• 제목/요약/키워드: Instrumental characterization

검색결과 34건 처리시간 0.032초

Comparing of 5-Nonylsalicylaldoxime and Salicylaldehyde Characterization Using Magnesium Salt Formylation Process

  • Pouramini, Zeinab;Moradi, Ali
    • 대한화학회지
    • /
    • 제56권3호
    • /
    • pp.357-362
    • /
    • 2012
  • 5-Nonylsalicylaldoxime and salicylaldehyde are two derivatives of phenolic compounds which are very applicable materials in industries. Formerly the formylation of phenolic derivatives were carried out by Rimer-Tiemann method. In this work both of these two materials were synthesized by magnesium meditated formylation technique and their structural characterizations were compared by instrumental analysis technique. In order to achieve a selectively orthoformylated product, the hydroxyl group of nonylphenol (or phenol) was first modified by magnesium methoxide. The nonylphenol magnesium salt was then formylated by paraformaldehyde. The oximation reaction was finally applied to the prepared nonylsalicylaldehyde magnesium salt by liquid extracting via water and acid washing and other extractions. The solvent was finally removed by evaporation under reduced pressure. Some instrumental analysis such as $^1H$-NMR, GC/MS and FT-IR spectra were taken on the product in order to interpret the reaction characterization quantitatively and qualitatively. The formaldehyde and oxime functional groups of two compounds were investigated through $^1H$-NMR and FT-IR spectra and were compared. The yield of methoxilation was very good and the yields of formylation and oximation reactions were about 90%and 85% respectively. The orthoselectivity of formylation reaction were evaluated by comparing of the relevant spectra. The GC/MS spectra also confirmed the obtained results.

기기분석에 의한 염료 구조 및 무기배합제 조성에 대한 접근 (Instrumental Characterization of Dyes and their Inorganic Additives)

  • 최은경;이은경;조영달
    • 한국섬유공학회:학술대회논문집
    • /
    • 한국섬유공학회 2002년도 봄 학술발표회 논문집
    • /
    • pp.139-142
    • /
    • 2002
  • Color Index의 염료 분류 방법은 chemical type에 따라 25개 구조 분류(예로, 아조, 안트라퀴논, tryarylmethane 등) 그리고, 염료의 응용 범위에 따라 19개 속명(Acid, Direct, Disperse, Reactive 등)을 사용한다. 상품화되어 있는 수많은 염료는 현재 생산 회사의 상품명과 Color Index generic name을 보편적으로 사용하고 있으나, 체계적인 화학명은 복잡할 뿐 만 아니라, 상업적 이유로 많은 경우 밝히지 않고 있다. (중략)

  • PDF

A Study on the Characterization on Some Semiconuctor Materials by Neutron Activation Analysis. Characterization of Semiconductor Silicon

  • 이철;권오천;김호근;이종두;정구순
    • Bulletin of the Korean Chemical Society
    • /
    • 제10권1호
    • /
    • pp.30-32
    • /
    • 1989
  • Traces of nine elements, gold, arsenic, cobalt, chromium, copper, europium, hafnium, sodium and antimony in commercially available silicon crystals were determined by the instrumental neutron activation analysis using the single comparator method. The values of the concentrations of these elements in both single and polycrystals were found to decrease significantly to a low limiting level by simply washing and etching surface contaminants having been introduced during various steps of sample preparation and irradiation. However, the chromium levels in polycrystals were not easily decreased, these depending upon the cutting tools employed. The Sb-doped content in each semiconductor has been compared with the associated quantities such as the concentration and the conductivity range given by the sample donor. Uncertainty in the sodium analysis due to the fission neutron reaction by silicon itself was discussed.

