• Journal of the Korean Chemical Society
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• v.55 no.2
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• pp.230-234
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• 2011

The present study describes the synthesis of 4,5-dihydro-6-(4-methoxy-3-methylphenyl)-3(2H)-pyridazinone derivatives. The synthesis of the first target compound, 4,5-dihydro-6-(4-methoxy-3-methylphenyl)-3(2H)-pyridazinone (1), was achieved by Friedel-Crafts acylation of o-cresyl methyl ether with succinic anhydride and subsequent cyclization of the intermediary g-keto acid with hydrazine hydrate. Condensation of compound 1 with aromatic aldehydes in the presence of sodium ethoxide affords the corresponding 4-substituted benzyl pyridazinones (3a-d). The dihydropyridazinone 1 underwent dehydrogenation upon treatment with bromine/acetic acid mixture to give (4). Pyridazine (5) has been synthesized upon the reaction of pyridazinone (1) with 1,3-diphenyl-2-propen-1-one under the Michael addition reaction. N-dialkylaminomethyl derivatives 6a-b have been obtained from the reaction of pyridazinone 1 with formaldehyde and secondary amine, whereas reaction of 1 with formaldehyde gives N-hydroxymethyl derivative (7). This study also includes the synthesis of the 3-chloropyridazine derivative 8 in excellent yield by heating pyridazinone 3b in phosphorus oxychloride. The behaviour of the chloro derivative toward sodium azide, benzyl amine and anthranilic acid was also studied. The proposed structures of the products were confirmed by elemental analysis, spectral data and chemical evidence.

• Journal of Surface Science and Engineering
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• v.50 no.5
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• pp.411-420
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• 2017

In this paper, two methods of making the Pd-added $SnO_2$ ($Pd-SnO_2$) powder with pure tetragonal phase by the hydrazine method were suggested and compared in terms of crystal structure, surface morphology, and alcohol gas response. One of the addition methods is to use $PdCl_2$ as a Pd source, the other is to use Pd-based organic with oleylamine (OAM). When Pd concentration was increased from 0 to 5 wt%, the average grain size of $Pd-SnO_2$ made with Pd-OAM were decreased from 32 to 12 nm. In the case of using with $PdCl_2$, grain size of the $PdCl_2$ fell to less than 10 nm. However, agglomerated and extruded surface morphology was observed for the films with Pd addition over 4 wt%. The crack-free $Pd-SnO_2$ thick films were able to successfully fill the $30{\mu}m$ gap of patterned Pt electrodes by optimized ink dropping method. Also, the 2 wt% $Pd-SnO_2$ thick film made with PdCl2 showed gas responses ($R_{air}/R_{gas}$) of 3.7, 5.7 and 9.0 at alcohol concentrations of 10, 50 and 100 ppm, respectively. On the other hand, the prepared 3 wt% $Pd-SnO_2$ thick film with Pd-OAM exhibited very excellent responses of 3.4, 6.8 and 12.2 at the equivalent measurement conditions, respectively. The 3 wt% $Pd-SnO_2$ thick film with Pd-OAM has a specific surface area of $31.39m^2/g$.

• Clean Technology
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• v.25 no.1
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• pp.14-18
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• 2019

In general after the etching process, waste etching solution contains metals. (ex. Nickel (Ni), Chromium (Cr), Zinc (Zn), etc.) In this work, we proposed a recycling process for waste etching solution and refining from waste liquid contained nickel to make nickel metal nano powder. At first, the neutralization agent was experimentally selected through the hydrolysis of impurities such as iron by adjusting the pH. We selected sodium hydroxide solution as a neutralizing agent, and removed impurities such as iron by pH = 4. And then, metal ions (ex. Manganese (Mn) and Zinc (Zn), etc.) remain as impurities were refined by D2EHPA (Di-(2-ethylhexyl) phosphoric acid). The nickel powders were synthesized by liquid phase reduction method with hydrazine ($N_2H_4$) and sodium hydroxide (NaOH). The resulting nickel chloride solution and nickel metal powder has high purity ( > 99%). The purity of nickel chloride solution and nickel nano powders were measured by EDTA (ethylenediaminetetraacetic) titration method with ICP-OES (inductively coupled plasma optical emission spectrometer). FE-SEM (field emission scanning electron microscopy) was used to investigate the morphology, particle size and crystal structure of the nickel metal nano powder. The structural properties of the nickel nano powder were characterized by XRD (X-ray diffraction) and TEM (transmission electron microscopy).

