• Title, Summary, Keyword: silanization

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Quantitative Analysis of the Degree of Silanization by the Ninhydrin Method and its Application to the Immobilization of GL-7-ACA Acylase and Cellulolytic Enzyme

  • Park, Seung-Won;Kim, Yong-In;Chung, Koo-Hun;Kim, Seung-Wook
    • Journal of Microbiology and Biotechnology
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    • v.11 no.2
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    • pp.199-203
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    • 2001
  • A simple quantitative method to measure the degree of silanization was developed, based on the reaction of ninhydrin with the silanization reagent (3-aminopropyltriethoxysilane, 3-APTES). At low concentrations (0.001-0.005%, v/v) of 3-APTES, a good linearity was obtained when 3-APTES reacted with undiluted ninhydrin for 30 min. On the other hand, at high levels of 3-APTES, a linearity was obtained when 3-APTES reacted with 3-fold diluted ninhydrin for 20 min. The reliability of regression curves mentioned above was expressed as a regression coefficient ($R^2$) of more than 0.99. Immobilization of different enzymes was introduced via silanization by using the 3-APTES in order to confirm the validity of the ninhydrin method. When yield for each step in the immobilizatio process were compared, yields of both glutaraldehyde and protein were founc to have the same tendency to silanization. These results shw that the ninhydrin method was suitable for quatitative analysis of silanization and that yields of immobilization could be pre-estimated by measuring silanization levels using the ninhydrin method.

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Effects of hydrogen peroxide pretreatment and heat activation of silane on the shear bond strength of fiber-reinforced composite posts to resin cement

  • Pyun, Jung-Hoon;Shin, Tae-Bong;Lee, Joo-Hee;Ahn, Kang-Min;Kim, Tae-Hyung;Cha, Hyun-Suk
    • The Journal of Advanced Prosthodontics
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    • v.8 no.2
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    • pp.94-100
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    • 2016
  • PURPOSE. To evaluate the effects of hydrogen peroxide pretreatment and heat activation of silane on the shear bond strength of fiber-reinforced composite posts to resin cement. MATERIALS AND METHODS. The specimens were prepared to evaluate the bond strength of epoxy resin-based fiber posts (D.T. Light-Post) to dual-curing resin cement (RelyX U200). The specimens were divided into four groups (n=18) according to different surface treatments: group 1, no treatment; group 2, silanization; group 3, silanization after hydrogen peroxide etching; group 4, silanization with warm drying at $80^{\circ}C$ after hydrogen peroxide etching. After storage of the specimens in distilled water at $37^{\circ}C$ for 24 hours, the shear bond strength (in MPa) between the fiber post and resin cement was measured using a universal testing machine. The fractured surface of the fiber post was examined using scanning electron microscopy. Data were analyzed using one-way ANOVA and post-hoc analysis with Tukey's HSD test (${\alpha}=0.05$). RESULTS. Silanization of the fiber post (Group 2) significantly increased the bond strength in comparison with the non treated control (Group 1) (P<.05). Heat drying after silanization also significantly increased the bond strength (Group 3 and 4) (P<.05). However, no effect was determined for hydrogen peroxide etching before applying silane agent (Group 2 and 3) (P>.05). CONCLUSION. Fiber post silanization and subsequent heat treatment ($80^{\circ}C$) with warm air blower can be beneficial in clinical post cementation. However, hydrogen peroxide etching prior to silanization was not effective in this study.

The senstivity characteristics of cholesterol sensor by immobilization methods of the enzyme (효소 고정화 방법에 따른 콜레스테롤 센서의 감도 특성)

