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A study on the development of phthalate plasticizers CRM in ABS resin (ABS 중 phthalates 가소제 CRM 개발에 대한 연구)

  • Jung, Jung-Sul;Park, Jung-Woo;Yoo, Seok;Kweon, Seong-Il;Hong, Sung-Taeg;Sun, Yle-Shik;Park, Cheon-Min;Choi, Chang-Hyoo
    • Analytical Science and Technology
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    • v.25 no.5
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    • pp.273-283
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    • 2012
  • Phthalate plasticizers are regulated by RoHS, REACH and CPSC as hazardous substances. Responding to these international environmental restrictions, we developed ABS certified reference material (CRM) for determination of phthalate plasticizers such as DMP, DEP, DBP, BBP, DEHP and DnOP. The candidate material has been made with ABS resin widely used in electric and electronic products and 6 kinds of phthalate plasticizers. The making of the material involved a series of processes like extruding, cooling, pelletizing, and drying using twin screw extruder. Then it has been certified according to ISO Guide 35. Using isotope dilution-gas chromatography/mass spectrometry (ID-GC/MS), homogeneity, short-term stability, and long-term stability were evaluated. The certified values were determined by using primary reference material (PRM) of KRISS for traceability. From now on, we will provide ABS CRM to national and international companies and research institutes after certification as certified reference material and registering on COMAR (code of reference material).

1,3-bisdicyanovinylindane 색소를 이용한 선택적 $Hg^{2+}$ 감지 특성

  • Kim, Su-Ho;Kim, Young-Sung;Kim, Sung-Hoon;Son, Young-A
    • Proceedings of the Korean Society of Dyers and Finishers Conference
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    • 2009.11a
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    • pp.19-20
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    • 2009
  • 최근 화학, 물리, 생명과학, 전기, 전자등의 다양한 분야에 활발하게 연구가 이루어지고 있는 초분자 화학은 선택적 분자인지를 위한 효율적인 골격구조와 나아가 다양한 계에 응용할 수 있다. 초분자 화학의 분자인지 과정의 특징은 일반적으로 수용체 (receptor 혹은 host)가 목표가 되는 기질 (substrate, analyte, 혹은 guest)에 대하여 선택적으로 식별하고 반응하는 것이다. 비공유 결합성 상호작용에 의하여 이루어지는 초분자 화학의 분자 인지 과정의 특징은 일반적으로 수용체 (receptor 혹은 host)가 목표가 되는 기질 (substrate, analyte, 혹은 guest)에 대하여 선택적으로 식별하고 반응하는 것이다. 이는 공유결합을 이용하는 분자화학과는 차별화 된 것이다. 수용체는 간단한 구조의 화합물 및 금속 이온들과 같은 기질과 가역적으로 상호 작용할 수 있는 착물을 형성한다. 최근들어 급격한 산업화가 진행되어 환경문제가 심각하게 대두 되어져 왔고, 그 중에서 특히 수은이나 카드뮴에 의한 질병, 납에 의한 중독 등 중금속에 의한 오염이 크게 나타남에도 불구하고, 현재 그러한 중금속을 검출함에 있어 많은 비용과 시간이 드는 문제점이 있다. 또한 우리에게 이로운 금속은 효율적 분석을 통해 환경계와 의료계에 많은 도움을 줄 것으로 사례되므로 화학센서 기술의 개발은 절실히 요구되어지고 있다. 이에 새로운 1,3-bisdicyanovinylindane 을 통해 $Hg^{2+}$ 금속의 감지 여부 알아보고, 그 특성을 파악하고자 한다. 1,3-indandion (2.18g, 14.9mmol), malononitrile (2.95g, 44.7mmol), ethanol 50ml를 20분간 상온에서 용해시킨다. 후에 sodium trihydrate acetate(3.05g)을 첨가한 후 5시간 동안 환류반응 시킨다. 이 과정에서 얻어진 용액을 필터과정을 통하여 에서 합성 반응 중에 생성된 불순물(1,3-dicyanovinylindane-1-one, monocondensation)을 제거한다. 필터과정을 통해 걸러진 미 반응 물질을 제�G 용반응욕액을 증류수(100ml)를 이용하여 희석시키고 난 후 염산을 이용, 산성화 시켜 고체 생성물을 얻어낸다. 이렇게 생성된 고체 생성물은 다시 필터 및 건조를 통하여 회색의 고체 화합물을 얻어낸다. 1,3-bisdicyanovinylindane과 금속이온에 대한 감응도를 확인하기 위하여 metanol/water(1:2)을 용매로 하여 금속이온의 농도를 변화시켜 발색특성을 살펴보았다. 본 색소화합물과 Hg2+에 대한 UV 흡광도 변화 적정결과와 그 화합물의 상태 살펴본 결과 금속이온이 0.2ml씩 더 참가되면서 색의 변화를 뚜렷하게 나타내었다. 반면 그 밖에 이온($Fe^{3+}$, $Ag^{2+}$, $Pd^{2+}$, $Zn^2$, $Fe^{2+}$, $Cu^{2+}$, $Pb^{2+}$)은 UV 흡광도 변화가 적거나 변화 자체가 없었다. 하지만 과량의 $Fe^{3+}$, $Ag^{2+}$, $Pd^{2+}$는 색상 변화를 나타내었으며,이와 같은 흡광도 변화는 금속에 따라 약간의 차이가 있지만, 420nm를 등흡수점으로 하여, 580nm의 파장 영역에 있는 흡수 밴드의 세기는 감소하는 반면 400nm 파장 영역에 있는 흡수 밴드의 세기가 증가하였다. 1,3-bisdicyanovinylindane 화합물은 다양한 생물계 및 환경계에서 요구되는 micro mol에서 milli mol 농도 영역의 $Hg^{2+}$ 이온의 선택적이고 민감한 검출과 정량적인 분석에 유용하게 사용될 수 있을 것이다.

