• Bulletin of the Korean Chemical Society
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• v.14 no.6
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• pp.696-700
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• 1993

Gold bonding wire of 0.076 mm in diameter used in semiconductor industry, is dissoved in aqua regia. The solution is then evaporated to near dryness several times with a few drops of HCl added to prepare the final sample solution in 5% HCl. The gold matrix is separated from trace impurities by controlled potential deposition. The whole electrolysis has been carried out inside a clean bench. An optimum potential is found to be +0.25 V to give more than 99.9% Au matrix removal with better than 90 analytes remaining in the electrolyte solution. Isotope dilution calibration is employed to get the best accuracy and precision. Analytical results are presented with determination limits of the analytical method.

• Journal of the Mineralogical Society of Korea
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• v.23 no.4
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• pp.281-295
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• 2010

This paper deals with magnetic susceptibility, mineralogy, soil properties (pH, EC, CEC, loss on ignition), iron and manganese oxides, the content and partitioning of heavy metals (As, Cd, Cr, Cu, Ni, Pb, Zn), and their mutual relationship in the soil samples of an unpolluted, abandoned mine area, and industrial complex area. The various minerals derived from weathered bedrock were identified by X-ray diffraction in the unpolluted soil samples, except for the magnetic minerals. XRD analysis also revealed the existence of hematite and magnetite related to mine tailings and waste rocks in the abandoned mine area samples. The industrial complex area samples had carbonate minerals, such as calcite and dolomite, that might be due to anthropogenic deposition. The sum of the reducible, oxidizable, and residual fractions was over 80% for the abandoned mine area samples and over 50% for the industrial complex area samples using the sequential extraction method. The industrial complex area samples had a relatively high carbonate fraction that was associated with carbonate minerals. The content of aqua regia-extractable Fe, Mn, As, and Zn had a high positive correlation with the content of the dithionite-citrate-bicarbonate (DCB)-extractable method related to Fe/Mn oxide phases. The 54% and 58% of aqua regia-extractable Fe and As content, respectively, acted together with the concentrations of the DCB-extractable phases. Magnetic susceptibility values of total samples ranged from 0.005 to $2.131{\times}10^{-6}m^3kg^{-1}$. The samples including iron oxide minerals, such as hematite and magnetite, had a high magnetic susceptibility. The magnetic susceptibility showed a significant correlation with the heavy metals, Cd (r=0.544, p<0.05), Cr (r=0.714, p<0.01), Ni (r=0.645, p<0.05), Pb (r=0.703, p<0.01), and Zn (r=0.496, p<0.01), as well as Fe (r=0.608, p<0.01) and Mn (r=0.615, p<0.01). The aqua regia-extractable Fe and Mn content had a significant positive correlation with Cd, Cr, Cu, Ni, and Zn. However, the DCB-extractable Fe and Mn content had a significant positive correlation with As and Ni, indicating that the heavy metals were associated with Fe and Mn oxide minerals.

• 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.

• Applied Chemistry for Engineering
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• v.10 no.4
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• pp.568-575
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• 1999

Two different digestion procedures for the simultaneous determination of major and platinum-group element(PGE) in spent automobile catalysts containing PGE and silicates by inductively coupled plasma atomic emission spectrometry(ICP-AES) are compared. Combinations of mixed aids using HF, $HNO_3$, HCl, $HClO_4$, $H_2O_2$, and $H_3BO_3$ are utilized for the hot plate dissolution method and the closed-vessel microwave digestion method, The latter method has been shown to be relatively superior in terms of recovery, analysis time, and amount of aqua regia (3 parts HCl + part $HNO_3$ required to dissolve PGE in comparison with conventional open vessel hot-plate dissolution. The best results were drawn from the following conditions: In closed Teflon PFA vessels under microwave heating with temperature/pressure regulation, a 0.25 g portion of sample was digested in 2 mL of HF, 2 mL of $HNO_3$ and 6mL of HCl under the pressure of 200 psi(13.79 bar) at $180^{\circ}C$ for 1hr, followed by a second digestion stage with 16 mL of 5%(w/v) boric acid under the pressure of 20 psi(1.38 bar) at $100^{\circ}C$ for 10 min. After the microwave heating, the sample was post-treated with 10 mL of aqua regia twice by hot-plate heating. This condition gives the PGE recovery within 85~110% and the relative standard deviations within 2%. The method developed can therefore be regarded as an alternative method for routine analysis of spent automobile catalysts.