Analysis of Zirconium and Nickel Based Alloys and Zirconium Oxides by Relative and Internal Monostandard Neutron Activation Analysis Methods

  • Shinde, Amol D.;Acharya, Raghunath;Reddy, Annareddy V.R.
    • Nuclear Engineering and Technology
    • /
    • 제49권3호
    • /
    • pp.562-568
    • /
    • 2017
  • Background: The chemical characterization of metallic alloys and oxides is conventionally carried out by wet chemical analytical methods and/or instrumental methods. Instrumental neutron activation analysis (INAA) is capable of analyzing samples nondestructively. As a part of a chemical quality control exercise, Zircaloys 2 and 4, nimonic alloy, and zirconium oxide samples were analyzed by two INAA methods. The samples of alloys and oxides were also analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES) and direct current Arc OES methods, respectively, for quality assurance purposes. The samples are important in various fields including nuclear technology. Methods: Samples were neutron irradiated using nuclear reactors, and the radioactive assay was carried out using high-resolution gamma-ray spectrometry. Major to trace mass fractions were determined using both relative and internal monostandard (IM) NAA methods as well as OES methods. Results: In the case of alloys, compositional analyses as well as concentrations of some trace elements were determined, whereas in the case of zirconium oxides, six trace elements were determined. For method validation, British Chemical Standard (BCS)-certified reference material 310/1 (a nimonic alloy) was analyzed using both relative INAA and IM-NAA methods. Conclusion: The results showed that IM-NAA and relative INAA methods can be used for nondestructive chemical quality control of alloys and oxide samples.

Characterization of neutron spectra for NAA irradiation holes in H-LPRR through Monte Carlo simulation

  • Kyung-O Kim;Gyuhong Roh;Byungchul Lee
    • Nuclear Engineering and Technology
    • /
    • 제54권11호
    • /
    • pp.4226-4230
    • /
    • 2022
  • The Korea Atomic Energy Research Institute (KAERI) has designed a Hybrid-Low Power Research Reactor (H-LPRR) which can be used for critical assembly and conventional research reactor as well. It is an open tank-in-pool type research reactor (Thermal Power: 50 kWth) of which the most important applications are Neutron Activation Analysis (NAA), Radioisotope (RI) production, education and training. There are eight irradiation holes on the edge of the reactor core: IR (6 holes for RI production) and NA (2 holes for NAA) holes. In order to quantify the elemental concentration in target samples through the Instrumental Neutron Activation Analysis (INAA), it is necessary to measure neutron spectrum parameters such as thermal neutron flux, the deviation from the ideal 1/E epithermal neutron flux distribution (α), and the thermal-to-epithermal neutron flux ratio (f) for the irradiation holes. In this study, the MCNP6.1 code and FORTRAN 90 language are applied to determine the parameters for the two irradiation holes (NA-SW and NA-NW) in H-LPRR, and in particular its α and f parameters are compared to values of other research reactors. The results confirmed that the neutron irradiation holes in H-LPRR are designed to be sufficiently applied to neutron activation analysis, and its performance is comparable to that of foreign research reactors including the TRIGA MARK II.

하이브리드 증착 시스템을 이용한 나노복합체 Ti-Si-N 박막의 특성 연구 (Characterization of Nanocomposite Ti-Si-N Films Prepared by a Hybrid Deposition System of A If and Sputtering Techniques)

  • 윤순영;최성룡;이미혜;김광호
    • 한국표면공학회지
    • /
    • 제36권2호
    • /
    • pp.122-127
    • /
    • 2003
  • Ti - Si - N hard films were deposited on SKD11 steel substrates by a hybrid deposition system, where TiN was deposited by AIP method while Si was incorporated by sputtering one. The microstructure of Ti-Si-N films was revealed to be a composite of TiN crystallites and amorphous Si3N4 by instrumental analyses. The highest hardness value of about 45 Gpa was obtained at the Si content of around 7.7 at.%. With increase of Si content, the size of TiN crystallites was reduced and their distribution was changed from aligned to randomly orientated states. Surface roughness of Ti-Si-N film also decreased with increase of Si content.

