• Title/Summary/Keyword: spectroscopic techniques

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Effect of Solution Annealing Heat Treatment on the Localized Corrosion Resistance of Inconel 718 (Inconel 718의 국부 부식 저항성에 미치는 용체화 열처리의 영향)

  • Yoonhwa Lee;Jun-Seob Lee;Soon Il Kwon;Jungho Shin;Je-hyun Lee
    • Corrosion Science and Technology
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    • v.22 no.5
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    • pp.359-367
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    • 2023
  • The localized corrosion resistance of the Ni-based Inconel 718 alloy after solution heat treatment was evaluated using electrochemical techniques in a solution of 25 wt% NaCl and 0.5 wt% acetic acid. Solution heat treatment at 1050 ℃ for 2.5 hours resulted in an increased average grain diameter. Both Ti carbides (10 ㎛ diameter) and Nb-Mo carbides (1 - 9 ㎛ diameter) were distributed throughout the material. Despite heat treatment, the shape and composition of these carbides remained consistent. An increase in solution temperature led to a decrease in pitting potential value. However, the pitting potential value of solution heat-treated Inconel 718 was consistently higher than that of as-received Inconel 718 at all tested temperatures. Localized corrosion initiation occurred at 0.4 VSSE in a temperature environment of 80 ℃ for both as-received and solution heat-treated Inconel 718 alloys. X-ray photoelectron spectroscopic analysis indicated that the composition of the passive film formed on specimen surfaces remained largely unchanged after solution heat treatment, with O1s, Cr2p3/2, Fe2p3/2, and Ni2p3/2 present. The difference in localized corrosion resistance between as-received and solution heat-treated Inconel 718 alloys was attributable to microstructural changes induced by the heat treatment process.

Non-contact Stress Measurement in Steel Member using Piezospectroscopy (압분광법을 이용한 강재의 비접촉식 응력측정)

  • Kim, Jongwoo;Kim, Namgyu
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.23 no.3
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    • pp.92-95
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    • 2019
  • In this paper, a novel laser-based non-contact and non-destructive stress measurement technique is newly proposed for measuring stress in steel structural members. As the demand of stress monitoring in structural members is increased, various non-destructive techniques are being applied to the field of structural health monitoring. Spectroscopic techniques are non-contact technique and widely used for chemical identification of target materials. Especially, piezospectroscopic technique is a residual stress measurement technique in thermal barrier coatings. Although the piezospectroscopic technique has high possibility of measuring structural stress in steel members, the technique has been rarely applied to this field. In this paper, piezospectroscopy-based stress measurement technique is, therefore, proposed for measuring stress in steel structural member. To do that, alumina particles have been coated onto a specimen of a structural steel rod using a thermal spray coating technique. And then, an uniaxial compression test has been conducted to the specimen to collect each fluorescence spectrum under different loading conditions. Finally, the linear relation of spectral shift and applied compressive stress of the specimen has been experimentally established.

Study on Manufacturing Techniques and Conservation for Earthenware Horn Cups with a Horse Head Decoration(Treasure) (보물 도기 말머리장식 뿔잔의 제작 기법 연구와 보존처리)

