• 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+.

• 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.

• Bulletin of the Korean Chemical Society
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• v.25 no.2
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• pp.177-181
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• 2004

A PVC membrane electrode for silver ion based on a new cone shaped calix[4]arene (CASCA) as membrane carrier was prepared. The electrode exhibits a Nernstian response for $Ag^+$ over a wide concentration range ($1.0{\times}10^{-1}-8.0{\times}10^{-6}$M) with a slope of 58.2 {\pm}$ 0.5 mV per decade. The limit of detection of the sensor is $5.0{\times}10^{-6}$M. The sensor has a very fast response time (~5 s) in the concentration range of ${\leq}=1.0{\times}10^{-3}$ M, and a useful working pH range of 4.0-9.5. The proposed sensor displays excellent discriminating ability toward $Ag^+$ ion with respect to common alkali, alkaline earth, transition and heavy metal ions. It was used as an indicator electrode in potentiometric titration of $Ag^+$ with EDTA and in direct determination of silver ion in wastewater of silver electroplating.

• Analytical Science and Technology
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• v.10 no.4
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• pp.256-263
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• 1997

The new naphthol-containing hexadentate ligands, 1,12-bis (2-naphthol)- 2,5,8,11-tetraazadodecane 4HCl (nptr) and 1,14-bis(2-naphthol)- 2,6,9,13- tetraazatetradodecane .4HCl (npptr) were synthesized and characterized by elemental analysis, IR, NMR, and mass spectrometry. Acid dissociation constants and stability constants of Co(II), Ni(II). Cu(II), and Zn(II) complexes were determined at $25.0^{\circ}C$ and ionic strength ($\mu$)=0.10M($KNO_3$) by potentiometry. The relationship between basicity and stability constants of ligands containing aliphatic amines and 2-naphthol were studied.

• Journal of the Korean Magnetic Resonance Society
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• v.10 no.1
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• pp.115-125
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• 2006

Hippuryl-L-histidyl-L-leucine(HHL) is widely used as a substrate of angiotensin converting enzyme(ACE) cleaving the neurotransmitter angiotensin(I) to the octapeptide angiotensin(II). The structure of the substrate molecules should provide information regarding the geometric requirements of the ACE active site. For the purpose of determination of in vivo reaction, metallo(Cu, Zn)-HHL complexes were synthesized and the degree of complex formation were identified by MALDITOF, ESI mass spectrometric analysis. Tn addition, the pH-dependent species distribution curves were obtained by potentiometric titration. Nitrogen atoms of imidazole ring and oxygen atom of caboxylate groups in the peptide chain were observed to be participated in the metal complex formation. After purification of complexes further structural characterization were made by utilizing UV-Vis, electrochemical methods and NMR. Complete NMR signal assignments were carried out by using 2D-spectrum techniques COSY, TOCSY, NOESY, HETCOR. A complex that two imidazole and carboxylate groups are asymmetrically participating to coordination mode was predicted to the solution-state structure of $Cu(II)-HHL_2$ based on $^{13}C-NMR$ signal assignment and NOE information.

• Bulletin of the Korean Chemical Society
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• v.26 no.1
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• pp.38-42
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• 2005

Bis(2-methylbenzaldehyde)butane-2,3-dihydrazone(TDSB) was used as new N-N Schiff's base which plays the role of an excellent ion carrier in the construction of a La(III) membrane sensor. The best performance was obtained with a membrane containing, 30% poly(vinyl chloride), 60% benzyl acetate, 6% TDSB and 4% sodium tetraphenyl borate. This sensor reveals a very good selectivity towards La(III) ions over a wide variety of cations, including alkali, alkaline earth, transition and heavy metal ions. The proposed electrode exhibits a Nernstian behavior (with slope of 19.8 mV per decade) over a wide concentration range (1.0 ${\times}$ 10$^{-5}$-1.0 ${\times}$ 10$^{-1}$ M). The detection limit of the sensor is 7.0 ${\times}$ 10$^{-6}$ M. It has a very short response time, in the whole concentration range ($\sim$5 s), and can be used for at least twelve weeks in the pH range of 3.0-9.4. The proposed sensor was successfully applied as an indicator electrode for the potentiometric titration of a La(III) solution, with EDTA. It was also successfully applied in the determination of fluoride ions in three mouth wash preparations.

