Choi, Ki Young;Kim, Dong Won;Kim, Chang Suk;Park, Byung Bin;Choi, Suk Nam;Hong, Choon Pyo;Ryu, Hae Il
Journal of the Korean Chemical Society
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v.44
no.5
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pp.403-409
/
2000
The formation and dissociation rates of $Zn^{2+}$ Complexes with l,4,7,10-tetraaza-13,16-diox-acyclooctadecane-N,N',N",N'"-tetraacetic acid (1), 1,4,7,10-tetraaza-13,16- dioxacyclooctadecane-N,N',N",N'"-tetramethylacetic acid (2), and 1,4,7,10-tetraaza-13,16- dioxacyclooctadecane-N,N',N",N'"-tetrapropionic acid(3) have been measured by stopped-flow and conventional spectrophotometry. Observations were made at 25.0$\pm$0.1 $^{\circ}C$ and at an ionic strength of 0.10 M NaClO$_4$. The formation reactions of $Zn^{2+}$ ion with 1 and 2 took place by the rapid formation of an intermediate complex (ZnH$_3L^+$) in which the $Zn^{2+}$ ion is incompletely coor-dinated. This might then lead to be a final product in the rate-determining step.ln the pH range 4.76-5.76, the diprotonated (H2L2-) form is the kinetically active species despite of its low concentration. The stability con-stants (log$K_{(ZnH$_3$3$L^+$)}$) and specific water-assisted rate constants (koH) of intermediate complexes have been deter-mined from the kinetic data. The dissociation reactions of $Zn^{2+}$ complexes of 1,2, and 3 were investigated with $Cu^{2+}$ ions as a scavenger in acetate buffer. All complexes exhibit acid-independent and acid-catalyzed con-tributions. The effect of buffer and $Cu^{2+}$ concentration on the dissociation rate has also been investigated. The ligand effect on t dissociation rate of $Zn^{2+}$ complexes is discussed in terms of the side-pendant armsand the chelate ring sizes of the ligands.
The extraction of trace cobalt, copper, nickel, cadmium, lead and zinc in urine samples of organic and alkali metal matrix into chloroform by the complex with a dithizone was studied for graphite furnace AAS determination. Various experimental conditions such as the pretreatment of urine, the pH of sample solution, and dithizone concentration in a solvent were optimized for the effective extraction, and some essential conditions were also studied for the back-extraction and digestion as well. All organic materials in 100 mL urine were destructed by the digestion with conc. $HNO_3$ 30 mL and 30% $H_2O_2$ 50 mL. Here, $H_2O_2$ was added dropwise with each 5.0 mL, serially. Analytes were extracted into 15.0 mL chloroform of 0.1% dithizone from the digested urine at pH 8.0 by shaking for 90 minutes. The pH was adjusted with a commercial buffer solution. Among analytes, cadmium, lead and zinc were back-extracted to 10.00 mL of 0.2 M $HNO_3$ from the solvent for the determination, and after the organic solvent was evaporated, others were dissolved with $HNO_3-H_2O_2$ and diluted to 10.00 mL with a deionized water. Synthetic digested urines were used to obtain optimum conditions and to plot calibration-eurves. Average recoveries of 77 to 109% for each element were obtained in sample solutions in which given amounts of analytes were added, and detection limits were Cd 0.09, Pb 0.59, Zn 0.18, Co 0.24, Cu 1.3 and Ni 1.7 ng/mL, respectively. It was concluded that this method could be applied for the determination of heavy elements in urine samples without any interferences of organic materials and major alkaline elements.
