• Title/Summary/Keyword: 왕수

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Recovery of Tungsten from WC-Co Hardmetal Sludge by Aqua regia Treatment (WC-Co 초경합금(超硬合金) 슬러지로부터 왕수처리(王水處理)를 이용한 텅스텐의 회수(回收))

  • Kim, Ji-Hye;Kim, Eun-Young;Kim, Won-Back;Kim, Byung-Su;Lee, Jae-Chun;Shin, Jae-Soo
    • Resources Recycling
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    • v.19 no.4
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    • pp.41-50
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    • 2010
  • A fundamental study was carried out to develop a process for recycling tungsten and cobalt from WC-Co hardmetal sludge generated in the manufacturing process of hardmetal tools. The complete extraction of cobalt and simultaneous formation of tungstic was achieved by treating the sludge using aqua regia. The effect of aqua regia concentration, reaction temperature and time, pulp density on cobalt leaching and tungstic acid formation was investigated. The complete leaching of cobalt was attained at the optimum conditions: 100 vol.% aqua regia concentration, $100^{\circ}C$ temperature, 60 min. reaction time and 400 g/L pulp density. A complete conversion of tungsten carbide of the sludge to tungstic acid was however, obtained at the pulp densities lower than 150 g/L under the above condition. The progress of reaction during the aqua regia treatment of the sludge was monitored through the XRD phase identification of the residue. The metallic impurities in the tungstic acid so produced could be further removed as insoluble residues by dissolving the tungsten values in ammonia solution. The ammonium paratungstate($(NH_4)_{10}{\cdot}H_2W_{12}O_{42}{\cdot}4H_2O$) of 99.85% purity was prepared from the ammonium polytungstate solution by the evaporation crystallization method.

Removal of Iron and Phosphorus from Metallurgical Grade Silicon by Melting with Ca and Aqua Regia Leaching (칼슘 첨가(添加)-용융(溶融) 금속급(金屬級) 실리콘의 왕수(王水) 침출(浸出)에 의한 철(鐵)과 인(憐)의 제거(除去))

  • SaKong, Seong-Dae;Sohn, Ho-Sang
    • Resources Recycling
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    • v.20 no.5
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    • pp.34-39
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    • 2011
  • Metallurgical grade silicon(MG-Si) was melted with Ca at 1500$^{\circ}C$ under Ar atmosphere. The sample was cooled at 10 $^{\circ}C$/min to room temperature and leached in aqua regia. In the present study, the effect of Ca addition and conditions of acid leaching on removal of Fe and P in MG-Si were investigated. CaSi$_2$ phase was formed at the grain boundary of MG-Si melting with Ca. Also FeSi$_2$ phase was precipitated in CaSi$_2$ phase. By the formation of CaSi$_2$ phase, 97% of Fe and 66 % of P were removed from Ca added MG-Si with the particle size of 600~850${\mu}m$ by aqua regia(more than 30%) leaching.

Preparation Method for Atomic Absorption Spectrophotometry of Food Samples -Comparison of Dry, Wet and Aqua-regia Methods- (원자흡광분석(原子吸光分析)을 위한 식품시료(食品試料) 전처리방법(前處理方法) -왕수액(王水液) 처리법(處理法)과 건식(乾式) 및 습식분해법과(濕式分解法)의 비교(比較)-)

  • Woo, Soon-Ja;Ryoo, Si-Saeng
    • Korean Journal of Food Science and Technology
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    • v.15 no.3
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    • pp.225-230
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    • 1983
  • Aqua-regia method is reported for simultaneous determination of potassium, sodium, calcium, magnesium, zinc, manganese, copper and iron in high-fat fish tissue. Samples are digested with conc nitric and conc hydrochloric acid in a volumetric flask. After digestion, aqua-regia extracts of samples are analyzed by direct flame atomic absorption spectrophotometry. The aqua-regia method is compared with dry ashing method and $H_{2}SO_{4}-HNO_{3}$ method. For quantiative determination of calcium, magnesium and zinc, the aqua-regia method and dry ashing method are superior to $H_{2}SO_{4}-HNO_{3}$ method. In case of the other elements-potassium, sodium, manganese, copper and iron-the three methods gave the similar results. Because samples can be processed by aqua-regia method easily, rapidily, cheaply and safely, aqua-regia method is suitable for the routine preparation of a large number of samples simultaneously.

