• Title/Summary/Keyword: potentiometric titration

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Surface Charge Density and Acidic Characteristics of $SO_4^{2-}/Al_2O_3$ ($SO_4^{2-}/Al_2O_3$의 표면전하밀도와 산적특성)

  • 함영민;홍영호;장윤호
    • Journal of the Korean Ceramic Society
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    • v.30 no.11
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    • pp.933-940
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    • 1993
  • SO42-/Al2O3 powder was prepared by the coprecipitation method from the Al(NO3)3.9H2O and NH4OH and followed by being treated with various concentrations of sulfuric acid. The characterization of these powders was performed with XRD, BET and FT-IR. The surface charge density at alumina/KCl(aq) interface was measured by potentiometric titration method. From the experimental data it was shown that acid strength, specfic surface area, and structure of surface treated alumina were independent on the amount of exchanged SO42-. However, the acid amounts of alumina were increased with the amounts of SO42- formed on alumina surface. The relation between the acid amount of SO42- ion exchanged alumina surface and the surface charge density for SO42-/Al2O3/KCl(aq) interface was investigated.

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Effective Uranyl Binding by a Dihydroxyazobenzene Derivative. Ionization of Uranium-Bound Water

  • 이관표;장보빈;서정훈
    • Bulletin of the Korean Chemical Society
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    • v.17 no.9
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    • pp.814-819
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    • 1996
  • In search of simple host molecules for uranyl ion which form 1: 1-type complexes with high formation constants that can be used either in extraction of uranium from seawater or in catalysis of biologically important organic reactions, the uranophile activities of dihydroxyazobenzene derivative 1 were studied. Uranyl ion and 1 form a 1: 1-type complex with a very large formation constant. The formation constant was measured at pH 7-11.6 by competition experiments with carbonate ion. From the resulting pH dependence, ionization constants of the two aquo ligands coordinated to the uranium of the uranyl complex of 1 were calculated. The ionization constants were also measured by potentiometric titration of the uranyl complex of 1. Based on these results, the pKa values of the two aquo ligands were estimated as 7.1 and 11.0, respectively. At pH 7.5-9.5, therefore, the complex exists mostly as monohydroxo species. Under the conditions of seawater, 1 possesses greater affinity toward uranyl ion compared with other uranophiles such as carbonate ion, calixarene derivatives, or a macrocyclic octacarboxylate. In addition, complexation of 1 with uranyl ion is much faster than that of the calixarene or octacarboxylate uranophiles.

Thallium(I)-Selective Electrodes Based on Calix[4]pyrroles

  • Park, Gyeong Sun;Jeong, Seong Uk;Lee, Sim Seong;Kim, Jae Sang
    • Bulletin of the Korean Chemical Society
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    • v.21 no.9
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    • pp.909-912
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    • 2000
  • Thallium(I) selective electrodes based on meso-alkyl substituted calix[4]pyrroles such as, meso-octamethyl-calix[4]pyrrole (L1), meso-octaethylcalix[4]pyrrole (L2) and meso-tetraspirocyclohexylcalix[4]pyrrole (L3) as sensor molecules have been pre pared and tested. The conditioned electrode (E4) incorporating L3gave best results with a wide working concentration range of 10-5.5 ~10-1 M near-Nernstian slope of 56.0 mV/decade of activity and detection limit of 10-6.0 M. This electrode exhibited a fast response time of 30 s and high selectivity over Na+ , K+ and other metal ions with only Ag+ interfering. The electrode works well in the pH range 2.0-11.0 and can be successfully employed for the determination of Tl+.This proposed electrode was also used as an indicator electrode in potentiometric titration of Tl+.

An Eurpium(III) Hydrolytic Catalyst Favoring Anionic Phosphate Esters over Phosphate Triester'

  • Yun, Chang Won;O, Sun Jin;Jeon, Yeong Jin;Choe, Yeong Seo;Son, Yun Gyeong;HwangBo, Seok;Gu, Ja Gang;Park, Jun Won
    • Bulletin of the Korean Chemical Society
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    • v.22 no.2
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    • pp.199-204
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    • 2001
  • A Cryptate (221) having a short alcohol pendant (2) was metallated with europium(Ⅲ) in anhydrous condition, and its hydrolytic activity for phosphate esters at neutral pH was examined. While the activity for the phosphate diester and monoester is comparable to that of the parent metal complex [1Eu]3+, its hydrolytic activity towards a phosphate triester is significantly suppressed. Potentiometric titration and luminescence spectroscopic studies for the equilibrium behavior of the complex in solution suggest that a dimer formation through the metal hydroxides as well as the pendant alcohol is likely to happen. The low hydrolytic activity for the triester seems to be associated with the dimer formation.

