• Journal of the Korean Applied Science and Technology
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• v.31 no.4
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• pp.642-652
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• 2014

The synthesis of octenyl succinyl ${\beta}$-gucan (OSA-${\beta}$-glucan) was carried out and its interfacial properties at the oil-water interface and in emulsion systems were investigated. An aqueous ethanol system as a reaction media was used to facilitate the synthesis process; 10% (w/w) ethanol found to be the best as it showed a maximum degree of substitution (DS: 0.0132). FT-IR showed a characteristic absorption spectrum at $1736cm^{-1}$, indicating the esterification of octenyl succinyl groups to ${\beta}$-glucan backbone. As for interfacial tension measurements, it was decreased with increasing concentration of OSA-${\beta}$-glucan in the aqueous phase and when NaCl was added to aqueous OSA-${\beta}$-glucan solution in the range of 0.01 M to 0.1 M and also when pH was raised (pH 3 ~ pH 9). In systems of emulsion stabilized with OSA-${\beta}$-glucan, fat globule size found to decrease with increasing concentration of OSA-${\beta}$-glucan, showing a critical value of about $0.32{\mu}m$ at 0.5 wt%. When the OSA-${\beta}$-glucan emulsions were stored, it was found that fat globule size was increased with storage time and particularly pronounced increase was observed in emulsion with 1% OSA-${\beta}$-glucan, possibly due to depletion flocculation. Results of creaming stability evaluated by light scattering technique showed that it was more stable in emulsions containing smaller fat globule size. Surface load of OSA-${\beta}$-glucan in emulsions increased with increasing concentration of OSA-${\beta}$-glucan, suggesting a multilayer adsorption.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.9 no.1
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• pp.23-40
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• 1999

The analysis of thiodiglycolic acid in urine has been used as an index of biological exposure to vinyl chloride. Unfortunately thiodiglycolic acid has a strong hydrophilic character, because it has two carboxylic groups, so that it can only be extracted with organic solvent with a great difficulty. Underivatized thiodiglycolic acid tends to tail because of non-specific interaction with the inert support. Therefore, esterification is the obvious first choice for derivatization of thiodiglycolic acid, particularly for gas chromatography. In this study, the focus of interest is to compare two method of esterifications (methylation and silylation). Methylation is to make the methyl ester of thiodiglycolic acid by reaction with diazomethane. Silylation is to make the trimethylsilyl ester of thiodiglycolic acid by reaction with N-trimethylsily-ldiethylamine. The results and conclusions are as the following: 1. The detection limit (sensitivity) of methylated thiodiglycolic acid was $5.00{\mu}g/m{\ell}$ and silylated thiodiglycolic acid was $3.07{\mu}g/m{\ell}$ by gas chromatography with flame ionization detector. 2. The optimal liquid-liquid extraction of thiodiglycolic acid was as following: To each of the tubes, $15m{\ell}$ of urine, concentrated sulfuric acid (pH 1 - 2) and 5 gsodium sulfate were added. The samples was extracted three times with $5m{\ell}$ ethylacetate each time. 3. The methylated thiodiglycolic acid was more stable than silylated thiodiglycolic acid in extractional solvent which contained humidity. 4. The precision (pooled coefficient of variation for 4 days) of the analysis was 0.07324 in methylated thiodiglycolic acid with external standard calibration, and 0.07033 in methylated thiodiglycolic acid with internal standard calibration. 5. The precision (pooled coefficient of variation for 4 days) of the analysis was 0.10914 in silylated thiodiglycolic acid with external standard calibration, and 0.13602 in silylated thiodiglycolic acid with internal standard calibration. From the above results, the analysis of methylated thiodiglycolic acid was more sensitive (limit of detection) than silylated thiodiglycolic acid by gas chromatography. However, the methylated thiodiglycolic acid was stable in the humidity and was separated sharply on chromatogram. Also, analysis of methylated thiodiglycolic acid was more precise (pooled coefficient of variation for 4 days) than silylated thiodiglycolic acid. In conclusion, it is established that the analysis of methylated thiodiglycolic acid is appropriate for biological monitoring of exposure to vinyl chloride.

