• 한국환경보건학회지
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• 제31권1호
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• pp.73-78
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• 2005

A determination method of trace Ni(II) and Zn(II) in aqueous solution was studied and developed by adsorbing on titanium dioxide. For this purpose, several conditions were optimized such as the pH of sample solution, adsorption time, the types and concentration acid, and desorption time. The titanium dioxide was added in sample solution which was pH adjusted. Then, the sample solution was stirred for 5 minutes. This mixture was stored in room temperature for 30 minutes to allow adsorption. After filtering and washing the titanium dioxide, the analytes were dissolved from the titanium dioxide on membrane filter by an ultrasonic vibration for 10 minutes in 1.0 M $HNO_3$ solution. Then, this sample solution was analysed using ICP-AES. The adsorption equilibrium was achieved in 30 minutes. The desorption was the most of effective with 1.0 M(mol/l) nitric acid solution, and desorption time was 10 minutes. This procedure was applied for the analysis of two real samples, i.e., brown seaweed and tangle. The recoveries of Ni(II) and Zn(II) in spiked samples were 89.4${\sim}$98.9% for analytes.

• 분석과학
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• 제11권3호
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• pp.174-178
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• 1998

Formaldehyde와 resorcinol을 반응시켜 chelating 수지를 제조하였다. 이 수지는 Pb(II)나 Ni(II)와 같은 전이금속에 대해 높은 흡착능을 나타내었다. Pb(II), Ni(II), Co(II), Fe(II)와 Zn(II)의 흡착과 탈착율을 batch법으로 구하였다. 이 수지의 중요한 특성은 금속 이온과 수지의 수소 이온간의 교환과정이다. 금속이온의 흡착과 탈착의 메카니즘은 수지의 작용기인 수소 이온의 탈착과 금속 이온간의 교환반응으로 생각된다. 이 수지를 이용하여 전이금속을 농축시키고, 다른 이온들로부터 Pb(II)를 분리하는데 적용해 보았다.

• Bulletin of the Korean Chemical Society
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• 제32권2호
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• pp.444-450
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• 2011

A novel method that utilizes poly(5-methyl-2-thiozyl methacrylamide-co-2-acrylamido-2-methyl-1-propanesulfonic acid-co-divinylbenzene) [MTMAAm/AMPS/DVB] as a solid-phase extractant was developed for simultaneous preconcentration of trace Cd(II), Co(II), Cr(III), Cu(II), Fe(III), Mn(II), Ni(II), Pb(II), and Zn(II) prior to the measurement by flame atomic absorpiton spectrometry (FAAS). Experimental conditions for effective adsorption of the metal ions were optimized using column procedures. The optimum pH value for the simultaneously separation of the metal ions on the new adsorbent was 2.5. Effects of concentration and volume of elution solution, sample flow rate, sample volume and interfering ions on the recovery of the analytes were investigated. A high preconcentration factor, 100, and low relative standard deviation values, $\leq$1.5% (n = 10), were obtained. The detection limits (${\mu}gL^{-1}$) based on the 3s criterion were 0.18 for Cd(II), 0.11 for Co(II), 0.07 for Cr(III), 0.12 for Cu(II), 0.18 for Fe(III), 0.67 for Mn(II), 0.13 for Ni(II), 0.06 for Pb(II), and 0.09 for Zn(II). The validation of the procedure was performed by the analysis of two certified reference materials. The presented method was applied to the determination of the analytes in various environmental samples with satisfactory results.

• 한국표면공학회지
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• 제37권2호
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• pp.99-109
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• 2004

The effect of trace metallic additives on microstructure, glossiness and hardness of Zinc electrodeposits was investigated by using sulfate bath and flow cell system. The preferred orientation of Zn deposits with Mg-Fe additives was (10$\ell$)+(002) mixed texture, while that of Zn deposits with Mg-Fe-Cr additives was ( $10\ell$). The preferred orientation of Zn deposits with Mg-Fe-X(X:Ni,Co) additives changed from ($10\ell$)+(002) to ($10\ell$) with increasing Mg additive from 5 to 10 g/$\ell$. The surface morphology of the Zinc deposits was closely related to the preferred orientation of the deposits. The glossiness of Zn deposits with Mg-Fe additives was similar to that of pure Zn deposit. The glossiness of Zn deposits with Mg-Fe-X(X:Ni,Cr) additives was lower than that of Zn deposits with Mg-Fe additives, while that of Zn deposits with Mg-Fe-Co additives was higher than that of Zn-Mg-Fe deposits. The hardness of Zn deposits with Mg-Fe-X(Ni,Co,Cr) increased with current density and amount of Mg additive. Hardness of Zn deposits was decreased and increased in comparison with Zn-Mg-Fe deposits for Mg-Fe-Co and Mg-Fe-Cr additives, respectively.

