• Analytical Science and Technology
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• v.7 no.3
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• pp.379-386
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• 1994

The elution behaviors in reversed-phase liquid chromatography were investigated thermodynamically for 2-hydroxy-arylazopyrazolone chelates with Ni(II), Cu(II), Co(III), Cr(III) on Novapak $C_{18}$ column. There was a good linear dependence of the capacity factor(k') on the variations of column temperature in van't Hoff plot. From this result, it was confirmed that the retention mechanism of these chelates in the reversed phase liquid chromatography system was invariant under the condition of various temperatures. For the most cases of the chelates studied, the dependence of capacity factor(1n k') on enthalpy$(-{\Delta}H)^{\circ}$, calculated by van't Hoff plot showed a good linearity(r=0.980~0.999) except [Pm(2-OH_(5-Cl)PaPz](r=0.787) and also the compensation temperatures(${\beta}$) showed constant values. The range of compensation temperature values calculated from the slope of $-{\Delta}H^{\circ}$ vs 1n k' plots was 374.3~806.9K. It was suggested that the retention of metal-2-hydroxy-arylazopyrazolone chelates in the reversed phase liquid chromatography system was largely affected by the hydrophobic effect.

• Korean Chemical Engineering Research
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• v.59 no.2
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• pp.296-303
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• 2021

The objective of this study is to investigate the applicability of a Cu-supported honeycomb catalyst as a catalyst for decomposition of a low toxic liquid propellant based on ammonium dinitramide (ADN). A mixture of copper, lanthanum, and alumina was supported on the honeycomb support by wash coating to prepare a Cu-La-Al/honeycomb catalyst. We elucidated that the effect of metal loading on the physicochemical properties of Cu-La-Al/honeycomb catalyst and catalytic performance in decomposition of the ADN-based liquid propellant. As the number of wash coatings increased, the amount of active metal Cu was increased to 4.1 wt%. The BET surface area of the Cu-La-Al/honeycomb catalyst was in the range of 3.1~4.1 ㎡/g. The micropores were hardly present in Cu-La-Al/honeycomb catalysts, however, the mesopores and macropores were well developed. The Cu (2.7 wt%)-La-Al/honeycomb catalyst exhibited the highest activity in the decomposition of the ADN-based liquid propellant, which is attributed to the largest surface area, the largest pore volume, and the well-developed mesopores and macropores.

• Analytical Science and Technology
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• v.7 no.1
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• pp.103-114
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• 1994

The elution behaviors of Ni(II), Cu(II), Co(II), and Cr(II) in 1-phenyl-3-methyl-4(2-hydroxy-5-X-phenylazo)-5-pyrazolone, [Pm(2-OH)(5-X)PaPz](X=H, $CH_3$, $NO_2$, Cl) chelates have been studied by reversed phase HPLC. Thirteen metal-[Pm(2-OH)(5-X)PaPz] chelates were prepared and characterized by UV, IR, MS, and ICP spectroscopic methods. These metal-2-hydroxyarylazopyrazolone chelates were successfully separated on Novapak-$C_{18}$ column using methanol/water mixtures as a mobile phases. It was found that the chelates were eluted properly in an acceptable range of the capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of the capacity factor(log k') on the volume fraction of water in the binary mobile phase showed a good linearity. Also, there was a good linear dependence of the capacity factor on the liquid-liquid extraction distribution ratio($D_c$) in methanol-water/n-pentadecane extraction system by the batch method. It suggested that the retention of the chelates in the reverse phase liquid chromatographic system be largely due to the solvophobic effect.

