• Journal of Food Hygiene and Safety
• /
• v.34 no.2
• /
• pp.140-147
• /
• 2019

An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

• Journal of the Korean Ceramic Society
• /
• v.39 no.3
• /
• pp.286-293
• /
• 2002

Microstructure and the electrical porperties of a ZnO-based multilayered chip-type varistor(abbreviated as MLV) with Ag/Pd(7:3) inner electrode have been studied as a function of firing of temperature. At 1100$^{\circ}$C, inner electrode layers began to show nonuniform thickness and small voids, which resulted in significant disappearance of the electrode pattern and delamination at 1100$^{\circ}$C. MLVs fired at 950$^{\circ}$C showed large degradation in leakage current, probably due to incomplete redistribution of liquid and transition metal elements in pyrochlore phase decomposition. Those fired at 1100$^{\circ}$C and above, on the other hand, revealed poor varistor characteristics and their reproductibility, which are though to stem from the deformation of inner electrode pattern, the reaction between electrode materials and ZnO-based ceramics, and the volatilization of $Bi_2O_3$. Throughout the firing temperature range of 950∼1100$^{\circ}$C, capacitance and leakage current increased while breakdown voltage and peak current decreased with the increase of firing temperature, but nonlinear coefficient and clamping ratio kept almost constant at ∼30 and 1.4, respectively. In particular, those fired between 1000$^{\circ}$C and 1050$^{\circ}$C showed stable varistor characteristics with high reproducibility. It seems that Ag/Pd(7:3) alloy is one of the electrode materials applicable to most ZnO-based MLVs incorporating with $Bi_2O_3$ when cofired up to 1050$^{\circ}$C.

• KSBB Journal
• /
• v.14 no.1
• /
• pp.82-90
• /
• 1999

In order to eventually fabricate an analytical system for infectious microorganisms, we synthesized major immunochemical components, utilized them for the construction of model system, and investigated an assay concept for bacterial whole cells. For the preparation of system components, a polyclonal antibody, against Salmonella thompson as model analyte, purified by immuno-affinity chromatography was used to chemically link to streptavidin or an enzyme, horseradish peroxidase(HRP). The antibody and streptavidin was modified with sulfosuccinimidyl 4-[N-maleimidomethyl]cyclohexane-1-carboxylate and N-succinimidyl-3-[2-pyridyldithio]propionate(subsequently activated by dithiotheritol), respectively. The modified components were reacted to synthesize antibody-streptavidin conjugates which were then purified on a two-layer chromatography column of diaminobiotin gel and Sephadex G-100. For antibody-HRP conjugates, HRP molecules were activated by $NalO_4$ oxidation and then coupled to immunoglobulin. After stabilizing with ($NaCNBH_3$, the conjugates were purified by size exclusion chromatography on Biogel A5M column. To devise a model system, such produced components were combined with a dot-blotter in which a nitrocellulose membrane($12{\mu}m$ pre size) with immobilized biotin was already located. The analyte (S. thompson cells) was reacted with the both antibody conjugates in a liquid phase, and the complexes formed were captured on the membrane surfaces by applying vacuum in the bottom compartment of the blotter to invoke biotin-streptavidin reaction. Under optimal conditions, the system enabled to identify the analytical concept for bacterial whole cells, and the lower limit of detection was approximately $1{\mu}g/m{\ell}$($10^5-10^6$ cells/m$m{\ell}$). The controlling factors were the concentrations of each antibody conjugate that caused agglutination in the presence of analyte as they increased.