• 한국환경보건학회지
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• 제24권3호
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• pp.1-5
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• 1998

A spectrophotometric method was developed for the acidic solution stripped after an extraction of 0.5 to 2.5 ppm of Lead(II) from 50 mL of $Na_2S_2O_3$ solution into chloroform as the ion-pairs formed between their thiosulfate complexes and alkylamine, Aliquat336. Pb(II) in the stripped solution forms an complex with DDTC in pH 7.3 buffer solution, and was developed in yellow by copper replacement. The ydlow-colored solution have the maximum absorbance at 435 nm in the measurement of absorbance by UV-Visible spectrophotometer. The interference ions such as Fe(III), Hg (II), Al(III), Co, Cu, Ni, Zn, Ca, Sn, have great effects on the extraction, but they were overcomed by the usage of adequate masking agents before an extraction. At last, a good result was obtained in applying this method to synthetic water.

• 분석과학
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• 제9권4호
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• pp.364-372
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• 1996

해수 중 U(VI) 등과 같은 미량 금속이온의 선택적인 분리, 농축 및 회수를 위하여 XAD-16-[2-(2-thiazolylazo)-p-cresol](TAC)형 킬레이트 수지에 대한 몇 가지 금속이온의 흡착 및 탈착 특성을 용리법으로 조사하였다. 금속이온의 흡착에 미치는 흐름속도, pH 및 완충 용액의 농도에 대한 영향을 조사하여 흡착 최적 조건을 결정하였다. 킬레이트 수지에 대한 금속이온의 총괄 흡착 용량을 조사한 결과 각각 0.41mmol U(VI)/g resin, 0.55mmol Th(IV)/g resin, 0.43mmol Cu(II)/g resin 및 0.32mmol Zr(IV) /g resin이었다. pH 5.0에서 돌파점 용량과 총괄 용량으로부터 얻은 금속이온의 용리 순서는 Th(IV)>Cu(II)>U(VI)>Zr(IV)>Pb(II)>Ni(II)>Zn(II)>Cd(II)>Mn(II)이었다. $HNO_3$, HCl, $HClO_4$, $H_2SO_4$ 및 $Na_2CO_3$ 등의 탈착제에 의한 탈착특성을 조사한 결과 Zr(IV)을 제외한 대부분의 금속이온들에 대하여 2M $HNO_3$이 탈착효율이 높게 나타났으며, 1M $H_2SO_4$ 용액을 사용하면 Zr(IV)의 탈착 및 회수가 가능하였다. 또한 킬레이트수지를 이용하여 미량의 U(VI) 이온이 함유된 인공 해수 시료를 용리시키고 회수한 결과 96% 이상의 높은 회수율을 나타내었다.

• 분석과학
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• 제10권4호
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• pp.282-290
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• 1997

XAD-16-[4-(2-thiazolylao)]orcinol (TAO)형 킬레이트 수지에 대한 U(VI), Tb(IV), Zr(IV), Cu(II), Pb(II), Ni(II), Zd(II), Cd(II) 및 Mn(II) 이온의 흡착 및 탈착 특성을 용리법으로 조사하였다. 각 금속이온의 총괄용량과 pH 변화에 따르는 혼합 금속이온의 분리능 및 금속이온의 최적 흡착 조건을 조사하기 위하여 금속이온의 흡착에 미치는 흐름속도, 완충용액의 농도에 대한 영향을 검토하였다. 킬레이트 수지에 의한 금속이온의 총괄 흡착 용량은 각각 0.35nmol U(VI)/g resin, 0.49nmol Th(VI)/g resin, 0.41nmol Cu(II)/g resin 및 0.31nmol Zr(IV)/g resin이었다. 그리고 pH 5.0에서 돌파점 용량과 총괄 용량으로부터 얻은 금속이온의 용리순서는 Th(IV)>Cu(II)>U(VI)>Zr(IV)>Pb(II)>Ni(II)>Zn(II)>Mn(II)>Cd(II)이었다. 흐름속도 0.28mL/min 및 pH 2~5범위에서 혼합 금속이온을 분리한 결과 pH가 증가함에 따라 이들 이온의 군분리가 가능하였다. 한편, $HNO_3$, HCl, $HClO_4$, $H_2SO_4$ 및 $Na_2CO_3$ 등의 탈착제에 의한 탈착특성을 조사한 결과 2M $HNO_3$는 Zr(IV)을 제외한 대부분의 금속이온들은에 대하여 높은 탈착효율을 나타냈으며, 1M $H_2SO_4$ 용액을 사용하면 Zr(IV)의 탈착 및 회수가 가능하였다. 또한 킬레이트 수지를 이용하여 미량의 U(VI) 이온이 함유된 인공 해수 시료를 용리시키고 회수한 결과 94%이상의 높은 회수율을 나타내었다. 아울러 XAD-16-TAO 킬레이트 수지는 희토류 금속의 혼합시료를 2M $HNO_3$ 용액으로 용리시키면 U(VI)의 선택적인 분리, 농축 및 회수에 유용함을 알 수 있었다.

