• 한국식품저장유통학회지
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• 제16권3호
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• pp.371-375
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• 2009

ESR spectroscopy에 의한 방사선 조사 건조향신료의 조사여부의 정확한 판별에 필요한 기초자료를 얻고자 방사선 조사 유래의 cellulose radical에 대한 parameter를 분석하였다. 건조향신료 분말 4종(고추, 마늘, 양파, 후추)에 대하여 0, 1, 5, 10 kGy의 $^{60}Co$ 감마선을 조사한 후 ESR signal을 분석하였다. 방사선 조사된 4종의 건조향신료는 모두 방사선 조사 유래의 triplet signal인 cellulose radical을 나타내면서 center signal($g_2=2.00673$)은 좌우 3.0455 mT 간격의 특이적인 signal을 보였다. 조사시료에서 나타난 hyperfine triplet signal(cellulose radical)의 g-value, center field 및 저-고자장 signal의 간격은 조사선량이 변화하여도 일정하였으므로 이들 parameter들은 cellulose radical의 고유 특성임을 확인 하였다. 이로써 감마선 조사시료와 비조사 시료 간의 구별이 분명하였다. ESR signal intensity는 조사선량이 증가함에 따라 유의적으로 증가하였다($R^2=0.8452{\sim}0.9854$). 이상의 결과에서 cellulose radical의 parameter 분석은 건조향신료의 ESR 분석에서 조사여부의 판별에 대한 신뢰성을 뒷받침 해 주었다.

• Journal of the Korean Wood Science and Technology
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• 제43권5호
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• pp.613-627
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• 2015

Simple methods of conductometric titration and infrared spectroscopy were used to quantify the surface carboxyl content of cellulose fibrils isolated by 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO)-mediated oxidation. The effects of different cellulose sources, post or assisted-sonication oxidation treatment, and the amount of sodium hypochlorite addition on the carboxyl content of cellulose were reported. This study showed that post sonication treatment had no influence on the improvement of surface carboxyl charge of cellulose macrofibrils (CMFs). However, the carboxyl content increased for the isolated cellulose nanofibrils (CNFs). Thus the carboxyl content of CNFs is different from those of their corresponding bulk oxidized cellulose and CMFs. Filter paper as a CNF source imparted a higher surface charge than did hardwood bleached kraft pulp (HWBKP) and microcrystalline cellulose (MCC). It was considered that the crystallinity and microstructure of the initial cellulose affected oxidation efficiency. In addition, the carboxyl content of cellulose was successfully controlled by applying sonication treatment during the oxidation reaction and adjusting the amount of sodium hypochlorite.

• Current Research on Agriculture and Life Sciences
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• 제31권4호
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• pp.250-255
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• 2013

As a renewable nanomaterial, cellulose nanocrystal (CNC) isolated from wood grants excellent mechanical properties in developing high performance nanocomposites. This study was undertaken to compare the reinforcing efficiency of two different CNCs, i.e., cellulose nanowhiskers (CNWs) and cellulose nanofibrils (CNFs) from hardwood bleached kraft pulp (HW-BKP) as reinforcing agent in polyvinyl alcohol (PVA)-based nanocomposite. The CNWs were isolated by sulfuric acid hydrolysis while the CNFs were isolated by 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO)-mediated oxidation. Based on measurements using transmission electron microscopy, the individual CNWs were about $6.96{\pm}0.87nm$ wide and $178{\pm}55nm$ long, while CNFs were $7.07{\pm}0.99nm$ wide. The incorporation of CNWs and CNFs into the PVA matrix at 5% and 1% levels, respectively, resulted in the maximum tensile strength, indicating different efficiencies of these CNCs in the nanocomposites. Therefore, these results suggest a relationship between the reinforcing potential of CNCs and their physical characteristics, such as their morphology, dimensions, and aspect ratio.