  • KWON, Ohyoung;HAM, Chulhee;YU, Jia;KIM, Hanseul;PARK, Changyuel
    • Korean Journal of Heritage: History & Science
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    • v.55 no.1
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    • pp.51-61
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    • 2022
  • Earthenware horn cups with horse head decorations were excavated from Tomb No. 7 of Bokcheon-dong, Dongraegu, Busan Metropolitan City. Made of earth in the shape of a horn, these cups are considered to have been used to drink alcohol or beverage. Large numbers of earthenware horn cups of various shapes were excavated from tombs located in the old territories of Silla and Gaya. A pair of earthenware horn cups were excavated from Tomb No. 7, and the two cups are almost identical in overall shapes and manufacturing techniques despite different sizes. Conservation treatment was carried out for the bigger one of the two horn cups this time. There are two cracks toward the horse head decorations around the mouth with missing parts observed. The chest of the horse touches the ground with one side decorating the horse head and the other side facing the conical mouth of the horn cup. It is in the U shape, striking a balance based on two legs attached behind. The surface of the horn cup was made with a potter's wheel, and the connection to the horse head has traces of cutting and trimming. The horse head is expressed realistically with its features including the ears, eyes, nose, and mouth well apprehended and its color is grey This study intended to investigate manufacturing techniques of the artifact by examining its internal structure through the condition survey in a non-destructive way. CT imaging was used to figure out its manufacturing techniques and to diagnose its condition, and accordingly the scientific conservation treatment was conducted to stabilize the artifact. The precise diagnosis on conservation condition found that there are two chips in the spout with their cracks extended. One of the chips is connected with separation added to the crack. The material which has been used for connection in the past was collected for the infrared spectroscopic analysis, which was identified to be nitrocellulose resin for the connection. Therefore, this conservation treatment focused on removing the old material and preventing the spread of cracks. Before conservation treatment, the condition survey and scientific examination for the artifact were carried out to secure data about the earthenware horn cup with horse head decorations(Treasure). Based on them, effective plans for its conservation treatment was sought for and then existing adhesive was safely removed, and restoration material was selected to take into account its reversibility. In addition, the conservation treatment according to optimal methodologies was conducted through the consultation meeting with experts.

Optical Properties of Oxotitanium (Ⅳ) Meso-tetrakis(4-sulfonatophenyl)porphyrin Intercalated into the Layered Double Hydroxides (LDH) Studied by Laser Spectroscopy

  • Ryu, Su-Young;Yoon, Min-Joong;Choy, Jin-Ho;Hwang, Sung-Ho;Frube, Akihiro;Asahi, Tsuyoshi;Hiroshi, Masuhara
    • Bulletin of the Korean Chemical Society
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    • v.24 no.4
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    • pp.446-452
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    • 2003
  • Some new nanohybrid materials have been synthesized by intercalating the oxotitanium(IV) meso-tetrakis(4- sulfonatophenyl) porphyrin$(O=Ti^{(IV)} TSPP)$ into the Zn/Al layered double hydroxides (LDHs), and their structures and photophysical properties have been investigated by various laser spectroscopic techniques. According to the XRD pattern of the synthesized nanohybrid materials, the macrocycle plane of $O=Ti^{(IV)}$ TSPP are grafted perpendicular to the LDH layers. The $O=Ti^{(IV)}$ TSPP-intercalated LDH exhibits band broadening of the absorption spectrum and a blue shift of Q-band as compared to that observed in solution. Resonance Raman spectral measurements demonstrate that the positively charged LDHs give rise to a slight decrease of the electronic density of the porphyrin ring accompanying a small change of the electronic distribution of the $O=Ti^{(IV)}$ TSPP. Consequently the LDH environment affects the energies of the two highest occupied molecular orbitals (HOMOs) of the $O=Ti^{(IV)}$) TSPP, $a_{1u}$ and $a_{2u}$, producing a mixed orbital character. Being consistent with these electronic structural changes of $O=Ti^{(IV)}$ TSPP in LDH, both the fluorescence spectral change and the fsdiffuse reflectance transient measurements imply that the photoexcitation of the $O=Ti^{(IV)}$ TSPP intercalated into LDH undergoes fast relaxation to the O=Ti(IV) $TSPP^+-LDH^- $charge transfer (CT) state within a few picoseconds, followed by a photoinduced electron transfer between the O=Ti(IV) TSPP and LDHs with a rate constant greater than %1×10^{10}S^{-1}$. No evidence is found for back electron transfer. In conclusion, the $O=Ti^{(IV)}$ TSPP intercalated LDH seems to be a possible candidate for an artificial reaction center for an efficient solar energy conversion system.

