• Applied Chemistry for Engineering
• /
• v.35 no.5
• /
• pp.385-389
• /
• 2024

For high-purity purification of indole (IN) contained in crude methylnaphthalene oil (CMNO), this study was reviewed by adopting the re-extraction method using n-hexane as an enrichment method of IN contained in the extract phase recovered from equilibrium extraction of CMNO and formamide aqueous solution. The raw material (extract phase) contained three types of nitrogen-containing compounds (NCCs): quinoline (QU), isoquinoline (IQU), and IN; and four types of bicyclic aromatic compounds (BACs): naphthalene, 2-methylnaphthalene, 1-methylnaphthalene, and biphenyl (BP). The distribution coefficient and selectivity of IN showed almost constant values regardless of the change in the initial volume fraction of the re-extraction solvent to the raw material. Compared to the distribution coefficient of IN, those of two types NCCs excluding IN and three types BACs excluding BP, respectively, are about 4~7 times and 190~394 times higher. In addition, the concentration of IN in the raffinate oil recovered through equilibrium n-hexane re-extraction run of the batch co-current five-stage under constant re-extraction was 54.6%, which was approximately 2.5 times higher than that of the raw material. From the excellent IN enrichment efficiency of this study, the re-extraction method using n-hexane was expected to be a new IN enrichment method that can be an alternative to the distillation method.

• Applied Chemistry for Engineering
• /
• v.35 no.5
• /
• pp.468-472
• /
• 2024

This study experimentally examined the separation performance of indole (IN) contained in crude methyl naphthalene oil (CMNO) by methanol extraction and then compared these results with formamide extraction. CMNO containing about 4.36% IN, which is attracting attention as an intermediate raw material such as medicine, essential amino acids, and perfumes, was used as a raw material, and methanol aqueous solution was used as a solvent, respectively. The increase in the initial volume fraction of water in the solvent (y_w,0) sharply decreased the distribution coefficient (m_IN) and yield (Y_IN) of IN, but conversely increased the selectivity of IN in reference to 2-methylnaphthalene (2MNA). An increase in the initial volume ratio of solvent to feed (E₀/R₀) increased m_IN, Y_IN, and 𝛽_IN,2MNA. In the range of 0.1 ≤ y_w,0 ≤ 0.3, m_IN and Y_IN of methanol extraction were approximately 1.9~5.9 times and 1.8~3.6 times greater than those of formamide extraction, respectively, whereas 𝛽_IN,2MNA of formamide extraction were 4.6~8.2 times greater than those of methanol extraction.

• Applied Biological Chemistry
• /
• v.49 no.4
• /
• pp.322-327
• /
• 2006

Food constituents analysis of Acer tegmentosum. Maxim.(Acer TM) stem was carried out according to AOAC method, and the antiradical activity on DPPH and cytotoxicity on human cell lines (AGS, HepG2, A549, MCF-7 and Chang) for the 80% ethylalcohol(EtOH) extracts of Acer TM stem were studied. The antiradical activity on DPPH radical of the ethylacetate(EtOAc) fraction of the bark showed a higher activity than that of $\alpha$-tocopherol, ascorbic acid and BHT. The inhibition activity of the 80% EtOH extracts from Acer TM stem on human cancer cell lines by SRB assay indicated a dose-dependent growth inhibition on most human carcinoma cells. The growth inhibition rate of each human cancer cell line showed 91.3% to AGS, 75.0% to A549, 74.1% to HepG2, and 70.2% to MCF-7 cells, respectively, when the 80% EtOH extract(1 mg/ml) of Acer TM stem was added.

• Journal of Soil and Groundwater Environment
• /
• v.14 no.4
• /
• pp.23-32
• /
• 2009

The sorption of europium (Eu (III)) onto kaolinite and the influence of humic acids over a range of pH 3 ~ 11 has been studied by batch adsorption experiment (V/m = 250 : 1 mL/g, $C_{Eu(III)}\;=\;1\;{\times}\;10^{-5}\;mol/L$, $C_{HA}\;=\;5{\sim}50\;mg/L$, $P_{CO2}=10^{-3.5}\;atm$). The concentrations of HA and Eu(III) in aqueous phase were measured by UV absorbance at 254nm (e.g., $UV_{254}$) and ICP-MS after microwave digestion for HA removals, respectively. Results showed that the HA sorption onto kaolinite was decreased with increasing pH and their sorption isotherms fit well with the Langmuir adsorption model (except pH 3). Maximum amount ($q_{max}$) for the HA sorption at pH 4 to 11 was ranged from 4.73 to 0.47 mg/g. Europium adsorption onto the kaolinite in the absence of HA was typical, showing an increases with pH and a distinct adsorption edge at pH 3 to 5. However in the presence of HA, Eu adsorption to kaolinite was significantly affected. HA was shown to enhance Eu adsorption in the acidic pH range (pH 3 ~ 4) due to the formation of additional binding sites for Eu coming from HA adsorbed onto kaolinite surface, but reduce Eu adsorption in the intermediate and high pH above 6 due to the formation of aqueous Eu-HA complexes. The results on the ternary interaction of kaolinte-Eu-HA are compared with those on the binary system of kaolinite-HA and kaolinite-Eu and adsorption mechanism with pH was discussed.