• Analytical Science and Technology
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• v.5 no.4
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• pp.389-399
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• 1992

Liquid Chromatographic behavior of Pd(II) in Isonitrosoethylacetoacetate lmine, $Pd(IEAA-NR)_2$ (R=H, $CH_3$, $C_2H_5$, $n-C_3H_7$, $C_6H_5-CH_2$, $n-C_4H_9$) chelates were investigated by reversed-phase HPLC on Micropak MCH-5 column using methanol/water as mobile phase. The optimum conditions for the separation of $Pd(IEAA-NR)_2$ chelates were examined with respect to the effect of the flow rate, sample solvent, mobile phase strength and column temperature. It wass found that metal chelates were properly eluted in an acceptable range of capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of the logarithm of capacity factor(k') on the volume fraction of water in the binary mobile phase was examined. Also, the dependence of k' on the liquid-liquid extration distribution ratio($D_c$) in methanol-water/n-alkane extration system was investigated. Both kinds of dependence are linear, which susggests that the retention of the electroneutral metal chelate is largely due to the solvophobic effect. Standard adsorption enthalpy changes (${\Delta}H^{\circ}$) and standard adsorption entropy changes (${\Delta}S^{\circ}$) of Pd(II) Isonitrosoethylacetoacetate imine chelates on Micropak MCH-5 column were calculated by measuring capacity factor with changing temperature of the column.

• Analytical Science and Technology
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• v.6 no.1
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• pp.107-119
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• 1993

The purpose of this study is to investigated the elution behavior of platinoid metal acetylacetonates, which is the key to elucidate their retention mechanism and optimize their RPLC separation conditions. The retention data of four platinoid metal acetylacetonates have been measured on four different columns in methanol-water and acetonitrile-water systems. The retention of uncharged platinoid metal acetylacetonates is interpreted by solvophobic effect. The retention of platinoid metal acetylacetonates is also greatly influenced by the geometric structure of the complexes. The square planar chelates, $Pd(acac)_2$, $Pt(acac)_2$, are retained longer than the octahedral chelates, $Rh(acac)_3$, $Ir(acac)_3$. It is likely due to that square planar chelates show greater interaction with nonpolar stationary phase than octahedral chelates. The results of van't Hoff plots have shown that platinoid metal acetylacetonates is operated on the same retention mechanism in the temperature range of $25{\sim}45^{\circ}C$. The study of the retention mechanism by the enthalpy-entropy compensation phenomenon has indicated that the retention mechanism of octahedral chelates and square planar chelates do not vary with the composition change of methanol-water mobile phase, respectively. In acetonitrile-water mobile phase, however, the retention mechanism is observed to be more complicated. Optimum condition for the separation of four platinoid metal acetylacetonates is found to be 40% methanol, polymeric C18 column, and $45^{\circ}C$.

• Clean Technology
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• v.26 no.3
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• pp.196-203
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• 2020

In this study, a Cu/hexaaluminate catalyst was prepared by a co-precipitation method, and then a binder was added to form a pellet. A catalyst in which Ni and Ru promoters were added to a Cu/hexaaluminate pellet catalyst was prepared. This study focused on examining the effect of the addition of Ni and Ru promoters on the properties of Cu/hexaaluminate catalysts and the decomposition reaction of ADN-based liquid monopropellants. Cu/hexaaluminate catalysts had few micropores and well-developed mesopores. When Ru was added as a promoter to the Cu/hexaaluminate pellet catalyst, the pore volume and pore size increased significantly. In the thermal decomposition reaction of ADN-based liquid monopropellant, the decomposition onset temperature was 170.2 ℃. Meanwhile, the decomposition onset temperature was significantly reduced to 93.5 ℃ when the Cu/hexaaluminate pellet catalyst was employed. When 1% or 3% of Ru were added as a promoter, the decomposition onset temperatures of ADN-based liquid monopropellant were lowered to 91.0 ℃ and 83.3 ℃, respectively. This means that the Ru promoter is effective in lowering the decomposition onset temperature of the ADN-based liquid monopropellant because the Ru metal has excellent activity in the decomposition reaction of ADN-based liquid monopropellant, simultaneously contributing to the increase of the pore volume and pore size. After the thermal treatment at 1,200 ℃ and decomposition of ADN-based liquid monopropellant were repeatedly performed, it was confirmed that the addition of Ru could enhance the heat resistance of the Cu/hexaaluminate pellet catalyst.