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Preparation and Current-Voltage Characteristics of Well-Aligned NPD (4,4' bis[N-(1-napthyl)-N-phenyl-amino] biphenyl) Thin Films (분자배열된 4,4' bis[N-(1-napthyl)-N-phenyl-amino] biphenyl 증착박막 제조와 전기적 특성)

  • Oh, Sung;Kang, Do-Soon;Choe, Youngson
    • Applied Chemistry for Engineering
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    • v.17 no.6
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    • pp.591-596
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    • 2006
  • Topology and molecular ordering of NPD(4,4'-bis-[N-(1-naphthyl)-N-phenyl-amino]biphenyl) thin films deposited under magnetic field with post-deposition annealing were investigated. NPD was deposited onto ITO glass substrates via thermal evaporation process in vacuum. It is of great importance for highly oriented organic/metal films to have improved device performances such as higher current density and luminance efficiency. AFM (Atomic Force Microscope) and XRD (X-Ray Diffraction) analyses were used to characterize the topology and structure of oriented NPD films. The multi-source meter was used to observe the current-voltage characteristics of the ITO (Indium-Tin Oxide) / NPD (4,4'bis[N-(1-napthyl)-N-phenyl-amino]-biphenyl) / Al (Aluminum) device. While NPD thin films deposited under magnetic field were not molecularly well aligned according to the XRD results, the films after post-deposition annealing at $130^{\circ}C$ were well-oriented. AFM images show that NPD thin films deposited under magnetic field had a smoother surface than those deposited without magnetic field. The current-voltage performance of NPD thin films was improved due to the enhanced electron mobility in the well-aligned NPD films.

