• Title/Summary/Keyword: Gravimetry.

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Determination of Bi Impurity in Lead Stock Standard Solutions by Hydride-generation Inductively Coupled Plasma Mass Spectrometry

  • Park, Chang J.
    • Bulletin of the Korean Chemical Society
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    • v.25 no.2
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    • pp.233-236
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    • 2004
  • Total impurity analysis of a primary standard solution is one of the essential procedures to determine an accurate concentration of the standard solution by the gravimetry. Bi impurity is determined in Pb standard solutions by inductively coupled plasma mass spectrometry (ICP-MS). The direct nebulization of the Pb standard solution produces a significant amount of the Pb matrix-induced molecular ions which give rise to a serious spectral interference to the Bi determination. In order to avoid the spectral interference from the interferent $^{208}PbH^+$, the hydride generation method is employed for the matrix separation. The Bi hydride vapor is generated by reaction of the sample solution with 1% sodium borohydride solution. The vapor is then directed by argon carrier gas into the ICP after separation from the mixture solution in a liquid-gas separator made of a polytetrafluoroethylene membrane tube. The presence of 1000 ${\mu}$g/mL Pb matrix caused reduction of the bismuthine generation efficiency by about 40%. The standard addition method is used to overcome the chemical interference from the Pb matrix. Optimum conditions are investigated for the hydride-generation ICPMS. The detection limit of this method is 0.5 pg/mL for the sample solutions containing 1000 ${\mu}$g/mL Pb matrix.

A Study on the Preparation of Thermoplastic Powder Coating Material and Its Flame Retardancy (열가소성 분말 코팅소재 제조 및 난연특성 연구)

  • Lee, Soon-Hong;Chung, Hwa-Young
    • Journal of the Korean Society of Safety
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    • v.25 no.3
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    • pp.45-52
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    • 2010
  • The purpose of this study is application to flame retardant powder coating(FRPC) material consisting of ammonium polyphosphate(APP) and magnesium hydroxide($Mg(OH)_2$) as a halogen free flame retardant into thermoplastic resin(LDPE-g-MAH). For improvement of adhesion, LDPE-g-MAH was synthesized from low density polyethylene(LDPE) and maleic anhydride(MAH). The mechanical properties as melt flow index, pencil hardness, cross-hatch adhesion and impact resistance of FRPC were measured. Also, the limited oxygen index(LOI) values were measured 17.3vol%, 31.1vol% and 33.7vol% for LDPE-g-MAH, FRPC-3(APP 15wt%, $Mg(OH)_2$ 15wt%) and FRPC-5(APP 30 wt%), respectively. The thermo gravimetry/differential thermal analysis(TG/DTA) of FPRC-3 was observed endothermic peak at $340^{\circ}C$ and $450^{\circ}C$, it was confirmed predominant thermal stability though the wide temperature range by APP and $Mg(OH)_2$. It was showed V-0 grade for FRPC-3 and FRPC-4(APP 20wt%, $Mg(OH)_2$ 10wt%) that a char formation and drip suppressing effect, and combustion time reduced by UL94(vertical burning test). It was confirmed that flame retardancy was improved with the synergy effect because of char formation by APP and $Mg(OH)_2$.

Gasification reactivity of Chinese Shinwha Coal Chars with Steam (스팀을 이용한 중국산 신화 석탄 촤 가스화 반응에 관한 연구)

  • Kang, Min-Woong;Seo, Dong-Kyun;Kim, Yong-Tak;Hwang, Jung-Ho
    • Journal of the Korean Society of Combustion
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    • v.15 no.1
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    • pp.22-29
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    • 2010
  • In this study, carbon conversion was measured using an electronic mass balance. In a lab scale furnace, each coal sample was pyrolyzed in a nitrogen environment and became coal char, which was then gasified with steam under isothermal conditions. The reactivity of coal char was investigated at various temperatures and steam concentrations. The VRM(volume reaction model), SCM(shrinking core model), and RPM(random pore model) were used to interpret experimental data. For each model the activation energy(Ea), pre-exponential factor (A), and reaction order(n) of the coal char-steam reaction were determined by applying the Arrhenius equation into the data obtained with thermo-gravimetric analysis(TGA). According to this study, it was found that experimental data agreed better with the VRM and SCM for 1,000 and $1,100^{\circ}C$, and the RPM for 1,200 and $1,300^{\circ}C$. The reactivity of chars increased with the increase of gasification temperature. The structure parameter(${\psi}$) of the surface area for the RPM was obtained.