• Bulletin of the Korean Chemical Society
• /
• v.28 no.10
• /
• pp.1675-1682
• /
• 2007

Large colorless single crystals of faujasite-type zeolite with diameters up to 200 μm have been synthesized from gels with the composition of 3.58SiO2:2.08NaAlO2:7.59NaOH:455H2O:5.06TEA:1.23TCl. Two of these, colorless octahedron about 200 μm in cross-section have been treated with aqueous 0.1 M TlC2H3O2 and KNO3 in order to prepare Tl+- and K+-exchanged faujasite-type zeolites, respectively, and then determined the Si/Al ratio of the zeolite framework. The crystal structures of |Tl71|[Si121Al71O384]-FAU and |K53Na18|[Si121Al71O384]-FAU per unit cell, a = 24.9463(2) and 24.9211(16) A, respectively, dehydrated at 673 K and 1 × 10-6 Torr, have been determined by single-crystal X-ray diffraction techniques in the cubic space group Fd m at 294 K. The two single-crystal structures were refined using all intensities to the final error indices (using only the 905 and 429 reflections for which Fo > 4σ(Fo)) R1/R2 = 0.059/0.153 and 0.066/0.290, respectively. In the structure of fully Tl+-exchanged faujasite-type zeolite, 71 Tl+ ions per unit cell are located at four different crystallographic sites. Twenty-nine Tl+ ions fill site I' in the sodalite cavities on 3-fold axes opposite double 6-rings (Tl-O = 2.631(12) A and O-Tl-O = 93.8(4)o). Another 31 Tl+ ions fill site II opposite single 6-rings in the supercage (Tl-O = 2.782(12) A and O-Tl-O = 87.9(4)o). About 3 Tl+ ions are found at site III in the supercage (Tl-O = 2.91(6) and 3.44(3) A), and the remaining 8 occupy another site III (Tl-O = 2.49(5) and 3.06(3) A). In the structure of partially K+-exchanged faujasite-type zeolite, 53 K+ ions per unit cell are found at five different crystallographic sites and 18 Na+ ions per unit cell are found at two different crystallographic sites. The 4 K+ ions are located at site I, the center of the hexagonal prism (K-O = 2.796(8) A and O-K-O = 89.0(3)o). The 10 K+ ions are found at site I' in the sodalite cavity (K-O = 2.570(19) A and O-KO = 99.4(9)o). Twenty-two K+ ions are found at site II in the supercage (K-O = 2.711(9) A and O-K-O = 94.7(3)o). The 5 K+ ions are found at site III deep in the supercage (K-O = 2.90(5) and 3.36(3) A), and 12 K+ ions are found at another site III' (K-O = 2.55(3) and 2.968(18) A). Twelve Na+ ions also lie at site I' (Na-O = 2.292(10) and O-Na-O = 117.5(5)o). The 6 Na+ ions are found at site II in the supercage (Na-O = 2.390(17) A and O-Na-O = 113.1(11)o). The Si/Al ratio of synthetic faujasite-type zeolite is 1.70 determined by the occupations of cations, 71, in two single-crystal structures.