  • Song, Min-Jung;Yoon, Dong-Hwa;Jin, Joon-Hyung;Min, Nam-Ki;Hong, Suk-In
    • Proceedings of the KIEE Conference
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    • pp.1935-1937
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    • 2003
  • 최근 콜레스테롤 센서는 전극 상에 효소를 고정화 하는 방식을 이용하여 센서의 집적도를 높이는 시도가 이루어지고 있다. 이러한 전극 상의 효소고정화 방식으로 entrapment, cross liking, covalently binding 등이 있다. 본 논문에서는 이러한 효소 고정화 방식-전도성 고분자인 P3MT를 사용하여 entrap시키는 방법과 silanization을 이용한 covalent bonding 시키는 방법-에 따른 전기화학 센서의 감도 특성에 관한 연구를 수행하였다. 전도성 고분자를 사용한 고정화 방법은 cyclic voltammograms으로 scan rate 10 mA/s, potential 0.5-1.3V의 조건하에서 P3MT를 Polymerization하고, 효소 고정화를 위해 chromoampermeter로 potential 0.6V에서 900초 동안 수행하였다. silanization을 이용한 covalent bonding 시키는 방법은 nitric acid로 Pt 전극표면을 산화시키고, APTER로 silanization 공정을 시행하였다. 효소 고정화를 위해 전해질로는 0.1M Phosphate buffer solution을 사용하여 cyclic voltammograms으로 scan rate 50 mA/s 전위 0.0-0.7V의 조건 하에서 수행하였다. 이 결과 전도성 고분자를 이용한 고정화 방법에서의 senstivity가 0.89 ${\mu}A/mM{\cdot}cm^2$이고, silanization을 이용한 효소 고정화 방법에서는 1.51 ${\mu}A/mM{\cdot}cm^2$였다. 이처럼 후자의 방법에서 더 좋은 감도 특성이 나타났다. 따라서, silanization을 이용한 고정화 방법이 센서 제작 방식으로 더 적합하다고 사료된다.

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Effects of post surface conditioning before silanization on bond strength between fiber post and resin cement

  • Mosharraf, Ramin;Ranjbarian, Parisa
    • The Journal of Advanced Prosthodontics
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    • v.5 no.2
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    • pp.126-132
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    • 2013
  • PURPOSE. Post surface conditioning is necessary to expose the glass fibers to enable bonding between fiber post and resin cement. The purpose of the present study was to evaluate the effect of different surface conditioning on tensile bond strength (TBS) of a glass fiber reinforced post to resin cement. MATERIALS AND METHODS. In this in vitro study, 40 extracted single canal central incisors were endodontically treated and post spaces were prepared. The teeth were divided into four groups according to the methods of post surface treatment (n=10): 1) Silanization after etching with 20% $H_2O_2$, 2) Silanization after airborne-particle abrasion, 3) Silanization, and 4) No conditioning (Control). Adhesive resin cement (Panavia F 2.0) was used for cementation of the fiber posts to the root canal dentin. Three slices of 3 mm thick were obtained from each root. A universal testing machine was used with a cross-head speed of 1 mm/minute for performing the push-out tests. Two-way ANOVA and Tukey post hoc tests were used for analyzing data (${\alpha}$=0.05). RESULTS. It is revealed that different surface treatments and root dentin regions had significant effects on TBS, but the interaction between surface treatments and root canal regions had no significant effect on TBS. There was significant difference among $H_2O_2$ + Silane Group and other three groups. CONCLUSION. There were significant differences among the mean TBS values of different surface treatments. Application of hydrogen peroxide before silanization increased the bond strength between resin cements and fiber posts. The mean TBS mean values was significantly greater in the coronal region of root canal than the middle and apical thirds.

Effect of silane activation on shear bond strength of fiber-reinforced composite post to resin cement