Ability of non-destructive assay techniques to identify sophisticated material partial defects

  • Lloyd, Cody;Goddard, Braden
    • Nuclear Engineering and Technology
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    • v.52 no.6
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    • pp.1252-1258
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    • 2020
  • This study explores the ability of non-destructive assay techniques to detect a partial material defect in which 100 g of plutonium are diverted from the center of a 1000 g can of PuO2 powder. Four safeguards measurements techniques: neutron multiplicity counting, calorimetry, gravimetry, and gamma ray spectroscopy are used in an attempt to detect the defect. Several materials are added to the partial defect PuO2 can to replicate signatures of the diverted material. 252Cf is used to compensate for the doubles neutron counts, 241Am is used to compensate for the decay heat, and aluminum is used to compensate for the weight. Although, the doubles and triples difference before and after diversion are statistically indistinguishable with the AWCC in fast and thermal mode, the difference in the singles counts are statistically detectable in both modes. The relatively short half-life of 252Cf leads to a decrease (three sigma uncertainty) in the doubles neutron counts after 161 days. Combining this with the precise quantity of 241Am needed (10.7 g) to mimic the heat signature and the extreme precision in 252Cf mass needed to defeat neutron multiplicity measurements gives reassurance in the International Atomic Energy Agency's ability to detect partial material defects.

Specimen Geometry Effects on Oxidation Behavior of Nuclear Graphite

  • Cho, Kwang-Youn;Kim, Kyung-Ja;Lim, Yun-Soo;Chung, Yun-Joong;Chi, Se-Hwan
    • Carbon letters
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    • v.7 no.3
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    • pp.196-200
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    • 2006
  • Graphite has hexagonal closed packing structure with two bonding characteristics of van der Waals bonding between the carbon layers at c axis, and covalent bonding in the carbon layer at a and b axis. Graphite has high tolerant to the extreme conditions of high temperature and neutron irradiations rather than any other materials of metals and ceramics. However, carbon elements easily react with oxygen at as low as 400C. Considering the increasing production of today of hydrogen and electricity with a nuclear reactor, study of oxidation characteristics of graphite is very important, and essential for the life evaluation and design of the nuclear reactor. Since the oxidation behaviors of graphite are dependent on the shapes of testing specimen, critical care is required for evaluation of nuclear reactor graphite materials. In this work, oxidation rate and amounts of the isotropic graphite (IG-110, Toyo Carbon), currently being used for the Koran nuclear reactor, are investigated at various temperature. Oxidation process or principle of graphite was figured out by measuring the oxidation rate, and relation between oxidation rate and sample shape are understood. In the oxidation process, shape effect of volume, surface area, and surface to volume ratio are investigated at $600^{\circ}C$, based on the sample of ASTM C 1179-91.

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CORROSION BEHAVIOR OF NI-BASE ALLOYS IN SUPERCRITICAL WATER

  • Zhang, Qiang;Tang, Rui;Li, Cong;Luo, Xin;Long, Chongsheng;Yin, Kaiju
    • Nuclear Engineering and Technology
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    • v.41 no.1
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    • pp.107-112
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    • 2009
  • Corrosion of nickel-base alloys (Hastelloy C-276, Inconel 625, and Inconel X-750) in $500^{\circ}C$, 25MPa supercritical water (with 10 wppb oxygen) was investigated to evaluate the suitability of these alloys for use in supercritical water reactors. Oxide scales formed on the samples were characterized by gravimetry, scanning electron microscopy/energy dispersive spectroscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. The results indicate that, during the 1000h exposure, a dense spinel oxide layer, mainly consisting of a fine Cr-rich inner layer ($NiCr_{2}O_{4}$) underneath a coarse Fe-rich outer layer ($NiFe_{2}O_{4}$), developed on each alloy. Besides general corrosion, nodular corrosion occurred on alloy 625 possibly resulting from local attack of ${\gamma}$" clusters in the matrix. The mass gains for all alloys were small, while alloy X -750 exhibited the highest oxidation rate, probably due to the absence of Mo.