Second Order Nonlinear Optical Polyimides Containing Organic Chromophores with an Oxadiazole Segment (옥사디아졸 결합의 유기 발색단이 도입된 이차비선형 광학 이미드 고분자)

  • Do, Jung Yun;Kim, Bong Gun;Kwon, Ji-Yun
    • Applied Chemistry for Engineering
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    • v.18 no.1
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    • pp.77-83
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    • 2007
  • It is essential that second order nonlinear optical materials have low optical propagation losses in the wavelengths of second harmonic generation for practical applications in waveguides. Three dipolar chromophores substituted with nitro, cyano, and alkyl sulfone as an electron withdrawing group were prepared. The UV-Vis absorption spectra of the cyano and alkylsulfone chromophores showed a blue-shift compared to the nitro chromophore. The introduction of oxadiazole segment in the chromophore structure led to similar spectral shift. The blue-shift can produce low optical loses at second harmonics. The chromophores were successfully attached to a polyimide, yielding side chain polymers. The nonlinear optical property of the prepared optical polymers was determined by measuring electro-optic coefficient at 1.55 mm. The polymers exhibited high glass transition temperature of over $185^{\circ}C$ and thermal stability to $300^{\circ}C$ through differential scanning calorimeter analysis and thermal gravimetric analysis.

Effect of applied current density on the corrosion damage with galvanostatic corrosion experiment of aluminum alloy for ship (선박용 알루미늄 합금의 정전류 부식 시험에 의한 부식 손상에 미치는 인가 전류밀도의 영향)

  • Kim, Yeong-Bok;Park, Il-Cho;Lee, Jeong-Hyeong;Kim, Seong-Jong
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.106-106
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    • 2018
  • 해양환경용 선박재료는 전기화학적인 부식을 발생시키는 염소이온($Cl^-$)이 다량 포함된 부식 환경에 장기간 노출되어 있어 부식에 대해 취약하다. 따라서 우수한 내식성 및 내침식성을 가진 재료를 선정하는 것은 매우 중요하다. 알루미늄 합금은 충분한 강도와 부동태 피막 형성으로 인해 내식성이 우수하여 해양환경용 선박 재료로서 널리 이용되고 있으며, 이에 따른 부식 특성에 관한 연구도 활발히 이뤄지고 있다. 그러나 선박에서는 부식에 의한 손상뿐만 아니라 전식에 의한 부식 손상도 발생할 수 있다. 특히 선미 부분은 프로펠러의 동합금과 알루미늄 합금의 이종금속 간 전위차에 의한 전식이 발생하여 선체의 다른 부위에 비해 부식이 더 심하게 진행될 수도 있다. 또한 전식은 해안 부두에 접안된 선박의 용접 시미주전류(stray current)에 의한 부식손상이 발생할 수 있으나 이에 대한 연구는 미미한 실정이다. 따라서 본 연구는 해양환경에서의 전식을 인위적으로 모사할 수 있는 부식 정전류 시험법을 이용하여 다양한 크기의 전식 손상을 유발시켰으며, 해양환경 하에서 선박재료로 주로 사용되는 알루미늄 합금인 Al5083-H321, Al5052-O, Al6061-T6에 대한 전식 특성을 비교, 분석하였다. 실험 방법으로 작동전극은 각 재료의 시험편을 $2cm{\times}2cm$ 으로 절단하여 sand paper # 2000 번까지 연마 후 아세톤과 증류수로 세척하고 건조하였으며, 제작된 시험편은 자체 제작한 홀더를 이용하여 $1cm^2$만 노출시킨 후 정전류 가속 실험을 실시하였다. 기준전극은 은/염화은(Ag/AgCl) 전극을, 대응전극은 백금(Pt) 전극을 사용하였다. 정전류 가속 조건은 $0.001mA/cm^2$, $0.1mA/cm^2$, $1mA/cm^2$, $5mA/cm^2$, $10mA/cm^2$의 전류 밀도를 천연해수에서 30분간 인가하였다. 각 재료에 대한 전식 특성은 실험 전후의 무게 감소량으로 전식의 저항 특성을 확인하였다. 그리고 3D 현미경으로 표면 손상 경향과 깊이를 측정하였으며, 주사전자현미경 (SEM)을 통해 표면 형상을 미시적으로 관찰하였다. 부식 정전류 시험 결과 모든 시편에서 $0.01mA/cm^2$에서 미세한 국부적인 부식이 일어났으며, 전류밀도가 증가할수록 표면 전반에 부식이 진행되고 성장하였다. 그리고 모든 인가 전류밀도의 조건에서 Al6061-T6가 5000계열(Al5083-H321, Al5052-O)보다 더 우수한 내식성을 나타났다.

