• Textile Coloration and Finishing
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• v.6 no.2
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• pp.24-29
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• 1994

In order to investigate the crystallization in silk fibroin induced by acid treatment and its photo-yellowing reduction effect. silk fibroin were immersed in PH 3.5~4.0 sulfuric acid and 0.01N hydro-chloric acid at 2$0^{\circ}C$, and the changes of crystallinity were measured by infrared spectroscopy, X-ray diffraction. Yellowness index caused by UV irradiation were also observed. The results are as follows : 1. ${\beta}$-form transition occurs when the silk fibroin are immersed at 2$0^{\circ}C$ in pH 3.5~4.0 sulfuric acid and 0.01N hydro-chloric acid. Formation of new hydrogenbond in molecules on the amorphous region induced ${\beta}$-form structure, and increased crystallinity. 2. Crystallization owing to $\beta$-form transition reduced the initial yellowness index by ultraviolet irradiation.

• Fashion & Textile Research Journal
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• v.4 no.2
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• pp.198-202
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• 2002

Degummed silk from Bombyx mori was dissolved in 9.3M lithium bromide solution. The regenerated silk fibroin films were completely ${\alpha}$-randomcoil type as shown by x-ray diffraction and infrared spectroscopy. The structural changes in silk fibroin induced by immersion into methanol and dilute hydrochloric acid and its photo-yellowing effect was studied. The changes of crystallinity were measured by infrared spectrometer. Yellowness index caused by ultraviolet irradiation were observed as a function of the structural change on silk fibroin. On treatment with methanol, ${\alpha}$-randomcoil silk film is converted to the ${\beta}$-form structure. After the treatment of hydrochloric acid on ${\beta}$-form structure in silk induced by immersion into methanol, ${\beta}$-form in silk fibroin is partially decreased. Crystallization owing to ${\beta}$-form transition reduced the initial yellowness index by ultraviolet irradiation. A little ${\beta}$-form structure in silk fibroin increased the initial yellowness in comparison with more ${\beta}$-form structure.

• Journal of Sericultural and Entomological Science
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• v.37 no.2
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• pp.142-153
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• 1995

This study is undertaken to investigate proper condition and dissolution method of silk fibroin to use it functional material as powder or membrane. Silk fibroin was dissolved with calcium chloride ethanol aqueous solution and hydrochloric acid. When silk fibron was dissolved with calcium chloride ehanol aqueous solution, main chain of silk fibroin was degradaded and molecular conformation was changed. Silk fibroin powder was made from silk fibroin solution. It showed lower thermal decomposition temperature and crystallinity than those of native silk fibroin. And Its molecular conformation was random coil structure. By acid gydrolysis, main chain of silk fibroin was attacked randomly. Silk fibroin powder from hydrolysate showed high crystallinity and thermal decomposition temprature. $\beta$-form molecular conformation was found by IR and X-ray diffraction. Silk fibroin powder form dissolved part with hydrochloric acid showed low thormal decomposition temperature but high crystallinity. During acid hydrolysis, transition of molecular structure of silk fibroin occurred, and it changed to $\alpha$-helix. Silk fibroin film was achieved by casting silk fibroin solution by ehanol solution or saturated vapor treatment, and its molecular conformation changed to $\beta$structure.

• Textile Coloration and Finishing
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• v.9 no.6
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• pp.18-25
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• 1997

The change of crystalline structure and mechanical properties of i-PP films which had before isothermally annealed at various temperature and times have been studied. The following results were abtain The crystallinity and crystallite size of the samples showed increasing above the annealing temperature of 13$0^{\circ}C$ and these are equilibrated after an annealing time of 30min. When the crystalline form was at annealling condition were below 13$0^{\circ}C$, 2min, subsequently achieving an $\alpha$, $\beta$ mixing form and at 13$0^{\circ}C$, 10min, the crystalline form entered an $\alpha$ form transition. It is achieved a typical $\alpha$ form at 15$0^{\circ}C$. The value of T'm was increasing until 13$0^{\circ}C$ but it was not founded at 15$0^{\circ}C$. The slopes which represented crystalline form in an Avrami plot differed from each other within the range of this experiment.

