• Resources Recycling
• /
• v.19 no.4
• /
• pp.41-50
• /
• 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.

• Korean Journal of Food Science and Technology
• /
• v.15 no.3
• /
• pp.225-230
• /
• 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.

• Resources Recycling
• /
• v.3 no.1
• /
• pp.17-24
• /
• 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.

• Journal of the Mineralogical Society of Korea
• /
• v.26 no.1
• /
• pp.45-54
• /
• 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.

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

• Analytical Science and Technology
• /
• v.23 no.6
• /
• pp.511-517
• /
• 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.

• Proceedings of the KSR Conference
• /
• 2007.11a
• /
• pp.1236-1241
• /
• 2007

The feasibility of soil washing was investigated in the laboratory to treat heavy metals-contaminated railway soil. Various organic acids including ethylene diamine tetraacetic acid (EDTA) and citric acid as well as inorganic acids such as hydrochloric acid (HCl) and phosphoric acid were tested to evaluate washing efficiency. Generally, inorganic acid showed higher removal efficiency compared to organic acids. Specially, EDTA, which are well known as most effective washing agent to remove heavy metals from soil, was not efficient to remove heavy metals in this study. Among washing agents tested in this study, HCl was most effective. The removal of Cd, Cu, and Pb was high, however, that for Zn and Ni was less than 30% with 0.5 M HCl. This difference comes from analytical methods (Korean Standard Test Method for Soil). Aqua regia was used to extract Zn and Ni, however 0.1 N HCl was used for other metals. As a result, simple washing technology is not effective, to treat railway contaminated soil with heavy metals.

• Journal of the Korean Chemical Society
• /
• v.15 no.4
• /
• pp.191-197
• /
• 1971

Ruthenium content in highly purified palladium metal (99.9%) was determined by counting $^{105}Rh$ nuclide which was produced by $^{104}Ru(n,{\gamma};{\beta}^-)^{105}Rh$ nuclear reaction. Palladium sample and ruthenium standard were irradiated by neutron with the Pneumatic Transfer System of TRIGA MARK II reactor. Palladium and ruthenium were dissolved by treating with aqua-regia and by fusing with sodium peroxide flux respectively. $^{105}Rh$ was separated through anion and cation exchange resin columns. The ruthenium content was determined by comparing the $^{105}Rh$ activities, obtained from the palladium sample, with that from pure ruthenium standard. The detection limit of ruthenium by the present method is about 1 ppm of ruthenium in 10 mg of palladium, which is approximately 40 times more sensitive than that of the conventional radioactivation method which employs $^{102}Ru(n,{\gamma})^{103}Ru$ nuclear reaction.

• Proceedings of the Korean Institute of Surface Engineering Conference
• /
• 2018.06a
• /
• pp.93.2-93.2
• /
• 2018

최근 기후 변화 문제로 $CO_2$배출량 억제 정책에 따라 열전재료가 다양한 분야에 크게 주목 받고 있다. 열전 모듈은 전류를 흘려 온도차를 발생시키는 펠티어 효과와 온도차를 전력으로 변환하는 제백 효과를 이용한다. 열전발전용에 적용되는 상용 열전모듈의 경우, 열전소자의 접합부의 수는 수십 개 이상이다. 따라서 단 한 개의 접합 불량 열전소자가 모듈 전체의 열전성능에 큰 영향을 미친다. 현재 상용화 된 Bi-Te계 열전 모듈은 Bi-Te의 Te와 Sn계 솔더의 주성분인 Sn이 $250^{\circ}C$ 부근에서 취성의 Sn-Te계 금속 화합물을 형성한다고 알려져 있다. 이 때 생성된 Sn-Te 화합물은 열전모듈의 접합강도를 약화시키고 이로 인해 열전모듈의 접합 신뢰성을 크게 저하 시킬 수 있다. 이를 해결하기 위해 솔더와 소자 사이에 확산방지층이 적용되고 있으며, 이 중에서 니켈합금이 가장 널리 적용되고 있다. 니켈층을 형성시키는 방법 중에서, 무전해 도금법은 간단하게 열전소자 표면 위에 도금 층을 균일한 두께로 만들어 낼 수 있다. 하지만, 니켈 도금층과 Bi-Te 소자 간에 화학적 결함이 존재하지 않기 때문에, 무전해 니켈 도금층의 밀착성이 떨어진다. 이 때. 소자 표면에 거칠기 효과(anchor effect)를 부여하기 위해 물리적 샌딩법을 사용하는데 이 방법의 경우 소자에 크랙 같은 손상을 미쳐 열전모듈의 신뢰성 저하를 가져온다. 그러므로 거칠기 효과를 부여하면서 소자에 손상을 최소화하는 습식 식각법을 개발하여 Bi-Te계 열전소자의 표면 조도를 조절하고 무전해 Ni-P 도금을 실시하였다. 그리고 열처리 유무에 따른 열전모듈의 접합강도를 측정하였으며, 제작한 열전 모듈의 접합부 및 파단부의 계면 분석하여 무전해 Ni-P도금을 위한 습식식각법(wet etching법)에 대하여 검토하였다. N-type은 질산과 구연산의 혼합수용액에, P-type은 왕수에 습식 식각처리를 해서 적당히 표면 조도를 조절한 후에 EPMA로 분석을 해본 결과 니켈 도금층과 Bi-Te 소자 간에 anchor effect가 부여 된 것을 확인했다. 습식 식각에 의해서 제조된 열전모듈의 접합강도는 종래의 알루미나 샌딩법으로 제조한 열전모듈 보다 높은 접합강도를 나타내었다.

• Journal of the Korea Academia-Industrial cooperation Society
• /
• v.14 no.8
• /
• pp.3597-3601
• /
• 2013

In this study, a wet cleaning process, P II, using aqua-regia and sulfuric acid mixture with oxidant agent ($K_2S_2O_8$, $P_2O_5$, $KMnO_4$, $H_2O_2$ etc) is proposed to remove the metastable phase of graphite such as graphene and DLC for high quality synthetic diamonds. The process employed the conventional acid cleaning process (P I) as well as P I+P II to remove the graphite related impurities from the 200um-diamond powders synthesized at 7GPa-$1500^{\circ}C$-5minutes. The degree of cleaning after P I and P I+P II has been observed by naked-eye, optical microscopy, micro-Raman spectroscopy, and TGA-DTA. After P I+P II, the color of diamond became more vividly yellow with enhanced saturation with naked eye and optical microscopy analysis. Moreover, the disappearance of diamond-like-carbon (DLC) peak ($1440cm^{-1}$) observed by Raman spectroscopy confirmed the decrease in amount of remaining impurities. TGA-DTA results showed that the graphite impurities first started to dissolve at $770.91^{\circ}C$ after PI process. However, the pyrolysis started at $892.18^{\circ}C$ after P I+P II process because of the dissolution of pure diamonds. This result proved the effective dissolution of the metastable phase of graphite. We expect that the proposed P II process may enhance the quality of diamonds through effective removal of surface impurities.