• 제목/요약/키워드: potentiometry

검색결과 79건 처리시간 0.023초

전이금속 이온과 Macrocyclic Ligand 사이의 반응에 관한 속도론적 연구 질소원자와 산소원자를 포함하는 거대고리 리간드를 중심으로 (Kinetic Studies of Reaction of Transion Metal Ion with Macrocyclic Ligands. Containing Nitrogen and Oxygen Donor Atoms)

  • 김진호;조문환;현동호;박휴범;김시중;이인종
    • 대한화학회지
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    • 제34권5호
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    • pp.418-423
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    • 1990
  • 새로이 합성된 거대고리 리간드 1,15,18-triaza-3,4;12,13-dibenzo-5,8,11-trioxa cycloeicosane (NdienOdienH$_4$)와 이미 합성된 거대고리 리간드 1,12,15-triaza-3,4;9,10-dibenzo-5,8-dioxa cycloheptadecane (NdienOenH$_4$)와 1,15-diaza-3,4;12,13-dibenzo-5,8,11-trioxa cycloheptadecane (NenOdienH$_4$)를 25$^{\circ}C$ 수용액에서 전위차계를 이용하여 양성자 첨가반응의 평형상수를 구하였다. 또한 위의 세 가지 리간드 각각과 Co(Ⅱ), Ni(Ⅱ), Cu(Ⅱ)의 금속이온과의 착물을 합성하여 25$^{\circ}C$수용액에서 안정도 상수를 전위차법으로 구하였다. 그리고 위의 착물 수용액에 에틸렌 디아민용액을 가해 착물의 리간드 치환반응 속도상수를 분광광도법으로 측정하였다. 그리고 활성화에너지와 활성화파라메타(${\{Delta}H^{\neq}$, ${\{Delta}S^{\neq}$)를 구하여 이 반응계의 타당한 메카니즘을 제안하였다.

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이온선택성 멤브레인을 이용한 양액 내 질산태 질소 및 칼륨 측정 (Sensing NO3-N and K Ions in Hydroponic Solution Using Ion-Selective Membranes)

  • 김원경;박두산;김영주;노미영;조성인;김학진
    • Journal of Biosystems Engineering
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    • 제35권5호
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    • pp.343-349
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    • 2010
  • Rapid on-site sensing of nitrate-nitrogen and potassium ions in hydroponic solution would increase the efficiency of nutrient use for greenhouse crops cultivated in closed hydroponic systems while reducing the potential for environmental pollution in water and soil. Ion-selective electrodes (ISEs) are a promising approach because of their small size, rapid response, and the ability to directly measure the analyte. The capabilities of the ISEs for sensing nitrate and potassium in hydroponic solution can be affected by the presence of other ions such as calcium, magnesium, sulfate, sodium, and chloride in the solution itself. This study was conducted to investigate the applicability of two ISEs consisting of TDDA-NPOE and valinomycin-DOS PVC membranes for quantitative determinations of $NO_3$-N and K in hydroponic solution. Nine hydroponic solutions were prepared by diluting highly concentrated paprika hydroponic solution to provide a concentration range of 3 to 400 mg/L for $NO_3$-N and K. Two of the calibration curves relating membrane response and nutrient concentration provided coefficients of determination ($R^2$) > 0.98 and standard errors of calibration (SEC) of < 3.79 mV. The use of the direct potentiometry method, in conjunction with an one-point EMF compensation technique, was feasible for measuring $NO_3$-N and K in paprika hydroponic solution due to almost 1:1 relationships and high coefficients of determination ($R^2$ > 0.97) between the levels of $NO_3$-N and K obtained with the ion-selective electrodes and standard instruments. However, even though there were strong linear relationships ($R^2$ > 0.94) between the $NO_3$-N and K concentrations determined by the Gran's plot-based multiple standard addition method and by standard instruments, hydroponic $NO_3$-N concentrations measured with the ISEs, on average, were about 10% higher than those obtained with the automated analyzer whereas the K ISE predicted about 59% lower K than did the ICP spectrometer, probably due to no compensation for a difference between actual and expected concentrations of standard solutions directly prepared.

1, 14-Bis(2-hydroxybenzyl)-2, 6, 9, 12-tetraazatetradecane.tetrahydro-chloride 구리착물의 합성, 안정도상수, X-ray 구조 및 전기화학적 연구 (Synthesis, Stability Constants, X-ray Structure and Electrochemical Studies of Copper (II) 1, 14-Bis (2-hydroxybenzyl)-2, 6, 9, 12-tetraazatetradecane.tetrahydrochloride Complex)