• Applied Chemistry for Engineering
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• v.33 no.6
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• pp.600-605
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• 2022

In this study, nitrogen oxide (NO_x) removal experiments were performed using a graphene based ceramic filter coated with a V₂O₅-WO₃-TiO₂ catalyst. Graphene oxide (GO) was prepared by Hummer's method using graphite, and the reduced graphene oxide was produced by reducing with hydrazine (N₂H₄). Vanadium (V), Tungsten (W), and Titanium (Ti) were coated by the sol-gel method, and then a metal oxide-supported filter was prepared through a calcination process at 350 ℃. A NO_x removal efficiency test was performed for the catalytic ceramic filters with UV light in a humid condition. When graphene oxide (GO) and reduced graphene oxide (rGO) were present on the filter, the NOx removal efficiency was superior to that of the conventional ceramic filter. Most likely, this is due to an improvement in the adsorption properties of NOx molecules on graphene coated surfaces. As the concentration of graphene increased, higher NO_x removal efficiency was confirmed.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.32 no.6
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• pp.239-245
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• 2022

Reduced graphene oxide (rGO) has attracted many attention and applications due to its excellent electrochemical ability. Therefore, standardization of rGO through structural and thermal analysis facilitates quality improvement and management, enabling users to increase efficiency and reduce relevant costs. For rGO and graphene-related materials, it is very important to determine the number of layers and define the resulting difference in physical properties. In this study, 3~4 layers of rGO-1 and 9~10 layers of rGO-2 were obtained from graphene oxide (GO) through a hydrazine reduction process. For the prepared rGOs, X-ray diffraction (XRD) pattern obtained a diffraction peak at 2θ≈25° related to (002) reflection was used to calculate the layer numbers by determining interlayer distance and FWHM value. To reduce the angular uncertainty, XRD data analysis was performed with angle correction using standard reference materials for X-ray powder diffraction analysis. Precise interlayer distance and number of layers were determined using OriginLab and open-source XRD diffraction analysis programs using the angle-corrected diffraction data. TG-DSC thermal analysis was performed to further standardize the physical properties of rGO samples.

• Korean Chemical Engineering Research
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• v.44 no.1
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• pp.65-72
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• 2006

Recent technical advances in the biorecognition engineering and the microparticle fabrication may enable us to develop the single step purification using magnetic particle, because of its simplicity, efficacy, ease of automation, and process economics. In this study, we used commercial magnetic particles from Seradyn, Inc. (Indianapolis, USA). It was ca. 2.8 micron in diameter, consisted of polystyrene core and magnetite coating, and its surface had carboxyl groups. The model, capture protein was IgG and anti-IgG was used as the ligand molecule. We studied the different surfaces ('nude', ester-activated, and anti-IgG coated) for their biorecognition of IgG. At a high pH condition, we could reduce non-specific binding. Also anti-IgG immobilized magnetic particle could capture IgG more selectively. We attempted 'oriented immobilization' of anti-IgG, in which the polysaccharides moiety near the C-terminus was selectively oxidized and linked to the hydrazine-coated MP, to improve the efficacy of biorecognitive binding. Using this method, the IgG capturing ability was improved by ca. 2 fold. From the binary mixture of the IgG-insulin, IgG could be more selectively captured. In summary, the oriented immobilization of oxidized anti-IgG proved to be as effective as the streptavidin-biotin system and yet simpler and cost-effective. This immobilization method can find its applications in protein biochips and biotargeting.