• 한국응용과학기술학회지
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• 제25권4호
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• pp.459-468
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• 2008

Methyl methacrylate(MMA) was grafted onto microcrystalline cellulose(MCC) with ceric ammonium nitrate(CAN) as a redox initiator at the various conditions. The cellulose triacetate(CTA) composite films added MCC and MMA-grafted MCC powders were prepared on a glass plate. The graft yield(GY) and graft efficiency(GE) of the grafted MCC were calculated with the simple equations by the weight balance method. The double bond of C=O on the grafted MCC surfaces was confirmed by the fourier transform infrared spectroscopy with attenuated total reflection(FT-IT ATR) spectrophotometer. After grafting, the degree of crystallinity of cellulose powders was decresed by judging from x-ray diffraction(XRD) data. Scanning electron microscope(SEM) photos showed the only solvent and CAN solution could change the roughness of MCC powders and the effect of powder dispersions in composite matrix. The tensile strength of MCC/CTA composite films was decreased with increase of MCC powder contents. When 5% grafted MCC was added, the tensile strength of grafted MCC/CTA composite films was increased from 82.3 MPa to 97.2 MPa. The thermal property of powders was also analyzed by the thermogravimetric analysis(TGA).

• Journal of the Korean Wood Science and Technology
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• 제42권2호
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• pp.119-129
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• 2014

This work undertook to prepare nanofibers of cellulose nanofibrils (CNF)/polyvinyl alcohol (PVA) composite by electrospinning, and characterize the electrospun composite nanofibers. Different contents of CNFs isolated from hardwood bleached kraft pulp (HW-BKP) by 2,2,6,6-tetramethylpiperidine-1-oxy radical (TEMPO)-mediated oxidation were suspended in aqueous polyvinyl alcohol (PVA) solution, and then electrospun into CNF/PVA composite nanofibers. The morphology and dimension of CNFs were characterized by transmission electron microscopy (TEM), which revealed that CNFs were fibrillated form with the diameter of about $7.07{\pm}0.99$ nm. Morphology of the electrospun nanofiber observed by field-emission scanning electron microscopy (FE-SEM) showed that uniform CNF/PVA composite nanofibers were manufactured at 1~3% CNF contents while many beads were observed at 5% CNF level. Both the viscosity of CNF/PVA solution and diameter of the electrospun nanofiber decreased with an increase in CNF content. The diameter and its distribution of the electrospun nanofibers helped explain the differences observed in their morphology. These results show that the electrospinning method was successful in preparing uniform CNF/PVA nanofibers, indicating a great potential for manufacturing consistent and reliable cellulose-based nanofibrils for scaffolds in future applications.

• Journal of the Korean Wood Science and Technology
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• 제23권3호
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• pp.23-27
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• 1995

Several characteristic results of physical and optical properties of paper treated by UV light were obtained in the previous papers(Kim et al. 1988). In this paper, folding endurance and brightness of paper prepared by spraying photostabilizer were examined in order to elucidate photodegradation phenomena, UV light absorber and radical scavenger were most effective in preventing of folding endurance decrease. These results may be indicated that depolymerization of cellulose and hemicellulose chains leading to degradation of paper mechanical properties mainly caused by radical reaction. Ineffective hydroperoxide decomposer may be explained because of auto-oxidation reactions before forming stable compound from hydroperoxide.

• Current Research on Agriculture and Life Sciences
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• 제31권1호
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• pp.18-24
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• 2013

This work attempted to fabricate organic/inorganic nanocomposite by combining organic cellulose nanofibrils (CNFs), isolated by 2,2,6,6-tetramethylpiperidine-1-oxy radical (TEMPO)-mediated oxidation of native cellulose with inorganic nanoclay. The morphology and dimension of CNFs, and tensile properties and thermal stability of CNF/clay nanocomposites were characterized by transmission electron microscope (TEM), tensile test, and thermogravimetry (TG), respectively. TEM observation showed that CNFs were fibrillated structure with a diameter of about $4.86{\pm}1.341nm$. Tensile strength and modulus of the hybrid nanocomposite decreased as the clay content of the nanocomposite increased, indicating a poor dispersion of CNFs or inefficient stress transfer between the CNFs and clay. The elongation at break increased at 1% clay level and then continuously decreased as the clay content increased, suggesting increased brittleness. Analysis of TG and derivative thermogravimetry (DTG) curves of the nanocomposites identified two thermal degradation peak temperatures ($T_{p1}$ and $T_{p2}$), which suggested thermal decomposition of the nanocomposites to be a two steps-process. We think that $T_{p1}$ values from $219.6^{\circ}C$ to $235^{\circ}C$ resulted from the sodium carboxylate groups in the CNFs, and that $T_{p2}$ values from $267^{\circ}C$ to $273.5^{\circ}C$ were mainly responsible for the thermal decomposition of crystalline cellulose in the nanocomposite. An increase in the clay level of the CNF/clay nanocomposite predominately affected $T_{p2}$ values, which continuously increased as the clay content increased. These results indicate that the addition of clay improved thermal stability of the CNF/clay nanocomposite but at the expense of nanocomposite's tensile properties.

