• Bulletin of the Korean Chemical Society
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• 제22권4호
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• pp.337-348
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• 2001

This article gives an overview of a recently developed channel system, frit-inlet asymmetrical flow field-flow fractionation (FI-AFlFFF), which can be applied for the separation of nanoparticles, proteins, and water soluble polymers. A conventiona l asymmetrical flow FFF channel has been modified into a frit-inlet asymmetrical type by introducing a small inlet frit near the injection point and the system operation of the FI-AFlFFF channel can be made with a great convenience. Since sample components injected into the FI-AFlFFF channel are hydrodynamically relaxed, sample injection and separation processes proceed without interruption of the migration flow. Therefore in FI-AFlFFF, there is no requirement for a valve operation to switch the direction of the migration flow that is normally achieved during the focusing/relaxation process in a conventional asymmetrical channel. In this report, principles of the hydrodynamic relaxation in FI-AFlFFF channel are described with equations to predict the retention time and to calculate the complicated flow variations in the developed channel. The retention and resolving power of FI-AFlFFF system are demonstrated with standard nanospheres and protreins. An attempt to elucidate the capability of FI-AFlFFF system for the separation and size characterization of nanoparticles is made with a fumed silica particle sample. In FI-AFlFFF, field programming can be easily applied to improve separation speed and resolution for a highly retaining component (very large MW) by using flow circulation method. Programmed FI-AFlFFF separations are demonstrated with polystyrene sulfonate standards and pululans and the dynamic separation range of molecular weight is successfully expanded.

• Bulletin of the Korean Chemical Society
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• 제27권3호
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• pp.413-418
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• 2006

Sodium hyaluronate (NaHA), water soluble polymer having ultra-high molecular weight, is characterized by using on-line frit inlet asymmetrical flow field-flow fractionation (FI-AFlFFF) and multiangle light scattering (MALS). This study demonstrates the capability of power programming FI-AFlFFF for the separation of NaHA and the applicability of FI-AFlFFF with MALS for the characterization of molecular weight distribution and their structural information. Since sample injection and relaxation in FI-AFlFFF are achieved by using hydrodynamic relaxation, separation of high molecular weight polymers can be achieved smoothly without halting the separation flow. Experiments are carried out with the two different NaHA products (a raw NaHA sample and a thermally degraded NaHA product) and molecular weight distribution and conformations in solution are determined. Influence of sample filtration on the change of molecular weight distribution is also discussed.

• 분석과학
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• 제25권6호
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• pp.476-482
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• 2012

황사입자들은 수 나노미터에서 수 마이크론 사이의 크기를 가지는 것으로 알려져 있다. 황사가 환경 및 인체 건강에 미치는 영향은 황사 입자의 크기에 의존한다. 입자가 작을수록 멀리까지 이동하며, 인체의 호흡기관 깊숙이 침투한다. 침강장-흐름 분획법(sedimentation field-flow fractionation, SdFFF)은 채널 내 포물선형태의 흐름(parabolic flow profile)과 외부에서 가해지는 원심력의 상호작용을 이용하여 나노 및 마이크론 크기의 입자들의 분리를 제공한다. 본 연구에서는 황사입자의 크기별 분리와 특성분석을 위한 steric 모드 침강장-흐름 분획법(Sd/StFFF)의 응용 가능성을 테스트하였다. 이를 위하여 다양한 Sd/StFFF 파라미터들을(유속, stop-flow time, 원심력의 세기, 등) 최적화 하였다. Sd/StFFF 보정곡선의 $R^2$값은 0.9983으로 높은 직선성을 보였으며, 실험결과는 Sd/StFFF가 마이크론 입자의 크기별 분리에 우수함을 보여주었다. 광학현미경(optical microscopy, OM)을 이용하여 황사입자들의 크기와 모양을 조사하였다. 황사가 진할 때에는 약할 때보다 입자크기가 증가함을 보여주었다. 또한 비가 올 때에는 건조할 때보다 입자크기가 감소하였는데, 이는 입자 표면에 흡착되어 있는 성분들이 빗물에 의해 제거되었기 때문인 것으로 보여진다. 본 연구의 결과는 Sd/StFFF가 황사와 같이 환경입자의 크기특성분석에 유용함을 보여준다.

• Bulletin of the Korean Chemical Society
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• 제28권4호
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• pp.613-618
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• 2007

Pollens are known to be an allergen. They penetrate human respiratory system, triggering a type of seasonal allergic rhinitis called pollen allergy (hey fever). The purpose of this study is to test two field-flow fractionation (FFF) techniques, gravitational FFF (GrFFF) and sedimentation FFF (SdFFF), for their applicability to sizecharacterization of micron-sized pollens. Both GrFFF and SdFFF are elution techniques, providing sequential elution of particles based on size. They allow the size distribution as well as the mean size of the sample to be determined from the elution time. In this study, GrFFF and SdFFF were used to determine the size distribution of Paper Mulberry and Bermuda Grass pollens. For the Paper Mulberry pollen, the mean size obtained by GrFFF is 12.7 μm, and agrees rather well with the OM data with the relative error of 8.0%. For the Bermuda Grass pollen, the mean size obtained by GrFFF is 32.6 μm with the relative error of 12.3%. The mean sizes determined by SdFFF are 12.4 (relative error = 10.1%) and 27.1 μm (relative error = 5.2%) for the Paper Mulberry and the Bermuda Grass pollen, respectively. Although SdFFF tends to yield more accurate size distribution due to lower band broadening under the field strength higher than 1 G, the sizes determined by GrFFF were not significantly different from those by SdFFF.

• 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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• 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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• 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.

• 분석과학
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• 제24권4호
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• pp.249-255
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• 2011

물의 흡수에 의한 전분알갱이의 swelling은 물과 친화력이 있는 새로운 부분의 노출에 의하여 구조적인 변화로써 점진적으로, 때로는 갑작스럽게 변화를 일으킨다. 이러한 이유로 인해서, 물과의 접촉 시간에 따르는 전분 알갱이의 크기 또는 모양의 변화에 관심을 가진다. 중력 장-흐름 분획법(gravitation field-flow fractionation, GrFFF)은 마이크론 범위의 크기를 가지는 입자들을 분리하는 데에 유용한 분리기술이다. 본 연구에서는 감자와 고구마 전분알갱이들의 크기와 크기 분포도를 결정하는 데에 있어서 GrFFF의 응용가능성을 검사하고자 한다. GrFFF를 이용하여 물과의 접촉 시간에 따르는 전분 알갱이들의 크기분포도 변화를 모니터하였다. GrFFF로부터 얻어진 전분알갱이들의 크기 및 크기분포는 광학현미경(optical microscopy, OM) 결과와 비교하였다. 결과적으로 감자와 고구마 전분의 swelling은 물과의 접촉시간이 증가함에 따라 전분알갱이의 크기가 증가하며, 전분의 종류가 달라지면 swelling 속도가 달라짐을 확인하였다.

• 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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• 제33권2호
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• pp.711-713
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• 2012