• Title/Summary/Keyword: 용해법

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Low Dilution Glass Bead Digestion Technique for the Trace Element Analysis of Rock Samples (저희석 유리구 용해법에 의한 암석시료 미량원소 분석법)

  • Park, Chan-Soo;Shin, Hyung-Seon;Oh, Hae-Young;Moon, Jong-Hwa;Cheong, Chang-Sik
    • The Journal of the Petrological Society of Korea
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    • v.20 no.3
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    • pp.161-172
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    • 2011
  • Open beaker digestion method is routinely used as the sample preparation technique for trace element determination of rock samples by inductively coupled plasma mass spectrometry, With this method, however, dissolution of Zr and Hf is not always guaranteed especially when the samples contain refractory minerals. In this study, glass bead digestion technique was compared with conventional open beaker digestion technique for the sample preparation of three USGS rock standards such as AGV-2, BHVO-2, and G-3. Thirty trace elements including rare earth elements were analysed by ICP-MS and ICP-AES. There were no clear differences in analytical results for the AGV-2 and BHVO-2 standards between the two techniques, but Zr, Hf, Y, and middle- to heavy- rare earth element concentrations of the G-3 standard prepared by open beaker digestion technique were significantly lower than the recommended values. This can be attributed to the presence of refractory mineral zircon. On the contrary, all the analytical results of the G-3 standard prepared by glass bead digestion technique were in good agreement with the recommended values, indicating complete dissolution of zircon. The analytical results show that the volatile elements such as Pb and Zn were not lost during the preparation of glass bead. Low dilution glass bead digestion technique described here will be very helpful to enhance precision and accuracy of trace element analysis for geological samples containing refractory minerals.

암석 용해방법에 따른 미량원소 분석결과 비교

  • 최만식;정창식;박계헌
    • The Journal of the Petrological Society of Korea
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    • v.3 no.1
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    • pp.41-48
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    • 1994
  • Three USGS rock standards (G-2, W-2, and BHVO-1) are decomposed by three different methods, such as open beaker, microwave oven, and alkali fusion method, to compare the effect of decomposition methods for trace elememt analysis in the rock samples. Solubilized trace elements are measured with inductively coupled plasma mass spectrometer (ICP-MS). Generally the analytical results of trace elements between open beaker and microwave digestion method are not different. In case of alkali fusion method, some volatile elements such as Pb, Cu, and Rb are considerably lost. Using acid digestion method, Zr and Hf concentrations are lowered in case that these elements are concentrated in refractory minerals. The concentrations of rare earth elements are generally consistent with the recommended values, but due to large dilution factor, there are some analytical problems in alkali fusion method.

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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.

진공밀폐 용해법으로 제조된 $La_zCo_4Sb_{12}$ Skutterudite의 열전특성

  • Park, Gwan-Ho;Yu, Sin-Uk;Sin, Dong-Gil;Lee, Go-Eun;Jeon, Bong-Jun;Lee, U-Man;Kim, Il-Ho
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.321-321
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    • 2013
  • 열전재료는 열과 전기의 변환이 상호 가역적으로 일어나는 현상을 갖는 재료로서, 사용온도별로 여러 가지 재료가 개발되고 있다. 중온 영역에서 우수한 열전특성을 보이는 skutterudite는 격자 내에 2개의 공극을 갖고 있고 이에 적절한 원자를 충진하여 포논산란을 유도하고, PGEC(phonon-glass and electron-crystal) 개념을 적용하여 재료의 열적인 성질과 전기적인 성질을 동시에 제어함으로써 열전성능의 향상을 도모할 수 있는 재료이다. 본 연구에서는 챔버 내부 기체를 연속적으로 뽑아내어 진공도를 유지하는 방식이 아닌, 석영관을 앰플화한 진공밀폐 용해법을 사용하였다. 진공밀폐 용해법은 성분원소의 산화와 휘발을 억제하는데 있어 매우 유용한 공정이다. 용해를 통해 얻어진 잉곳을 용해와 동일한 방법으로 석영관에 밀봉하여 873 K에서 100시간 동안 진공열처리를 실시하였다. 또한, 합성된 잉곳의 기계적 특성 향상을 위해 $75{\mu}m$ 이하로 파쇄하여 진공 열간 압축 소결하였다. La가 충진된 $La_zCo_4Sb_{12}$ Skutterudites 단일상을 합성하여 La의 충진량(z)에 따른 열전특성과 전자이동특성을 조사하였다.

