• Title/Summary/Keyword: Trace $H_2O$ and $O_2$

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Studies on Determination of trace amount of Se in Volcanic Rocks by Atomic Absorption Spectrophotometry (원자 흡수 분광광도법에 의한 화산암중 극미량의 Se정량에 관한 연구)

  • Kim, Chan-Kook;Sung, Hak-Je;Chung, Kang-Sup;Yamaya, Kazuhisa
    • Analytical Science and Technology
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    • v.12 no.6
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    • pp.484-489
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    • 1999
  • The extraction of trace amounts of Se in volcanic rock was investigated using the hydride generation method and atomic absorption spectrophotometry. The powdered rock, 1.0 g, was decomposed with the mixture of $HClO_4$, $HNO_3$ and HF in an acid digestion bomb at $140^{\circ}C$ for 2 hours. For the reduction of Se(VI) to Se(IV) in the solution, 10 mL of 6 M HCl and 0.2 mL of 1 M KBr were added to the solution and the mixture was heated for 30~45 minutes. $H_2Se$ was produced by adding 3% $NaBH_4$ as a strong reducing agent, extracted by nitrogen gas, and was absorbed twice into $KMnO_4$solution. The contents of Se in the solution were determined by generation/AAS. According to the proposed method, 1.0 ng or more of Se was quantitatively extracted and Se levels of 2.5 ng/g or more in rock samples could be determined. For example, Se in a rhyolite was determined with the precision of $19.5{\pm}1.3ng/g$(95% confidence, n=6).

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Determination of Trace Anions in Concentrated Hydrogen Peroxide by Direct Injection Ion Chromatography with Conductivity Detection after Pt-Catalyzed On-Line Decomposition

  • 김도희;이보경;이동수
    • Bulletin of the Korean Chemical Society
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    • v.20 no.6
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    • pp.696-700
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    • 1999
  • A method has been developed for the determination of trace anion impurities in concentrated hydrogen peroxide. The method involves on-line decomposition of hydrogen peroxide, ion chromatographic separation and subsequent suppressed-type conductivity detection. H2O2 is decomposed in Pt-catalyst filled Gore-Tex membrane tubing and the resulting aqueous solution containing analytes is introduced to the injection valve of an ion chromatograph for periodic determinations. The oxygen gas evolving within the membrane tubing escapes freely through the membrane wall causing no problem in ion chromatographic analysis. Decomposition efficiency is above 99.99% at a flow rate of 0.4mL/min for a 30% hydrogen peroxide concentration. Analytes are quantitatively retained. The analysis results for several brands of commercial hydrogen peroxides are reported.

High Temperature Oxidation Behavior of Nickel and Iron Based Superalloys in Helium Containing Trace Impurities

  • Tsai, C.J.;Yeh, T.K.;Wang, M.Y.
    • Corrosion Science and Technology
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    • v.18 no.1
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    • pp.8-15
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    • 2019
  • A high-temperature gas-cooled reactor (HTGR) is recognized as the best candidate reactor for next generation nuclear reactors. Helium is used to be the coolant in the core of the HTGR with temperature expected to exceed $900^{\circ}C$ at the core outlet. Several iron- and nickel-based superalloys, including Alloy 800H, Hastelloy X, and Alloy 617, are potential structural materials for intermediate heat exchanger (IHX) in an HTGR. Oxidation behaviors of three selected alloys (Hastelloy X, Alloy 800H, and Alloy 617) were investigated at four different temperatures from $650^{\circ}C$ to $950^{\circ}C$ under helium environments with various concentrations of $O_2$ and $H_2O$. Preliminary results showed that chromium oxide as the primary protective layer was observed on surfaces of the three tested alloys. Based on results of mass gain and SEM analyses, Hastelloy X alloy exhibited the best corrosion resistance in all corrosion tests. Further details on the oxidation mechanism of these alloys are presented in this study.

A Study on Treatment of Wastes from the Uranium Ore Dissolution/purification and Nuclear Fuel Powder Fabrication (우라늄 정광의 용해/정제 및 핵연료 분말 가공공정에서 발생된 폐액의 처리에 관한 연구)

  • Jeong, Kyung-Chai;Hwang, Seong-Tae
    • Applied Chemistry for Engineering
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    • v.8 no.1
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    • pp.99-107
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    • 1997
  • This study Provides the treatment methods of liquid wastes from the dissolution/purification process of nuclear fuel raw material and the fabrication process of nuclear fuel powder. One of the treatment methods is to process liquid waste from uranium raw material dissolution/purification process. This waste, of the strong acid, can be reused to dissolve the fine ADU particles in filtrate which is ADU waste of pH 8.0 converted from AUC waste after recovery of uranium. To dissolve the fine ADU particles, ADU filtrate was pretreated to pH 4.0 with the dissolution/purification waste, and then mixed with the lime to pH 9.2 and aged for 30 minutes. From this processing, uranium content of the filtrate was decreased to below 3ppm. The waste from fuel powder fabrication is emulsified solution dispersed with fine oil droplets. This emulsion was destroyed effectively by adding and mixing the nitric acid with rapid heating at the same time. After this processing, $Na_2U_2O_7$ compound is produced by addition of NaOH. Optimum condition of this processing was shown at pH 11.5, and uranium content of the filtrate was analyzed to 5ppm. To remove the trace of uranium in the filtrate, lime should be added. Otherwise, 4N nitric acid was used to destroy the emulsion directly, and then lime was added to this waste. Uranium content of the treated filtrate was below 1 ppm. In addition to these wastes, the trace of uranium in filtrate after recovery of uranium from the AUC waste which is produced during PWR power preparation, is treated with NaOH to takeup fluorine(F) in the waste because fluorine is valuable and toxic material. In the finally treated waste, uranium was not detected.

