• 제목/요약/키워드: Dynamic Light Scattering (DLS)

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[Retraction]Characterization of carbon black nanoparticles using asymmetrical flow field-flow fractionation (AsFlFFF)

  • Kim, Kihyun;Lee, Seungho;Kim, Woonjung
    • 분석과학
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    • 제32권3호
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    • pp.77-87
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    • 2019
  • High viscosity carbon black dispersions are used in various industrial fields such as color cosmetics, rubber, tire, plastic and color filter ink. However, carbon black particles are unstable to heat due to inherent characteristics, and it is very difficult to keep the quality of the product constant due to agglomeration of particles. In general, particle size analysis is performed by dynamic light scattering (DLS) during the dispersion process in order to select the optimum dispersant in the carbon black dispersion process. However, the existing low viscosity analysis provides reproducible particle distribution analysis results, but it is difficult to select the optimum dispersant because it is difficult to analyze the reproducible particle distribution at high viscosity. In this study, dynamic light scattering (DLS) and asymmetrical flow field-flow fractionation (AsFlFFF) analysis methods were compared for reproducible particle size analysis of high viscosity carbon black. First, the stability of carbon black dispersion was investigated by particle size analysis by DLS and AsFlFFF according to milling time, and the validity of analytical method for the selection of the optimum dispersant useful for carbon black dispersion was confirmed. The correlation between color and particle size of particles in high viscosity carbon black dispersion was investigated by using colorimeter. The particle size distribution from AsFlFFF was consistent with the colorimetric results. As a result, the correlation between AsFlFFF and colorimetric results confirmed the possibility of a strong analytical method for determining the appropriate dispersant and milling time in high viscosity carbon black dispersions. In addition, for nanoparticles with relatively broad particle size distributions such as carbon black, AsFlFFF has been found to provide a more accurate particle size distribution than DLS. This is because AsFlFFF, unlike DLS, can analyze each fraction by separating particles by size.

[Retraction]Size measurement and characterization of ceria nanoparticles using asymmetrical flow field-flow fractionation (AsFlFFF)

  • Kim, Kihyun;Choi, Seong-Ho;Lee, Seungho;Kim, Woonjung
    • 분석과학
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    • 제32권5호
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    • pp.173-184
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    • 2019
  • As the size of semiconductors becomes smaller, it is necessary to perform high precision polishing of nanoscale. Ceria, which is generally used as an abrasive, is widely used because of its uniform quality, but its stability is not high because it has a high molecular weight and causes agglomeration and rapid precipitation. Such agglomeration and precipitation causes scratches in the polishing process. Therefore, it is important to accurately analyze the size distribution of ceria particles. In this study, a study was conducted to select dispersants useful for preventing coagulation and sedimentation of ceria. First, a dispersant was synthesized and a ceria slurry was prepared. The defoamer selection experiment was performed in order to remove the air bubbles which may occur in the production of ceria slurry. Dynamic light scattering (DLS) and asymmetrical flow field-flow fractionation (AsFlFFF) were used to determine the size distribution of ceria particles in the slurry. AsFlFFF is a technique for separating nanoparticles based on sequential elution of samples as in chromatography, and is a useful technique for determining the particle size distribution of nanoparticle samples. AsFlFFF was able to confirm the presence of a little quantities of large particles in the vicinity of 300 nm, which DLS can not detect, besides the main distribution in the range of 60-80 nm. AsFlFFF showed better accuracy and precision than DLS for particle size analysis of a little quantities of large particles such as ceria slurry treated in this study.

