• Proceedings of the Korean Institute of Surface Engineering Conference
• /
• 2014.11a
• /
• pp.216-218
• /
• 2014

자동차용 고광택 크롬 도금 박리액에는 질산과 유가금속인 구리 및 니켈이 다량 함유되어 있는 것으로 알려져 있다. 질산($HNO_3$) 및 유가금속은 고가이며 유독하므로 경제적 및 친환경적으로 반드시 회수하여 재활용하여야 한다. 본 연구에서는 도금박리액으로부터 질산과 구리, 니켈을 용매 추출법을 이용하여 분리하였다. 수상에 존재하는 질산의 농도는 0.01 ~ 1N NaOH를 이용하여 적정하여 분석하고, 금속의 농도는 ICP-MS 및 ICP-AES 등을 이용하여 분석하였다. 도금 박리액을 분석한 결과 Cu(76850mg/L), Ni(51990 mg/L)이 함유되어 있음을 알 수 있었다. 용액 내 질산의 양을 NaOH 용액을 이용하여 적정법으로 측정하였을 때, 질산의 양은 대략 1.02 M 임을 알 수 있었다. 50 % Tributylphosphate (TBP)를 이용하여 3단 추출한 유기층의 용액을 증류수를 이용하여 3회의 역추출을 하였을 때, 원액으로부터 48.1 %의 질산을 회수할 수 있음을 알 수 있었으며, 순도는 99.5% 이상이었다. 질산 회수 후 용액 내에 남은 구리와 니켈은 ISE-106로 구리를 추출하여 니켈을 분리한 후 황산을 이용해 역추출 하였다. 회수된 구리는 NaOH를 이용하여 pH를 조절하고 수산화구리 형태로 침전시킨 후 $N_2H_4$를 이용하여 환원시켰고, 온도와 pH 및 환원제를 이용하여 다양한 조건 하에 구리 분말을 제조하였다. 구리를 추출하여 라피네이트 용액으로 분리된 니켈은 $NaBH_4$를 이용하여 환원시켰고, 다양한 조건 하에서 니켈 분말을 제조하였다. 환원 된 분말은 분석결과 99%의 순수한 분말임을 알 수 있었다.

• Bulletin of the Korean Chemical Society
• /
• v.29 no.2
• /
• pp.417-421
• /
• 2008

The efficient synthesis of four mesitylene-based receptors 1-4 and their potentiometric response characteristics to alkali metal, alkaline earth metal, and transition metal ions, under various pH conditions are outlined. Receptor 1-based electrode exhibited more sensitive response to Ag+ ion (49 mV/decade of range from 10-6 to 10-2 M) than the 2-based electrode (47 mV/decade of range from 3 ´ 10-5 to 10-2 M), while the 3- and 4-based ones revealed sub-Nernstian below 40 mV/pAg+. All electrodes showed substantial responses to Ag+ ion under acidic condition, but there was almost nil-response to other transition metal ions (Fe2+, Co2+, Zn2+, Ni2+, Pb2+, Cd2+, Cu2+ and Hg2+). The association constant of receptor 1 toward Ag+ ion, measured by 1H NMR titration, showed the largest value (200 M-1) among the tested receptors. The results were interpreted with semi empirically-modeled structures.