• Journal of the Korean Chemical Society
• /
• v.35 no.2
• /
• pp.119-127
• /
• 1991

The protonation and the metal ion complexation of 15 to 18 membered diaza crown ether such as 1,12-diaza-3, 4 : 9, 10-dibenzo-5, 8-dioxacyclopentadecane(NtnOenH$_4$), 1,13-diaza-3,4 : 10,11-dibenzo-hydroxy-5,9-dioxacyclohexadecane(NtnOtnH$_4$), 1,13-diaza-3,4 : 10,11-dibenzo-15-hydroxy-5,9-dioxacyclohexadecane(Ntn(OH)OtnH$_4$), 1,15-diaza-3,4 : 12,13-dibenzo-5,8,11-trioxacycloheptadecane (NenOdienH$_4$) and 1,15-diaza-3,4 : 12,13-dibenzo-5,8,11-trioxacyclooctadecane(NtnOdienH$_4$) were studlied by potentiometry and NMR spectroscopy. The protonation constants were used to predict basicity of crown ethers. The sequence of the basicity was NenOdienH$_4$ < Ntn(OH)OtnH$_4$ < NtnOenH$_4$ < NtnOtnH$_4$ < NtnOdienH$_4$. Changes on the basicity were explained in terms of the effects of substituents and the degree of twistness of the macrocyclic ring. The sequence of the complex stabilities were Co(II) < Ni(II) < Cu(II) < Zn(II) for the transition metal complexes and Cd(II) < pb(II) < Hg(II) for the post-transition metal complexes. These changes on the stabilities were dependent on the basicity of the ligand and cavity size of the ring. For the heavy post-transiton metal complexes and Zn(Ⅱ) complex, the former factor was predominent and for the other transition metal complexes, the latter was affected on the stabilities. $^1$H and $^{13}$C-NMR studies for heavy post-transition metal complexes indicated that the nitrogen atom has greater affinity on metal ions than oxygen atom and the planarity of the rings was losed by the complexation with metal ions.

• Journal of the Korean Chemical Society
• /
• v.40 no.7
• /
• pp.474-482
• /
• 1996

Two crystal structures of the vacuum dehydrated $Ag^+$-exchanged zeolite X have been determined by single-crystal X-ray diffraction techniques in the cubic space group Fd3 at 21(1)$^{\circ}C$ (a=24.922(1)${\AA}$ and a=24.901(1)${\AA}$, respectively). Each crystal was ion exchanged in flowing streams of aqueous $AgNO_3$ for three days. The first crystal was dehydrated at 300$^{\circ}C$ and $2{\times}10^{-6$torr for two days. The second crystal was similarly dehydrated at 350$^{\circ}C$. Their structures were refined to the final error indices, $R_1=0.095\;and\;R_2=0.092$ with 227 reflections, and $R_1=0.096\;and\;R_2=0.087$ with 334 reflections, respectively, for which I > 3${\sigma}$(I). In the first crystal, Ag species are found at five different crystallographic sites: sixteen $Ag^+$ ions fill the site I, the center of the double 6-ring, thirty-two Ag0 atoms fill the I' site in the sodalite cavities opposite double six-rings, seventeen $Ag^+$ ions lie at the 32-fold site II' inside the sodalite cavity at the single six-oxygen ring in the supercage, fifteen Ag+ ions lie at the 32-fold site II, in the supercage, and the remaining twelve $Ag^+$ ions lie at site III' in the supercage at a little off two-fold axes. In the second crystal, all Ag species are located similarly as crystal 1; 16 at site I, 28 at site I', 16 at site II, 16 at site II', 6 at site III and 6 at site III'. Total 88 silver species were found per unit cell. The remaining four Ag atoms were migrated out of the zeolite framework to form small silver crystallites on the surface of the zeolite single crystal. In the first structure, the numbers of Ag atoms per unit cell are approximately 32.0 and these may form tetrahedral $Ag_4$ clusters at the centers of the sodalite cavities. The probable four-atom cluster is stabilized by coordination to two $Ag^+$ ions. The Ag-Ag distance in the cluster, ca. 3.05 ${\AA}$, is a little longer than 2.89 ${\AA}$, Ag-Ag distance in silver metal. At least two six-ring $Ag^+$ ions on sodalite cavity (site II') must necessarily approach this cluster and this cluster may be viewed as a distorted octahedral silver cluster, (Ag6)2+.

• Korean Journal of Environmental Agriculture
• /
• v.12 no.1
• /
• pp.51-57
• /
• 1993