• Journal of the Korean Ceramic Society
• /
• v.41 no.10 s.269
• /
• pp.783-787
• /
• 2004

Microwave dielectric properties and the microstructure of $Ba_5Nb_4O_{15}$ ceramics with $PbO-B_2O_3-SiO_2$ glass frit were investigated to reduce the sintering temperature of $Ba_5Nb_4O_{15}$ ceramics as a function of the amount of glass frit from $0.5wt\%$ to $10wt\%$ and the sintering condition. The sintered density and the microwave dielectric properties of $Ba_5Nb_4O_{15}$ ceramics were remarkably changed with the amount of glass fit which existed as a liquid phase and assisted the densification. $Ba_5Nb_4O_{15}$ with $3wt\%$ $PbO-B_2O_3-SiO_2$ glass frit sintered at $900^{\circ}C$ for 2 h showed dielectric constant (K) of 41.4, a quality factor (Q $\times$f) of 13,485 GHz, and a Temperature Coefficient of resonant Frequency (TCF) of 9 ppm/$^{\circ}C$. Due to no trace of physical and chemical reaction between this composition and Ag electrode cofired at $900^{\circ}C$ for 2 h, this ceramics can be a good candidate for the multilayer dielectric filter.

• Resources Recycling
• /
• v.20 no.1
• /
• pp.54-60
• /
• 2011

The spherical artificial aggregates (AAs) with a diameter of 8 mm, which contains fly ashes discharged from the fluidized bed combustion in a thermal power plant and clay were manufactured by direct sintering method at $1050{\sim}1250^{\circ}C$ for 10 minutes. The effect of fly ash contents on the bloating phenomenon in the AAs was analyzed. The AAs containing fly ash of the amount under 50 wt% showed the black-coring and bloating phenomena. The AAs containing fly ash of the amount over 5Owt%, however, the specific gravity was increased and the color of specimens fully changed to black. These color change phenomena were caused from the formation of FeO by the reduction reaction of almost $Fe_2O_3$ component by the excessive reducing atmosphere formed simultaneously with the rapid emission of the gases generated from the high contents of unburned carbon of with increasing the added fly ash amount. Specific gravity was decreased as fly ash contents increased in the case of sintering at the same temperature condition. Water absorption of all specimens except of the specimens containing 10 wt% fly ashes decreased with increasing sintering temperature. These were because a liquid phase was formed as the increasing the sintering temperature. In the case of the specimens manufactured in this study containing fly ashes discharged from the fluidized bed combustor in a the thermal power plant and 10~90 wt% of clay, the specific gravity was 0.9~1.8 and the water absorptivity was 8~60%, therefore it is considered that those results can be applied to the light or heavy aggregates.

• KSCE Journal of Civil and Environmental Engineering Research
• /
• v.14 no.3
• /
• pp.655-668
• /
• 1994

Conventional deodorization filters using soil and compost reach the capacity limitation of deodorization in short period, because its removal mechanism primarily depends on adsorption. Therefore, in this study the experiment was performed on the removal of ammonia which is a strong inorganic malodor, frequently emitted from night soil treatment plants and sewage treatment plants, by seeding activated sludges on the bio-peat containing higher organic contents, water conservation capacity, permeability and lower pressure drop. As a result, in raw peat filter natural ammonia outlet was observed in consequence of pH increase resulted from ammonia ionizing in liquid phase. Ammonia removal mechanism primarily depended on the adsorption onto the anion colloidal substances in peat. In peat bio-filter, theoretical ammonium salts ratio was higher than that of raw peat, resulted from slight pH increase by microorganism activity, however, the experimetal value of ammonia-nitrogen accumulated in bio-peat was lower than that of raw peat because of nitrification by nitrifying bacteria. In the initial reaction period, adsorption was predominant in the ammonia removal mechanism, but nitrification was conspicuous after the middle period. Mass balance of nitrogen was established using experimental data of input $NH_3$ loading, output $NH_3$ loading, $NH_4{^+}$-N, $NO_x$-N, and Org-N. The critical time of unsteady state, which is the maximum activating point of microorganism in bio-filter, was determined using experimental data, and the ammonia adsorption curve was computed using regression analysis. On the basis of the results obtained by above analysis, the delay days for the saturation of adsoption capacity in peat bio-filter was calculated.