• Analytical Science and Technology
• /
• v.19 no.4
• /
• pp.309-315
• /
• 2006

Two piperazine-templated metal sulfate complexes, $(C_4N_2H_{12})[Ni(H_2O)_6](SO_4)_2$, I and ($C_4N_2H_{12}$) $[Co(H_2O)_6](SO_4)_2$, II, have been synthesized by hydro/solvothermal reactions and their crystal structures analyzed by single crystal X-ray diffraction methods. Complex I crystallizes in the monoclinic system, $P2_1/n$ space group, a=12.920(3), b=10.616(2), $c=13.303(2){\AA}$, ${\beta}=114.09(1)^{\circ}$, Z=4, $R_1=0.030$ for 3683 reflections; II: monoclinic $P2_1/n$, a=12.906(3), b=10.711(2), $c=13.303(2){\AA}$, ${\beta}=114.10(2)^{\circ}$, Z=4, $R_1=0.032$ for 4010 reflections. The crystal structures of the piperazine-templated metal(II) sulfates demonstrate zero-dimensional compound constituted by diprotonated piperazine cations, metal(II) cations and sulfate anions. The structures of complex I and II are substantially isostructural to that of the previously reported our piperazine-templated copper(II) sulfate complex $(C_4N_2H_{12})[Cu(H_2O)_6](SO_4)_2$. The central metal(II) atoms are coordinated by six water molecules in the octahedral geometry. The crystal structures are stabilized by three-dimensional networks of the $O_{water}-H{\cdots}O_{sulfate}$ and $N_{pip}-H{\cdots}O_{sulfate}$ hydrogen bonds between the water molecules and sulfate anions and protonated piperazine cations. Based on the results of thermal analysis, the thermal decomposition reactions of the complex I was analyzed to have three distinctive stages whereas the complex II proceed through several stages.

• Korean Journal of Environmental Agriculture
• /
• v.20 no.1
• /
• pp.20-27
• /
• 2001

Stream water chemistry in the abandoned Boeun Jeil coal mine area was studied for a period of 3 months, including rainy and dry season. The stream waters were a nearly neutral and slightly alkali condition, and $Mg-SO_4$ type with Mg>Ca>Na>K and $SO_4>HCO_3>Cl>NO_3$. Chemical composition of the stream water was quite irregular during the experimental period. Concentrations of Na, K, $HCO_3$, U, Sr, and Cr decreased by $10{\sim}30%$ during rainy season, caused by dilution effects with rain. The concentration of Ca, Mg, $NO_3$, Cd, and Co increased during the rainy season, caused by more easily dissolved from bedrocks or mine drainage with slightly acidic condition than dry season. The stream water was enriched in Mg, Ca, $HCO_3$, $SO_4$, Al, Fe, Zn, Ni, Co, Cr, Cd, Sr and U. Concentrations of Na, Mg, Ca, $SO_4$, $HCO_3$, Fe, Zn, Ni, Sr, and U decreased linearly with distance from the mine adit. These elements were strongly controlled by dilution of unpolluted water influx and/or adsorption on the clay minerals and iron oxyhydroxide precipitates. This mine area exhibited two main weathering processes ; 1) oxidation with acidification derived from Fe sulphides, and 2) pH buffering due to Ca and Mg carbonate dissolution. This weathering processes were followed by adsorption of metals on iron oxyhydroxides and precipitation.

• Korean Journal of Environment and Ecology
• /
• v.26 no.5
• /
• pp.694-706
• /
• 2012

The purpose of this study was to offer the raw data for conservation and restoration of aquatic ecosystem by surveying and analysing a water quality, sediment, benthic macroinvertebrate, fish and hydrophyte in Junam reservoir. In the result of analysing the water quality, pH was 8.2~8.4, 6.0~7.5mg/${\ell}$ in COD, 10.0~10.3mg/${\ell}$ in SS, 8.3~11.5mg/${\ell}$ in DO, 0.1mg/${\ell}$ in T-P and 1.2~1.3mg/${\ell}$ in T-N. In case of the sediments, Cd was 0.47~0.52mg/kg, 7.08~7.43mg/kg in Cu, 0.22~0.32mg/kg in As, 0.02~0.03mg/kg in Hg, 6.20~7.45mg/kg in Pb, 32.80~39.70mg/kg in Ni, 513.0~543.0mg/kg in F and 137.0~140.0mg/kg in Zn. $Cr^{6+}$ was not detected. The benthic macroinvertebrates were 432 individuals including 3 phyla, 5 classes, 9 orders, 26 families, 33 genera and 39 species, and the ecological score of benthic macroinvertebrate community(ESB) was 25. The fishes were 8 families and 14 species, and the invasive alien species were 2 taxa including Micropterus salmoids and Lepomis macrochirus. The hydrophytes were 63 taxa including 28 families, 42 genera, 56 species, 1 subspecies and 6 varieties. The emergent plants were 38 taxa(60.3%), 5 taxa(7.9%) in floating-leaved plants and each 10 taxa(15.9%) in free-floating plants and submerged plants.