Evaluation of Environment Imapcts on TiN-ZrCo Composites Hydrogen Seperation by Material Life Cycle Assessment (TiN-ZrCo 복합수소 분리막의 제조와 환경성 평가)

  • KIM, MINGYEOM;AHN, JOONGWOO;HONG, TAEWHAN
    • Transactions of the Korean hydrogen and new energy society
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    • v.28 no.6
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    • pp.627-634
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    • 2017
  • In this study, Material life cycle evaluation was performed to analyze the environmental impact characteristics of TiN-ZrCo membrane manufacturting process. Gabi was used as software. The Eco-Indicator 99 methodology was used to evaluate the 11 impact categories and the 10 impact categories using the CML 2001 methodology. Precursor TiN was synthesized by sol-gel method and zirconium was coated by ball mill method. The metallurgical, physical and thermodynamic characteristics of the membranes were analyzed by using Scanning Electron Microscope (SEM), Energy Dispersive X-ray (EDS), X-ray Diffraction (XRD), Thermo Gravimetry/Differential Thermal Analysis (TG/DTA), Brunauer, Emmett, Teller (BET) and Gas Chromatograph System (GP). As a result of the characterization and normalization, the environmental impacts of each category of impacts were GWP 100 years with the highest environmental impact of 99.9%.

Preparation and characterization of ceria nanofibers obtained by electrospinning

  • Hwang, A.R.;Park, J.Y.;Koh, S.W.;Kang, Y.C.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.08a
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    • pp.70-70
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    • 2010
  • Cerium oxide nanofibers have been of great interest in fundamental level study. We fabricated polyvinylpyrollidone (PVP) and cerium nitrate nanofibers composite applying a mixed solution of PVP and cerium nitrate hydrate (Ce(NO3)3) with various cerium concentration from 8.87 to 35.5wt% by electrospinning process. Electrospinning method is a simple and cost-effective process to make nanoand submicro nanofiber fabrication. We applied 0.69 kV/cm of electric field between the capillary and a drum collector covered with aluminum foil. Cerium oxide nanofibers were obtained after calcination of PVP/Ce(NO3)3 nanofibers composite at 573, 873 and 1273K, which were chosen by thermal gravimetry analysis. The obtained nanofibers were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS). When the viscosity of the electrospinning solution was high named over 60 cP, only nano and submicro-sized cerium oxide fibers were collected. X-ray photoelectron spectroscopy (XPS) was performed for investigation of the chemical nature of the obtained ceria nanofibers. After we calcined the PVP/ceria nanocomposites, metallic cerium was oxidized to cerium oxide including ceria.

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Chemical Compositions and Pyrolysis Characteristics of Oil Shales Distributed in Korea

  • Yang, Moon Yul;Yang, Myoung Kee;Lee, Sang Hak;Wakita, Hisanobu
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.487-492
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    • 1995
  • The chemical compositions and pyrolysis characteristics of oil shales and source rocks distributed in the southwestern and southeastern parts of the Korean peninsular have been investigated. In order to compare the results of Korean samples with those of shales giving high oil yields, two Colorado oil shale samples and one Paris source rock samples were also investigated. Chemical compositions of the samples were analysed by means of gravimetry, CHN analysis, X-ray diffraction method, inductively coupled plasma atomic emission spectrometry and atomic absorption spectrometry. A custom made pyrolyser and a Rock-Eval system were used for the pyrolysis studies. Pyrolyses of the samples were carried out by means of a temperature controlling device to $600^{\circ}C$ at a heating rate of $5^{\circ}C/min$ with a helium flow rate of $1200m{\ell}/min$. The results of pyrolysis study indicated that Colorado shale samples belong to type I and all the other samples belong to type II.

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Effect of Copper Substitution on Structural and Magnetic Properties of NiZn Ferrite Nanopowders

  • Niyaifar, Mohammad;Shalilian, Hoda;Hasanpour, Ahmad;Mohammadpour, Hory
    • Journal of Magnetics
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    • v.18 no.4
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    • pp.391-394
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    • 2013
  • In this study, nickel-zinc ferrite nanoparticles, with the chemical formula of $Ni_{0.3}Zn_{0.7-x}Cu_xFe_2O_4$ (where x = 0.1- 0.6 by step 0.1), were fabricated by the sol-gel method. The effect of copper substitution on the phase formation and crystal structure of the sample was investigated by X-ray diffraction (XRD), thermo-gravimetry (TG), differential thermal analysis (DTA), Fourier transform infrared spectrometry (FT-IR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The XRD result shows that due to the reduction of Zn content,the crystallite size of the sample increased. The results of the vibration sample magnetometer (VSM) exhibit an increase in saturation magnetization value (Ms) for samples with x ${\leq}$ 0.3 and a linear decrease for samples with x > 0.3. The variation of saturation magnetization and coercivity of the samples were then studied.