• Journal of Food Hygiene and Safety
• /
• v.31 no.6
• /
• pp.432-438
• /
• 2016

Ethoxyquin (EQ, 1,2-dihydro-6-ethoxy-2,2,4-trimethyl-quinoline) is quinoline-based antioxidant used in the animal feed and food industry to protect the raw materials and final products against oxidation. In recent years the use of synthetic antioxidants in fishmeal ingredients carry-over to farmed fish fillets has received increasing attention in food safety. This study was conducted to develop an analytical method to determine EQ in aquatic products. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with 1 N HCl (in case of flatfish extracted with 1 N HCl containing 10% acetonitrile). Then, solid phase extraction (SPE) was used for the cleanup. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.99, analyzed at 0.005-0.2 mg/kg concentration. The developed method was validated according to the Codex Alimentarius Commission (CAC) guideline. The limits of quantitation for EQ were 0.01 mg/kg. Average recoveries ranged from 81.3% to 107%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was below 10%. The analytical method was characterized with high accuracy and acceptable sensitivity to meet CODEX guideline requirements and would be applicable to analyze the EQ residue in aquatic products.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.22 no.1
• /
• pp.57-63
• /
• 2012

$Al_2TiO_5$ ceramics were sintered by a solid-state reaction. LAS (${\beta}$-spodumene) and $Fe_2O_3$ were added to the $Al_2TiO_5$ composition for enhancement of sintering behavior such as mechanical strength and thermal shock resistance. The sintered body was much densified by addition of LAS and $Fe_2O_3$ because LAS formed the liquid-phase and $Fe_2O_3$ suppressed the grain growth. We have systematically investigated the sintering characteristics, microstructures, mechanical properties, and thermal shock resistance according to the change of the amount of additive. When the additive of LAS (20 wt%)-$Fe_2O_3$ was added to $Al_2TiO_5$, it confirmed that superior mechanical properties of the fracture strength of over 120 MPa and the thermal shock resistance of over $1,200^{\circ}C$ were achieved.

• Applied Chemistry for Engineering
• /
• v.5 no.1
• /
• pp.160-175
• /
• 1994

Fibrous potassium hexatitanate whisker with the size of $ID=0.5{\sim}1{\mu}m$ and length=$100{\sim}1000{\mu}m$ (aspect ratio=100~1000) was produced through the reaction between titanium dioxide and potassium carbonate using the slow-cooling calcination followed by water leaching treatment. The optimum condition for the production of fibrous potassium titanate was calcination temperature of $1100^{\circ}C$ for 5hrs, $TiO_2$ mole ratlo to $K_2CO_3$ of 4.5 and slow-cooling rate of $0.5^{\circ}C/min$ to $860^{\circ}C$. Fibrous crystal are grown by the association between the solid potassium titanate and liquid phase during the slow-cooling process. The Proper water leaching condition for removing of K component was leaching time of 10hrs in boiling water. Pressurizing of the mixture of $K_2CO_3$ and $TiO_2$ to be calcinated became effective on the growth of fibrous crystal.

• Journal of the Korean Ceramic Society
• /
• v.25 no.3
• /
• pp.207-216
• /
• 1988

Effect of $SO_3$ on the formation of $C_3S$ and its properties were investigated through studies for diffusion of reacting component, the size variation of $C_3S$ and compositional change of the phases in the clinker. When less than 2.0% of $SO_3$ was added to the clinker composition, the formation of $C_3S$ was enhanced, however, addition of more than 2.0% of $SO_3$ rather restrained the reaction remarkably. The diffusion coefficient of Si into the melt was about $3.6~4.2{\times}10^{-7}Cm^2$/sec and it was slightly decreased with the amount of $SO_3$. The crystal size of $C_3S$ formed in the clinker was grown gradually according to the amount of $SO_3$, when more than 1.0% of $SO_3$ was added. With increasing of $SO_3$ content in the clinker composition of CaO and decreasing of $SiO_2$ were found in the melt of the clinker. Consequently, it is considered that the decreasing of $C_3S$ formation is caused by dissolution and transportation of CaO component into liquid phase is interrupted.