• Title/Summary/Keyword: Borohydride

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The Extraction and Derivatization of Organotins in Water Sample by Gas Chromatograph/Mass Spectrometer (기체크로마토그래프/질량분석기에 의한 물시료 중 Organotin의 추출 및 유도체 반응에 관한 연구)

  • Hong, Jee-Eun;Lee, Kang-Jin;Pyo, Hee Soo;Park, Song-Ja;Lee, Won
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.636-645
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    • 2000
  • A method is described for the determination of organotins in water samples by GC/MS. Optimized derivatization methods for ethylation and hydrogenation of organotins were surveyed according to various reaction conditions such as time, pH and concentration of reagents. The organotins were extracted with n-hexane in presence of 0.1% tropolone and hydrogenated with sodium borohydride. Extraction recoveries of organotins with hydrogenation were in the range of 61-112%. After ethylation, organotins in water samples were extracted by liquid-liquid extraction (LLE) and solid-phase extraction (SPE). Using LLE, extraction recoveries were in the range of 74-113%. The recoveries ranged from 61-97% in the case of SPE with styrene-divinylbenzene copolymers. Method detection limits of hydrogenated and ethylated organotins ranged from 0.05 to 0.5 ng/ml and from 0.02 to 0.05 ng/ml, respectively.

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Characteristic of Hydrogen Generation from Solid-State NaBH4 and Fuel Cell Operation for Fuel Cell Aircraft (연료전지 항공기를 위한 고체상태 NaBH4의 수소발생 및 연료전지 구동 특성)

  • Lee, Chung-Jun;Kim, Tae-Gyu
    • Journal of the Korean Society for Aeronautical & Space Sciences
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    • v.39 no.9
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    • pp.858-865
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    • 2011
  • This paper describes the characteristics of hydrogen generation from solid-state $NaBH_4$ and fuel cell operation for fuel cell aircraft. The solid-state $NaBH_4$ was used for a high hydrogen storage density, and was reacted with hydrochloric acid to generate hydrogen. The hydrogen generation rate for the solid-state $NaBH_4$ reaction was measured at various conditions. As a result, the hydrogen generation rate was increased with the feed rate and concentration of hydrochloric acid, while not be affected by the reaction temperature. A fuel cell was connected with the solid-state $NaBH_4$ hydrogen generator. The stable power output was obtained at the gradual and sudden increases of electric loads.

Determination of Selenium in Milk by ICP-OES (ICP-OES를 이용한 우유의 Selenium 분석)

  • 김효중;박종길;신정걸;백영진
    • Food Science of Animal Resources
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    • v.23 no.4
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    • pp.356-360
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    • 2003
  • The purpose of this paper was to determine the quantity of selenium in milk by inductively coupled plasma optical emission spectrometry. The sample was digested in teflon vessel containing nitric-hydrogen peroxide acid mixture. After digestion, the sample is treated with additional hydrochloric acid. Total selenium was reduced with sodium borohydride and concentrated hydrochloric acid in a simplified hydride generation(HG) manifold. The optimum conditions of HG are 2 M for HCl, 1.5% for NaBH$_4$, 1.2 mL/mim for sample flow. Recovery rates by the standard addition method were 88.0% at 10 ppb and 92.2% at 10 ppm. The relative standard deviations were 4.8 and 3.2%, respectively. This method showed a good accuracy and precision. And so it was highly suitable for determination of small quantity of selenium in milk.

Preparation of Copper Nanoparticles Protected by Chemisorption via Thiol Group (Thiol기의 화학흡착을 이용한 구리 나노입자의 제조)

  • Kim, Jung-Teag;Ju, Chang-Sik
    • Korean Chemical Engineering Research
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    • v.46 no.6
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    • pp.1069-1074
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    • 2008
  • In this work, we made a study for the 3D SAM formation of octanethiol, decanethiol, and dodecanethiol on copper nanoparticles and we verified stability of the copper particle depending on the ratio of dodecanethiol to copper. The reaction was performed in a one-phase system under nitrogen atmosphere and the thiolated copper particles could be obtained by centrifugation. We could confirm that the nanoparticles consisted of a spherical shape of 3~6 nm from TEM images. FT-IR, XPS and TGA results showed that alkanethiols were chemisorbed via thiol group and the packing density of the alkanethiols on copper surface increased with the alkyl chain lengths. XRD patterns gave us useful information about superlattice formations. Finally, $Cu_2O$ was formed when the molar ratio of dodecanethiol to copper is less than unity and copper nanoparticles formed more compact 3D SAMs when the molar ratio of dodecanethiol to copper was 1.25.