  • Kim, Hyun-Dong;Lee, Joo-Hee;Ahn, Kang-Min;Kim, Hee-Sun;Cha, Hyun-Suk
    • The Journal of Advanced Prosthodontics
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    • v.5 no.2
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    • pp.104-109
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    • 2013
  • PURPOSE. Among the surface treatment methods suggested to enhance the adhesion of resin cement to fiberreinforced composite posts, conflicting results have been obtained with silanization. In this study, the effects of silanization, heat activation after silanization, on the bond strength between fiber-reinforced composite post and resin cement were determined. MATERIALS AND METHODS. Six groups (n=7) were established to evaluate two types of fiber post (FRC Postec Plus, D.T. Light Post) and three surface treatments (no treatment; air drying; drying at $38^{\circ}C$). Every specimen were bonded with dual-curing resin cement (Variolink N) and stored in distilled water for 24 hours at $37^{\circ}C$. Shear-bond strength (MPa) between the fiber post and the resin cement were measured using universal testing device. The data were analyzed with 1-way ANOVA and by multiple comparisons according to Tukey's HSD (${\alpha}$=0.05). The effect of surface treatment, fiber post type, and the interactions between these two factors were analyzed using 2-way ANOVA and independent sample T-tests. RESULTS. Silanization of the FRC Postec Plus significantly increased bond strength compared with the respective non-treated control, whereas no effect was determined for the D.T. Light Post. Heat drying the silane coupling agent on to the fiberreinforced post did not significantly improve bond strength compared to air-syringe drying. CONCLUSION. The bond strength between the fiber-reinforced post and the resin cement was significantly increased with silanization in regards to the FRC Postec Plus post. Bond strength was not significantly improved by heat activation of the silane coupling agent.

Quantitative Analysis of Silanization Degree of Silica Nanoparticles Modified with Bis[3-(trimethoxysilyl)propyl]amine Coupling Agent (Bis[3-(trimethoxysilyl)propyl]amine 커플링제로 개질된 실리카 나노입자의 실란화도 정량 분석)

  • Jeon, Ha-Na;Kim, Jung-Hye;Ha, Ki-Ryong
    • Polymer(Korea)
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    • v.36 no.3
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    • pp.372-379
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    • 2012
  • In this study, we treated silica nanoparticles with bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to modify their surfaces. We investigated the effects of BTMA hydrolysis time, BTMA concentration and BTMA treatment time on the degree of silanization reaction of silica nanoparticles. We used Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to obtain quantitative data. We found the decrease of isolated Si-OH peak intensity at 3747 $cm^{-1}$ and the increase of $-CH_2 $stretching and bending peaks with increasing hydrolysis time, concentration and treatment time of BTMA. EA analysis results also supported this trend. We found a strong effect of BTMA concentration on the degree of silanization of the silica particles, but weak effects of the hydrolysis time and the treatment time.

Effect of 1,3-Diphenyl-guanidine (DPG) Mixing Step on the Properties of SSBR-silica Compounds

  • Lim, Seok-Hwan;Lee, Sangdae;Lee, Noori;Ahn, Byeong Kyu;Park, Nam;Kim, Wonho
    • Elastomers and Composites
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    • v.51 no.2
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    • pp.81-92
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    • 2016
  • 1,3-Diphenylguanidine (DPG) is commonly used as a secondary accelerator which not only acts as booster of cure but also activating silanization reaction. The aim of this study is to increase the interaction between silica and rubber by using DPG. In this study, mixing was proceeded in two steps. The T-1 compound is mixed DPG with silica and silane coupling agent in the kneader at high temperature which is named as $1^{st}$ mixing step. T-3 compound is mixed DPG with curatives in the two-roll mill at low temperature which is named as $2^{nd}$ mixing step. The T-2 compound is mixed a half of DPG in $1^{st}$ mixing step and the remainder is mixed in $2^{nd}$ mixing step. Total DPG content was equal for all compounds. When DPG is mixed with silica, silane coupling agent during the $1^{st}$ mixing step, a decrease in cure rate and an increase in scorch time can be seen. This indicates that DPG is adsorbed on the surface of silica. during rubber processing. However, bound rubber content is increased and dynamic properties are improved. These results are due to the highly accelerated silanization reaction. However, there are no significant difference in 100%, 300% modulus.