하이브리드 증착 시스템에 의해 합성된 나노복합체 Ti-Al-Si-N 박막의 미세구조와 기계적 특성 (Microstructural and Mechanical Characterization of Nanocomposite Ti-Al-Si-N Films Prepared by a Hybrid Deposition System)

  • 박인욱;최성룡;김광호
    • 한국표면공학회지
    • /
    • 제36권2호
    • /
    • pp.109-115
    • /
    • 2003
  • Quaternary Ti-Al-Si-N films were deposited on WC-Co substrates by a hybrid deposition system of arc ion plating (AIP) method for Ti-Al source and DC magnetron sputtering technique for Si incorporation. The synthesized Ti-Al-Si-N films were revealed to be composites of solid-solution (Ti, Al, Si)N crystallites and amorphous Si3N4 by instrumental analyses. The Si addition in Ti-Al-N films affected the refinement and uniform distribution of crystallites by percolation phenomenon of amorphous silicon nitride, similarly to Si effect in TiN film. As the Si content increased up to about 9 at.%, the hardness of Ti-Al-N film steeply increased from 30 GPa to about 50 GPa. The highest microhardness value (~50 GPa) was obtained from the Ti-Al-Si-N film haying the Si content of 9 at.%, the microstructure of which was characterized by a nanocomposite of nc-(Ti,Al,Si) N/a$-Si_3$$N_4$.

Preparation and Characterization of Silk Fibroin Nanoparticles

  • Kweon, Hae-Yong;Yeo, Joo-Hong;Woo, Soon-Ok;Han, Sang-Mi;Jo, You-Young;Lee, Kwang-Gill
    • International Journal of Industrial Entomology and Biomaterials
    • /
    • 제20권1호
    • /
    • pp.25-28
    • /
    • 2010
  • Silk fibroin was conjugated with methoxypoly(ethylene glycol) derivatives to prepare silk nanoparicles. Conjugation of SF with PEG was examined with various instrumental analyses. Nuclear magnetic resonance spectrometry and amino acid analysis showed that serine and tyrosine residues in SF were reacted with PEG and resulted in increasing molecular weight. The sizes and shapes of SF nanoparticles observed by transmission electronmicroscope were ranged about 150-400 nm in diameter and spherical morphology. UV/VIS spectrometry showed SF nanoparticles might be outer PEG and inner SF structure.

3Y-TZP의 기계적 특성에 미치는 산화물 조성 및 첨가제의 영향 (Effects of Composition and Additives on the Mechanical Characteristics of 3Y-TZP)

  • 박미정;양성구;강종봉
    • 한국세라믹학회지
    • /
    • 제43권10호
    • /
    • pp.640-645
    • /
    • 2006
  • Monoclinic zirconia and yttria were mixed with a stoichiometric composition of 3Y-TZP (3 mol% Yttria-stabilized Tetragonal Zirconia Polycrystal). The specimen was sintered at 1350$\sim$1450$^{\circ}C$ and mechanical characterization and microstructure analysis were conducted. Microhardness and fracture toughness were shown as 1357.4 Hv and 8.56 MPa $m^{1/2}$. respectively. Without alumina, they were 1311 Hv and 10.02 MPa $m^{1/2}$ respectively. By mixing two different oxides, it was possible to obtain high values of microhardness and fracture toughness. It was possible that was turned out nano-scale particle using the co-milling of high mechanical energy.

Synthesis and Characterization of Phthalocyaninatometal (PcM, M=$Fe^{2+}$, $Co^{2+}$ Complexes with Monodenate Aromatic Isocyanide Ligands

  • 임윤묵;박하선;송수호;박찬조;유하일;이종기;양현수
    • Bulletin of the Korean Chemical Society
    • /
    • 제20권6호
    • /
    • pp.701-704
    • /
    • 1999
  • Metallophthalocyanines [PcM, Pc: phthalocyanine, M: Fe 2+ , Co 2+ ] were reacted with α-isocyanonaphthalene( α-in) and α-isocyanoanthracene (α-ia) to form monomeric complexes. The synthesis and coordination behaviour of the isocyanides as a ligand (L) are discussed. All the products were characterized by spectroscopic methods and instrumental analysis. The electrical conductivities of these complexes, which were not treated with dopant, were attributed to the metal-ligand electron delocalization in the PcML2 complexes. The complexes have an enlarged macrocycle where the π-electron back donating ability of PcM is stronger than the σ-electron coordinating ability of the isonitrile ligands. Their electrical conductivities were measured as σRT = 2.1×10 -9 ~3×10 -10 S/cm. Also thermal stability was investigated in this study.