• Title/Summary/Keyword: Liquid-phase reduction

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Speciation of Chromium in Water Samples with Homogeneous Liquid-Liquid Extraction and Determination by Flame Atomic Absorption Spectrometry

  • Abkenar, Shiva Dehghan;Hosseini, Morteza;Dahaghin, Zohreh;Salavati-Niasari, Masoud;Jamali, Mohammad Reza
    • Bulletin of the Korean Chemical Society
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    • v.31 no.10
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    • pp.2813-2818
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    • 2010
  • A novel method was developed for the speciation of chromium in natural water samples based on homogeneous liquid-liquid extraction and determination by flame atomic absorption spectrometry (FAAS). In this method, Cr(III) reacts with a new Schiff's base ligand to form the hydrophobic complex, which is subsequently entrapped in the sediment phase, whereas Cr(VI) remained in aqueous phase. The Cr(VI) assay is based on its reduction to Cr(III) by the addition of sodium sulfite to the sample solution. Thus, separation of Cr(III) and Cr(VI) could be realized. Homogeneous liquid-liquid extraction based on the pH-independent phase-separation process was investigated using a ternary solvent system (water-tetrabutylammonium ion ($TBA^+$)-chloroform) for the preconcentration of chromium. The phase separation phenomenon occurred by an ion-pair formation of TBA and perchlorate ion. Then sedimented phase was separated using a $100\;{\mu}L$ micro-syringe and diluted to 1.0 mL with ethanol. The sample was introduced into the flame by conventional aspiration. After the optimization of complexation and extraction conditions such as pH = 9.5, [ligand] = $1.0{\times}10^{-4}\;M$, [$TBA^+$] = $2.0{\times}10^{-2}\;M$, [$CHCl_3$] = $100.0\;{\mu}L$ and [$ClO_4$] = $2.0{\times}10{-2}\;M$, a preconcentration factor (Va/Vs) of 100 was obtained for only 10 mL of the sample. The relative standard deviation was 2.8% (n = 10). The limit of detection was sufficiently low and lie at ppb level. The proposed method was applied for the extraction and determination of chromium in natural water samples with satisfactory results.

Synthesis of Nano Sized Cobalt Powder from Cobalt Sulfate Heptahydrate by Liquid Phase Reduction (액상환원공정을 이용한 황산코발트로부터의 코발트 나노분말 합성)

  • An, Se-Hwan;Kim, Se-Hoon;Lee, Jin-Ho;Hong, Hyun-Seon;Kim, Young-Do
    • Korean Journal of Materials Research
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    • v.21 no.6
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    • pp.327-333
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    • 2011
  • Nanostructured cobalt materials have recently attracted considerable attention due to their potential applications in high-density data storage, magnetic separation and heterogeneous catalysts. The size as well as the morphology at the nano scale strongly influences the physical and chemical properties of cobalt nano materials. In this study, cobalt nano particles synthesized by a a polyol process, which is a liquid-phase reduction method, were investigated. Cobalt hydroxide ($Co(OH)_2$), as an intermediate reaction product, was synthesized by the reaction between cobalt sulphate heptahydrate ($CoSO_4{\cdot}7H_2O$) used as a precursor and sodium hydroxide (NaOH) dissolved in DI water. As-synthesized $Co(OH)_2$ was washed and filtered several times with DI water, because intermediate reaction products had not only $Co(OH)_2$ but also sodium sulphate ($Na_2SO_4$), as an impurity. Then the cobalt powder was synthesized by diethylene glycol (DEG), as a reduction agent, with various temperatures and times. Polyvinylpyrrolidone (PVP), as a capping agent, was also added to control agglomeration and dispersion of the cobalt nano particles. The optimized synthesis condition was achieved at $220^{\circ}C$ for 4 hours with 0.6 of the PVP/$Co(OH)_2$ molar ratio. Consequently, it was confirmed that the synthesized nano sized cobalt particles had a face centered cubic (fcc) structure and with a size range of 100-200 nm.

A Study on the Liquid Phase Sintering of Tungsten-Nickel-Manganese alloy (텅스텐-니켈-망간 합금의 액상소결에 관한연구)

  • Hong, Mun-Hui;Lee, Seong;Roh, Jun-Ung;Paik, Un-Hyeong
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 1995.11a
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    • pp.25-25
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    • 1995
  • Liquid phase sintering of 90W-6Ni-4Mn alloy has been investigated as functions of sintering atmosphere, heating rate, and reduction temperature. The present work accounts for the thermodynamic oxidatiodreduction reactions of constituent powders of W, Ni and Mn. By discounting these reactions, the previous investigations would obtain only the alloy with large pores and the lowered relative sintered density, by the liquid phase sintering under a dry hydrogen atmosphere. the sintering cycle consisted of a rapid heating to reduction temperatures under high purity nitrogen atmosphere, and holding for 4 hours and sintering at $1260^{\circ}C$ for 1 hour under a dry hydrogen gas. The relative density of the sintered alloy increased with increasing heating rate. As the reduction temperature increased, the relative density increased to the lm theotical density at the duction temture above $1150^{\circ}C$. The mimsturcatre of sintered alloys has been analysed by a scanning election microscope. The sintered density was compared with those obtained from the other investigators. It was found that the reduction $1150^{\circ}C$ results in the lowered densification of 90W-6Ni-4Mn alloy. This is caused by the fact that reducing reactions of W and Ni oxides contained in W an Ni powders concomitantly leads to oxidizing reaction of Mn powder the oxidized Mn is hardly reduced at sintering temperature and thereby remains large pores in the alloy. It is concluded that the W-Ni-Mn alloy with full density can be obtained by the precise control of atmosphere, heating rate, and sintering temperature.

