system with chiral separation. 2.05% of D-glutamic acid and 2.93% of D-alanine were found in milk.

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Seasonal Variation and Natural Attenuation of Trace Elements in the Stream Water Affected by Mine Drainage from the Abandoned Indae Mine Areas (인대광산 지역 광산배수에 영향을 받은 하천에서 미량원소의 계절적인 수질변화와 자연저감)

  • Kang, Min-Ju;Lee, Pyeong-Koo;Choi, Sang-Hoon
    • Economic and Environmental Geology
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    • v.40 no.3 s.184
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    • pp.277-293
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    • 2007
  • Seasonal and spatial variations in the concentrations of trace elements, pH and Eh were found in a creek watershed affected by mine drainage and leachate from several waste rock dumps within the As-Pb-rich Indae mine site. Because of mining activity dating back to about 40 years ago and rupture of the waste rock dumps, this creek was heavily contaminated. Due to the influx of leachate and mine drainage, the water quality of upstream reach in this creek was characterized by largest seasonal and spatial variations in concentrations of Zn(up to $5.830 mg/{\ell}$), Cu(up to $1.333 mg/{\ell}$), Cd(up to $0.031 mg/{\ell}$) and $SO_4^{2-}$(up to $173 mg/{\ell}$), relatively acidic pH values (3.8-5.1) and highly oxidized condition. The most abundant metals in the leachate samples were in order of Zn($0.045-13.909 mg/{\ell}$), Fe($0.017-8.730mg/{\ell}$), Cu($0.010-4.154mg/{\ell}$) and Cd($n.d.-0.077mg/{\ell}$), with low pH(3.1-6.1), and high $SO_4^{2-}$(up to $310 mg/{\ell}$). The mine drainage also contained high concentrations of Zn, Cu, Cd and $SO_4^{2-}$ and remained constantly near-neutral pH values(6.5-7.0) in all the year. While the leachate and mine drainage might not affect short-term fluctuations in flow, it may significantly influence the concentrations of chemicals in the stream. The abundance and chemistry of Fe-(oxy)hydroxide within this creek indicated that the Fe-(oxy)hydroxide formation could be responsible for some removal of trace elements from the creek waters. Spatial and seasonal variations along down-stream reach of this creek were caused largely by the influx of water from uncontaminated tributaries. In addition, the trace metal concentrations in this creek have been decreased nearly down to the background level at a short distance from the discharge points without any artificial treatments after hydrologic mixing in a tributary. The nonconservative(i.e. precipitation, adsorption, oxidation, dissolution etc.) and conservative(hydrologic mixing) reactions constituted an efficient mechanism of natural attenuation which reduces considerably the transference of trace elements to rivers.