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Evaluation on Natural Background of the Soil Heavy Metals in Korea (우리나라 토양의 중금속 자연배경농도 평가)

  • Yoon, Jeong-Ki;Kim, Dong-Ho;Kim, Tae-Seung;Park, Jong-Gyum;Chung, Il-Rok;Kim, Jong-Ha;Kim, Hyuk
    • Journal of Soil and Groundwater Environment
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    • v.14 no.3
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    • pp.32-39
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    • 2009
  • This study was conducted in order to get the scientific background for soil pollution criteria. The 92 soil samples derived from various geological units were taken and analyzed to survey natural heavy metal background levels using aqua regia digestion method and 0.1N HCl extraction method. From these results, the average natural contents of metals were 0.287 mg/kg for Cd, 15.26 mg/kg for Cu, 18.43 mg/kg for Pb, 25.36 mg/kg for Cr, 54.27 mg/kg for Zn, 17.68 mg/kg for Ni, 6.83 mg/kg for As by the aqua regia method, and 0.040 mg/kg for Cd, 0.48 mg/kg for Cu, 3.06 mg/kg for Pb, 0.09 mg/kg for Cr, 1.54 mg/kg for Zn, 0.27 mg/kg for Ni, 0.089 mg/kg for As by the 0.1N HCl extraction method. Ratios of soluble contents and total contents were Cd 0.14, Cu 0.03, Pb 0.17, Cr 0.004, Zn 0.03, Ni 0.02, As 0.013 and the correlation coefficients of soluble contents and total contents were 0.24(As), 0.88(Cd), 0.43(Cr), 0.65(Cu), 0.70(Pb), 0.61(Ni), 0.24(Zn). The correlation factor decreased in the order of Cd > Pb > Cu > Ni > Cr > Zn $\approx$ As.

Separation of Nitric Acid and Gold from Gold Bearing Aqua Regia Solution by Solvent Extraction with TBP(tributyl phosphate) (금이 함유된 왕수용액으로부터 TBP(tributyl phosphate) 용매추출에 의한 질산과 금의 분리)

  • Bae, Mooki;Srivastava, Rajiv R.;Kim, Sookyung;Lee, Jae-chun
    • Resources Recycling
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    • v.26 no.1
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    • pp.51-58
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    • 2017
  • The present study to develop a process for extracting nitric acid and gold from aqua regia leach solution using TBP(tributyl phosphate) was conducted. The pure aqua regia was used to investigate the extractive behavior of nitric acid depending on the concentration of extractant, concentration ratio of nitric and hydrochloric acid. The extraction rate of nitric acid and gold from the gold bearing aqua regia was also examined. The theoretical extraction number was verified by counter current using the number of operations and the phase ratio obtained from McCabe-Thiele diagram. Stripping experiments were carried out for continuous recovery of nitric acid and gold in loaded organic. Considering the effect of extraction acid and gold, the simulation showed that greater than 99.9% extraction of $103.0mg{\cdot}L^{-1}$ gold and 98.0% of $151.2g{\cdot}L^{-1}$ nitric acid could be attained in a two and three-stage counter-current extraction at an O/A phase ratio of 1:0.85. Distilled water and sodium thiosulfate were used as the nitric acid and gold stripping solution. The stripping rates were 99.5% and 92.0%, respectively. The study revealed that the recovery of nitric acid and gold from gold bearing aqua regia was a plausible approach through simultaneous extraction and continuous stripping of nitric acid and gold.

Analysis of heavy metals from soils with magnetite immobilized functional groups (기능성기가 결합된 자성체를 이용한 토양의 중금속 분석)