Proton Affinity Distributions of Humic Acid Extracted from Upland and Paddy Soils (논·밭토양으로부터 추출한 Humic Acid의 수소이온 친화력 분포)

  • Jeong, Chang-Yoon;Park, Chan-Won;Kim, Jeong-Gyu;Lim, Soo-Kil
    • Korean Journal of Soil Science and Fertilizer
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    • v.32 no.4
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    • pp.429-439
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    • 1999
  • Potentiometric titration data were collected for some humic acids purified from Korean upland and paddy soils over a range of pH (3.0 - 11.0) with $NaNO_3$ background electrolyte concentrations (0.01, 0.10, 0.50 and 1.00 M). The data were applied to model A and V which included both intrinsic heterogeneity of humic materials and electrostatic interaction influences on binding sites. The elemental analysis were conducted for various type of humic samples. The $E_4/E_6$ ratio proposed negative correlation with the total carboxyl groups ($r^2$= 0.9988). The charge ($cmol_c\;kg^{-1}$) on the humic acids became more negative as the ionic strength increased. In both continuous and batch titrations, the ionic strength effect was greater in Namweon series (pH 6.39) than others at pH 5.00. The effect of ionic strength on surface charge appears to be greater in batch titrations. This could suggest that continuous titrations do not represent an equilibrium state and the effects of electrolyte concentration was not fully realized during the course of titrations. Both models described experimental data obtained from continuous and batch titrations well over a range of ionic strengths. Model A is more simpler than model V but adaptes more fitted parameters. Thus, the observed change in apparent binding constants with surface charge is regarded solely due to electrostatic influences rather than functional group heterogeneity. However, Model V is more mechanistically realistic in a number of discrete ligand binding sites.

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Surface Chemical Properties of Aqueous Kaolinite and Halloysite: Surface Complexation Modeling (수용액 내 캐올리나이트와 할로이사이트의 표면화학 특성: 표면복합반응 모델링)

  • 장세정;김수진
    • Journal of the Mineralogical Society of Korea
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    • v.17 no.2
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    • pp.157-168
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    • 2004
  • The surface chemical properties of aqueous kaolinite and halloysite were studied using a potentiometric titration experiment and a computer program FITEQL3.2. Among the surface complexation models a constant capacitance model was selected for this study. The 2 sites - 3 p $K_{a}$ s model, in which the surfaces were assumed to have tetrahedral and octahedral sites, was reasonable for the description of the experimental data. The surface charges of both minerals were negative above pH of 4. The higher the pH, the lower the proton surface charge densities of both minerals. The ≡ $SiO^{[-10]}$ site played an important role in cation adsorption in acid and neutral pH range; whereas the ≡ Al $O^{[-10]}$ site was in an alkaline pH range. The optimized intrinsic constants of kaolinite, p $K_{a2(Si)}$$^{int}$, p $K_{al(Al)}$$^{int}$ and p $K_{a2(Al)}$$^{int}$ were 4.436, 4.564, and 8.461 respectively, and those of halloysite were 7.852, 3.885, and 7.084, respectively. The total Si and Al surface sites concentrations of kaolinite were 0.215 and 0.148 mM, and those of halloysite were 0.357 and 0.246 mM. The ratio of Si and Al surface site densities ([≡SiOH]:[≡AlOH]) of both minerals was 1 : 0.69. The total surface site density of kaolinite, 3.774 sites/n $m^2$, was 1.6 times larger than that of halloysite, 2.292 sites/n $m^2$./TEX>.

Study on Adsorption Features of Arsenic onto Lepidocrocite (레피도크로사이트(lepidocrocite) 표면의 비소 흡착 특성 규명)

  • Lee, Woo-Chun;Jeong, Hyeon-Su;Kim, Ju-Yong;Kim, Soon-Oh
    • Economic and Environmental Geology
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    • v.42 no.2
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    • pp.95-105
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    • 2009
  • Systematic studies are performed for arsenic adsorption on synthesized lepidocrocite. The synthesized lepidocrocite with high surface area of $94.8\;g/m^2$ has shown that the point of zero charge(PZC) is 6.57 determined by potentiometric titration, suggestive of high capacity of arsenic removal. Results show that arsenite[As(III)] uptake by synthesized lepidocrocite is greater than that of arsenate[As(V)] at pH $2{\sim}12$, indicating that the lepidocrocite has high affinity toward arsenite rather than arsenate. Adsorption of arsenate decreases with increasing pH from 2 to 12, whereas arsenite sorption increases until pH 8.0, and then decreases dramatically with increasing pH, suggesting that changes in surface charge of the lepidocrocite as a function of pH playa important role in aresinc uptake by the lepidocrocite. Upon kinetic experiments, our results demonstrate that both arsenite and arsenate sorption on the lepidocrocite increases rapidly for the first 4 h followed by little changes during the duration of the experiment, showing that adsorption plays a key role in aresenic uptake by the lepidocrocite. Our results also show that power function and elovich models are the best fit for the adsorption kinetics of arsenite and aesenate on the lepidocrocite.

