• Carbon letters
• /
• v.12 no.4
• /
• pp.229-235
• /
• 2011

Isotactic polyacrylonitrile (PAN) with triad isotacticity of 0.53, which was determined by $^{13}C$ NMR, using dialkylmagnesium as an initiator, was successfully synthesized. Isothermal treatment of iso-PAN was conducted in air at 200, 220, 250 and $280^{\circ}C$. Structural evolutions and chemical changes were studied with Fourier transformation infrared and wide-angle X-ray diffraction during stabilization. A new parameter $CNF={I_{2240cm}}^{-1}/ ({I_{1595cm}}^{-1}+f^*{I_{1595cm}}^{-1})$ was defined to evaluate residual nitrile groups. Crystallinity and crystal size were calculated with X-ray diffraction dates. The results indicated that the nitrile groups had partly converted into a ladder structure as stabilization proceeded. The rate of reaction increased with treatment temperature; crystallinity and crystal size decreased proportionally to pyrolysis temperature. The iso-conversional method coupled with the Kissinger and Flynn-Wall-Ozawa methods were used to determine kinetic parameters via differential scanning calorimetry analysis with different heating rates. The active energy of the reaction was 171.1 and 169.1 kJ/mol, calculated with the two methods respectively and implied the sensitivity of the reaction with temperature.

• Journal of the Korean Wood Science and Technology
• /
• v.23 no.3
• /
• pp.1-7
• /
• 1995

The crystal transformation from cellulose I to cellulose II during alkaline swelling of waste wood, which has been used for cultivating oak mushroom(Cortinellus edodes (Berk.) Ito et Imai), was investigated and compared to that of normal wood by a series of X-ray diffraction analysis. When the sapwood of cultivated wood was treated with 20% NaOH solution for 2 hours, the cellulose I can be easily transformed into Na-cellulose I than normal wood or heartwood of cultivated wood. Certainly the formation of Na-cellulose in wood is proportional to alkali swelling duration, and the formation of cultivated sapwood was faster than that of the other woods. Cellulose I in the sapwood of cultivated wood was easily transformed into cellulose II during mercerization, but the sapwood of normal wood and the heartwood of cultivated wood hardly converted to cellulose II. Namely, most of Na-cellulose I in normal wood can be reconverted to cellulose I in the process of washing and drying. Therefore, it can be concluded from this study that in cell wall lignin and hemicellulose can prevent the alkaline swelling of cellulose in wood and the transformation from cellulose I to cellulose II as well.

• Bulletin of the Korean Chemical Society
• /
• v.30 no.5
• /
• pp.1021-1025
• /
• 2009

A novel supramolecular network containing binuclear copper unit $[Cu(phen)_{2}({\mu}-ID\;A)Cu(phen){\cdot}(NO_{3})](NO_{3}){\cdot}4(H_{2}O)$ (1) was synthesized through the self-assembly of iminodiacetic acid ($H_2IDA$) and 1,10-phenanthroline (phen) in the condition of pH = 6. It has been characterized by the infrared (IR) spectroscopy, elemental analysis, single crystal X-ray diffraction, and thermogravimetric analysis (TGA). 1 shows a 2-D supramolecular structure assembled through strong and unique $\pi-\pi$ packing interactions. Density functional theory (DFT) calculations show that theoretical optimized structures can well reproduce the experimental structure. The TGA and powder X-ray diffraction (PXRD) curves indicate that the complex 1 can maintain the structural integrity even at the loss of free water molecules. The magnetic property is also reported in this paper.

• YAKHAK HOEJI
• /
• v.12 no.3_4
• /
• pp.41-49
• /
• 1968

The optimum reaction conditions for the preparation of the precipitated calcium carbonate of an average particle size of 0.05.mu. in diameter was set in which the Box-Wilson Plan was applied. The reaction conditions are as follows; 1) concentration of milk of lime; 6.56% w/w 2) temperature; 14.24.deg. C #) velocity of carbon dioxide introducing; 1.95l/min. The crystal form was found that of calcite in X-ray diffraction analysis. The particle size was determined by the sedimentation volume measurement. The shape was identified by the elctron micro-diffraction pattern and the electron microscopic photographs.