Effect of particle size of TiO2 and octyl-methoxycinnamate (OMC) content on sun protection factor (SPF)

  • Choi, Jaeyeong;Kim, Suyeon;Kim, Woonjung;Eum, Chul Hun;Lee, Seungho
    • 분석과학
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    • 제30권4호
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    • pp.159-166
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    • 2017
  • Exposure to UV light, i.e., UV-A (320-400 nm) or UV-B (290-320 nm) radiation, can cause skin cancer. Titanium dioxide ($TiO_2$) effectively disperses UV light. Therefore, it is used as a physical UV filter in many UV light blockers. Usually, the $TiO_2$ content in commercialized UV blockers is 25 % at most. To block UV-B, a chemical UV blocker, octyl-methoxy cinnamate (OMC) is used. OMC is commonly used in combination with $TiO_2$. In this study, $TiO_2$ and OMC were mixed in different proportions to produce UV blockers with different compositions. Also the changes in the sun protection factor (SPF) based on the composition and $TiO_2$ particle sizes were investigated. In order to analyze the $TiO_2$ particle size, dynamic light scattering (DLS) and asymmetrical flow field-flow fractionation (AsFlFFF) were used. The results showed that the SPF was influenced by the proportion of $TiO_2$ and OMC, where the proportion of $TiO_2$ induced a more significant influence. In addition, changes in the $TiO_2$ particle size based on the proportion of OMC were observed.

Phase Behavior of a PEO-PPO-PEO Triblock Copolymer in Aqueous Solutions: Two Gelation Mechanisms

  • Park, Moon-Jeong;Kookheon Char;Kim, Hong-Doo;Lee, Chang-Hee;Seong, Baek-Seok;Han, Young-Soo
    • Macromolecular Research
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    • 제10권6호
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    • pp.325-331
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    • 2002
  • Phase behavior of a PEO-PPO-PEO (Pluronic P103) triblock copolymer in water is investigated using small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), dynamic light scattering (DLS) and rheology. Pluronic P103 shows apparent two gel states in different temperature regions. The first sol-to-gel transition at a lower temperature (i.e., the hard gel I state) turns out to be the hexagonal microphase as evidenced by the combined SANS and SAXS and the frequency dependence of both G′ and G" in rheology. In contrast to the hard gel I, the second sol-to-gel transition (i. e., the hard gel II state) at a higher temperature represents the block copolymer micelles in somewhat disordered state rather than the ordered state seen in the hard gel I. Moreover, turbidity change depending only on the temperature with four distinct regions is observed and the large aggregates with size larger than 5,000 nm are detected with DLS in the turbid solution region. Based upon the present study, two different gelation mechanisms for aqueous PEO-PPO-PEO triblock copolymer solutions are proposed.

Sizes and Structures of Micelles of Cationic Octadecyl Trimethyl Ammonium Chloride and Anionic Ammonium Dodecyl Sulfate Surfactants in Aqueous Solutions

  • Kim, Hong-Un;Lim, Kyung-Hee
    • Bulletin of the Korean Chemical Society
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    • 제25권3호
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    • pp.382-388
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    • 2004
  • The sizes and structures of micelles formed in aqueous solutions of cationic octadecyl trimethyl ammonium chloride (OTAC) and anionic ammonium dodecyl sulfate (ADS) surfactants were investigated using smallangle neutron scattering (SANS), self-diffusion coefficients by pulsed-gradient spin-echo (PGSE) NMR, and dynamic light scattering (DLS) methods. SANS and DLS data indicate that their structures are spherical at concentrations as high as 300 mM. As the total surfactant concentration increases, the peaks of SANS spectra shift to higher scattering vector and become sharper, indicating that the intermicellar distance decreases and its distribution becomes narrower. This is due to more compact packing of surfactant molecules at high concentrations. The intermicellar distance of around 100 ${\AA}$ above 200 mM corresponds approximately to the diameter of one micelle. The sizes of spherical micelles are 61 ${\AA}$ and 41 ${\AA}$ for 9 mM OTAC and 10 mM ADS, respectively. Also the self-diffusion coefficients by PGSE-NMR yield the apparent sizes 96 ${\AA}$ and 31 ${\AA}$ for micelles of 1 mM OTAC and 10 mM ADS, respectively. For ADS solutions of high concentrations (100-300 mM), DLS data show that the micelle size remains constant at $25{\pm}2{\AA}$. This indicates that the transition in micellar shape does not take place up to 300 mM, which is consistent with the SANS results.