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Optimization of Endoglucanase Production from Fomitopsis pinicola Mycelia (Fomitopsis pinicola 균사체로부터 Endoglucanase의 최적생산)

  • Gu, Ji-Min;Park, Sang-Shin
    • Microbiology and Biotechnology Letters
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    • v.41 no.2
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    • pp.145-152
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    • 2013
  • The culture conditions to maximize the production of endoglucanase (EC 3.2.1.4) from the brown rot fungus Fomitopsis pinicola MKACC 54347 mycelia were investigated. Among the tested media for endoglucanase production, Mandel's mineral salts medium (MSM; 1% cellulose, 0.1% peptone, 0.14% $(NH_4)_2SO_4$, 0.03% urea, 0.2% $KH_2PO_4$, 0.03% $MgSO_4{\cdot}7H_2O$, 0.03% $CaCl_2$, and 0.1% trace metal solution (19.8 mM $FeSO_4$, 13.0 mM $MnSO_4$, 12.2 mM $ZnSO_4$, and 15.4 mM $CoCl_2$)) produced the highest activity of the enzyme. To optimize the medium composition for enzyme activity, the effects of various carbon, nitrogen, phosphorus, and inorganic sources were investigated in MSM. Maximal enzyme production was accomplished using a medium containing 2% carboxymethyl cellulose (CMC), 2% yeast extract, 0.2% $KH_2PO_4$, 0.03% $MnSO_4$, and 0.3% trace metal solution. Different physiological conditions, like incubation period and temperature, were also examined to assess their influence on enzyme production. Enzyme production from F. pinicola reached its highest level after cultivation for 8 days at $25^{\circ}C$. Nondenaturing polyacrylamide gel electrophoresis (PAGE), followed by the endoglucanase activity staining using CMC as the substrate, was performed to identify the endoglucanase under the culture conditions studied. Zymogram analysis of the culture supernatant revealed an endoglucanase band with a molecular mass of 52 kDa. The optimum pH and temperature for enzyme activity were $55^{\circ}C$ and pH 5.0, respectively.

Purification and Characterization of Oxidase Induced from Thiobacillus neapolitanus R-10 (Thiobacillus neapolitanus R-10으로 부터 산화 효소의 분리 정제와 특성)

  • Weon, Yong-Don;Kim, Dong-Suck;Ryu, Beung-Ho
    • Journal of Environmental Science International
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    • v.5 no.1
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    • pp.43-50
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    • 1996
  • Thiobacillus neopolitanus R-10, which produces a active thiosulfate oxidase was isolated from nightsoil. The optimal culture conditions of Thiobacillus neopolitanus R-10 for the production of enzyme was determined as followed: 0.8% $Na_2S_2O_3$, 0.2% $KH_2PO_4$, 0.2% $K_2HPO_4$, 0.04% $Na_2CO_3$, 0.02% $MgSO_4$.$7H_2O$, 2ml trace elements solution, ann PH 6.5 at 3$0^{\circ}C$ and 72hr cultivation. The oxidase was successively purified 83 folds yield by ${(NH_2)}_2SO_4$ fractionation, DEAE-Cellulose, Sephadex A-50 column chromatogrophy and gel Sephadex G-150 gel filteration with yield of 5.9%. The molecular weight of purified enzyme was estimated to be 43.000 dalton by SDS-polyacrylamide gel electrophoresis and gel filteration column chromatography The enzyme activity was highest at 40t and PH 7.0 The enzyme activity was relatively high by $\beta$-mercaptoethanol but strongly inhibited by cysteine.

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Spectrophotometric Determination of Ultra trace Tri & Hexavalent Chromium by Using on-line Flow Injection Analysis with Dual Pre-concentration Column

  • Jung, Sung-Woon;Lim, Hyun-Woo;Kang, Chul-Ho;Choi, Yong-Wook
    • Bulletin of the Korean Chemical Society
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    • v.32 no.9
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    • pp.3437-3442
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    • 2011
  • An on-line flow injection analysis with dual pre-concentration method was developed to determine the ultra trace tri and hexavalent chromium in water. In this system, the cation and anion pre-concentration columns were combined with a 10-port injection valve and then used to separate and concentrate Cr (III) and Cr (VI) selectively. The two species of concentrated chromium were sequentially eluted and determined by using HCl-KCl buffer of pH 1.8 as an eluent. Cr (III) was oxidized by hydrogen peroxide to Cr (VI). It was detected spectrophotometrically at 548 nm by complexation with DPC (diphenylcarbazide). Several factors such as concentration of $H_2O_2$, DPC and coil length in reaction condition were optimized. The linear range for Cr (III) and Cr (VI) was 0.1-50 ${\mu}g$/L. The limit of detections ($3{\sigma}$) of Cr (III) and Cr (VI) were 52 ng/L and 44 ng/L under the optimized FIA system, and their recoveries 98% and 103%, respectively. This method was applied to analyze contamination level of chromium species in tap water, groundwater and bottled water.