Synthesis of Sub-Micron 2SnO·(H2O) Powders Using Chemical Reduction Process and Thermal Calcination (화학적 합성법을 이용한 마이크론 이하급 2SnO·(H2O) 분말의 합성과 하소 특성)

  • Chee, Sang-Soo;Lee, Jong-Hyun
    • Korean Journal of Materials Research
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    • v.23 no.11
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    • pp.631-637
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    • 2013
  • Synthesis of sub-micron $2SnO{\cdot}(H_2O)$ powders by chemical reduction process was performed at room temperature as function of viscosity of methanol solution and molecular weight of PVP (polyvinylpyrrolidone). Tin(II) 2-ethylhexanoate and sodium borohydride were used as the tin precursor and the reducing agent, respectively. Simultaneous calcination and sintering processes were additionally performed by heating the $2SnO{\cdot}(H_2O)$ powders. In the synthesis of the $2SnO{\cdot}(H_2O)$ powders, it was possible to control the powder size using different combinations of the methanol solution viscosity and the PVP molecular weight. The molecular weight of PVP particularly influenced the size of the synthesized $2SnO{\cdot}(H_2O)$ powders. A holding time of 1 hr in air at $500^{\circ}C$ sufficiently transformed the $2SnO{\cdot}(H_2O)$ into $SnO_2$ phase; however, most of the PVP (molecular weight: 1,300,000) surface-capped powders decomposed and was removed after heating for 1 h at $700^{\circ}C$. Hence, heating for 1 h at $500^{\circ}C$ made a porous $SnO_2$ film containing residual PVP, whereas dense $SnO_2$ films with no significant amount of PVP formed after heating for 1 h at $700^{\circ}C$.

Efficiency of a Direct Absorption Solar Collector using Ag Nanofluids Synthesized by Chemical Reduction Method (화학적 환원법으로 제조된 은나노유체를 사용한 직접흡수식 태양열 집열기의 효율)

  • Lee, Seung-Hyun;Park, Yong-Jun;Choi, Tae Jong;Jang, Seok Pil
    • Journal of the Korean Solar Energy Society
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    • v.34 no.5
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    • pp.65-72
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    • 2014
  • In this paper, the water-based Ag nanofluids are synthesized by the chemical reduction method and their extinction coefficients are measured by an in-house developed measurement device. The Ag nanofluids are manufactured by the chemical reduction method with the mixing of silver nitrate ($AgNO_3$) and sodium borohydride ($NaBH_4$) in an aqueous solution of polyvinyl pyrrolidone (PVP). The extinction coefficients of Ag nanofluids are measured by means of the in-house developed apparatus at a wavelength of 632.8nm according to the particle volume fractions. The results show that the extinction coefficient of water-based Ag nanofluids increases with the increase of nanoparticle concentrations. Finally, the temperature field and efficiency of direct absorption solar collector (DASC) are analytically estimated based on the measured extinction coefficient of water-based Ag nanofluids. The results indicate that the direct absorption solar collectors using nanofluids have the feasibility to improve the efficiency of conventional flat-plate solar collectors without using an absorber plate.

Moisturizing Property and Physiological Activity of Chitosan Oligosaccharide (키토산 올리고당의 보습성과 생리활성에 관한 연구)

  • 하병조;이옥섭
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.25 no.1
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    • pp.6-22
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    • 1999
  • Chitosan oligosaccharide having physiological activity, such as cell proliferation and wound healing, was prepared by NaNO$_2$ oxidation-NaBH$_4$ reduction from natural chitosan. After deamination by NaNO$_2$ oxidation, the reducing-end residue from NaBH$_4$ was converted to alditol unit, and the reduction was checked by MBTH reagent. The resulting chitosan oligosaccharide had a degree of polymeration of 2-6 from HPLC analysis. From moisture absorption test at relative humidity of 43% and 81%, the moisture absorption ability was 63% and 57%. Moisture retention ability at relative humidity of 43%, silica gel emvironment, was 98% and 97% respectively. Cell proliferation was showed In the range of 0.000032~0.01%, wound healing effect was also appeared in the concentration of 2% and 20%. Antioxidative effect ($SC_{50}$/) was 3213 ppm. Chitosan oligosaccharide was compatible with most of ingredients used in cosmetic products.