• Journal of the Korean Chemical Society
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• v.10 no.3
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• pp.114-118
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• 1966

The glass electrode was empirically calibrated in dioxane-and ethanol-water mixed solvents, by means of which the pH-meter reading could be converted to stoichiometric hydrogen ion concentration. By the potentiometric titration method, the thermodynamic dissociation constants of hydrogen cupferrate (HCup) with variations of ionic concentration in aqueous solution were determined, and by the extrapolation of the constants the new thermodynamic $pK_a$ value, 3.980${\pm}$0.006, at zero ional concentration was obtained. The thermodynamic dissociation constants of HCup in dioxane-and ethanol-water solution were also potentiometrically determined with the changes in composition of organic solvents at 0.01 and 0.05 of the ionic strength(${mu}$) and 25 $^{\circ}C$. The empirical formula of the constants with mole fraction(n) of the organic solvent are as follow: Dioxane-water solution. $pK_a$= 12.96n + 4.10 at ${\mu}$ = 0.01, n = 0.0228∼0.171 $pK_a$= 12.05n + 4.23 at ${\mu}$ = 0.05, n= 0.0228∼0.171 Ethanol-water solution, $pK_a$= 4.0ln + 4.26 at ${\mu}$= 0.01, n= 0.0395∼0.262 $pK_a$= 3.83n + 4.34 at ${\mu}$= 0.05, n= 0.0395∼0.262

• Bulletin of the Korean Chemical Society
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• v.34 no.10
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• pp.3088-3092
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• 2013

A novel PVC membrane sensor for perindopril based on perindopril-phosphotungstate ion pair complex was prepared. The influence of membrane composition (i.e. percent of PVC, plasticizer, ion-pair complex, and kind of plasticizer), inner solution, pH of test solution and foreign cations on the electrode performance was investigated. The optimized membrane demonstrates Nernstian response ($30.9{\pm}1.0$ mV per decade) for perindopril cations over a wide linear range from $9.0{\times}10^{-7}$ to $1{\times}10^{-2}$ M at $25^{\circ}C$. The potentiometric response is independent of the pH in the range of 4.0-9.5. The proposed sensor has the advantages of easy preparation, fast response time. The selectivity coefficients indicate excellent selectivity for perindopril over many common cations (e.g., $Na^+$, $K^+$, $Mg^{2+}$, $Cu^{2+}$, $Ni^{2+}$, rhamnose, maltose, glycine and benzamide. The practical applications of this electrode was demonstrated by measuring the concentrations of perindopril in pure solutions and pharmaceutical preparations with satisfactory results.

• Bulletin of the Korean Chemical Society
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• v.31 no.10
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• pp.2980-2984
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• 2010

A new poly (vinyl chloride) (PVC) membrane electrode that is highly selective to $Mn^{+2}$ ions was prepared using N,N'-bis(2'-pyridinecarboxamide)-1,2-ethane ($bpenH_2$) as a suitable neutral carrier. This concentration range ($1.0{\times}10^{-5}$ to $1.0{\times}10^{-1}\;M$) with Nernstian slope of $29.3{\pm}0.5\;mV$ per decade. The detection limit and the response time of electrode were $8.0{\times}10^{-6}\;M$ and (${\leq}15\;s$) respectively. The membrane can be used for more than two months without observing any divergence. The electrodes exhibited excellent selectivity for $Mn^{+2}$ ion over other mono-, di- and trivalent cations. Selectivity coefficients were determined by the matched potential method (MPM). The electrode can be used in the pH range from 4.0 - 9.0. The isothermal coefficient of this electrode amounted to 0.00023 V/$^{\circ}C$. The stability constant (log $K_s$) of the $Mn^{+2}$ - $bpenH_2$ complex was determined at $25^{\circ}C$ by potentiometric titration in mixed aqueous solution. The proposed electrode was applied to the determination of $Mn^{+2}$ ions in real samples.

• Bulletin of the Korean Chemical Society
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• v.31 no.6
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• pp.1699-1703
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• 2010

The Schiff base N,N'-bis(pyridin-2-ylmethylene)benzene-1,2-diamine [BPBD] has been synthesized and explored as ionophore for preparing PVC-based membrane sensors selective to the silver ($Ag^+$) ion. Potentiometric investigations indicate high affinity of this receptor for silver ion. The best performance was shown by the membrane of composition (w/w) of ionophore: 1 mg, PVC: 33 mg, o-NPOE: 66 mg and additive were added 50 mol % relative to the ionophore in 1 mL THF. The sensor works well over a wide concentration range $1{\times}10^{-3}$ to $1.0{\times}10^{-7}$ M by pH 6 at room temperature (slope 58.6 mV/dec.) with a response time of 10 seconds and showed good selectivity to silver ion over a number of cations. It could be used successfully for the determination of silver ion content in environmental and waste water samples.