• Polymer(Korea)
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• v.24 no.3
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• pp.314-325
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• 2000

Thermal degradation of thermoplasitc polyurethane modified polycarbonate has been investigated by means of DSC, GPC and FT-IR techniques. The polyurethanes used in this study are TPU-35 and TPU-53 containing 35.5 and 53.4 wt% of hard segments, respectively. The more content of hard segment, the higher the glass transition temperature (T$_{g}$) of TPU was observed. On the other hand, the T$_{g}$ of the TPU modified PC decreased with the content of TPU and the annealing temperature regardless of the hard segment contents. The latter behavior nay arise from the thermal degradation of TPU upon annealing process: the observed thermal degradation temperatures were at 240 and 25$0^{\circ}C$ for the PC/TPU-35 and PC/TPU-53, respectively. The molecular weight, molecular weight distribution and viscosity agree well with the DSC measurement, which implicates a thermal degradation of TPU. In addition, thermal stability of the TPU modified PC linearly decreased with an incorporation of TPU. Transesterification or any interaction was not observed using FT-IR: the evidence was no frequency shift or any variance betwere the carbonyl stretching and NH group. For the specimens prepared below the degradation temperature, the enhancement of the thickness dependent impact strength of the PC/TPU blend was observed, and the morphology of the two blends was compared.d.

• Applied Chemistry for Engineering
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• v.25 no.3
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• pp.318-323
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• 2014

In order to analyze the effect of maleic anhydride (MAH) content and styrene monomer (SM)/MAH mole ratio on reactive extrusion of maleic anhydride grafted random polypropylenes (MAH-g-rPP), MAH-g-rPPs were prepared by using a twin screw extruder. MAH contents were 0.5, 1.0, 3.0, and 5.0 phr and SM/initiator mole ratio was 0.0, 1.0, and 2.0. Dicumyl peroxide (DCP) was used as an initiator. The graft degree of MAH was confirmed by the existence of carbonyl group (C = O) stretching peak at $1700cm^{-1}$ from FT-IR spectrum. The degree of graft reaction increased up to 3.0 phr MAH and showed the optimum value at 1.0 SM/MAH mole ratio from the area ratio of C = O and C-H stretching peak. Thermal and crystallization properties of MAH-g-rPP and PP/MAH-g-rPP/pulp composites were investigated by DSC, TGA, XRD, and POM. There was a decrease in non-isothermal crystallization temperature of PP/MAH-g-PP/pulp composites. Based on tensile properties and SEM pictures for the fractured surface of PP/MAH-g-PP/pulp composites, MAH content of 1.0 wt% and SM/MAH mole ratio of 1.0 were the optimum formulation as the compatibilizer. The rheological properties of the composites were measured by dynamic Rheometer to compare the processability of the composites with and without compatibilizer. The power law index showed slightly low value at the composites with compatibilizer.

• Bulletin of the Korean Chemical Society
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• v.14 no.4
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• pp.439-444
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• 1993

The aerobic oxidation of the Fe(II) complex of 1,4,8,11-tetraazacyclotetradecane, [Fe(cyclam)$(CH_3CN)_2](ClO_4)_2$, in MeCN in the presence of a few drops of $HClO_4$ leads to low spin Fe(III) species [Fe(cyclam)$(CH_3CN)_2](ClO_4)_3$. The Fe(III) cyclam complex is further oxidized in the air in the presence of a trace of water to produce the deep green binuclear bismacrocyclic Fe(II) complex $[Fe_2(C_{20}H_{36}N_8)(CH_3CN)_4](ClO_4)_4{\cdot}2CH_3CN$. The Fe(II) ions of the complex are six-coordinated and the bismacrocyclic ligand is extensively unsaturated. $[Fe_2(C_{20}H_{36}N_8)(CH_3CN)_4](ClO_4)_4{\cdot}2CH_3CN$ crystallizes in the monoclinic space group $P2_1/n$ with a= 13.099 (1) ${\AA}$, b= 10.930 (1) ${\AA}$, c= 17.859 (1) ${\AA}$, ${\beta}$= 95.315 $(7)^{\circ}$, and Z= 2. The structure was solved by heavy atom methods and refined anisotropically to R values of R= 0.0633 and $R_w$= 0.0702 for 1819 observed reflections with F > $4{\sigma}$ (F) measured with Mo K${\alpha}$ radiation on a CAD-4 diffractometer. The two macrocyclic units are coupled through the bridgehead carbons of ${\beta}$-diimitie moieties by a double bond. The double bonds in each macrocycle unit are localized. The average bond distances of $Fe(II)-N_{imine}$, $Fe(II)-N_{amine}$, and $Fe(II)-N_{MeCN}$ are 1.890 (5), 2.001 (5), and 1.925 (6) ${\AA}$, respectively. The complex is diamagnetic, containing two low spin Fe(II) ions in the molecule. The complex shows extremely intense charge transfer band in the near infrared at 868 nm with ${\varepsilon}$= 25,000 $M^{-1}cm^{-1}$. The complex shows a one-electron oxidation wave at +0.83 volts and two one-electron reduction waves at -0.43 and-0.72 volts vs. Ag/AgCl reference electrode. The complex reacts with carbon monoxide in $MeNO_2$ to form carbonyl adducts, whose $v_{CO}$ value (2010 $cm^{-1}$) indicates the ${\pi}$-accepting property of the present bismacrocyclic ligand.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.284-289
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• 2017