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Homogenization Analysis of Problems related to Quartz Dissolution and Hydroxide Diffusion (석영광물의 용해 및 수산화 이온의 확산에 관한 균질화해석)

  • Choi, Jung-Hae;Ichikawa, Yasuaki
    • The Journal of Engineering Geology
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    • v.20 no.3
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    • pp.271-279
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    • 2010
  • Time-dependent behavior similar to secondary deformation related to mineral dissolution is easily observed when performing a laboratory pressure experiment. In this research, to observe the dissolution of quartz found in bentonite used as buffer material for the geological disposal of high-level waste (HLW) under conditions of high pH, we calculated the diffusion of $OH^-$ ions and the behavior of quartz dissolution using the homogenization analysis method. The results reveal that the rate of quartz dissolution is proportional to the temperature and interlayer water thickness. In particular, in a high-pH environment, the reacted area (and therefore the dissolution rate) increases with decreasing interlayer water thickness.

Preparation and Characterization of Water-Soluble Glass Through Melting Process(II) : Dissolution Characteristics, Bactericidal Effects and Cytotoxicity (용융법에 의한 수용성 유리의 제조 및 특성(II) : 용해 특성, 살균 효과 및 세포 독성)

  • 오승한;조종호;최세영;오영제
    • Journal of the Korean Ceramic Society
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    • v.34 no.1
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    • pp.13-22
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    • 1997
  • Water-soluble phosphate glasses containing Ag and Cu ion were prepared through melting process. Dis-solution characteristics, bactericidal effect and cytotoxicity were investigated with composition and time in D. I. water using the powdered sample. Surface change were observed with increasing dissolution time us-ing the bulk specimen. Dissolution amount was maximum at the molar Ag:Cu ratio of 1 and increased with increasing time. The behavior of dissolution was total dissolution from the early stage. But no new layer was observed at the glass surface during dissolution. The bactericidal effect for pseudomonas sp, e. coli, sta-phylococcus aureus, and salmonella increased with increasing dissolution amount and therefore great bac-tericidal effect appeared. The result of cytotoxicity experiment to L929 showed that solution with more than 10 ppm of Ag ion had strong cytotoxicity.

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Characterization of Graphene Transparent Conducting Film Fabricated on Self-Assembled Monolayers/Polyethylene Terephthalate

  • Go, Yong-Hun;Jeong, Dae-Seong;Adhikari, Prashanta Dhoj;Cha, Myeong-Jun;Jeon, Seung-Han;Park, Jong-Yun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.380.1-380.1
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    • 2014
  • 열 화학기상증착법은 여러 가지 그래핀의 제작방법 중 대면적으로 양질의 그래핀을 효과적으로 합성할 수 있는 방법으로 널리 이용되고 있다. 이 방법으로 그래핀을 합성할 경우, 주요 변수로 성장 온도와 촉매 금속이 있으며 이를 적절히 조절함으로써 합성되는 그래핀의 결정성과 층수를 조절할 수 있다[1-3]. 본 연구에서는 탄소 용해도가 작은 두꺼운 촉매 금속 기판 위에 선택적인 위치에 탄소 용해도가 큰 얇은 촉매 금속을 증착하여 그래핀의 층수를 적절하게 제어하고자 한다. 그래핀을 합성하기 위해 온도를 증가시키는 과정에서 두 층의 촉매 금속은 표면 에너지를 낮추기 위해 합금을 형성하게 되며, 이 때 탄소 용해도가 변화할 것으로 예상된다. 이 변화하는 탄소 용해도에 맞추어 탄소 공급원인 메탄 가스를 주입하는 시기를 적절히 조절하게 되면, 합성되는 그래핀의 층수 조절이 가능할 것이라 예상한다. 탄소 용해도가 큰 금속으로 니켈을, 탄소 용해도가 작은 금속으로 구리를 선택하였다. 우선 니켈의 확산 거리를 계산하여 메탄 가스를 주입하는 적절한 온도를 결정하였으며, 이 온도를 기준으로 표면에서의 니켈의 함량을 분석하였다. 니켈의 함량과 표면에서의 탄소의 구성비의 관계를 조사한 결과, 본 실험에서 이용한 방법으로 그래핀의 층수를 조절하는 것이 가능하다는 것을 확인하였다.

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