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Monitoring of the Transfer of Tetrachloroaurate(III) Ions by Thin-layer Electrochemistry and Electrochemical Deposition of Metallic Gold over a Graphite Electrode

  • Song, Ji-Seon;Shin, Hyo-Sul;Kang, Chan
    • Bulletin of the Korean Chemical Society
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    • v.29 no.10
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    • pp.1983-1987
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    • 2008
  • This study demonstrates the electrochemical conversion of the synthetic procedure of monolayer-protected clusters using a thin toluene layer over an edge plane pyrolytic graphite electrode. A thin toluene layer with a thickness of 0.31 mm was coated over the electrode and an immiscible liquid/liquid water/toluene interface was introduced. The transfer of the tetrachloroaurate ($AuCl_4^-$) ions into the toluene layer interposed between the aqueous solution and the electrode surface was electrochemically monitored. The $AuCl_4^-$ ions initially could not move through into the toluene layer, showing no reduction wave, but, in the presence of the phase transfer reagent, tetraoctylammonium bromide (TOABr), a cathodic wave at 0.23 V vs. Ag/AgCl was observed, indicating the reduction of the transferred $AuCl_4^-$ ions in the toluene layer. In the presence of dodecanethiol together with TOABr, a self-assembled monolayer was formed over the electro-deposited metallic gold surface. The E-SEM image of the surface indicates the formation of a highly porous metallic gold surface, rather than individual nanoparticles, over the EPG electrode.

Melting of Ice Inside a Horizontal Cylinder under the Volume Change (수평원관내 체적변화를 고려한 얼음의 용용시 전열특성에 관한 연구)

  • 조남철;김동춘;이채탈;임장순
    • Korean Journal of Air-Conditioning and Refrigeration Engineering
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    • v.13 no.12
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    • pp.1266-1274
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    • 2001
  • Heat transfer phenomena during melting process of the phase change material (ice) was studied by numerical analysis and experiments. In a horizontal ice storage tube, the natural convection caused an increase in melting rate. However, the reduction of the heating surface area caused a decrease in melting rate. Therefore, during the melting process of ice in a horizontal cylinder, the reduction of the heating surface area should be considered. Under the same heating wall and initial water temperature condition, the melting rate became higher for $V_s/V_tot/=0.545 \;than \;that\; for\; V_s/V_tot$/=1.00 due to the difference in the reduction of heating surface area. A modified melting model considering the equivalent thermal conductivity of liquid phase and volume reduction was proposed. The results of the model were compared with the measured values and found to be in good agreement.

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Creep-Rupture and Fatigue Properties of Transient Liquid Phase Bonded Joints of Ni-Base Single Crystal Superalloy (액상확산접합한 Ni기 단결정 초내열합금의 크리프 파단 및 피로특성)

  • 김대업
    • Journal of Welding and Joining
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    • v.19 no.1
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    • pp.82-87
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    • 2001
  • The creep-rupture and low cycle fatigue properties of transient liquid phase bonded joints of Ni-base single crystal superalloy, CMSX-2 was investigated using MBF-80 insert metal. The (100) orientation of bonded specimen was aligned perpendicular to the joint interface. CMSX-2 was bonded at 1523K for 1.8ks in vacuum, optimum bonding condition. The creep rupture strength and rupture lives of the joints were the almost identical to ones of the base metal. SEM observation of the fracture surfaces of joints after creep rupture test revealed that the fracture surfaces classified three types of region, ductile fracture surface, cleavage fracture surface and interfacial fracture surface. The low cycle fatigue properties of the joints were also the same level as those of base metal. The elongation and reduction of area values of joints were comparable to those of base metal while fell down on creep rupture condition of high temperature.

