• 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.

• Bulletin of the Korean Chemical Society
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• 제32권4호
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• pp.1315-1320
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• 2011

Whey protein (WP) is a mixture of proteins, and is of high nutritional values. WP has become an important source of functional ingredients in various health-promoting foods. In this study, size-exclusion chromatography (SEC) and asymmetrical flow field-flow fractionation (AsFlFFF) were used for separation and analysis of whey proteins. It was found that a lab-prepared WP from raw milk is mostly of ${\beta}$-lactoglobulin with small amount of higher molecular weight components, while a commercial whey protein isolate (WPI) powder contains relatively larger amount of components other than ${\beta}$-lactoglobulin, including IgG and protein aggregates. Results suggest that AsFlFFF provides higher resolution for the major whey proteins than SEC in their normal operation conditions. AsFlFFF could differentiate the BSA and Albumin, despite a small difference in their molecular weights, and also was able to separate much smaller amount of aggregates from monomers. It is noted that SEC was able to show the presence of low molecular weight components other than the major whey proteins in the WP samples, which AsFlFFF could not show, probably due to the partial loss of those low molecular weight species through the membrane.

• 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.

• Bulletin of the Korean Chemical Society
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• 제24권9호
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• pp.1339-1344
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• 2003

Flow field-flow fractionation (FlFFF) is a technology to separate the molecules by size in an open channel. Molecules with different size have different diffusivities and are located vertically in different positions when passing through an open channel. In this study, hollow fiber membranes instead of conventional rectangular channels have been used as materials for the open channel and this change would decrease the cost of manufacturing. FlFFF is a useful technique to characterize the biopolymeric materials. Retention time, diffusion coefficients and Stokes radius of analysis can be calculated from the related simple equations. Hollow-fiber flow field-flow fractionation (HF-FlFFF) has been used for the characterization and separation of protein mixture in a phosphate buffer solution and has demonstrated the potential to be developed into a disposable FlFFF channel. The important indexes for the analytical separation are selectivity, resolution and plate height. The optimized separation condition for protein mixture of Ovalbumin, Alcohol dehydrogenase, Apoferritin and Thyroglobulin is ${\dot V}_{out}/{\dot V}_{rad}=0.65/0.85\;mL/min$.

• Bulletin of the Korean Chemical Society
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• 제27권9호
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• pp.1433-1438
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• 2006

An AsFlFFF channel was designed and built, and then tested for analysis of pullulans and proteins. Pullulans and proteins having various nominal molecular weights were injected at various conditions of the cross-flow rate ($F_c$) and the channel-out flow rate ($F_{out}$). The retention (measured by the retention ratio R) and the zone broadening (measured by the plate height H) were measured, and then compared with theory. When the incoming flow rate, $f_{in}$ (and thus $F_{out}$) was varied with $F_c$ fixed at 2.5 mL/min, the plate height measured for the pullulan with nominal molecular weight (M) of about 100,000 showed the trend expected by the longitudinal diffusion theory (H decreases with increasing flow rate). In contrast, when $F_{out}$ was varied with the flow rate ratio, $F_c/F_{out}$, fixed constant at 5, the plate height measured for the same sample showed the trend expected from the non-equilibrium theory (H increases with increasing flow rate). Calibration plots (log D vs. log M) obtained with pullulans and proteins were not coincide, probably due to the difference in molecular conformation, suggesting the analysis of pullulans and proteins using AsFlFFF requires independent calibration. It was found that the linearity of the protein-calibration plot was improved by using a buffer solution as the carrier.

• 대한환경공학회지
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• 제35권11호
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• pp.835-860
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• 2013

최근 들어 나노기술의 발전에 따라 다양한 산업 및 상업분야에서 나노물질의 사용이 급증하고 있다. 이러한 나노물질이 환경에 유출되어 사람의 건강 및 생태계에 악영향을 줄 수 있다는 문제가 지속적으로 제기되어 왔다. 이에 따라 다양한 환경매질 내에서 나노물질의 거동특성 및 생독성 등에 대한 평가들이 요구되어진다. 이러한 평가들이 진행되기 위해서 필연적으로 다양한 매체 내에서 존재하는 나노물질을 효과적으로 분리하고 이들의 특성을 정량화하는 기술들이 수반되어야 한다. 본 논문에서는 이러한 나노물질의 분리기술들 중 시료의 교란이 비교적 적고 전처리과정이 단순한 장-흐름 분획기술을 이용한 나노물질 분리에 대한 국내외 선행연구들을 살펴보았다. 특히 가장 많이 활용되어온 흐름 장-흐름 분획기를 중심으로 기본원리를 살펴보고 분리대상인 나노물질의 종류에 따라서 지금까지 수행되어온 연구들을 분류하고 분석해 봄으로써 이 분야의 연구자들에게 실제적인 정보를 제공하고자 한다. 장-흐름 분획기를 이용하여 다양한 환경매질로부터 나노물질을 효과적으로 분리하기 위해서 분리대상인 나노물질의 종류와 특성을 고려한 전처리, 적절한 멤브레인과 운반용액의 선택, 흐름조건의 최적화 등이 중요한 것으로 조사되었다. 뿐만 아니라 분리 후 나노물질의 특성을 정량화하기 위해서 다양한 검출기 및 분석기와의 연계가 필수적으로 보인다. 하지만 아직까지 일부 환경매질에만 국한되어 연구가 진행되었으며, 또한 분리대상인 나노물질의 종류도 극히 제한적인 것으로 조사되었다. 특히 이러한 나노물질에 대한 분리 및 측정에 대한 국내 연구는 매우 부족한 실정이며 나노물질 사용량이 급증하고 있는 현실을 고려하면 이 분야에 대한 연구가 절실히 요구된다.

• 한국응용과학기술학회지
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• 제34권2호
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• pp.357-366
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• 2017

천연색소는 색을 발현할 수 있는 물질로서 식품, 화장품, 의약품 등에 사용된다. 천연색소는 동 식물에서 추출하여 만들기 때문에 크기가 균일하지 않으며 특히 적색색소의 경우, 다른 색의 색소에 비해 친유성이 강해 수용액 상태에서 쉽게 응집이 되는 경향이 있다. 또한 응집에 의한 크기변화로 인해 색의 재현이 어려운 문제점이 있다. 적색색소로 기존에 사용했던 동물성 색소인 코치닐 추출 색소는 알레르기를 유발하고 식용으로서의 거부감이 있는 등의 문제점으로 인하여 사용이 기피되는 추세이다. 본 연구에서는 적색의 식물성 색소인 라이코펜 추출물과 치자황색소를 사용하였고 Ball-milling을 이용하여 색소의 크기를 균일하게 만든 후 Asymmetrical flow field-flow fractionation(AsFlFFF), Dynamic light scattering(DLS)를 이용하여 크기를 분석하고 색차계를 이용하여 색을 확인하는 연구를 진행하였다. 실험결과 milling 전에는 색소 입자의 크기가 크고 크기분포가 넓었으나, milling 후에는 크기가 감소하고 크기분포가 좁아짐을 확인하였다. 색차계 측정 결과, milling 시간이 증가함에 따라 밝기, 적색도, 황색도가 높아져서 밝은 적색을 나타내었다.

• 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.