• Journal of the Mineralogical Society of Korea
• /
• v.32 no.4
• /
• pp.287-301
• /
• 2019

Preservation of the original form is the principle for conservation, management and utilization of cultural heritages. Thus, non-destructive analysis of these samples are important field of the conservation science. In this study, examined the applicability of nondestructive surface X-ray diffraction analysis (ND-XRD) for cultural heritage by materials (rock specimen, jade stone, pigment painted specimen, earthen artifact, metal artifact). In result, all type of sample is recorded suitable X-ray diffraction patterns for identifying mineral composition in case of surface condition with adequate particle size and arrangement. And diffraction pattern is reflected surface information than matrix. Therefore, ND-XRD is thought to be applicable not only mineral identification but also interpretation of manufacturing technique and alteration trend about layered sample (in horizontally or vertically). Whereas some exceptional diffraction patterns were recorded due to overlapping information on specific crystal planes. It caused by skip the sample treatment (powdering and randomly orientation). It could be advantageously used for mineral identification, such as preferred orientation of clay minerals. In contrast, irregular diffraction pattern caused by single crystalline effect is required careful evaluation.

• Proceedings of the Korean Vacuum Society Conference
• /
• 2016.02a
• /
• pp.379.2-379.2
• /
• 2016

The Ni oxide/PVP nanofibers were synthesized by sol-gel and electrospinning technique. The obtained Ni oxide/PVP (polyvinylpyrrolidone) nanofibers were calcined to remove the PVP compound at 873 and 1173 K. The Ni oxide/PVP nanofibers were analyzed by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). The SEM images showed that the mat form was prepared by calcination of Ni oxide/PVP nanofibers at 873 K. And the crystal structure of Ni oxide at 1173 K was also confirmed by SEM images. XRD results shows the crystallinity of metallic Ni and NiO. TEM images also verified the crystal phase of Ni and Ni oxide. XP spectra revealed that the oxidation state of Ni to conclude the chemical composition of Cu oxide nanofibers.

• Korean Journal of Pharmacognosy
• /
• v.27 no.3
• /
• pp.207-211
• /
• 1996

Cumambrin A has been isolated from the dried flowers of Chrysanthemum boreale Makino. The complete $^1H$ and $^{13}C$ NMR assignment of cumambrin A was achieved from two-dimensional $^1H$-$^1H$ COSY and $^{13}C$-$^1H$ COSY spectra with the aid of homonuclear and heteronuclear double resonance experiments. The its structure has been verified by single crystal X-ray diffraction.

• Archives of Pharmacal Research
• /
• v.8 no.1
• /
• pp.1-6
• /
• 1985

The crystal structure or $\gamma$-hydroxy-$\betha$-aminobutyric acid was determined by MULTAN system with X-ray intensity data on a diffractometer and refined by the least-squares method to an R-value 0.034 for 711 reflections. The crystals were orthorhombic, space group $P2_{1}2_{1}2_{1}$, Z = 4, with a = 10.220, b = 8.257 and c = 6.556$\AA$. The molecule takes the zwitterionic form and skeletal conformation is trans-transform. The molecules are held together by intra-and intermolecular NH-O and OH--O hydrogen bonds.

• Bulletin of the Korean Chemical Society
• /
• v.18 no.1
• /
• pp.38-43
• /
• 1997

Poly(ethylene 2, 6-naphthalate-co-tetramethylene 2, 6-naphthalate) (PEN/PBN) copolymers were synthesized and studied by 13C NMR spectroscopy, DSC analysis and X-ray diffraction. A minimum in the melting point vs. composition curve was found at approximately 60 mol% tetramethylene 2, 6-naphthalate. The PEN/PBN copolymers were shown to be statistically random throughout the range of 1, 4-butanediol compositions. The melting point depression behavior of annealed PEN/PBN copolymers depended upon the sequence propagation probability, PS, which is suggested by indivisual crystal formation of two pure comonomers; that is, ethylene-naphthalate-ethylene, EE, and tetramethylene-naphthalate-tetramethylene, BB. However, it can be seen from the X-ray curve that the peaks of PEN/PBN copolymers appear from a crystal lattice which is governed only by the rich component between two different aliphatic units in the copolymer composition.

• Bulletin of the Korean Chemical Society
• /
• v.12 no.5
• /
• pp.525-529
• /
• 1991

A simple route is described for the selective functionalization of calixarene at the para positions of phenyl rings. Calix[4]arene tetraacetate 2, obtained from the treatment of calix[4]arene with acetic anhydride, undergoes Fries rearrangement to yield the diametrically para substituted p-diacetylcalix[4]arene 3 in 80% yield. The crystal and molecular strucutre has been determined by X-ray diffraction method. The crystals are orthorhombic, space group Pna21, with a = 11.121 (3), b = 10.374 (3), c = 21.690 (6) $\AA$ and Z = 4. The structure was solved by direct method and refined by full-matrix least-squares methods to final R of 0.036 for 1795 observed reflections. Each hydroxyl hydrogen atom is disordered over two positions. The macrocycle exists in the cone conformation which is determined by the strong circular intramolecular flip-flop type hydrogen bonds of phenolic OH, while crystal packing effects of the diametrically para-acetyl substituents seem to be responsible for the distortion of the cone conformation.