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Electrocatalytic Effect of Dioxygen Reduction at Glassy Carbon Electrode Modified with Schiff Base Co(II) Complexes (Schiff Base Co(II) 착물이 변성된 유리질 탄소전극에서 산소 환원의 전기촉매 효과)

  • Seong, Jeong-Sub;Chae, Hee-Nam;Choi, Yong-Kook
    • Analytical Science and Technology
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    • v.11 no.6
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    • pp.460-468
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    • 1998
  • Schiff base ligands such as $SOPDH_2$, $SNDH_2$, $EBNH_2$, and $PBNH_2$ and their Co(II) complexes such as [$Co(II)(SND)(H_2O)_2$], [$Co(II)(SOPD)(H_2O)_2$], [$Co(II)(EBN)(H_2O)$], and [$Co(II)(PBN)(H_2O)$] have been synthesized. The mole ratio of Shiff base ligand to cobalt(II) for the Co(II) complexes was found to be 1:1. Also these complexes have been configurated with hexa-coordination. Reduction of dioxygen was investigated by cyclic voltammetry at glassy carbon electrodes modified with Schiff base Co(II) complexes in 1 M KOH aqueous solution. At modified glassy carbon electrode with Schiff base Co(II) complexes, reduction peak current of oxygen was increased and peak potential was shifted to more positive direction compared to bare glassy carbon electrode. The electrokinetic parameters such as number of electron and exchange rate constant were calculated from the results of cyclic voltammogrms. The reduction of dioxygen at glassy carbon electrode has been $2e^-$ reaction pathway. Exchange rate constant at glassy carbon electrode modified with Co(II) complexes was increased 2~10 times compared to bare electrode.

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Biomimetic Analysis on the Spider Silk Apparatus for Designing the Nanofiber-spinning Nozzle (나노섬유 방사노즐 설계를 위한 거미 실크 방적장치의 생체모사 분석)

  • Moon, Myung-Jin;Kim, Hoon;Park, Jong-Gu
    • Applied Microscopy
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    • v.42 no.2
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    • pp.67-76
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    • 2012
  • The biomimetic approach on the cuticular spinning nozzles of the major ampullate silk glands in the golden-web spider Nephila calvata has been attempted using various visualizing techniques of light and electron microscopes to improve the design of spinning nozzle for producing synthetic nanofibers spun from electrospinning apparatus. The major ampullate spigot which has the most effective nozzle system to produce nanofibers for dragline silk with high strength and elasticity is connected via the bullet type spigot on anterior spinneret with flexible terminal segment. The excretory duct which transports the liquid silk feedstock from ampulla to spigot is divided into 3 limbs by loops back on itself to form an S-shape morphology that is bundled in connective tissue. Final diameter of the nanofibers at nozzle was dramatically reduced by gradual narrowing of duct cuticle less than 10 times comparing to its original size of funnel region. Moreover, the funnel has a characteristic cuticular organization with porous microstructure which seems to be related to water removal from feedstock of silk precursors. High magnification electron micrographs also reveal the presence of the spiral grooves on the surface of the cuticular intima near the valve which presumed to reduce friction during rapid flow of liquid silk.