• Journal of Pharmaceutical Investigation
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• v.35 no.4
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• pp.279-285
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• 2005

Ground CS-891 (N-[1-(4-methoxyphenyl)-1-methylethyl]-3-oxo-4-aza-5a-androst-1-ene-$17{\beta}$-carboxamide) of poorly water soluble drug was obtained using a Heiko Seisakusho model TI-100 vibration mill, and samples with different crystallinity were prepared at mixture ratios of 10:0, 7:3, 5:5, 3:7 and 0:10 (intact;ground CS-891). Physicochemical characterizations were obtained using qualitative and quantitative X-ray diffractometry, different scanning calorimetry (DSC), scanning electron microscopy (SEM), Quantasorb surface area analyzer, and controlled atmosphere microbalance. With increase of amorphous CS-891 in mixture ratios, the intensities of X-ray diffraction peaks of crystalline CS-891 were decreased, whereas surface area, water absorption, and exothermic peaks in DSC were increased. The apparent solubility of ground CS-891 was $4.4\;{\mu}g/ml$ and the solubility of intact CS-891 was $3.1\;{\mu}g/ml$ at $37{\pm}1^{\circ}C$. The apparent precipitation rates of CS-891 in a supersaturated solution during the solubility test were increased with an increase of amorphous CS-891, and a crystalline form of CS-891 transformed from amorphous CS-891 after the solubility test was found by X-ray diffraction analysis, DSC and SEM. The dissolution profiles of CS-891 with different crystallinity at $37{\pm}1^{\circ}C$ by the USP paddle method were investigated, and the apparent dissolution rate constant of ground CS-891 was about 5.9-fold higher than that of intact CS-891. A linear relationships between the crystallinity of CS-891 and the apparent dissolution rate constant (r>0.96) were obtained.

• Journal of the Korean Society of Industry Convergence
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• v.2 no.2
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• pp.61-68
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• 1999

The variety of crystalline structure and mechanical properties of PP filament treated with dry heat treatment at different draw ratio has been studied. Crystalline structure and mechanical properties of annealed PP filament at different draw ratio has been examined by XRD, UTM, and density method. Heat treatment has been carried out $100^{\circ}C$, $120^{\circ}C$ $140^{\circ}C$ for 30min. in dry oven. From the results of this study, it found the following facts. It was found that the crystallinity and crystallite size of (110) plane of sample were increased with increasing of annealed temperature and draw ratio. The crystalline form of annealed sample which was undrawn showed ${\alpha}$, ${\beta}$ mixing form below $120^{\circ}C$ and showed ${\alpha}$ form at $140^{\circ}C$. But the crystalline form of annealed sample which was drawn showed ${\alpha}$ form at $120^{\circ}C$. Initial modulus and tensile strength were increased with increasing of annealing temperature, and the degree of orientation was decreased with decreasing of annealing temperature.

• Journal of the Korean Ceramic Society
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• v.41 no.12 s.271
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• pp.921-928
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• 2004

Calcium phosphate powders have been prepared by using $Ca(OH)_2\;and\;H_{3}PO_4$ solution under various conditions such as pH, calcination temperature, and reaction time. ${\beta}-TCP({\beta}-tricalcium phosphate)$and HAp(hydroxyapatite) were synthesized at pH=5.21 and pH > 7.62, respectively. From XRD results, $Ca(OH)_2\;and\;H_{3}PO_4$ solution reacted quickly to form HAp, which was structurally stable up to 16h. Calcination temperature having good crystallinity is revealed to be at $1200^{\circ}C$. SEM analysis showed that ${\beta}-TCP$ and HAp with needle type were synthesized at pH 5.21 and pH 7.62, respectively. However, at pH 9.16, tiny and homogeneous HAp having sphere was prepared and rearranged to show needle morphology. HAp synthesized at pH 9.16 was utilized as bonechina body and calcined. The sample was analyzed its crystallinity, water absorbtion, color, and shape to check physical properties.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.13 no.2
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• pp.56-62
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• 2003