• Membrane Journal
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• v.18 no.3
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• pp.234-240
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• 2008

This work demonstrates the preparation of proton conducting crosslinked polymer electrolyte membranes by blending polystrene-b-poly(hydroxyethyl acrylate) (PS-b-PHEA) and poly(vinyl alcohol) (PVA) at 1 : 1 wt ratio. The PHEA block of the diblock copolymer was crosslinked with PVA using sulfosuccinic acid (SA) via the esterification reaction between -OH of membrane and -COOH of SA, as confirmed by FT-IR spectroscopy. Ion exchange capacity (IEC) continuously increased from 0.14 to 0.91 meq/g with increasing concentrations of SA, due to the increasing portion of charged groups in the membrane. In contrast, the water uptake increased up to 20.0 wt% of SA concentration above which it decreased monotonically. The membrane also exhibited a maximum proton conductivity of 0.024 S/cm at 20.0 wt% of SA concentration. The maximum behavior of water uptake and proton conductivity is considered to be due to competitive effect between the increase of ionic sites and the crosslinking reaction according to the SA concentration.

• Membrane Journal
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• v.19 no.3
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• pp.228-236
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• 2009

ABA type triblock copolymer of poly(hydroxyl ethyl acrylate )-b-polystyrene-b-poly(hydroxyl ethyl acrylate), i.e. PHEA-b-PS-b-PHEA, was synthesized throughatom transfer radical polymerization (ATRP). This block copolymer was thermally crosslinked with 4,5-imidazole dicarboxylic acid (IDA) via the esterification between the -OH groups of PHEA in block copolymer and the -COOH groups of IDA. Upon doping with ${H_3}{PO_4}$ to form imidazole-${H_3}{PO_4}$ complexes, the proton conductivity of membranes continuously increased with increasing ${H_3}{PO_4}$ content. The PHEA-b-PS-b-PHEA/IDA/${H_3}{PO_4}$ polymer membrane with [HEA]:[IDA]:[${H_3}{PO_4}$]=3:4:4 exhibited a maximum proton conductivity of 0.01 S/cm at $100^{\circ}C$ under anhydrous conditions. Thermal gravimetric analysis (TGA) shows that the PHEA-b-PS-b-PHEA/IDA/${H_3}{PO_4}$ complex membranes were thermally stable up to $350^{\circ}C$, indicating their applicability in fuel cells.

• Applied Chemistry for Engineering
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• v.10 no.8
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• pp.1169-1174
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• 1999

2-Diazo-1-naphthoquinone-5-sulfonyl chloride(NQD-Cl) was synthesized from sodium 2-diazo-naphthoquinone-5-sulfonate by chlorination. NQD-Cl was esterified with hydroxybenzophenones to give several 1,2-naphthoquinone-(2)-diazide-5-sulfonic acid ester derivatives(NQD-esters). We have compared benzophenone derivatives with methoxy group to benzophenone derivatives with hydroxy group. Solubility of each NQD-ester was studied. Each of NQD-esters was formulated with novolac base resin and PS plates were manufactured. Photosensitivity, bleachability, compatible exposed time and relative sensitivity were determined by UV spectrophotometry, imaged by UV lithographic techniques, and the gray scale method. According to the number of substituted NQD group, it showed that relative sensitivity was different from gray scale method. NQD-esters with methoxy group showed a good solubility and higher sensitivity than commercial PS ones.

• Applied Chemistry for Engineering
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• v.19 no.5
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• pp.497-503
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• 2008

A variety of techniques has been employed in order to reduce problems caused by the crystallization of paraffin and saturated fatty acid esters in diesel fuel containing biodiesels. Methacrylate copolymers are known as additives which reduce the pour point and cold filtering plugging point (CFPP) of diesel fuels. This paper describes the synthesis, characterization and low temperature properties, having as an initial step the synthesis of the alkyl methacrylate monomers by esterification of methacrylic acid with C12, C18, and C22 fatty alcohols. The copolymerization of these monomers with styrene was then performed, with molar ratios of 30:70, 50:50 and 70:30 for styrene:alkyl methacrylate. All copolymers were characterized by $^1H-NMR$, FT-IR, and gel permeation chromatography (GPC). The poly(styrene-co-alkyl methacrylate)s (PStmSMAn) leads to a large reduction in the pour point and CFPP of poly(styrene-co-alkyl methacrylate) in ultra low sulfur diesel (ULSD) and BD5 with treated 100~5000 ppm of poly(styrene-co-alkyl methacrylate). BD5 fuel containing 5000 ppm of the copolymer (PSt82SMA18) showed a $25^{\circ}C$ and $9^{\circ}C$ reduction in their pour points and CFPP, respectively.