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Performance and Emission Characteristics of Liquid-Phase LPG Injection Engine with Different EGR Rate (EGR율 변화에 대한 액상 LPG분사 엔진의 운전 및 배출가스특성)

  • 염기태;우영민;장진영;박용국;배충식
    • Transactions of the Korean Society of Automotive Engineers
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    • v.11 no.5
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    • pp.7-14
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    • 2003
  • Exhaust Gas Recirculation (EGR) system is used to reduce NOx emission, to improve fuel economy, and to suppress knock since it offers the benefits of the inlet charge dilution. The effects of EGR was investigated on the performance and emission to reduce exhaust thermal load with a single cylinder liquid-phase LPG injection engine, in a wide range of EGR rate, engine conditions and LPG proportions. As EGR rate was increased, NOx was reduced while HC was increased. Pumping loss reduction by EGR improved bsfc and increased EGR lowered exhaust gas temperature. And, LPG proportions were made a difference on the performance and emission characteristics.

Sintering Mixtures in the Stage of Establishing Chemical Equilibrium

  • Savitskii, A.P.
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 1999.04a
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    • pp.5-5
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    • 1999
  • The Principal deficiency of the existing notion about the sintering-mixtures consists in the fact that almost no attention is focused on the Phenomenon of alloy formation during sintering, its connection with dimensional changes of powder bodies, and no correct ideas on the driving force for the sintering process in the stage of establishing chemical equilibrium in a system are available as well. Another disadvantage of the classical sintering theory is an erroneous conception on the dissolution mechanism of solid in liquid. The two-particle model widely used in the literature to describe the sintering phenomenon in solid state disregards the nature of the neighbouring surrounding particles, the presence of pores between them, and the rise of so called arch effect. In this presentation, new basic scientific principles of the driving forces for the sintering process of a two-component powder body, of a diffusion mechanism of the interaction between solid and liquid phases, of stresses and deformation arising in the diffusion zone have been developed. The major driving force for sintering the mixture from components capable of forming solid solutions and intermetallic compounds is attributed to the alloy formation rather than the reduction of the free surface area until the chemical equilibrium is achieved in a system. The lecture considers a multiparticle model of the mixed powder-body and the nature of its volume changes during solid-state and liquid-phase sintering. It explains the discovered S-and V-type concentration dependencies of the change in the compact volume during solid-state sintering. It is supposed in the literature that the dissolution of solid in liquid is realised due to the removal of atoms from the surface of the solid phase into the melt and then their diffusicn transfer from the solid-liquid interface into the bulk of liquid. It has been shown in our experimental studies that the mechanism of the interaction between two components, one of them being liquid, consist in diffusion of the solvent atoms from the liquid into the solid phase until the concentration of solid solutions or an intermetallic compound in the surface layer enables them to pass into the liquid by means of melting. The lecture discusses peculimities of liquid phase formation in systems with intermediate compounds and the role of the liquid phase in bringing about the exothermic effect. At the frist stage of liquid phase sintering the diffusion of atoms from the melt into the solid causes the powder body to grow. At the second stage the diminution of particles in size as a result of their dissolution in the liquid draws their centres closer to each other and makes the compact to shrink Analytical equations were derived to describe quantitatively the porosity and volume changes of compacts as a result of alloy formation during liquid phase sinteIing. Selection criteria for an additive, its concentration and the temperature regime of sintering to control the density the structure of sintered alloys are given.

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Reduction of Beating noise at LPLi pump (LPLi 연료펌프의 맥놀이 소음 저감 연구)

  • Gang, Tae-Sik;Sim, Jae-Gi
    • Proceedings of the Korean Society for Noise and Vibration Engineering Conference
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    • 2005.11b
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    • pp.161-165
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    • 2005
  • Until now LPG car has drived used to mixer and vaporizer. So LPG car always has problems back fire and when in the winter. LPG Car's Fuel consumption is rather than gasoline. But LPLi Fuel pump located in the fuel tank is directly injection in the engine. So Fuel consumption is better than LPG mixer system and result to reduced exhaust gas. In this paper to reduction of beating noise of LPLi(liquid phase LPG Injection) fuel pump. General speaking we know, beating noise is occur to near frequency each of pump. So we Modification of RPM through chang of amature turn number and area of dimension of the pump's body.

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Open-Loop Responses of Droplet Vaporization to Linear Normal Acoustic Modes

  • Kim, S.Y.;W.S. Yoon
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2004.03a
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    • pp.155-164
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    • 2004
  • In order for studying pressure-coupled dynamic responses of droplet vaporization, open-loop experiment of an isolated droplet vaporization exposed to pressure perturbations in stagnant gaseous environment is numerically conducted, Governing equations are solved for flow parameters at gas and liquid phases separately and thermodynamic parameters at the interfacial boundary are matched for problem closure. For high-pressure effects, vapor-liquid interfacial thermodynamics is rigorously treated. A series of parametric calculations in terms of mean pressure level and wave frequencies are carried out employing a n-pentane droplet in stagnant gaseous nitrogen. Results show that wave instability in view of pressure-coupled vaporization response seems more susceptible at higher pressures and higher wave frequencies. Mass evaporation rate responding to pressure waves is amplified with increase in pressure due to substantial reduction in latent heat of vaporization. Augmentation of perturbation frequency also enhances amplification due to the reduction of phase differences between pressure perturbation and surface temperature fluctuation.

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