Oxidized polyethylene wax (OPEW) is, one of the food additives, used as a coating agent in citrus fruits and nuts. OPEW is authorized to quantum satis in EU, USA, and is acceptable less than 250 mg/kg in Australia and New Zealand. But OPEW is unauthorized as a food additive in Korea. This study was to establish the analytical method of OPEW and demonstrate the effective application of various food samples. We first conducted to compare the various analytical method including acid value (AV), high temperature gel permeation chromatography (HT-GPC), matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF/MS), gas chromatography flame ionization detector (GC-FID) and fourier transform infrared spectroscopy (FT-IR). This result indicated that FT-IR spectrum of OPEW treated food sample displayed absorption bands for carbonyl group (C=O, $1714cm^{-1}$), ester group (C-O, $1463cm^{-1}$), aliphatic group (C-H, $2916cm^{-1}$). Furthermore, IR spectrum of OPEW treated food sample showed similar tendency with IR spectrum of OPEW standard. Therefore, it is confirmed that analytical method using FT-IR can be detected on analysis of OPEW in food. As a result of monitoring of 111 samples using established analytical method, OPEW was not detected in the food samples.

• Nuclear Medicine and Molecular Imaging
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• v.41 no.4
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• pp.326-334
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• 2007

Purpose: The estrogen receptor (ER), which is over-expressed in ER-positive breast tumors, has been imaged by positron emission tomography (PET) using $[^{18}F]$ labeled estrogen ligands, especially $[^{18}F]FES$. However, $[^{18}F]$ has relatively short-lived half-life ($t_{1/2}$ =1.8 h) and the labeling yield of radio-fluorination is usually low compared with $^{64}Cu\;(t_{1/2}=12.7\;h)$. 1,4,7,10-tetraazacyclododecane (cyclen) is used to form stable metal complexes with copper, indium, gallium, and gadolinium. With these in mind, we prepared cyclen-based Cu complexes which mimic estradiol in aspect of two hydroxyl groups. Materials and Methods: 1.7-Protected cyclen, 1.7-bis (benzyloxycarbonyl)-cyclen was synthesized according to the reported procedure. After introducing two 4-benzyloxybenzyl groups at 4,10-positions, the benzyloxycarbonyl and benzyl groups were removed at the same time by hydrogenation on Pd/C to give 1,7-bis(4-hydroxybenzyl)-1,4,7,10-tetraazacyclododecane (1). Results: The prepared ligand 1 was fully characterized by $^1H,\;^{13}C$ NMR, and mass spectrometer. The synthesized ligand was reacted with copper chloride and copper perchlorate to give copper complexes $[Cu(1)]^{2+}2(CIO_4^-)\;and\;[Cu(1)Cl]^+Cl^-$ which were confirmed by high-resolution mass (FAB). Conclusion: We successfully synthesized a cyclen derivative of which two phenol groups are located on trans position of N-atoms. And, two Cu(ll) complexes of +2 and +1 overall charge, were prepared as a potential PET tracers for ER imaging.