• Economic and Environmental Geology
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• v.53 no.3
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• pp.297-306
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• 2020

The red mud generated from bauxite during the Bayer alumina production process has been regarded as an industrial waste due to the high alkaline property and high content of Na. Despite of its environmental problem, various studies for recovery of the valuable resources from red mud has been also carried out because of high content (25.7 wt.% as Fe₂O₃ in this study) of iron in red mud. In order to recover the iron resource in the red mud, microwave heating experiments were performed with adding of activated carbon and elemental sulfur to the red mud. Through the microwave heating the powdered red mud mixtures converted to porous and vitrified solid aggregates. The vitrified aggregates produced by microwave heating are composed of goethite, zero valent iron (Fe⁰), pyrrhotite and pyrite. And then, the microwave heating samples were dissolved in the aqua regia solution, and Fe precipitates were obtained as a Fe-chlorides by adding of NaCl salt in the aqua regia solution. The Fe recovery rates in the Fe-chloride precipitates showed differences depending on the experimental mixture conditions, and Fe grades of the end products are 49.0 wt.%, 58.0 wt.% and 59.5 wt.% under mixture conditions of red mud, red mud + activated carbon, and red mud + activated carbon + elemental S, respectively. The Fe content of 56.0 wt.% is generally known as the grade value of Fe in a iron ore for iron production, and the Fe grades of microwave heating samples with adding activated carbon and elemental S in this study are higher than the grade value of 56.0 wt.%.

• 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.

• Economic and Environmental Geology
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• v.47 no.6
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• pp.645-655
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• 2014

In order to obtain pure metallic Te from gold concentrate, roasting treatment, hypochlorite leaching, Fe removal and electrolysis experiments were carried out. The contents of Au, Ag and Te from the concentrate sample and roasted sample were much more soluble in the hypochlorite solution than in aqua regia digestion, whereas the metals Pb, Zn, Fe and Cu were easier to leach with the aqua regia than the hypochlorite. With the addition of NaOH in the hypochlorite leaching solution prior to electrolysis, the Fe removal rate achieved was only 96% in the concentrate sample, while it reached 98% in the roasted sample. The results of electrolysis for 240 min, 98% of the metallic copper was recovered from the concentrate sample, while 99% was obtained from the roasted sample due to the removal of S by roasting. The amount of anode slime was also greater in the electrolytic solution with the roasted sample than with the concentrate sample. The results on the anode slime after the magnetic separation process showed the amount of metallic pure native tellurium recovered was greater in the roasted sample than in the concentrate sample.

• Resources Recycling
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• v.27 no.6
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• pp.23-29
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• 2018

Recently rapid economic growth and technological development have led to an increase in the generation of waste electrical and electronic equipment (WEEE). As the amount of electric and electronic waste generated increases, the importance of processing waste printed circuit boards (PCB) is also increasing. Various studies have been conducted to recycle various valuable metals contained in a waste PCB in an environmentally friendly and economical manner. To get anode slime containing Ag and Au, Anode copper prepared from PCB scraps was used by means of electro-refining. Ag and Au recovery was conducted by leaching, direct reduction, and ion exchange method. In the case of silver, the anode slime was leached at 3 M $HNO_3$, 100 g/L, $70^{\circ}C$, and Ag was recovered by precipitation, alkali dissolution, and reduction method. In the case of gold, the nitrate leaching residues of the anode slime was leached at 25% aqua regia, 200 g/L, $70^{\circ}C$, and Au was recovered by pH adjustment, ion exchange resin adsorption, desorption and reduction method. The purity of the obtained Au and Ag were confirmed to be 99.99%.

• Analytical Science and Technology
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• v.20 no.6
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• pp.516-523
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• 2007

Purification of silica mineral has been investigated by acid leaching of pulverized silica. A series of studies has been carried out on the effect of leaching silica powder as a function of the leaching time at the constant temperature of $80^{\circ}C$ in oxalic acid, aqua regia, and two mixed acids of HF/HCl, $HF/HNO_3$. The impurities of silica and leachantes were measured by neutron activation analysis (NAA), inductively coupled plasma atomic emission spectrometry (ICP-AES), atomic absorption spectrometry, x-ray fluorescence (XRF) method and wet analysis (WA). Certain metals, such as sodium, calcium, iron, aluminium and titanium, have been found in concentrations of hundreds or even thousands of mg/kg. Comparison of purification processes of silica and analytical methods of impurities in the silica was conducted in this study.

• Journal of Soil and Groundwater Environment
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• v.18 no.1
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• pp.112-122
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• 2013

Current status of soil contamination with fluorine and its source were investigated. The basic principles and procedures of various techniques for the analysis of fluorine contents in soil and solid phase samples were summarized in this review. Analysis of fluorine in solid matrices can be achieved by two types of techniques: (i) UV/Vis spectrophotometer or ion selective electrode (ISE) analysis after performing appropriate extraction steps and (ii) direct solid analysis. As the former cases, the standard method of Korean ministry of environment, alkali fusion-ISE method, pyrohydrolysis, oxygen bomb combustion, aqua regia digestion-automatic analysis, and sequential extraction-ISE method were introduced. In addition, direct analysis methods (i.e., X-ray fluorescence spectrometry and proton induced gamma-ray emission spectrometry) and atomic spectrometry combining with the equipment for introducing solid phase sample were also reviewed. Fluorine analysis techniques can be reasonably selected through site-specific information such as matrix condition, contamination level, the amount of samples and the principles of various methods for the analysis of fluorine presented in this review.