In order to evaluate the geochemical behaviors of elements with waste rocks in the abandoned Jangpoong Cu mine area, total concentration analysis and leaching experiments were performed. The content of elements within waste rocks compared with background values decreased in order of As>>Cu>Pb>Cd>Co. Leaching experiments were carried out at various extraction environments, considering the acid rain ($0.00001{\sim}0.001N\;HNO_3$) and the acid mine drainage ($0.001{\sim}0.1N$ HNO3). After 24 hours of reaction with different acidic solution, the leaching characteristics of waste rocks were classified into three types according to final pH of leaching solution. Type I refers to the case that the final pH of leaching solution was lower than that of the reaction solution due to the dissolution of acidic minerals from rocks, while type 2 and 3 refer to the case that the final pH maintained higher than that of the reaction solution. Theses types include in acid buffering minerals such as clay minerals and carbonate minerals. The leaching characteristics of the elements after the reaction could be categorized into As-Co-Fe, Cu-Mn-Cd-Zn, and Pb. As-Co-Fe started to get leached under 2.5 of pH regardless of changes in the final pH, and Cu-Mn-Cd-Zn showed different initial leaching pH according to the types of final pH changes. Based on the pH value where leaching started regardless of leaching concentration, the relative mobility of each element was in the order of Mn Zn>Cd>Cu>>Fe Co>As>Pb. Thus, more higher mobility elements(Zn, Mn and Cu) were leached by reacting with acid rain water. Acid mine drainage may result in distributions of elements having relatively less mobility(As, Fe, Co and Pb).
The chemical and optical absorption spectroscopic characters of pink and colorless tourmalines from San Diego mine in California, U.S.A., blue/green tourmalines from anonymous mine, Brazil, and brownis black tourmalines from Uncheon and Haksan mines in Korea have been studied using X-ray diffractometer, electron microprobe, optical absorption spectroscopy, and heat treatment. Least-squares refinements give unit cell diminsions : a = 15.96-16.01 ${\AA}$, c = 7.15-7.16 ${\AA}$ for the brownish black tourmalines, a = 15.82 - 15.87 ${\AA}$, c = 7.09 - 7.10 ${\AA}$ for pink tourmalines, and a = 15.88 - 15.94 ${\AA}$, c = 7.12 - 7.15 ${\AA}$ for blue green tourmalines. The colors of tourmalines are responsible for the transition elements. The pink color is attributed to the $Mn^{3+}$ ions, the blue-green to $Fe^{2+}$ and $Mn^{2+}$, bluish green to $Cu^{2+}$, and the brownish black to $Fe^{2+}$, $Fe^{2+}$ - $Fe^{3+}$, and $Fe^{2+}$ - $Ti^{4+}$. The $Mn^{3+}$ ions of pink color tourmalines are stabilized in the Y sites compressed along the O(1)H-O(3)H axis by Jahn-Teller distortion. Heating removes the pink or red component from tourmalines, producing the colorless stones from the pink and red ones. The bluish green samples change into the greenish blue ones and a certain yellowish green samples change into the light green ones by heat treatment. In the elbaite-schorl series, the concentration of Fe and Mn are variable depending on the color zones. The green zone is characterrized by the high content of Fe and Mn are variable depending on the color zones. The green zone is characterized by the high content of Fe, whereas the pink zone by the high content of Mn. Mn increases in deep yellow zone compared with yellow or colorless zones.
An effective extraction methods of a garlic were investigated in order to improve the functional properties of the extracts. The solid yield, electron donating ability (EDA), nitrite-scavenging effects (NSE), peroxide value (POV) and total thiosulfinates contents of garlic extracts were determined. In order to improve the functional properties of extracts prepared with several organic solvents and acids, concentration and pH adjustment of the selected solvent and addition of acids and salts to solvents were also examined. Among the solvents tested, the methanol and ethanol extracts were found to be the most effective on the base of functionality and solid yields. The highest EDA, NSE and thiosulfinate value were obtained with 50% ethanol. The pH control of solvent and addition of citric acid, NaCl and phosphates to 50% ethanol did not affect on the functionality of the extracts. Therefore the optimal solvent for the best functional properties of garlic extract was 50% ethanol.