• Korean Journal of Veterinary Research
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• v.37 no.1
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• pp.167-176
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• 1997

The present investigation was focussed mainly on the development of the tumors and proliferating cells on the intestinal tracts of 1, 2-dimethyl-hydrazine(DMH)-treated young or adult rats. 26 rats(Wistar, 14 young rats weighting approximately 130~180gm and 12 adult rats weighting approximately 500~550gm) were given subcutaneously once weekly with 20mg of DMH/kg body weight(BW)/week for 8~22 weeks. Individual body weight were recorded weekly at the same day and time. The rats were killed at 8, 13, 15. 17, 19, 21 and 22 weeks. The intestinal tracts were opened longitudinally and carefully examined for tumors. The localization, number, and size of tumors were noted. Tumor-bearing areas were dissected out and fixed on neutral buffered 10% formalin and normal-looking mucosa from 8~22 weeks rats were also taken for fixation. Paraffin sections were stained by H-E for histopathological examination or with immunohistochemical stain for bromodeoxyuridine(Brdur) positive cells. 1. The growth proportion of body weight appeared to be decreased in the DMH-treated young rats than in control young rats and body weight of DMH-treated adult rats appeared to be 13.4% or less lower than weighted on 0 week. 2. Macroscopically, the developed tumors in the intestinal tracts were not observed as early as the 13 weeks after DMH treatment. The number of developed tumors per rat was found to be 14.3, 18.8, 22.3 in 15, 17 and 22 weeks. The numbers of tumors in intestinal regions per rat were 2.1, 4.3, 5.4, 2.5 in duodenum, jejunum, ilium and colon on 15 weeks, 2.3, 6.4, 7.8, 2.3, on 17 weeks, and 2.7, 9.3, 9.0, 1.3 on 22 weeks, respectively and the ileum and jejunum were higher in appearance rate of tumors and tumor types are dome shapes and diameter of largest tumor were 6.3mm. 3. Histopathologically, intestinal mucosa were thickened by the irregular distorted and distended crypts following hyperplasia. The tumors developed on the mucosa and submucosa and were recognized to be adenocarcinoma. 4. Immunohistochemically, the labeling index(LI) was calculated as the ratio of the number of Brdur-labeled cells to the total number of column cells of the crypts with longitudinal axis. LI of Brdur positive cells per crypt were 5.6%, 8.0% on small intestine of control and 22 week group, respectively and 3.7%, 12.7% on large intestine of control and 22 week group, respectively and were appeared to be increase in 22 week group than in control group and to be more number of proliferating cells in 22 week group than in control group. 5. LI of Brdur positive cells in 1, 2, 3, 4, 5 segments of crypt column were 11.7%, 10.7%, 3.8%, 0.6%, 0% in small intestine of control group and 23.5%, 11.8%, 2.3%, 2.4%, 0.8% in small intestine of 22 week group, and 5.4%, 7.4%, 3.8%, 1.0%, 0.4% in large intestine of control group and 29.5%, 20.3%, 5.9%, 6.3%, 1.3% in large intestine of 22 week group respectively. So results indicate that the number of proliferating cells by DMH treatment increase and were concentrated on the 1, 2 segments of crypt columns.

• The Korean Journal of Nuclear Medicine
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• v.36 no.6
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• pp.333-343
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• 2002

Purpose: A new linker, hydrazino nicotinamide (HYNIC), was recently introduced for labelling of liposome with $^{99m}Tc$. In this study we synthesized HYNIC derivatized PEG (polyethylene glycol)-liposomes radiolabeled with $^{99m}Tc$. Materials and Methods: In order to synthesize HYNIC-DSPE (distearoyl phosphatidyl ethanolamine) which is a crucial component for $^{99m}Tc$ chelation, first of all succinimidyl 6-BOC-hydrazinopyridine-3-carboxylic acid was synthesized from 6-chloronicotinic acid by three sequential reactions. A DSPE derivative of succinimidyl 6-BOC-hydrazinopyridine-3-carboxylic acid was transformed into HYNIC-DSPE by HCI/dioxane. HYNIC-PEG-liposomes were prepared by hydration of the dried lipid mixture of EPC (egg phosphatidyl choline): PEG-DSPE : HYNIC-DSPE:cholesterol (1.85:0.15:0.07:1, molar ratio). The HYNIC-PEG-liposomes were labeled with $^{99m}Tc$ in the presence of $SnCl_2{\cdot}2H_2O$ (a reducing agent) and tricine (a coligand). To investigate the level of in vivo transchelation of $^{99m}Tc$ in the liposomes, the $^{99m}Tc$-HYNiC-PES-liposomes were incubated with a molar excess of DTPA, cysteine or glutathione solutions at $37^{\circ}C$ for 1 hour. The radiolabeled liposomes were also incubated in the presence of human serum at $37^{\circ}C$ for 24 hours. Results: 6-BOC-hydrazinopyridine-3-carboxylic acid was synthesized with 77.3% overall yield. The HYNIC concentration in the PEG-coated liposome dispersion was 1.08 mM. In condition of considering the measured liposomal size of 106 nm, the phospholipid concentration of $77.5\;{\mu}mol/m{\ell}$ and the liposomal particle number of $5.2{\times}10^{14}$ liposomes/ml, it is corresponded to approximate 1,250 nicotinyl hydrazine group per liposome in HYNIC-PEG-liposome. The removal of free $^{99m}Tc$ was not necessary because the labeling efficiency were above 99%. The radiolabeled liposomes maintained 98%, 96% and 99%, respectively, of radioactivity after incubation with transchelators. The radiolabeled liposomes possessed above 90% of the radioactivity in serum. Conclusion: These results suggest that the HYNIC can be synthesized easily and applied in labelling of PEG-liposomes with $^{99m}Tc$.