• Analytical Science and Technology
• /
• v.17 no.3
• /
• pp.199-210
• /
• 2004

A new polystyrene-divinylbenzene chelating resin containing 4,5-dihydroxy-naphthalene-2,7-disulfonic acid (chromotropic acid : CTA) as functional group has been synthesized and characterized. The sorption and desorption properties of this chelating resin for Cr(III) ion and Cr(VI) ion including nine metal bloodstain. As a results, FOB test kit could be effectively applied to identification of human blood at chelating resin was stable in acidic and alkaline solution. The Cr(VI) ion is selectively separated from Cr (III) ion at pH 2 and the maximum sorption capacity of Cr(VI) ion is 1.2 mmol/g. In the presence of anions such as $F^-$, $SO{_4}^{2-}$, $CN^-$, $CH_3COO^-$, $NO{_3}^-$, the sorption of Cr(VI) ion was reduced but anions such as $PO{_4}^{3-}$ and $Cl^-$ revealed no interference effect. The elution order of metal ions obtained from breakthrough capacity and overall capacity at pH 2 was Cr(VI)>Sn(II)>Fe(III)>Cu(II)>Cd(II)${\simeq}Pb(II){\simeq}Cr(III){\simeq}Mn(II){\simeq}Ni(II){\simeq}Al(III)$. Desorption characteristics for Cr(VI) ion was investigated with desorption agents such as $HNO_3$, HCl, and $H_2SO_4$. It was found that the ion showed high desorption efficiency with 3 M HCl. As the result, the chelating resin, XAD-16-CTA was successfully applied to separation and preconcentration of Cr (VI) ion from several metal ions in metal finishing works.

• Resources Recycling
• /
• v.9 no.4
• /
• pp.16-27
• /
• 2000

In order to produce raw material powder of advanced magnetic material by spray roasting process, newly modified spray roasting system was developed in this work. In this spray roasting system, raw material solution was effectively atomized and sprayed into the reaction furnace. Also, uniform temperature distribution inside reaction furnace made thermal decomposition process fully completed, and produced powder was effectively collected in cyclone and bag filter. This system equipped with apparatus which can purify hazard produced gas. In this study complex acid solution was prepared by dissolution of mill scale and ferro-Mn into the acid solution, and the pH of this complex acid solution was controlled about to 4. It was conformed that mill scale and ferro-Mn containing a lot of impurities such as $SiO_2$, P and Al could be used as raw material by reducing the impurities content of complex acid solution below 20 ppm. Complex oxide powder of Fe-Mn system was produced by spraying purified complex acid solution into the spray roaster through nozzle, and the variations of produced powder characters were studied by changing he reaction conditions such as reaction temperature, the injection velocity of solution and air, nozzle tip size and concentration of solution. The morphology of produced powder had spherical shape under the most experimental conditions, and concentration of solution. The morphology of produced powder has spherical shape under the most experimental conditions, and the composition and the particle size distribution were almost uniform, which tells the excellence of this spray roasting system. The grain size of most produced powder was below 100 nm. From the above results, it will be possible to produce ultra fine oxide powder from the chloride of Fe, Mn, Ni, Cu and rare earth by using this spray roasting system, and also to produce ultra fine pure metal powder by changing reaction atmosphere.