• Journal of the Korean Chemical Society
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• v.37 no.3
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• pp.344-350
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• 1993

25,26,27,28-Tetraacetoxycalix[4]arene·monohydrate is orthorhombic, space group Pbca with a = 14.979(4), b = 15.154(4), c = 27.890(3) ${\AA}$, Z = 8, V = 6330.6 ${\AA}^{-3}$, D$_c$ = 1.28 $g{\cdot}cm^{-3}$, (Mo K${\alpha}$) = 0.71069 ${\AA}$, ${\mu}$ = 0.86 cm$^{-1}$, F(000) = 2600, and R = 0.069 for 3376 unique observed reflections with I > 1.0 ${\sigma}$(I). The structure was solved by direct methods and refined by cascade diagonal least-squares refinement. All the C-H bond lengths(= 0.96 ${\AA}$), the methyl groups and the methylene groups are fixed and refined as the rigid groups with ideal geometry. The macrocycle exists in the 1,3 alternate conformation (by Conforth) making the angles of 110.7, 684, 113.7 and 68.8$^{\circ}$ between the benzene rings and the methylenic mean plane, and four each acetoxy groups are twisted away from their own benzene rings with the angles of 68.2, 97.6, 78.9 and 71.3$^{\circ}$, respectively. The relative dihedral angles between two opposite side of the benzene rings are 135.6$^{\circ}$ for the rings (1) and (3) and 135.2$^{\circ}$ for (2) and (4). A water molecule which has nearly the same height of the methylenic plane of the macrocycle in the c-axis, is located within the distances of 2.942(5) ${\AA}$ from the O(8) atom of the carbonyl group and 2.901 ${\AA}$ from, another O(2)(1/2-x, -1/2＋y, z). The shortest contact between the molecule is 3.193 ${\AA}$ from the O(4) to the C(3)(1/2＋x, 1/2-y,-z).

• Applied Chemistry for Engineering
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• v.21 no.4
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• pp.377-384
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• 2010

We perform a comparative study to investigate the properties of the new energetic chain extender (AzPD). A series of poly(glycidyl azide)/poly(tetramethylene oxide)-based energetic segmented polyurethane (GAP/PTMG ESPU) with different chain extender, which is 3-azidopropane-1,2-diol (AzPD), 1,4-butane diol (1,4-BD), or 1,5 pentane diol (1,5-PD), was synthesized by solution polymerization in dimethyl formamide (DMF) and their phase behaviors were investigated. The ESPUs were characterized with Fourier transform infrared-attenuated total reflection spectroscopy (ATR FT-IR), differential scanning calorimetry (DSC), and dynamic mechanical analysis (DMA). The results of the ATR FT-IR analysis of the urethane carbonyl group region showed that the 'free' C=O fraction was higher in GAP/PTMG AzESPU (0.5) than GAP/PTMG BDESPU (0.44) and GAP/PTMG PDESPU (0.41) for 7 days samples after preparation and that it was similar in the range of 0.26~0.29 for three 60 days ESPU samples. DMA curves of the GAP/PTMG AzESPU for 7 days samples showed amorphous polymers, but GAP/PTMG BDESPU and GAP/PTMG PDESPU showed viscoelastic behaviors with rubbery plateau and the flow region. However, DMA curves of the GAP/PTMG AzESPU for 60 days samples showed viscoelastic behaviors with rubbery plateau and the flow region like GAP/PTMG PDESPU, but GAP/PTMG BDESPU did not show the flow region. From phase behaviors with ATR FT-IR, DSC and DMA analysis, GAP/PTMG AzESPU showed good phase-mixing between components. However, it represented viscoelastic behavior of TPE similar to GAP/PTMG PDESPM according to phase equilibrium progress with aging time.

• Journal of Korean Society of Forest Science
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• v.45 no.1
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• pp.62-67
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• 1979

Ultraviolet microscopy of ultrathin sections of wood has proved to be one of the useful means for determining the lignin distribution in the various regions of the cell wall. Also, spectral approach and quantitative analysis of isolated compound middle lamella fraction from birch xylem have revealed that the lignin associated with the vessel secondary wall and middle lamella is composed predominantly of gualacylpropane units. Lignin deposited in the fiber and ray parenchyma secondary walls is composed mostly of syringylpropane units. The middle lamella lignin around fibers and ray cells contains both guaiacyl and syringyl propane quits. On the basis of the results above, this research was carried out to clarify the origin of milled wood lignin (MWL) by analysing the chemical characteristics of ML MWLs extracted at various milling stages. The amount of phenolic hydroxyl-, ${\alpha}$-carbonyl-, and methoxyl-group in the MWL's increases the milling time. And progressive mining contributes to the merease of ratio of syringylaldehyde to vanillin(S/V ratio) after nitrobenzene oxidation of MWL. Accordingly, It could be concluded that milled wood lignin extracted at the initial milling stage derives from compound middle lamella region of cell wall, whereas, with progressive milling, lignin of secondary wall of fiber is introduced gradually to milled wood lignin. These results are suggesting that heterogeneous chemical structure of lignins in hardwood exists. Although milled wood lignin at the initial stage seems to have lower molecular weight in comparison with milled wood lignin extracted at final milling stage from the result of Gel-filtration curves, further study would be required on molecular weight distribution of milled wood lignin in future.