Microenvironmental Optimizaton of Immobilized Invertase for Methyl- $\beta$ -D-Fructofuranoside Synthesis (Methyl- $\beta$ -D-Fructofuranoside 합성을 위한 고정화 전화당 효소의 미소환경 최적화)

  • 허주형;안형환
    • Journal of the Korea Safety Management & Science
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    • v.1 no.1
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    • pp.259-272
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    • 1999
  • In order to enhance the selectivity, productivity and yield of methyl fructoside, which was synthesized by enzymatic glycosylation of sucrose and methanol solution, controlling of surface property of solid support using different immobilization procedures optimized microenvironment of immobilized invertase. Silanization and polyethylene imine coating methods were adopted to give a hydrophobic and hydrophilic environment of immobilized invertase. As a result, polyethyleneimine coating method gave higher loading of enzyme, effective activity, and relative activity than silanization method, because it brought on increasing the functional density of amino group and enhancing the conservation of activity by regulating of hydrophilicity. And then, hydrophilic environment was possible to restraint the assessing of methyl fructoside molecule, which was more hydrophobic than sucrose, fructose, and glucose molecule in the reaction mixture, into .the active site of immobilizedinvertase. Consequently, hydrophilic microenvironment of immobilized invertase by polyethyleneimine coating obtained higher yield and productivity with increasing conversion than silanized and native invertase. Thus, this procedure optimized the microenvironment of immobilized invertase suitable for the enzymatic synthesis of methyl fructoside.

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Sensitivity dependence on the effective surface area for cholesterol biosensor fabricated by silanization process (실란화 공정으로 제작된 콜레스테롤 센서의 전극 표면적에 따른 감도 특성)

  • Song, M.J.;Yoon, D.H.;Jin, J.H.;Min, N.K.;Hong, S.I.
    • Proceedings of the KIEE Conference
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    • pp.2114-2116
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    • 2004
  • 센서의 소형화 되는 추세에 전극 면적은 sensitivity의 중요한 요인이다. 본 연구에서는 콜레스테롤을 측정하기 위해 각각 planar 전극과 porous 전극에 효소 고정화 방법으로 covalent binding인 silanization 공정을 이용하여 전극 면적에 따른 전기화학적 감도를 비교하였다. Handles-Sevcik equation을 이용하여 전극 면적을 구한 결과 planar 전극의 경우 0.1608 $cm^2$, porous 전극의 경우 0.5054 $cm^2$로 porous 전극 면적이 planar전극에 비해 약 3.1배 증가하였다. 또, planar 센서의 sensitivity는 0.08567 ${\mu}A/mM{\cdot}cm^2$이고 porous 센서의 sensitivity는 planar sensor에 비해 약 3.1배 증가한 0.2656 ${\mu}A/mM{\cdot}cm^2$였다. 따라서 porous sensor의 sensitivity의 증가는 전극 면적의 증가에 따른 것이라고 할 수 있다.

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Comparative evaluation of effects of different surface treatment methods on bond strength between fiber post and composite core

  • Mosharraf, Ramin;Yazdi, Najmeh Baghaei
    • The Journal of Advanced Prosthodontics
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    • v.4 no.2
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    • pp.103-108
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    • 2012
  • PURPOSE. Debonding of a composite resin core of the fiber post often occurs at the interface between these two materials. The aim of this study was to evaluate the effects of different surface treatment methods on bond strength between fiber posts and composite core. MATERIALS AND METHODS. Sixty-four fiber posts were picked in two groups (Hetco and Exacto). Each group was further divided into four subgroups using different surface treatments: 1) silanization; 2) sandblasting; 3) Treatment with 24% $H_2O_2$, and 4) no treatment (control group). A cylindrical plexiglass matrix was placed around the post and filled with the core resin composite. Specimens were stored in 5000 thermal cycles between $5^{\circ}C$ and $55^{\circ}C$. Tensile bond strength (TBS) test and evaluation using stereomicroscope were performed on the specimen and the data were analyzed using two-way ANOVA, Post Hoc Scheffe tests and Fisher's Exact Test (${\alpha}$=.05). RESULTS. There was a significant difference between the effect of different surface treatments on TBS ($P$ <.001) but different brands of post ($P$=.743) and interaction between the brand of post and surface treatment ($P$=.922) had no significant effect on TBS. Both silanization and sandblasting improved the bonding strength of fiber posts to composite resin core, but there were not any significant differences between these groups and control group. CONCLUSION. There was not any significant difference between two brands of fiber posts that had been used in this study. Although silanization and sandblasting can improve the TBS, there was not any significant differences between surface treatments used.