Antitumor Activity and Nephrotoxicity of the Novel Platinum(II) Coordination Complex (새로운 Platinum (II) Complex [Pt (II)(trans-d-dach)(DPPE)] $(NO_3)_2$의 항암효과 및 신독성에 관한 연구)

  • Jung Jee-Chang;Lee Moon-Ho;Chang Sung-Goo;Rho Young-Soo
    • The Korean Journal of Pharmacology
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    • v.31 no.1 s.57
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    • pp.103-114
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    • 1995
  • Platinum coordination complexes are currently one of the most compounds used in the treatment of solid tumors. However, its use is limited by severe side effects such as renal toxicity. Our platinum-based drug discovery program is aimed at developing drugs capable of diminishing toxicity and improving antitumor activity. We synthesized new Pt (Ⅱ) complex analogue containing 1,2-diaminocyclohexane (dach) as carrier ligand and 1,2-bis(diphenylphosphino) ethane (DPPE) as a leaving group. Furthermore, nitrate was added to improve the solubility. A new series of [Pt(trans-ddach)(DPPE).$2NO_3(PC)$ was synthesized and characterized by their elemental analysis and by various spectroscopic techniques [infrared (IR), $^{13}carbon$ nuclear magnetic resonance (NMR)]. PC demonstrated acceptable antitumor activity aganist P388, L-1210 lymphocytic leukemia cells and SK=OV3 human ovarian adenocarcinoma cells, and significant. activity as compared with that. cisplatin. The toxicity of PC was found quite less than thar of cisplatin using MTT, $[^3H]$ thymidine uptake and glucose consumption tests in rabbit proximal tubule cells, human kidney cortical cells and human renal cortical tissues. Based on these results, this novel platinum compound represent a valuable lead in the development of a new anticancer chemotherapeutic agent capable of improving antitumor activity and low toxicity.

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Real-time monitoring for blending uniformity of trimebutine CR tablets using near-infrared and Raman spectroscopy (근적외분광분석법과 라만분광분석법을 이용한 트리메부틴말레인산 서방정의 혼합 과정 모니터링)

  • Woo, Young-Ah
    • Analytical Science and Technology
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    • v.24 no.6
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    • pp.519-526
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    • 2011
  • Chemometrics using near-infrared (NIR) and Raman spectroscopy have found significant uses in a variety quantitative and qualitative analyses of pharmaceutical products in complex matrixes. Most of the pharmaceutical can be measured directly with little or no sample preparation using these spectroscopic methods. During pharmaceutical manufacturing process, analytical techniques with no or less sample preparation are very critical to confirm the quality. This study showed NIR and Raman spectroscopy with principal component analysis (PCA) was very effective for the blending processing control. It is of utmost importance to evaluate critical parameters related to quality of products during pharmaceutical processing. The blending is confirmed by off-line determination of active pharmaceutical ingredient (API) by a conventional method such as high performance liquid chromatography (HPLC) and UV spectroscopy. These analytical methods are time-consuming and ineffective for real time control. This study showed the possibility for the determination of blend uniformity end-point of CR tablets with the use of both NIR and Raman spectroscopy. The samples were acquired from six positions during blending processing with U-type blender from 0 to 30 min. Using both collected NIR and Raman spectral data, principal component analysis (PCA) was used to follow the uniformity of blending and finally determine the end-point. The variation of homogeneity of six samples during blending was clearly found and blend uniformity end-point was successfully confirmed in the domains of principal component (PC) scores.

In vitro Antitumor Activity of Ergosterol Peroxide Isolated from Cordyceps militaris on Cancer Cell Lines from Korean Patients (Cordyceps militaris로부터 분리한 Ergosterol Peroxide의 한국인 암세포주에 대한 항암작용)