• Applied Chemistry for Engineering
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• v.9 no.2
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• pp.207-213
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• 1998

On the basis of the previous study[1], miscibility were investigated and intermolecular interaction strength for the miscibility were relatively compared for the blends poly{2,2-(m-phenylene)-5,5'-bibenzimidazole}(PBI) with two aromatic polyimides (PIs) synthesized by another dianhydride. Aromatic PAAs were prepared by the reaction of condensation of two diamines, 4,4'-methylene dianiline(4,4'-MDA) and 4,4'-oxydianiline(4,4'-ODA) with 3,3',4,4'-diphenylsulfone tetracarboxylic dianhydride(DSDA) using DMAc, and then converted into PIs after curing. PBI/PAA blends were prepared by solution blending. Cast films or precipitated powders of the PBI/PAA blends were cared at a high temperature to transform into PBI/PIs blends. Miscibility and specific intermolecular interaction for miscibility in the blends were investigated, and compared with previous polyimide structures of PBI/PIs blends [1]. Two blends, PBI/DSDA+4,4'-MDA(Blend-V) and PBI/DSDA+4,4'-ODA(Blend-VI), were found miscible : the evidences were optically clear films, synergistic single composition dependent $T_g{\prime}s$, and frequency shifts of N-H stretching band as much as $39{\sim}40cm^{-1}$, and of C=O stretching band near 1730 and $1780cm^{-1}$, 5~6 and $3{\sim}4cm^{-1}$, respectively. The specific intermolecular interactions existing between PBI and PIs were relatively analyzed with the area(A) formed between the $T_g{\prime}s$ of the measured and that of the calculated by the Fox equation at all compositions, the ${\kappa}$ values in Gordon-Taylor equation obtained from the measured $T_g{\prime}s$, and differences of the frequency shifts in the functional N-H and carbonyl stretching band. From the results, the area(A) and the ${\kappa}$ values for Blend-V and VI were smaller than those for Blend-III and IV used in previous study[1]. Differences of the frequency shifts in the functional groups(N-H and C=O) also showed similar tendency. Thus, specific intermolecular interaction strength in terms of hydrogen bonding of PBI/PI blends is dependent upon chemical structures of PIs, that is, PIs it seems that $SO_2$ group in dianhydride(DSDA) has weaker hydrogen bond strength than those of C=O in BTDA. In other words, it implies that the former occupied bulk space than the latter due to the sterric effect.

• Journal of the Korean Society of Food Science and Nutrition
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• v.35 no.1
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• pp.61-67
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• 2006

The oxidative stability of lipids from eel (Anguilla japonica) fed diets containing different concentrations of conjugated linoleic acid (CLA) was studied. Eels, 3 weeks of age, with an average weight of 160 g, were randomly divided into 5 groups (5 fishes/group) by body weight, and assigned to one of the five CLA-supplemented diets at the following concentrations: 0, 0.5, 1.0, 2.5, and $5.0\%$ CLA. After 8 weeks of feeding, eels were sacrificed and the total lipid contents were extracted. The lipids from each treatment groups were stored at $37^{\circ}C$ for 5 weeks. Changes in the fatty acid profile, lipid class, weight gained, peroxide value (POV) and carbonyl value (COV) of the lipid from each treatment groups were analyzed weekly. The composition of CLA in the lipids of eels fed with 0.5, 1.0, 2.5, and $5.0\%$ CLA-supplemented diets were 0.5, 1.7, 3.3, and $6.2\%$, respectively After 4 weeks of storage, the proportion of polyunsaturated fatty acids (PUFAs) in the lipid of eels fed diets containing 1.0 and $2.5\%$ CLA were 15.3 and $14.8\%$, respectively. Whereas, lipid extracted from eels fed with 0.5 and $5.0\%$ CLA-supplemented diets contain 11.8 and $7.4\%$ PUFAs, respectively. Lipid from the control sample contained $9.0\%$ PUFAs. POV and COV were found to be the lowest in the lipids samples from 1.0 and $2.5\%$ CLA diets. These results indicate that lipids from diets containing 1.0 or $2.5\%$ CLA were more stable against oxidative rancidity relative to other concentrations, suggesting that these are the appropriate CLA concentrations for the production of stable eel lipids.