Epitaxial $Bi_4Ti_3O_{12}$ films on $SrTiO_3$(100), L$aA1O_3$(100) and MgO(100) were prepared by sol-gel process using metal naphthenate as a starting material. As-deposited films were pyrolyzed at $500^{\circ}C$ for 10 min In air and annealed at $750^{\circ}C$ for 30 min in air. Crystallinity and in-plane alignment of the film were investigated by X-ray diffraction $\theta$-2$\theta$ scan and P scanning. A field emission-scanning electron microscope and an atomic force microscope were used for characterizing the surface morphology and the surface roughness of the film. The film prepared on MgO(100) showed the most poor crystallinity and in-plane alignment, compared to those on the other substrates. While the films on $LaA1O_3$(100) and $SrTiO_3$(100) having high crystallinity and in-plane alignment showed the form of columnar grain growth, the film on MgO(100) which had poor crystallinity showed the form of acicula grain growth.

• Journal of Pharmaceutical Investigation
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• v.39 no.2
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• pp.97-106
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• 2009

Although lovastatin (LS) is widely used in the treatment of hypercholesterolemia, its bioavailability is known to be around 5%. This study was aimed to increase the solubility and dissolution-permeation rates of LS using solid dispersions (SDs) with bile salts. The solubilities of LS in water, aqueous bile salt solutions and non-aqueous vehicles were determined, and effects of bile salts on the cellulose or duodenal permeation of LS from SDs were evaluated using a horizontal permeation system. SDs were prepared at various ratios of LS to carriers, such as sodium deoxycholate (SDC), sodium glycocholate (SGC) and/or 2-hydroxypropyl-$\beta$-cyclodextrin (HPCD). The addition of bile salts (25 mM) in water increased markedly the solubility of LS by the micellar solubilization. Some non-aqueous vehicles were effective in solubilizing LS. From differential scanning calorimetric studies, it was found that the crystallinity of LS in SDs disappeared, indicating a formation of amorphous state. The SDs showed markedly enhanced dissolution compared with those of their physical mixtures (PMs) and drug alone. In the dissolution-permeation studies using a cellulose membrane, the donor and receptor solutions were maintained as a sink condition using pH 7.0 phosphate buffer containing 0.05% sodium lauryl sulfate (SLS). The flux of LS alone was nearly same as that of LS-SDC-HPCD (1:3:6) PM. However, the flux of LS-SDC-HPCD (1:3:6) SD slightly increased compared with drug alone and PM, suggesting that entrapment of LS in micelles does not significantly hinder the permeation across cellulose membrane. In the dissolution-duodenal permeation studies using a LS-HPCD-SDC (1:3:6) SD, the addition of various bile salts in donor solutions (25 mM) enhanced the permeation of LS markedly, and the fluxes were found to be $0.69{\pm}0.41$, $0.87{\pm}0.51$, $0.84{\pm}0.46$, $0.47{\pm}0.17$ and $0.68{\pm}0.32{\mu}g/cm^2/hr$ for sodium cholate (SC), SDC, SGC, sodium taurodeoxycholate (STDC) and sodium taurocholate (STC), respectively. The stepwise increase of donor SGC concentration increased the flux dose-dependently. From the relationship of donor SGC concentration and flux, the concentration of SGC initiating the permeation across the duodenal mucosa was calculated to be 11.1 mM, which is nearly same as the critical micelle concentration (CMC, 11.6 mM) of SGC. However, with no addition of bile salts and below CMC, the permeation was very limited and irratic, indicating that LS itself is very poor permeable. Higher protions of bile salt in SD such as LS-SDC or LS-SGC (1 : 49 and 1 : 69) showed highly promoted fluxes. In conclusion, SD systems with bile salts, which may form their micelles in intestinal fluids, might be a promising means for providing enhanced dissolution and intestinal permeation of practically insoluble and non-absorbable LS.