Objective of this research was to assess the influence of reaction time on the heavy metal-organic ligand complexation by employing kinetic models. Aqueous solutions of humic (HA) or fulvic acid (FA) were reacted with metal solutions with 1:1 ratio to form complexes. Efficiency of organic ligand on metal removal was determined by separating the precipitates from solution using $0.45\;{\mu}m$ filter paper. Complexation between Cu or Pb and HA or FA followed the first- or multiple first order kinetics, largely depending on metal concentration and kind of organic ligand. Amounts of precipitates were increased proportionally with reaction time but reached to quasiequilibrium where rate of precipitate formation was not varied with time. Copper-ligand complexation was, irrespective of ligand, fitted to the single first order kinetics at Cu concentrations lower than $300{\mu}M$, but this was fitted to the multiple first order kinetics at Cu concentrations higher than $300{\mu}M$. As increasing Cu concentrations, the precipitates formed more readily, judging from the increased rate constants (${\kappa}$). In the multiple first order kinetics, ${\kappa}$ was decreased as reaction steps proceeded. Most of Cu-ligand precipitates were formed within 15 min. FA precipitated Cu more rapidly than HA did. ${\kappa}$ for Pb-HA complexation was decreased but that for Pb-FA reaction was increased, as increasing Pb concentration. Most of Pb-organic ligand complexation occurred within 30 min. Afterwards, ${\kappa}$ values were relatively small and not affected much by time. Pb was precipitated by humic acid more readily than Cu when metal concnetrations were $200{\sim}300{\mu}M$. However, when metal concentrations were in the ranges of $400{\sim}500{\mu}M$, a reversed tendency was observed.

• Journal of the Mineralogical Society of Korea
• /
• v.30 no.2
• /
• pp.45-57
• /
• 2017

Two single crystals of fully dehydrated $Cd^{2+}$-exchanged zeolites Y were prepared by the exchange of ${\mid}Na_{75}{\mid}[Si_{117}Al_{75}O_{384}]-FAU$ ($Na_{75}-Y$, Si/Al = 1.56) with aqueous $0.05M\;Cd(NO_3)_2$ (pH = 3.65) at 294 K, followed by vacuum dehydration at 723 K (crystal 1) and a second crystal, similarly prepared, was exposed to zeolitically dried benzene for 72 hours at 294 K and evacuated (crystal 2). Their structures were determined crystallographically using synchrotron X-rays and were refined to the final error indices using $F_o$>$4{\sigma}(F_o)$ of $R_1/wR_2=0.040/0.121$ and 0.052/0.168, respectively. In crystal $1({\mid}Cd_{36}H_3{\mid}[Si_{117}Al_{75}O_{384}]-FAU)$, $Cd^{2+}$ ions primarily occupy sites I and II, with additional $Cd^{2+}$ ions at sites I', II', and a second site II. In crystal $2({\mid}Cd_{35}(C_6H_6)_{24}H_5{\mid}[Si_{117}Al_{75}O_{384}]-FAU)$, $Cd^{2+}$ ions occupy five crystallographic sites. The 24 benzene molecules are found at two distinct positions within the supercages. The 17 benzene molecules are found on the 3-fold axes in the supercages where each interacts facially with one of site IIa $Cd^{2+}$ ions. The remaining 7 benzene molecules lie on the planes of the 12-rings where each is stabilized by multiple weak electrostatic and van der Waals interactions with framework oxygens.

• The Korean Journal of Pesticide Science
• /
• v.7 no.3
• /
• pp.176-181
• /
• 2003

The leaching behaviour of [aniline-$^{14}C$]mefenacet in soil was investigated using glass columns (5 cm I.D. $\times$ 30 cm. H) packed with two types of soils with different physicochemical properties. $^{14}C$-Mefenacet (8.33 kBq) and mefenacet (in total, 1.05 mg/kg) were treated onto soil columns and rice plants (Oryza sativa L.) were grown for 17 weeks on these columns. Leachates from the columns were collected at the rate of 122.5 mL per week. $^{14}C$-Activities leached from soil A (OM, 3.1%; CEC, 86 mmol(+)/kg; texture, loam) columns with and without rice plants were 1.95 and 4.19% of the originally applied, whereas those from soil B (OM, 1.3%; CEC, 71 mmol(+)/kg; texture, loam) were 2.69 and 7.05%, respectively. These results indicated that larger amounts of $^{14}C$ were percolated from soil B with less organic matter and from the columns without vegetation. $^{14}C$-Activities absorbed by rice plants from soil A and B were 8.95 and 8.47%, respectively, most of which remained in the root and shoot excluding unhulled grains and ears without grains. $62\sim73%$ of the originally applied $^{14}C$ remained in the depth of $0\sim5cm$ in soil. The mass balance indicated that the losses by volatilization and/or mineralization amounted to $3.4\sim9.2%$ of the originally applied. $^{14}C$-Radioactivities in the aqueous phase of the leachates ranged from 59.4 to 97.7% of the radioactivities in leachates, showing the fast transformation of mefenacet to the polar metabolites.