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Reduction of Nitrate-nigrogen by Zero-valent Iron Adhered in Mesoporous Silicas (메조기공 실리카에 부착된 영가철을 이용한 질산성 질소의 환원)

  • Yeon, Kyeong-Ho;Lee, Seunghak;Lee, Kwanyong;Park, Yong-Min;Kang, Sang-Yoon;Lee, Jae-Won;Choi, Yong-Su;Lee, Sang-Hyup
    • Journal of Korean Society of Water and Wastewater
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    • v.21 no.1
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    • pp.139-147
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    • 2007
  • For environmental remediation of a contaminated groundwater plume, the use of zero-valent metal represents one of the latest innovative technologies. In this study, the effects of denitrification by zero-valent iron adsorbed in mesoporous silicas have been studied for groundwater contaminant degradation. The mesoporous silica was functionalized with 3-mercaptopropyltrimethoxysilane (MPTS) ligands and the zero-valent iron precipitated in the mesopore of granular silica was made by $FeCl_2$ and $NaBH_4$. Hydrogen was exchanged with $Fe^{2+}$ ions in the granular silicas. And then the ions were reduced by sodium borohydride in the mesoporous silicas. The surface area of the silica determined via the BET method ranged from 858 to $1275m^2/g$. The reductive reaction of nitrate-nitrogen indicated that the degradation of nitrate-nitrogen appeared to be pseudo first-order with the observed reaction rate constant kobs ($0.1619h^{-1}$) and to be directly proportional to the specific surface area. Therefore, the mesoporous silica with nano zero-valent iron proposed as a novel treatment strategy for contaminated groundwater was successfully implemented herein for the removal of nitrate-nitrogen.

Influence of Reducing Agents and Additives on the Synthesis of ZnSe Nanoparticles (ZnSe 나노분말 합성에 미치는 환원제와 첨가제의 영향)

  • Back, Geum Ji;Lee, Da Gyeong;Lee, Min Seo;Song, Ha Yeon;Hong, Hyun Seon
    • Journal of Powder Materials
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    • v.27 no.3
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    • pp.233-240
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    • 2020
  • Nano-sized ZnSe particles are successfully synthesized in an aqueous solution at room temperature using sodium borohydride (NaBH4) and thioglycolic acid (TGA) as the reducing agent and stabilizer, respectively. The effects of the mass ratio of the reducing agent to Se, stabilizer concentration, and stirring time on the synthesis of the ZnSe nanoparticles are evaluated. The light absorption/emission properties of the synthesized nanoparticles are characterized using ultraviolet-visible (UV-vis) spectroscopy, photoluminescence (PL) spectroscopy, and particle size analyzer (PSA) techniques. At least one mass ratio (NaBH4/Se) of the reducing agent should be added to produce ZnSe nanoparticles finer than 10 nm and to absorb UV-vis light shorter than the ZnSe bulk absorption wavelength of 460 nm. As the ratio of the reducing agent increases, the absorption wavelengths in the UV-vis curves are blue-shifted. Stirring in the atmosphere acts as a deterrent to the reduction reaction and formation of nanoparticles, but if not stirred in the atmosphere, the result is on par with synthesis in a nitrogen atmosphere. The stabilizer, TGA, has an impact on the Zn precursor synthesis. The fabricated nanoparticles exhibit excellent photo-absorption/discharge characteristics, suggesting that ZnSe nanoparticles can be alloyed without the need for organic solutions or high-temperature environments.

One-pot Syntheses of Metallic Hollow Nanoparticles of Tin and Lead

  • Lee, Gae-Hang;Choi, Sang-Il;Lee, Young-Hwan;Park, Joo-T.
    • Bulletin of the Korean Chemical Society
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    • v.30 no.5
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    • pp.1135-1138
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    • 2009
  • Hollow Sn and Pb nanoparticles have been prepared by a rapid injection of an aqueous solution of $SnCl_2$- poly(vinylpyrrolidone) (PVP, surfactant) and $Pb(OAc)_2${\cdot}$3H_2O-PVP$ into an aqueous solution of sodium borohydride (reducing agent) in simple, one-pot reaction at room temperature under an argon atmosphere, respectively. The two hollow nanoparticles have been fully characterized by TEM, HRTEM, SAED, XRD, and EDX analyses. Upon exposure to air, the black Pb hollow nanoparticles are gradually transformed into a mixture of Pb, litharge (tetragonal PbO), massicot (orthorhombic PbO), and $Pb_5O_8$. The order and speed of mixing of the reactants between the metal precursor-PVP and the reductant solutions and stoichiometry of all the reactants are crucial factors for the formation of the two hollow nanocrystals. The Sn and Pb hollow nanoparticles were produced only when 1:(1.5-2) and 1:3 ratios of the Sn and Pb precursors to $NaBH_4$ were employed with a rapid injection, respectively.