• Applied Biological Chemistry
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• v.17 no.2
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• pp.125-137
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• 1974

The chemical structure of glycolipid of Selenomonas ruminantium cell wall was to be elucidated. The bacterial cells were treated in hot TCA and the glycolipid fractions were extracted by the solvent $CHCl_3\;:\;CH_3OH$ (1 : 3). The extracted glycolipids fraction was further separated by acetone extraction. The acetone soluble fraction was named as the spot A-compound. The acetone insoluble but ether soluble fraction was named as the spot B-compound. These two compounds were examined for elucidation of their chemical structure. The results were as follows: 1. The IR spectral analysis showed that O-acyl and N-acyl fatty acids were linked to glucosamine moiety in the spot A-compound. However in the spot B-compound in addition to O and N-acyl acids phosphorus was shown to be attached to glucosamine. 2. It was recognized by gas liquid chromatography that spot A compound contained beta-OH $C_{13:0}$ fatty acid in predominance in addition to the fatty acid with beta-OH $C_{9:0}$, whereas the spot B compound was composed of the predominant fatty acid of beta-OH $C_{13:0}$ with small amount of beta-OH $C_{9:0}$. 3. According to the paper chromatographic analysis of hydrazinolysis products of the spot A compound, a compound of a similar Rf value as the chitobiose was recognized, which indicated a structure of two molecules glucosamine condensed. The low Rf value of the hydrazinolysis product of the spot B-compound confirmed the presence of phosphorus attached to glucosamine. 4. The appearance of arabinose resulting from. ninhydrin decomposition of the acid hydrolyzate of the spot A compound indicated that the amino group is attached to $C_2$ of glucosamine. 5. The amount of glucosamine in the N-acetylated spot A compound decreased in half of the original content by the treatment. with $NaBH_4$, indicating that there are two molecules of glucosamines in the spot A compound. The presence of 1, 6-linkage between two molecules of glucosamine was suggested by the Morgan-Elson reaction and confirmed by the periodate decomposition test. 6. By the action of ${\beta}-N-acetyl$ glucosaminidase the N-acetylated spot A compound was completely decomposed into N-acetyl glucosamine, whereas the spot B compound was not. This indicated the spot A compound has a beta-linkage. 7. When phosphodiesterase or phosphomonoesterase acted on $^{32}P-labeled$ spot B compound, $^{32}P$ was not released by phosphodiesterase, but completely released by phosphomonoesterase. This indicated that one phosphorus is linked to glucosamine moiety. 8. The spot A compound is assumed to have the following chemical structure: That is glucosaminyl, ${\beta}-1$, 6-glucosamine to which O-acyl and N-acyl fatty acids are linked, of which the predominant fatty acid is beta-OH $C_{13:0}$ fatty acid in addition to beta-OH $C_{9:0}$ fatty acid 9. The spot B compound is likely to have the linkage of $glucosaminyl-{\beta}-1$, 6-glucosamine to which phosphorus is linked in monoester linkage. Furthermore both O-acyl and N-acyl fatty acids contained beta-OH $C_{13:0}$ fatty acid predominantly in addition to beta-OH $C_{9:0}$ fatty acid.