  • Hyungsuk So;Nah, In-Wook;Hwang, Kyung-Yub
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2003.04a
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    • pp.156-156
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    • 2003
  • 유럽의 여러나라들의 경우 토양내 중금속의 허용치는 그 사용 목적에 따라 다르게 책정되고 있으며 1999년에 제정된 독일의 새로운 토양보전법에서도 토양의 사용목적별로 중금속 허용치를 달리 정하고 있다. 여기서 중금속 농도를 측정하기 위한 방법으로는 DIN(독일 공업규격)에서 정하고 있는 증류수추출법과 왕수추출법이 채택되고 있다. 그러나 이 2가지 방법들은 토양의 중금속분석에서 가장 큰 factor로 작용하는 것이 pH인데 반하여 pH가 7인 증류수와 pH가 0인 왕수를 사용함으로써 실제환경에 적용하기에는 많은 무리수를 내포하고 있으며 차츰 적당치 못한 것으로 판명되고 있다. 실질적인 중금속의 유해성 여부는 토양에서의 그 중금속의 용해도와 유동성으로 결정되는데 강한 산성비가 내린다고 가정하였을 때 비의 pH가 약 4 정도이고 이 경우 식물 뿌리 부분의 pH는 5 정도가 되므로 pH를 기준으로 할 때 잠재적으로 유동가능한 중금속을 분석하는 데에는 pH 4.5 에서 EDTA 추출이 가장 적당하고 또한 이를 토대로 토양내 중금속 허용치를 정하는 것이 합리적이라고 하겠다. 그러나 EDTA는 pH 4에서 부분적으로 Proton과 결합되어 Metal Chelate로의 능력을 잃게 되고 또한 식물 뿌리의 중금속 흡착을 Simulation할 수 없어 불리한 점이 있다. 또한 EDTA는 분해기간이 길고 인체에 해롭다는 것이 알려지고 있어 점점 사용이 어려워지고 있다. 본 연구에서는 토양에 함유된 유동가능한 중금속농도분석을 보다 적절히 하기 위한 방법으로 EDTA와 같이 Carboxyl기가 결합된 고분자 자성체를 이용해 토양의 중금속을 분석하는 것을 제안하였고 분석을 위한 중금속 추출 시 토양시료와 증류수 그리고 고분자 자성체만을 사용하여 근본적으로 토양에서 유동 가능성이 있는 중금속만을 추출하였다. 분석실험은 토양의 Cd2+ 와 Pb2+를 대상으로 행하여졌으며, 여러 토양에서 추출 분석한 결과를 EDTA분석결과와 비교하였다. 실험결과, 중금속은 매우 신속하게 고분자 자성체와 결합하였고, 그 후 자성체를 외부 자장으로 모은 후 산으로 용해시키고, 결합된 중금속은 Graphite furnace AAS로 분석함으로써 빠르고 효율적으로 분석실험을 수행할 수 있음을 알 수 있었다. 한편, 실험에서 나타난 수치들을 비교 검토한 결과 토양 분석시 sandy soil에서는 자성체를 이용한 분석이 EDTA에 의한 방법보다 더 높은 추출도를 보인 반면, silt 함량이 많은 토양의 경우에서 EDTA분석에서 더 높은 중금속 추출도를 보였다.

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Recovery of Precious Metals from Spent Catalyst Generated in Domestic Petrochemical Industry (한내 석유화학 폐촉매로부터 귀금속의 회수 연구)

  • 김준수;박형규;이후인;김성돈;김철주
    • Resources Recycling
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    • v.3 no.1
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    • pp.17-24
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    • 1994
  • Recovery of precious metal values from petrochemical spent catalyst is important from the viewpoint of environmental protection and resource recycling. Two types of spent catalysts were used in this study. One used in the manufacture of ethylene contains 0.3% Pd in the alumina substrate. The other used in oil refining contains 0.3% Pt and 0.3% Re. Both spent catalysts are roasted to remove volatile matters as carbon and sulfur. Then, metallic Pd powder from Pd spent catalyst is obtained in the course of grinding, hydrochloric acid or aqua regia leaching and cementation with iron. For the recovery of Pt and Re from Pt-Re spent catalyst, Pt and Re are leached with either HCI or aqua regia, first. Metallic Pt powder is recovered from the leach solution by cementation with Fe powder. Re in sulfide form is precipitated by the addition of sodium sulfide to the solution obtained after Pt recovery. It is found that 6N HCI can be successfully used as leaching agent for both types of spent catalyst. 6N HCI is considered to be better than aqua regia in consideration of reagent and equipment cost.