  • Kim, Ha-Won;Kim, Young-Ho;Cai, Xing Fu;Nam, Kyong-Suk;Lee, Seung-Jung;An, Hye-Suk;Jeong, Eun-Ho;Yun, Seung-Hyun;Sung, Su-Kyong;Lee, Sung-Jin;Hyun, Jin-Won
    • The Korean Journal of Mycology
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    • v.29 no.1
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    • pp.61-66
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    • 2001
  • Entomopathogenic fungus of Cordyceps militaris is famous of its medicinal efficacies. An antitumor compound was purified from the n-hexane extract of artificially cultivated fruiting bodies of C. militaris and identified as ergosterol peroxide $(5{\alpha},\;8{\alpha}-epidioxy-24(R)-methylcholesta-6,22-dien-3{\beta}-o1,\; C_{28}H_{44}O_3)$ mainly by $^1H\;and\;^{13}C-NMR$ spectroscopic techniques. When the antitumor activity of ergosterol peroxide was measured against 3 tumor cell lines from Korean cancer patients, it showed the most strong activity against gastric cancer SNU-l cell line 3 days after treatment. The 50% inhibitory concentrations $(IC_{50})$ of ergosterol peroxide 6 days after treatment were $75.8{\mu}g/ml$ for human gastric SNU-1 tumor cell line, $39.7{\mu}g/ml$ for human colorectal SNU-C4 tumor cell line and $32.7{\mu}g/ml$ for human hepatoma SNU-354 cell line.

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NIS quality analysis of pre- and post-harvest sugarcane.

  • Johnson, Sarah E.;Berding, Nils
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1621-1621
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    • 2001
  • The quality of sugarcane grown on the NE Australian tropical coast ($16^{\circ}$15'- $18^{\circ}$15' S Lat.) has declined markedly in the past seven years. This has been linked to dilution of mill-supply cane with increasing levels of non mature-stalk material consisting of leaves and sucker culms. The prime research objective was to examine the transition from the pre-harvest, in-field crop to harvested material sent for processing, in terms of quality and crop fraction proportions. A secondary objective was to quantify the effects of preharvest-season crop habit and culm condition on crop quality. Ten quadrat samples from each of 54 random crop sites (17 in 1999 and 37 in 2000), covering a wide range of variables (cultivar, crop class, and edaphic, topographic, climatic, and temporal factors) were collected immediately before harvest. Samples were partitioned into four fractions:- sound and unsound mature stalks (culms), sucker culms, and extraneous matter (leaves). Material harvested from each site was sampled and partitioned into four fractions:- sound and unsound billets (culm pieces), culm-spindle pieces, and leaf. In 2000, before harvest, 14 additional sites were sampled monthly, on three occasions, from March - June. Erect and non-erect culms were divided into sound and unsound classes. All samples were disintegrated and presented to a remote reflectance module of a scanning spectrophotometer using the BSES large cassette module. Near infra-red spectroscopic (NIS) analyses were developed for the rapid determination of quality components (Brix, commercial cane sugar (CCS), fibre, moisture, and polariscope reading). Calibrations for three material groups (culm (n = 639), non-culm (n = 496), and combined) were developed for all components using the 1999 data set. Two sub-sets (n = 178, and 190) of about 10% of the preharvest-season and harvest populations scanned in 2000 also were subjected to full routine laboratory analyses. The 1999 combined calibrations were excellent, but the culm calibrations produced consistently lower standard errors. Non-culm calibrations were marginally better than the combined for only CCS and pol. reading. Analysis of the 2000 culm data with calibrations using all 1999 and 2000 culm data resulted in better predictions relative to the 1999 culm calibrations. This also was true for the combined calibrations. Assessment of quality components in pre- and post-harvest sugarcane using NIS calibrations was more cost effective than using routine laboratory techniques. Outcomes from this NIS-facilitated research will have important economic consequences for the Australian sugarcane industry. Potential CCS present in mature culms is being discounted by dilution with leaves and sucker culms, threatening farm viability. The results question the efficacy of current harvesting technology. The CCS of harvested cane is improved only marginally over that of the in-field crop. Current harvesting technology requires either supplementary, innovative pre-mill processing or a design revolution to improve mill-supply cane quality, and therefore whole of industry economics. NIS-facilitated analyses, before the harvest season, highlighted the benefits of growing erect, sound crops. Loss of CCS then, can be minimized only by a combination of crop improvement and agronomic solutions, applied as part of sound on-farm management.