Lee In-Gyeong;Lee Pyeong-Koo;Choi Sang-Hoon;Kim Ji-Soo;So Chil-Sup
Economic and Environmental Geology
/
v.38
no.6
s.175
/
pp.699-705
/
2005
In order to identify the speciation of As and trace elements which are contained weathered waste rocks on the abandoned Jangpoong Cu mine area, five fraction sequential extraction was carried out. Concentrations of the extraction solutions which were acquaired each fraction were mesured by ICP-AES. Mineral characters of weathered waste rocks were determinated by XRD. The weathered waste rocks could divide into two types (Type I and type II). Type land type II weathered waste rocks are mainly composed of a quartz and a calcite, respectively. The most dominant speciation of As, Co and Fe is residual phase. Most of the speciation of Cd, Mn and Zn is residual phase for type I and Fe-Mn oxide phase for type II. In case of Cu, residual phase is predominant in type I and sulfide is predominet in type II. The most dominant speciation of Pb for type I and type II is associated with the residual phase and Fe-Mn oxide phase, respectively. At pH 4-7 range, the order of relative mobility considers Zn>Cu>Cd>Pb>Co>AS in type I, and Cd>Cu>Zn>Pb>As>Co in type II.
Jang, Hae Jong;Lee, Ye Rie;Lee, Kyung Ryul;Han, Sang-Beom;Kang, Seung Woo;Lee, Hee Joo
Analytical Science and Technology
/
v.19
no.3
/
pp.239-243
/
2006
This method is used for the determination of itraconazole in human plasma by liquid-liquid extraction and high performance liquid chromatography. Felodipine was used as an internal standard. After extraction of the plasma with diethyl ether, the centrifuged upper layer was then transferred. The supernantant was evaporated and then reconsituted with mobile phase. The mobile phase was composed of 10 mM ammonium acetate adjusted to pH 7 by phosphoric acid with a flow rate of 0.2 mL/min. A C18 reversed-phase column with a pre-column was used as the analytial column. Linear detection responses were obtained for itraconzole concentration range for 2~1,000 ng/mL. The correlation coefficient of linear regression($R^2$) was 0.9991, limit of quantification (LOQ) was 2 ng/mL, reproducibility was less than 10.8 %, and accuracy was 97.2~108.2%. This method has been successfully applied to the pharmacokinetic study of itraconazole in human plasma.
Batch scale experiments to investigate the efficiency of the solidification process for metal mine tailing treatment were performed. Portland and MSG (micro silica pouting) cements were used as solidifier and three kinds of mine tailings (located at Gishi, Daeryang, and Aujeon mine) were mixed with cements to paste solidified matrices. Single axis com-pressible strengths of solidified matrices were measured and their heavy metal extraction ratios were calculated to investigate the solidification efficiency of solidified matrices created in experiments. Solidified matrices ($5cm{\times}5cm{\times}5cm$) were molded from the paste of tailing and cements at various conditions such as different tailing/cement ratio, cement/water ratio, and different cement or tailing types. Compressible strengths of solidified matrices after 7, 14, and 28 day cementation were measured and their strengths ranged from 1 to $2kgf/mm^2$, which were higher than Korean limit of compressible strength for the inside wall of the isolated landfill facility ($0.21kgf/mm^2$). Heavy metal extractions from intact tailings and powdered matrices by using the weak acidic solution were performed. As concentration of extraction solution for the powdered solidified matrix (Portland cement + Gishi tailing at 1:1 w.t. ratio) decreased down to 9.7 mg/L, which was one fifth of As extraction concentration for intact Gishi tailings. Pb extraction concentration of the solidified matrix also decreased to lower than one fourth of intact tailing extraction concentration. Heavy metal extraction batch experiments by using various pH conditions of solution were also performed to investigate the solidification efficiency reducing heavy metal extraction rate from the solidified matrix. With pH 1 and 13 of solution, Zn and Pb concentration of solution were over the groundwater tolerance limit, but at pH $1{\sim}13$ of solution, heavy metal concentrations dramatically decreased and were lower than the groundwater tolerance limit. While the solidified matrix was immerged Into very acidic or basic solution (pH 1 and 13), pH of solution changed to $9{\sim}10$ because of the buffering effect of the matrix. It was suggested that the continuous extraction of heavy metals from the solidified matrix is limited even in the extremely high or low pH of contact water. Results of experiments suggested that the solidification process by using Portland and MSG cements has a great possibility to treat heavy metal contaminated mine tailing.