Sub-Micro Molar Monitoring of La3+ by a Novel Lanthanum PVC-Based Membrane Sensor Based on 3-Hydroxy-N'-(pyridin-2-ylmethylene)-2-naphthohydrazide

  • Ganjali, Mohammad Reza;Norouzi, Parviz;Yousefian, Nasrin;Faridbod, Farnoush;Adib, Mehdi
    • Bulletin of the Korean Chemical Society
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    • v.27 no.10
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    • pp.1581-1586
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    • 2006
  • A La (III) ion-selective membrane sensor has been fabricated from poly vinyl chloride (PVC) matrix membrane, containing 3-hydroxy-N'-(pyridin-2-ylmethylene)-2-naphthohydrazide (HPMN) as a neutral carrier, potassium tetrakis (p-chlorophenyl) borate (KTpClPB) as an anionic excluder and ortho-nitrophenyloctyl ether (NPOE) as a plasticizing solvent mediator. The effects of membrane composition and pH as well as the influence of the anionic additive on the response properties were investigated. The sensor with 30% PVC, 62% solvent mediator, 6% ionophore and 2% anionic additive, shows the best potentiometric response characteristics. It displays a Nernstian behavior (19.2 mV per decade) across the range of $1.0{\times}10^{-2}-1.0{\times}10^{-7}$ M. The detection limit of the electrode is $7.0{\times}10^{-8}$ M ($\sim$10 ng/mL) and the response time is 15 s from $1.0{\times}10^{-2}$ up to $1.0{\times}10^{-4} $M and 30 s in the range of $1.0 {\times}10^{-5}-1.0{\times}10^{-7}$ M. The sensor can be used in the pH values of 3.0-9.0 for about seven weeks. The membrane sensor was used as an indicator electrode in the potentiometric titration of lanthanum ions with EDTA. It was successfully applied to the lanthanum determination in some mouth wash preparations.

Organopalladium(II) Complexes as Ionophores for Thiocyanate Ion-Selective Electrodes

  • Kim, Dong-Wan;Lee, So-Hyun;Kim, Jung-Hwan;Kim, Jin-Eun;Park, Jong-Keun;Kim, Jae-Sang
    • Bulletin of the Korean Chemical Society
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    • v.30 no.10
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    • pp.2303-2308
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    • 2009
  • A thiocyanate poly(vinyl chloride) (PVC) membrane electrode based on [1,2-bis(diphenylphosphino)ethane]dihalopalladium( II), [(dppe)$PdX_2$, X = Cl ($L^1$), X = I ($L^2$)] as active sensor has been developed. The diiodopalladium complex, [(dppe)$PdI_2](L^2$) displays an anti-Hofmeister selectivity sequence: $SCN^-\;>\;I^-\;>\;{ClO_4}^-\;>\;Sal^-\;>\;Br^-\;>\;{NO_2}^-\;>\;{HPO_4}^-\;>\;AcO^-\;>\;{NO_3}^-\;>\;{H_2PO_4}^-\;>\;{CO_3}^{2-}$. The electrode exhibits a Nernstian response (-59.8 mV/decade) over a wide linear concentration range of thiocyanate ($(1.0\;{\times}\;10^{-1}\;to\;5.0\;{\times}\;10^{-6}$ M), low detection limit ($(1.1\;{\times}\;10^{-6}$ M), fast response $(t_{90%}$ = 24 s), and applicability over a wide pH range (3.5∼11). Addition of anionic sites, potassium tetrakis[p-chlorophenyl] borate (KTpClPB) is shown to improve potentiometric anion selectivity, suggesting that the palladium complex may operate as a partially charged carrier-type ionophore within the polymer membrane phase. The reaction mechanism is discussed with respect to UV-Vis and IR spectroscopy. Application of the electrode to the potentiometric titration of thiocyanate ion with silver nitrate is reported.

Determination of triflusal in raw material and capsules by HPLC

  • Pham, Thuy-Vy;Mai, Xuan-Lan;Lee, Ji-Hyeon;Lee, Jong-Ha;Jo, Hyeon-Ah;Kang, Jong-Seong;Woo, Mi Hee;Na, Dong-Hee;Chun, In-Koo;Kim, Kyeong Ho
    • Analytical Science and Technology
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    • v.31 no.4
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    • pp.143-148
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    • 2018
  • Currently, the Korean Pharmacopoeia (KP XI) recommends HPLC and potentiometric titration (which is less specific than HPLC) for the determination of triflusal content in capsules and raw materials, respectively. Additionally, the British Pharmacopoeia (BP 2017) and European Pharmacopoeia (EP 8.0), which include a monograph for triflusal in raw materials only, describe a titration method for the assay. The latest version of the United States Pharmacopoeia (USP 39) and Japanese Pharmacopoeia (JP 17) still have not published monographs for triflusal and its preparations. To improve the specificity and efficacy of the assay, we present an HPLC method to determine triflusal content in both raw materials and capsules. The proposed method was validated in accordance with the requirements of the International Conference on Harmonization. A good linear relationship was achieved for triflusal in the range of $200-1250{\mu}g/mL$ with a coefficient of determination of approximately 0.9996. The relative standard deviations (RSDs) of inter- and intraday precision were 0.73-1.12 % and 0.34-0.51 %, respectively. The recovery percentage of triflusal was in the range of 98.80-101.31 %. Because its system suitability, intermediate precision, and robustness were satisfactory, this method could be suitable for determining triflusal content in raw materials and capsules.