Chemical Analysis and Thermoelectric Properties of the PbSnTe Semiconductors (화학조성에 따른 PbSnTe계 반도체의 열전특성조사)

  • Oh, Kyu-Whan;Oh, Seung-Mo
    • Applied Chemistry for Engineering
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    • v.1 no.1
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    • pp.83-90
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    • 1990
  • The semiconducting $(Pb_1\;_xSn_x)_1$ $_yTe_y$, one of the low - temperature thermoelectric materials, has been prepared and its chemical composition and nonstoichiometry has been analyzed. The content of Pb in the specimens was determined by the complexometric back - titration method with EDTA and Pb(II) standard solutions. Te - content was analyzed with the redox titration method. The electrical conductivity and the thermoelectric power have also been measured by the DC 4 - probe and the heat-pulse technique, respectively. All of the specimens showed a nonstoichiometric behavior in their chemical compositions (Te excess), thus gave rise to a p - type semiconducting property, and the nonstoichoimetry became bigger as the Sn - content increased. The thermoelectric power vs. temperature results have been analyzed upon the basis of the Fermi level vs. temperature profiles in the saturation regime. The specimen of x=0.1 evolved a transition from p - to n - type property at about 670K, which has been explained by the fact that the mobility of electrons is bigger than that of holes in the temperature range of the intrinsic regime.

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Implementation of Low Frequency Welding Pre-heating System Using Induction Heating (유도가열 기법을 이용한 저주파 용접예열 시스템 구현)

  • Yang, Juyeong;Kim, Soochan;Park, Junmo
    • Journal of the Institute of Convergence Signal Processing
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    • v.19 no.2
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    • pp.61-67
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    • 2018
  • Welding preheating means that the surface of the base material to which the metal is welded before the main welding is heated to a constant temperature. It prevents the cracks of the adjacent influences such as reduction of material hardening degree by controlling the cooling rate, suppression of segregation of impurities, prevention of thermal deformation, and moisture removal. For this reason, it is a necessary operation for high quality welding. Induction heating is an efficient heating method that converts electric energy into heat energy by applying electromagnetic induction phenomenon. Compared with combustion heat generated by gas and liquid, it is clean, stable, and economical as well as rapid heating. It can be heated regardless of the shape, depth and material of the heating body by modifying the shape of the frequency and the coil with a simple structure. In this paper, we implemented a low frequency welding preheating system using induction heating technique and observed the temperature changes of coil resistance, inductance and automotive transmission parts according to the height of each transmission in winding coil for three kinds of automotive transmission parts. We confirmed that the change of current is a very important factor in the low frequency heating.

Structural and Electrochemical characterization of LiCoO2 Nano Cathode Powder Fabricated by Mechanochemical Process (기계 화학법에 의해 제작된 나노 LiCoO2 양극 분말의 구조 및 전기화학적 특성)

  • Choi, Sun-Hee;Kim, Joo-Sun;Yoon, Young-Soo
    • Journal of the Korean Ceramic Society
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    • v.41 no.1
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    • pp.86-91
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    • 2004
  • $LiCoO_2$ cathode powders with round particle shaped and nano grain sized of 70-300nm were synthesized by a mechanochemical method. The surface of Li-Co precursor prepared by freeze drying method was modified by $K_2SO_4$ coating and ball milling was used for the coating process. The precursor was crystallized to high temperature form of $LiCoO_2$ at $800^{\circ}C$ and the grain growth was inhibited by the $K_2SO_4$ coating effect. The $K_2SO_4$ coating was not decomposed at $800^{\circ}C$ and prevented the contact in the Li-Co precursor particles. The nano-sized $LiCoO_2$ powder had tetragonal phase and it affected the Li diffusion through the surface of particles. It means that the anode materials for hight performance battery should be satisfied not only small particle size but phase contol on the surface of particles. In this study, the powder characteristics and rate capabilities were compared with a commercial powder and the nano-sized $LiCoO_2$ powder fabricated by the mechanochemical method. And the crucial factor which affects on battery performance was also examined.