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Adsorption Characteristics of Nitrogen monoxide over Dealuminated and Alkali/Alkaline-earth Metal ion Exchanged Y-Zeolites (탈알루미늄 및 알칼리/알칼리토금속 양이온을 교환한 Y형 제올라이트의 NO흡착 특성)

  • Kim, Cheol-Hyun;Lee, Chang-Seop
    • Journal of the Korean Institute of Gas
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    • v.9 no.4 s.29
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    • pp.17-25
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    • 2005
  • The dealuminated and alkali/alkaline-earth metal exchanged Y-zeolites were prepared as a catalyst. Elemental compositions and structures of the prepared catalysts were analyzed by the various spectroscopic techniques such as inductively coupled plasma-atomic emission spectroscopy(ICP-AES), X-ray fluorescence(XRF) and X-ray diffraction(XRD), and the desorption behaviors of adsorbed species on the catalyst surfaces were investigated via NO-TPD experiment. Comparing with the composition of the starting material of NaY zeolite, the magnitudes of Si/Al ratio in catalytic materials were increased after dealumination. The Si/Al ratio of catalytic materials after dealumination followed by Cs and Ba cation exchange were additionally decreased. Dealumination to catalysts induced a destruction of basic frame due to a detachment of aluminum, which results in reducing framework structure, while increasing non-framework structure. This phenomenon becomes more serious with increasing time of steam treatment and even more significant for the cation exchanged catalysts. In NO-TPD experiments, the desorption peaks of NO which indicates an activity point of catalysts shifted to the low temperature region after dealumination and cation exchange. The desorption peaks of the NO-TPD profiles taken after steam treatment also shifted to the low temperature region as the steam treatment time increased. In dealuminated and cation exchanged Y-zeolites, the catalytic activities were more influenced by exchanged cation and the formation of non-framework structure.

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A New Class of Platinum (II) Complexes [Pt (trans-1-daeh) (DPPP)] $2NO_3$ and [Pt (trans-1-daeh)(DPPE)] $2NO_3$ Exhibiting Antitumor Activity and Nephrotoxieity (새로운 Platinum (II) Complex ([Pt (II)(trans-1-dach)(DPPP)] $(NO_3)_2$와 [Pt (II)(trans-1-dach)(DPPE)] $(NO_3)_2$의 항암효과 및 신독성에 관한연구)

  • Jung, Jee-Chang;Yoon, Chin-Hee;Chang, Sung-Goo;Lee, Kyung-Tae;Rho, Young-Soo
    • The Korean Journal of Pharmacology
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    • v.29 no.2
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    • pp.283-295
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    • 1993
  • Pt-complexes is currently one of the most compounds used in the treatment of solid tumors. However, its used is limited by severe side effects such as renal toxicity. Our platinum-based drug discovery program is aimed at developing drugs capable of diminishing toxicity and improving antitumor activity. We synthesized new Pt (II) complex analogues containing 1, 2-diaminocyclohexane (dach) as carrier ligand and 1, 3-bis (diphenylphosphino) propane (DPPP)/1,2-bis (diphenylphosphino) ethane (DPPE) as a leaving group. Furthermore, nitrate was added to improve the solubility. A new series of (KHPC-001) [Pt (trans-1-dach)(DPPP)] $2NO_3$ and (KHPC-002) [Pt (trans-1-dach)(DPPE)] $2NO_3$ were synthesized and characterized by their elemental analysis and by various spectroscopic techniques [infrared (IR), $^{13}carbon$ nuclear magnetic resonance (NMR)]. KHPC-001 and KHPC-002 demonstrated acceptable antitumor activity aganist P-388, L-1210 lymphocytic leukemia cells and significant activity as compared with that of cisplatin. The toxicity of KHPC-001 and KHPC-002 was found quite less than that of cisplatin using MTT, $[^3H]$ thymidine uptake and glucose consumption tests in rabbit proximal tubule cells and human kidney cortical cells.

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