Probe and Matrix Diffusion of Polystyrene Particle and Labeled Polyallylamine Hydrochlorate

  • Choi, Young-Wook;Sohn, Dae-Won
    • 한국고분자학회:학술대회논문집
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    • 한국고분자학회 2006년도 IUPAC International Symposium on Advanced Polymers for Emerging Technologies
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    • pp.205-205
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    • 2006
  • Adsorption behaviors of positively charged matrix (PAH) onto negatively charged probe (sulfate PS particle) were investigated using DLS (dynamic light scattering) and FPR (fluorescence photobleaching recovery) as view points of matrix and salt concentration. The system experienced sharp decrease of diffusion (flocculation) at dilute condition while the system underwent gradual decrease of diffusion above semi-dilute concentration. With FPR and viscometry experiments, we revealed the probe behaviors in polyelectrolyte solution were strongly affected by the coil overlap concentration (0.5 g/L PAH concentration).

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Preparation of Silica Hollow Composite Particles

  • Lee, Dong Hoon;Lee, Chang Hyun
    • Bulletin of the Korean Chemical Society
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    • 제35권11호
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    • pp.3303-3306
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    • 2014
  • A facile and effective approach has been developed to prepare hybrid hollow microspheres, via consecutive processes of pickering mini-emulsion polymerization for core-shell formation, and calcination of the sacrificial core. The resulting hollow composite particles have mono-layered shells. The morphology and size characteristics of synthesized composite particles were investigated, using dynamic light scattering (DLS) and scanning electron microscopy (SEM) measurements.

Synthesis of gold nanoparticles using Coffea Arabica fruit extract

  • Bogireddy, Naveen Kumar Reddy;Gomez, L. Martinez;Osorio-Roman, I.;Agarwal, V.
    • Advances in nano research
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    • 제5권3호
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    • pp.253-260
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    • 2017
  • We report a simple eco-friendly process for the synthesis of gold nanoparticles (AuNPs) using aqueous extract from Coffea Arabica fruit. The formation of AuNPs was confirmed using absorption spectroscopy and scanning electron microscopy images. FT-IR analysis demonstrates the major functional groups present in Coffee Arabica fruit extract before and after synthesizing AuNPs. The Face Center Cubic (FCC) polycrystalline nature of these particles was identified by X-Ray diffraction (XRD) analysis. Taking into account the contribution of the biomass surrounding the AuNPs, dynamic light scattering (DLS) results revealed an average particle size of ~59 nm.

Well-Defined Thermoresponsive Copolymers with Tunable LCST and UCST in Water

  • Jung, Seo-Hyun;Lee, Hyung-Il
    • Bulletin of the Korean Chemical Society
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    • 제35권2호
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    • pp.501-504
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    • 2014
  • A thermoresponsive polymer, poly(2-(dimethylamino)ethyl methacrylate) (PDMAEMA), was successfully synthesized by atom transfer radical polymerization (ATRP). Different amounts of 1,3-propanesultone were used as quaternization agent to transit the PDMAEMA into partially modified poly(zwitterions), resulting in p[DMAEMA-co-3-dimethyl(methacryloyloxyethyl)ammonium propanesulfonate] (PDMAEMA-co-PDMAPS). Molecular weight, molecular weight distribution, and degree of quarternization were determined by gel permeation chromatography (GPC) and 1H NMR spectroscopy. The transmission spectra of the 1.0 wt % aqueous solutions of the resulting polymers at 650 nm were measured as a function of temperature. Results showed that the lower critical solution temperature (LCST) and the upper critical solution temperature (UCST) could be easily controlled by the different composition of dimethylamino and zwitterion groups. The effect of partial quaternization on thermoresponsive properties was also studied by dynamic light scattering (DLS) with the same aqueous concentration (1.0 wt %) as employed for turbidimetry studies. The LCST and UCST values measured by DLS correlated well with those determined by turbidimetry.