• Bulletin of the Korean Chemical Society
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• 제24권12호
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• pp.1775-1780
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• 2003

A continuous flow system has been developed to determine trace Cu(II), Mn(II), Ni(II) and Zn(II) in a large volume of water samples by a solvent sublation technique. The mixed solution of 1,10-phenanthroline(phen) and thiocyanate ion was used as ligands for the formation of their ternary complexes. The continuous system was constructed in this laboratory with a peristaltic pump, a mini shaker, three mixing bottles and a flotation cell by connecting each part with a polyethylene tube. The flotation conditions such as the flow rate of sample solution and the injection rates of ligand, buffer and surfactant solutions have been investigated to obtain the best sublation efficiencies. Each solution flowed into the flotation cell through each polyethylene tube by the peristaltic pumps. The ternary complexes were floated and extracted into MIBK in a flotation cell of 2 L by bubbling a nitrogen gas. The absorbances of extracted analytes in MIBK were directly measured by graphite furnace-AAS. The concentrations of 1,10-phenanthroline and thiocyanate ion were $2.6\;{\times}\;10^{-3}$ M and $2.3\;{\times}\;10^{-2}$ M in the mixed solution, respectively. The pH of sample solution was adjusted to 5.0 with a buffer solution and 1%(m/v) sodium lauryl sulphate solution was added as a surfactant to support the effective flotation of the complexes. The $N_2$ gas was bubbled at 30 mL/min for 90 minutes for 20 L of sample. Reproducible results of less than 10% RSD and recoveries of 80-120% could be obtained in real samples.

• 약학회지
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• 제4권1호
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• pp.8-11
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• 1959

The method for the estimation of trace elements in hair is studied on this paper modifying the circular paper chromatography method shown by Giri and Balakrishnan for the estimation of vitamins from the multivitamin preparation. The elements studied are Ni, Al, Mn, Mg, Zn, Ca, Co, Cu, and Fe. The content of the element is estimated quantitatively by comparison the size and the color density of spots of the standard chromatogram prepared by the known amount of each standard substance and the chromatogram prepared from sample solution, after checking those chromatogram qualitatively. The comparative study has been made between the results from this method and the results from the other methods which are applying routinely at this laboratories. The experimental errors at each elements were within 10% limits. There was no interference between each elements. It is recommendable that this method can be applied to treat numerous speciemens saving times within experimental error of 10%.

• 자원환경지질
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• 제40권5호
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• pp.587-604
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• 2007

회동저수지의 호저퇴적물에 대하여 미량원소의 심도별 변화와 존재형태 및 이들의 상관관계에 대해서 알아보고자 하였다. 회동저수지의 5개 지점에서 깊이 21-41cm의 코어와 간극수를 채취하였다. 회동저수지 퇴적물 내 미량원소의 평균 총함량은 Zn $232{\pm}30.8mg/kg$, Cu $119{\pm}272mg/kg$, Pb $58.4{\pm}4.1mg/kg$, Ni $15.7{\pm}3.3mg/kg$ 및 Cd $1.6{\pm}0.3mg/kg$이었다. 회동저수지 안쪽으로 가면서 호저퇴적물 내 미량원소 함량이 감소하는 경향이 관찰되었다. 깊이에 따른 함량 변화는 시료채취 위치에 상관없이 Mn, Pb 및 Zn는 감소하는 반면, Cu와 Fe는 증가하였다. 간극수에 용해된 미량원소의 함량은 Fe>Mn>Cu>Zn의 순으로 낮았고 Cd, Ni 및 Pb는 검출되지 않았다. 간극수에 용해된 Zn, Cu, Fe 및 Mn 함량은 퇴적층의 하부로 가면서 증가하는 경향을 보여주고 있으며, 이는 상부로 미량원소가 확산되고 있음을 의미한다. 이러한 미량원소의 이동은 퇴적물-물과의 경계부분까지 전달될 것이며, 퇴적층 상부에서 비정질 철 및 망간 산화광물과 탄산염광물에 의하여 흡착되고 있다. 겉보기 분산계수 값을 이용한 결과, 각 미량원소의 상대적인 이동도는 Mn>Cu>Zn>Fe순이다. 연속추출결과, 미량원소의 표면집적이 비정질 산화광물형태와 탄산염광물 수반형태에 기인된 것임을 확인하였다. Cu, Fe, Mn 및 Zn의 간극수 내 함량은 호저퇴적물의 양이온교환형태와 밀접한 상관관계가 있음이 관찰되었다.