Lee, Kang Yeon;Kim, Kyoung Hoon;Baek, Youl Chang;Ok, Ji Un;Seol, Yong Joo;Han, Ki Jun;Park, Keun Kyu;Ryu, Ho Tae;Lee, Sang Suk;Jeon, Che Ok;Oh, Young Kyoon
Journal of Animal Science and Technology
/
v.55
no.1
/
pp.25-32
/
2013
The purpose of this study was to investigate the effects of mustard, which contains allyl isothiocyanate, on ruminal fermentation and methane emission in vitro. To this end, diluted ruminal fluid(30ml) was incubated anaerobically at $39^{\circ}C$ or 6, 12, and 24 h with or without seeds or powdered mustard. Either mustard seed or powdered mustard was weighed and serially (0, 3.33, 5.00, 6.67, and 8.33 g/L) mixed with ruminal fluid. Ammonia-N was increased (P < 0.05) by mustard treatment in a dose dependent manner. Regardless of concentration or form, mustard increased (P < 0.05) total VFA content but decreased (P < 0.01) pH compared to control group. Molar proportion of acetate (A) was decreased (P < 0.05) whereas propionate (P) was increased (P < 0.05) by mustard treatment, thereby A:P ratio was decreased (P < 0.05) compared to control group. Total gas production was increased (P < 0.01) in a linear manner by mustard treatment compared to control group. There was no effect of mustard powder, except 8.33 g/L level at 6 h, on methane emission. However, at 24 h, methane emission was reduced (P < 0.05) by 4.77% and 11.54% with 6.67 g/L and 8.33 g/L of mustard seeds supplementation, respectively. Altogether, these results suggest that mustard seeds containing allyl isothiocyanate may reduce methane production without disturbing ruminal fermentation.
Recently, Psychrobacter sp. ArcL13 strain showing the extracellular lipase activity was isolated from the Chuckchi Sea of the Arctic Ocean. However, due to the low expression levels of the enzyme in the natural strain, the production of recombinant lipase is crucial for various applications. Identification of the gene for the enzyme is prerequisite for the production of the recombinant protein. Therefore, in the present study, a novel lipase gene (ArcL13-Lip) was isolated from Psychrobacter sp. ArcL13 strain by gene prospecting using PCR, and its complete nucleotide sequence was determined. Sequence analysis showed that ArcL13-Lip has high amino acid sequence similarity to lipases from bacteria of some Psychrobacter genus (84-90%) despite low nucleotide sequence similarity. The lipase gene was cloned into the bacterial expression plasmid and expressed in E. coli. SDS-PAGE analysis of the cells showed that ArcL13-Lip was expressed as inclusion bodies with a molecular mass of about 35 kDa. Refolding was achieved by diluting the unfolded protein into refolding buffers containing various additives, and the highest refolding efficiency was seen in the glucose-containing buffer. Refolded ArcL13-Lip showed high hydrolytic activity toward p-nitrophenyl caprylate and p-nitrophenyl decanoate among different p-nitrophenyl esters. Recombinant ArcL13-Lip displayed maximal activity at $40^{\circ}C$ and pH 8.0 with p-nitrophenyl caprylate as a substrate. Activity assays performed at various temperatures showed that ArcL13-Lip is a cold-active lipase with about 40% and 73% of enzymatic activity at $10^{\circ}C$ and $20^{\circ}C$, respectively, compared to its maximal activity at $40^{\circ}C$.
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