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Evaluation of Analytical Results of Heavy Metal Concentrations in Soils from the Dalsung Mine Area, Korea (달성광산지역 토양의 중금속함량 분석결과의 평가)

  • 김경웅
    • Journal of the Korean Society of Groundwater Environment
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    • v.4 no.1
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    • pp.20-26
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    • 1997
  • This paper examines the influences of mining activities on the concentrations of heavy metals in soils in the vicinity of the Dalsung Cu-W mine, Korea. Geochemical surveys were undertaken in the Dalsung mine area and sampling of surface and subsurface soils was carried out. Samples were prepared using 0.1 N HCI, HNO$_3$-HClO$_4$, and aqua regia, and analyzed for Cd, Cu, Pb and Zn by Atomic Absorption Spectrometry. In addition, soil samples were sequentially extracted to investigate the chemical speciation of heavy metals in soils. Heavy metals are highly contaminated in soils in the vicinity of mining area ranging up to 28 $\mu\textrm{g}$/g Cd, 5000 $\mu\textrm{g}$/g Cu, 2390 $\mu\textrm{g}$/g Pb and 930 $\mu\textrm{g}$/g Zn by the method using HNO$_3$-HClO$_4$. The pollution indices calculated with the permissible levels are up to 49 in surface and subsurface soils, which are considered sufficient to raise environmental problems. However, the heavy metal levels by the method using 0.1 N HCl are not higher than Korean standard for soil contamination. It suggests that analytical methods and soil standard should be re-examined. From the results of the sequential extraction methods for metal speciation, total Cu, Pb and Zn concentrations may be determined by analytical methods using HNO$_3$-HClO$_4$ or aqua regia, and exchangeable phase of those metals by the method using 0.1 N HCl.

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Application of Roasting Pretreatment for Gold Dissolution from the Invisible Gold Concentrate and Mineralogical Interpretation of their Digested Products (비가시성 금정광의 효율적 용해를 위한 소성전처리 적용과 분해 잔유물에 대한 광물학적 해석)

  • Kim, Bong-Ju;Cho, Kang-Hee;Oh, Su-Ji;On, Hyun-Sung;Kim, Byung-Joo;Choi, Nag-Choul;Park, Cheon-Young
    • Journal of the Mineralogical Society of Korea
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    • v.26 no.1
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    • pp.45-54
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    • 2013
  • In order to dissolve Au, Ag, and other valuable metals from gold ore concentrate, raw gold concentrate was pre-treated by roasting and salt-roasting at $750^{\circ}C$. The roasted concentrate was treated with aqua regia digestion to dissolve the valuable metals and higher amount of Au, Ag, and valuable metals were extracted from the roasted concentrates than from the raw concentrate. Higher amount of these metals were also extracted from the salt-roasted concentrate than from the roasted concentrate. The results of the gold dissolution experiments showed that the gold dissolution was most efficient when particle size, roasting temperature, and the percentage of added salt in salt roasting were about $181{\sim}127{\mu}m$, $750^{\circ}C$, and was 20.0%, respectively. The XRD analysis suggests that quartz and pyrite were not destroyed even through roasting at $750^{\circ}C$ and decomposition with aqua regia. However, through salt roasting, pyrite was completely decomposed, whereas quartz could not be destroyed through salt-roasting at $750^{\circ}C$ and aqua regia digestion. Accordingly, it was expected that the gold contained in quartz can not be dissolved through salt-roasting and treatment with aqua regia.

Dissolution of vanadium pentoxide using microwave digestion system for determination of vanadium by ICP-AES (ICP-AES로 바나듐 측정을 위한 마이크로파 용해 장치를 이용한 오산화바나듐 용해)

  • Choi, Kwang-Soon;Park, Yang-Soon;Kim, Yeon-Hee;Han, Sun-Ho;Song, Kyu-Seok
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.511-517
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    • 2010
  • Dissolution procedure of vanadium pentoxide, which is widely used as a catalyst for production of sulfuric acid or an oxide reaction of the numerous organic compounds, was investigated. Reagent of vanadium pentoxide was completely dissolved in aqua regia-$H_2O_2$-HF solution, but plate type of vanadium pentoxide sample was not clearly dissolved with mixed acids. Thus, in order to establish the dissolution procedure for plate type of vanadium pentoxide, the solubility of vanadium pentoxide was investigated through comparison of acid treatment-fusion and microwave digestion methods. The optimized acid for dissolution of vanadium compound was found to be mixing acids of aqua regia, $H_2O_2$ and HF. Acid-fusion and microwave digestion methods have a similar property in the solubility of vanadium compound, but the latter was more quick and convenient procedure. The content of vanadium pentoxide was found to be $97.9{\pm}0.9%$ using an inductively coupled plasma atomic emission spectrometer after dissolution of a sample with the microwave digestion system.