• Journal of Industrial Technology
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• v.5
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• pp.21-26
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• 1985

본(本) 연구(硏究)는 주조(鑄造) 및 용접(溶接)을 통하여 제작(製作)된 화력발전용(火力發電用) 대형(大型)밸브에 발생한 결함(缺陷)의 원인(原因)을 규명하기 위하여 사용(使用)된 몇가지 기술에 대하여 언급하였다. 초음파(超音波) 비파괴검사(非破壞檢査)로써 내재(內在)되어 있는 균열의 위치(位置) 및 길이를 예측(豫測)하였다. 균열의 근원(根源)을 다치지 않게 보존(保存)한 채로 시험편(試驗片)에 대(對)하여 기계적 절단(絶斷)을 행하였다. 또한 균열의 원인(原因)을 직접 관찰할 수 있도록 액체 질소에서 낙추법(落錘法)을 써서 파단(破斷)시켰다. 동시(同時)에 균열의 측면양상(側面樣相)과 미세조직(微細組織)과의 관계를 금속현미경 및 전자현미경(SEM)을 통하여서 관찰하였다. 결론적으로 제조시(製造時) 도입(導入)된 결함(缺陷)은 용접과정중에 만들어진 것이 아니라 주조작업중(鑄造作業中)에 용융금속(溶融金屬)의 공급부족(共給不足)으로 인(因)하여 생긴 기공(氣孔)에서 출발(出發)하였음을 알 수 있었다.

• Journal of the KSME
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• v.28 no.4
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• pp.313-321
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• 1988

어떤 구조물이 반복하중을 받으면 피로파괴를 일으킨다. 만일 이 구조물이 부식환경 속에 앗 으면 불활성 분위기나 공기 중에서 보다 빨리 파괴에 이르게 된다. 이러한 현상을 흔히 부식 피로라고 한다. 부식피로에 크게 영향을 미치는 변수들을 대략 기계적 변수, 금속학적 변수, 환경 변수로서, 기계적 변수에는 최대응력 확대계수, 응력확대계수범위, 응력비, 반복하중 주파수, 반복하중파형, 응력상태, 잔류응력, 균열의 크기 및 모양 등이 있으며 금속학적 변수로는 합금 조성, 합금원소와 불순물의 분포, 미세조직과 결정구조, 열처리, 소성가공, 집합조직 등이며 환 경변수에는 온도, 환경의 형태(기체, 액체), 부식성분의 분압 또는 농도, 전기화학적 전위, pH, 수용성 환경의 점성, 피복, 부식억제제 등이 있다. 이와 같이 부식환경 속에 있는 구조물의 파 손을 이해하기 위하여는 응력부식과 부식피로를 공부하여야 한다. 이 현상은 매우 복잡한 문 제이기 때문에 아직도 완전히 이해되지 않은 상태이고 따라서 중요한 연구대상이 되고 있다. 여기서는 응력부식과 부식피로의 파괴역학적인 측면을 소개하고자 한다.

• Proceedings of the Korea Society for Energy Engineering kosee Conference
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• 2002.11a
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• pp.111-116
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• 2002

고온의 소듐을 냉각재로 사용하는 풀형 액체금속로인KALIMER[1]는 기존의 경수로에 비해 고온에서 운전되므로, 잔열제거계통은 공기 자연순환에 의해 격납용기(CV) 외벽을 직접 냉각하는 방식의 PSDRS(Passive Safety-grade Decay Heat Removal System)[1]를 사용하며, 특히 고온의 구조물 표면온도에 의해 대류전열 외에도 복사전열과정이 활발히 일어난다.(중략)

• Proceedings of the Korean Institute of Industrial Safety Conference
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• 2000.11a
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• pp.88-94
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• 2000

최근 플라스틱공업, 유기합성공업, 금속분체공업 및 사료공업 등의 기술이 진보함에 따라서 원료 및 제품을 분체로 취급하는 공정은 현저하게 증가되고 있는 실정이며, 미립자의 제조, 분쇄, 건조, 분급, 혼합 등의 신공정에서는 유동이나 부유상태로 취급하거나 고온 분위기하에서 처리하는 경우가 많다. 그리고 이에 수반하여 분진폭발 위험성이 상당히 인식되고는 있으나 가스 또는 액체에 의한 폭발 위험성만큼 충분히 알려져 있지 않고 있다. /sup 1)/ 분진에 대한 최초의 폭발기록/sup 2)/은 1785년 이탈리아의 제분공정에서 일어난 사고였다.(중략)