• Journal of the Korean Society of Marine Environment & Safety
• /
• v.28 no.1
• /
• pp.1-9
• /
• 2022

The effect of sediments in a waste dumping area on marine organisms was evaluated using sediment toxicity tests with a benthic amphipod (Monocorophium acherusicum) and bioluminescent bacterium (Vibrio fischeri) in accordance with the Korean Standard Method for Marine Wastes (KSMMW). Nine sites in the East Sea-Byeong, East Sea-Jeong, and Yellow Sea-Byeong areas were sampled from 2016 to 2019. The test results showed that the relative average survival rate (benthic amphipods) and relative luminescence inhibition rate (luminescent bacteria) were below 30%, which were judged to be "non-toxic." However, in the t-test, a total of 12 benthic amphipod samples (6, 1, 1, and 4 in 2016, 2017, 2018, and 2019, respectively) were significantly different (p<0.05) from the control samples. To identify the source of toxicity on benthic amphipods, a simple linear regression analysis was performed between the levels of eight heavy metals (Cr, As, Ni, Cd, Cu, Pb, Zn, and Hg) in sediments and the relative average survival rate. The results indicated that Cr had the highest contribution to the toxicity of benthic amphipods (p = 0.000, R2 = 0.355). In addition, Cr was detected at the highest concentration at the DB-85 station and exceeded the Marine Environment Standards every year. Although the sediments were determined as "not toxic" according to the ecotoxicity criteria of the KSMMW, the results of the statistical significance tests and toxicity identification evaluation indicated that the toxic effect was not acceptable. Therefore, revising the criteria for determining the toxic effect by deriving a reference value through quantitative risk assessment using species sensitivity distribution curves is necessary in the future.

• Journal of Conservation Science
• /
• v.32 no.1
• /
• pp.33-42
• /
• 2016

Modern cultural heritage were made with various materials. But there are no certain analysis for modern cultural heritage. Analysis on rickshaw from National Museum of Korean Contemporary History were carried out using P-XRF, species identification, paint film analysis, FT-IR and microscope observation. As a result Copper and Zinc were measured in metal parts. Nickel alloys were first used in the modern era for rickshaw. Wooden parts, Oak(Quercus spp.), bamboo(Phyllostachys spp.) and Hinoki cypress(Chamaecyparis spp.) were identified. Outer films were painted by 5 layers and inner films were painted by 3 layers. More simple painting process were performed on the inner part. Cotton and wool were identified by FT-IR. Also, cowhide were identified. Authenticity conservation and restoration could be carried out with the results.

• Analytical Science and Technology
• /
• v.10 no.3
• /
• pp.187-195
• /
• 1997

Chemically modified electrodes(CMEs) for Ag(I) were constructed by incoporating 1,5,9,13-tetrathiacyclohexadecane([16]-ane-$S_4$) with a conventional carbon-paste mixture composed of graphite powder and nujol oil. Ag(I) ion was chemically deposited onto the surface of the modified electrode with [16]-ane-$S_4$ by immersion of the electrode in the acetate buffer solution(pH=4.5) containing $5.0{\times}10^{-4}M$ Ag(I) ion. And then the electrode deposited with Ag(I) was reduced at -0.3V vs. S.C.E. Well-defined stripping voltammetric peaks could be obtained by scanning the potential to the positive direction. The CME surface was regenerated with exposure to 0.1M $HNO_3$ solution and was reused for the determination of Ag(I) ion. When deposition/measurement/regeneration cycles were 10 times, the response could be reproduced with relative standard deviation of 6.08%. In case of differential pulse stripping voltammetry, the calibration curve for Ag(I) was linear over the range of $5.0{\times}10^{-7}{\sim}1.5{\times}10^{-6}M$. And the detection limit was $2.0{\times}10^{-7}M$. Various ions such as Cd(II), Ni(II), Pb(II), Zn(II), Mn(II), Mg(II), EDTA, and oxalate(II) did not influence the determination of Ag(I) ion, except Cu(II) ion.