• Korean Journal of Food Science and Technology
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• v.40 no.5
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• pp.491-496
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• 2008

Properties of pectin extracted from flesh of Asian pear in 3 cultivars were investigated at different growth stages. The extraction yields of pectin by the acidic treatment decreased during the growth. The $L^*$ value of young fruit was lower than unripe and ripe fruit, and $a^*$ and $b^*$ value were higher in the same cultivars. The degree of esterification (DE) and intrinsic viscosity of pectin were 21.1-41.3% and 1.90-3.81 dL/g, respectively. The pectin extracted from flesh of pear showed about 30% glucose retarding effect. The DE value had a high correlation with retarding effect on glucose transport and intrinsic viscosity (p<0.01 and p<0.05). The intrinsic viscosity of the pectin seems to affect the retardation of glucose transport in blood. Pectin extracted from flesh of Asian pear by acidic treatment could be a good source to develop low calorie and functional food.

• Applied Chemistry for Engineering
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• v.7 no.3
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• pp.496-503
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• 1996

Aromatic and aliphatic copolyesters for the dispersing agent were synthesized by two stage reaction, esterification and polycondensation. Copolyesters were blended with PET in the melt state and their thermal and rheological properties were investigated. From GPC analysis Mn's and Mw's of copolyesters were about 30000 and 65000g/mol, respectively. From DSC experiment copolyesters had melting range of $90{\sim}150^{\circ}C$. Copolymer composition was in good agreement with comonomer feed ratio from $^1H$-NMR analysis. Copolyesters and SPA (standard sample) were blended with PET in the melt state. From DSC experiment, copolyesters and SPA were miscible with PET. From the dynamic melt viscosity experiment, melt viscosity of blended sample was increased as the content of aromatic copolyester was increased, while it was decreased as the content of aliphatic and SPA were increased. As for volume resistivity of dry color containing carbon black and copolyesters with dispersing time, aromatic copolyester showed highest value. It was conferred from this result that aromatic copolyester was the best dispersing agent for carbon black in PET resin.

• Korean Journal of Food Science and Technology
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• v.30 no.1
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• pp.125-131
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• 1998

The change of pectinesterase (PE) activity and pectin substances in fig fruit were investigated and low sugar jams prepared by various methods from fig fruit were compared. Fig fruit PE, which began to show the activity at the harvest time, was not inactivated and had slight activity during frozen storage at $-25^{\circ}C$. The amount of alcohol insoluble solid (AIS) and the degree of esterification (DE) of AIS were reduced by its own PE activity. However the intrinsic PE of fig fruit was not enough to make low-methoxyl pectin below 50% of DE. Fig pulp treated by its own PE and combination of fig PE and orange PE could make low-methoxyl pectin. After PE treatments, fig pulp adjusted below pH 4.0 by addition of citric acid kept red colour. Fig Jams processed by various methods had lower soluble solid $(31{\sim}49^{\circ}Brix)$ compared with conventional fig jam. Five kinds of fig jams out of those showed higher score than others in the sensory evaluation. For preparation of the five jams, the fig pulps with or without 1% pectin were treated at $50^{\circ}C$ for 25 minutes with addition of orange PE (200 units/400 g pulp). The treated pulps were added with 0.25% citric acid, 0.7% calcium and 20% cane sugar. The mixed pulps were prepared for jams containing low sugar by hot plate or microwave or refrigeration (excepting the mixed pulp without pectin).

• Polymer(Korea)
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• v.35 no.2
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• pp.166-170
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• 2011

This study reported the synthesis of perfluoropolyether intermediate (TP-$COOCF_3$) having a $CF_3$ functional group via electrophilic fluorine substituting direct fluorination from PFPE intermediate (TP-$COOCH_3$) having a $CH_3$ functional group, which was synthesized by the ring opening polymerization and methyl esterification of HFPO. The effects of reaction conditions such as the amount of solvent, fluorine partial pressure, reaction time, were investigated. The results showed that the yield of fluorination reaction became the highest when the reaction was carried out in a mild condition for a long reaction time, which also minimized side reactions. The sample was characterized by FTIR and NMR, which confirmed the synthesis of the final product, TP-$COOCF_3$, via direct fluorination converting $CH_3$ of TP-$COOCH_3$ to $CF_3$ of TP-$COOCF_3$ with 95.4% yield.