Impurity Analysis of Domestic $MnSO_4{\cdot}H_2O$ Introduced to Manganese Bath Method (망간용액조방법에 도입되는 국산 황산망간중의 불순물 분석)

  • Hwang, Sun-Tae;Lee, Kyung-Ju;Choi, Kil-Oung;Lee, Kwang-Woo;Woo, Jin-Chun;Lee, Ki-Bum
    • Journal of Radiation Protection and Research
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    • v.12 no.1
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    • pp.48-53
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    • 1987
  • The manganous sulphate bath method is widely used for measurements of neutron source strength. In this study, the analytical chemistry method based on the argon supported inductively coupled plasmas emission spectrometry was used for examining the impurity contents of domestic $MnSO_4{\cdot}H_2O$ the product of Chemical Industry, to induce $^{55}Mn(n,{\gamma})^{56}$ Mn reactions. From the analytical results, mainly potassium, cobalt, and zinc as well as trace amounts of cadmium, lithium, etc. have turned out to be the relevant impurities absorbing the neutrons, and the fraction of neutrons absorbed by the total impurities was calculated. The value obtained was about 1.37% of the neutrons captured by manganese.

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Preparation of Birnessite (δ-MnO2) from Acid Leaching Solution of Spent Alkaline Manganese Batteries and Removals of 1-naphthol (폐 알칼리망간전지의 산 침출액으로부터 버네사이트(δ-MnO2)의 제조 및 1-naphthol 제거)

  • Eom, Won-Suk;Lee, Han-Saem;Rhee, Dong-Seok;Shin, Hyun-Sang
    • Journal of Korean Society of Environmental Engineers
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    • v.38 no.11
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    • pp.603-610
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    • 2016
  • This work studies the synthesis of birnessite (${\delta}-MnO_2$), a catalyst of oxidative-coupling reactions, from the powder of spent alkaline manganese batteries (SABP, <8 mesh) and evaluate its reactivity for 1-naphthol (1-NP) removals. Manganese oxides using commercial reagents ($MnSO_4$, $MnCl_2$) and the acid birnessite (A-Bir) by McKenzie method were also synthesized, and their crystallinity and reactivity for 1-NP were compared with one another. 96% Mn and 98% Zn were extracted from SABP by acid leaching at the condition of solid/liquid (S/L) ratio 1:10 in $1.0M\;H_2SO_4+10.5%\;H_2O_2$ at $60^{\circ}C$. From the acid leaching solution, 69% (at pH 8) and 94.3% (pH>13) of Mn were separated by hydroxide precipitation. Optimal OH/Mn mixing ratio (mol/mol) for the manganese oxide (MO) synthesis by alkaline (NaOH) hydrothermal techniques was 6.0. Under this condition, the best 1-NP removal efficiency was observed and XRD analysis confirmed that the MOs are corresponding to birnessite. Kinetic constants (k, at pH 6) for the 1-NP removals of the birnessites obtained from Mn recovered at pH 8 (${Mn^{2+}}_{(aq)}$) and pH>13 ($Mn(OH)_{2(s)}$) are 0.112 and $0.106min^{-1}$, respectively, which are similar to that from $MnSO_4$ reagent ($0.117min^{-1}$). The results indicated that the birnessite prepared from the SABP as a raw material could be used as an oxidative-coupling catalyst for removals of trace phenolic compounds in soil and water, and propose the recycle scheme of SAB for the birnessite synthesis.

Determination of Trace Level Mercury in Bio-Materials by Square Wave Anodic Stripping Voltammetry (네모파 산화전극벗김 전압전류법을 이용한 생체시료 중의 미량 수은 분석)

  • Kim Il Kwang;Park Sung Woo;Han Jong Hyun;Kim Youn Geun;Chun Hyun Ja;Park Kyung Ok
    • Journal of the Korean Chemical Society
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    • v.37 no.5
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    • pp.477-482
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    • 1993
  • The determination of trace level mercury in bio-materials has been investigated by the square wave anodic stripping voltammetry (ASV)-technique at glassy carbon electrode. Prior to analysis, the bio-materials were digested with HNO3/H2SO4 mixture and KMnO4 was added to complete the oxidation. The detection limit of the mercury varied greatly with deposition time, deposition potential, pH and stirring rate. When deposition is carried out for 240 sec with 400 rpm stirring at -1.0 volts vs. Ag/AgCl, the detection limit was below $0.5\;ppb\;(2.5{\times}10^{-9} M)$. The method is recommended for trace level mercury analysis of biomaterials because this procedure is time saving and has higher sensitivity.

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