• Journal of Ginseng Research
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• 제36권3호
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• pp.308-313
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• 2012

Fresh (raw roots), white (dried), and red (steamed-drid) ginseng samples were gamma-irradiated at 0 to 7 kGy. Electron spin resonance (ESR) technique was used to characterize the irradiation status of the samples, targeting the radiation-induced cellulose radicals after different sample pretreatments. All non-irradiated samples exhibited a single central signal (g=2.006), whose intensity showed significant increase upon irradiation. The ESR spectra from the radiation-induced cellulose radicals, with two side peaks (g=2.0201 and g=1.9851) equally spaced (${\pm}3mT$) from the central signal, were also observed in the irradiated samples. The core sample analyzed after alcoholic-extraction produced the best results for irradiated fresh ginseng samples. In the case of irradiated white and red ginseng samples, the central (natural) and radiation-induced (two-side peaks corresponding to cellulose radical) signal intensities showed little improvement on alcoholic-extraction. The water-washing step minimized the effect of $Mn^{2+}$, but reduced the intensity of side peaks making them difficult to indentify. The effect of different origins was negligible, however harvesting year showed a clear effect on radiation-induced ESR signals.

• 한국염색가공학회지
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• 제5권3호
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• pp.173-181
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• 1993

Dyeing cotton fabric with direct dye (C. I. Direct Blue 15) by redox sytem of ammonium persulfate as an oxidant and glucose as reductant was studied. It was found that covalent bond between dye and cellulose molecule can be formed by free radical produced by the redox system in the dye bath, which enhanced significantly the color strength. The retained color strength after DMF extraction was much better in the presence than in the absence of the redox sytem. The optimum dyeing condition was 0.028 mol/$\ell$(APS/Glucose each) of redox concentration, 65$^{\circle}C$ of dyeing temperature and 60min of dyeing time. The color variation on the dyed sample had not been observed as a result of fixed ${\lambda}_max$.

• 한국식품영양과학회지
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• 제41권10호
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• pp.1454-1459
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• 2012

섬유소 식품 중 바질과 정향의 방사선 조사처리 여부 확인을 위한 전자스핀공명분석법(ESR)의 개선을 위해 동결건조(FD), 상압건조(OD), 알코올건조(AE), 알코올세척건조(WAE) 처리하여 cellulose radical을 확인하였다. 비 조사 시료는 모두 singlet signal($g_0$=2.006)을 나타내었고, 조사된 시료의 경우는 모두 singlet signal을 중심으로 두 개의 side peak($g_1$=2.023 and $g_2$=1.986)가 6 mT 간격으로 나타나 cellulose 유래의 signal을 확인할 수 있었다. AE, WAE 처리한 정향의 경우, 조사유래의 cellulose radical의 ESR intensity가 증가하였으며, central peak와 side peak의 비율도 판별에 매우 적합하였다. 그러나 FD 처리한 바질의 경우 ESR intensity는 가장 크게 나타났으나, signal ratio는 AE, WAE 처리하였을 때 더 이상적이었다. 또한 $Mn^{2+}$ signal 유래의 radical은 AE, WAE 처리한 시료에서 크게 감소하여, FD 및 OD에 비해 매우 명확한 조사여부 판별이 가능하였다. 따라서 AE, WAE 처리는 바질과 정향의 조사여부 판별방법을 크게 개선시키는 것으로 확인되었으며, 기타 향신료에 대해서도 ESR spectra 분석에 적용 가능할 것으로 판단되었다.