  • 김선덕;김준광;김성윤
    • 분석과학
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    • 제13권2호
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    • pp.173-178
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    • 2000
  • 두 개의 페놀기를 포함하는 열린 고리형태의 1, 14-Bis(2-hydroxybenzyl)-2, 6, 9, 12-tetraazatetradecane(bsated) 리간드를 염산염의 형태로 분리하여 원소 분석, 질량 스펙트럼 및 핵자기공명법으로 분석하였다. 합성된 리간드의 산 해리상수($logK^n{_H}$)와 $Cu^{2+}$, $Ni^{2+}$, $Co^{2+}$$Zn^{2+}$에 대한 안정도 상수($logK_{ML}$)를 전위차 적정법으로 결정하였다. 이때 온도는 $25^{\circ}C$ 및 이온강도는 0.10M($KNO_3$)로 고정시켰다. [Cu(bsated)] $(ClO_4)_2$ X-ray구조의 crystal data는 다음과 같다: Monoclinic space group $P2_1/n$, $a=17.856(4){\AA}$, $b=17.709(1){\AA}$, $c=8.539(2){\AA}$, $V=2700(2){\AA}$ with Z=4. tetrabutylammonium perchlorate 전해질의 dimethyl sulfoxide 용액속에서 [Cu(bsated)]$(ClO_4)_2$ 착물의 전기화학적 특성을 순환 전압-전류법 (CV)과 normal pulse voltammertry (NPV, 정상펄스전압전류법)으로 측정하였다.

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새로운 산소-질소(N2O2)계 네 자리 리간드의 합성과 전이금속 착물 안정도상수에 대한 치환기 효과 (Synthesis of new N2O2 tetradentate ligands and the substituent effect on the stability constants of the transition metal complexes)

  • 김선덕;진경록
    • 분석과학
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    • 제19권2호
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    • pp.131-141
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    • 2006
  • 새로운 산소-질소($N_2O_2$)계 네 자리 리간드 N,N'-bis(2-hydroxybenzyl)-ethylenediamine($H-BHE{\cdot}2HBr$)의 브롬산염을 합성하였다. 또한 $H-BHE{\cdot}2HBr$의 페놀기 5-위치에 치환기로 브롬, 염소, 메틸기 및 메톡시기를 가진 $Br-BHE{\cdot}2HBr$, $Cl-BHE{\cdot}2HBr$, $CH_3-BHE{\cdot}2HBr$$CH_3O-BHE{\cdot}2HBr$을 합성하였다. 그리고 페놀기 대신에 naphthalen-2-ol을 가진 $Nap-BHE{\cdot}2HBr$도 합성하였다. 합성된 리간드들의 양성자 해리는 수용액에서 전위차 적정한 결과 4 단계로 일어났으며, 계산된 각 리간드의 총괄 양성자 해리상수(${\log}{\beta}_p$) 값은 Br-BHE < Cl-BHE < H-BHE < Nap-BHE < $CH_3$-BHE < $CH_3O$-BHE의 순서로 Hammett 상수(${\sigma}_P$) 값의 순서와 비교적 같은 경향을 나타내었다. 전이금속(II) 이온들의 착물의 안정도상수(${\log}K_{ML}$) 값의 크기는 Co(II) < Ni(II) < Cu(II) > Zn(II) > Cd(II) > Pb(II)의 순서이었다. 또한 각 리간드들의 전이금속(II) 이온들의 착물 안정도상수(${\log}K_{ML}$) 값들의 크기 순서도 리간드의 총괄 양성자 해리상수(${\log}{\beta}_p$) 값과 서로 잘 일치하였다.

Dioxouranium(Ⅵ) 이온과 Hydrazide Schiff Base 리간드와의 착물형성에 관한 연구 (A Study on Complexation of Dioxouranium(Ⅵ) Ion with Hydrazide Schiff Base Ligands)

  • 차분희;허영애;최규성
    • 대한화학회지
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    • 제39권7호
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    • pp.538-542
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    • 1995
  • Hydrazide schiff base 리간드인 N,N'-oxalylbis(salicylalde hydehydrazone)(OBSH)과 N,N'-malonylbis(salicylaldehydehydrazone)(MBSH), N,N'-succinylbis(salicylaldehydehydrazone)(SBSH) 리간드들과 $UO_2^{2+}$ 이온과의 착물형성에 따르는 안정도상수와 열역학적 파라미터를 95% DMF 용액에서 전위차 적정법을 사용하여 측정하였다. 안정도상수의 크기는 SBSH$UO_2^{2+}$ 이온과의 착물형성에 대한 ΔH는 OBSH에 대해서는 음의 값을 갖는 발열반응임을 알 수 있었고, MBSH, SBSH에 대해서는 양의 값을 갖는 흡열반응임을 알 수 있었다. ΔS는 OBSH < MBSH < SBSH로 증가하였다.

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Novel Triiodide PVC-Based Membrane Sensor Based on a Charge Transfer Complex of Iodine and Bis(2-hydroxyacetophenone)butane-2,3-dihydrazone

  • Ganjali, Mohammad Reza;Norouzi, Parviz;Shirvani Arani, Simindokht;Salavati Niasari, Masoud
    • Bulletin of the Korean Chemical Society
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    • 제26권11호
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    • pp.1738-1742
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    • 2005
  • In this study a novel triiodide ion-selective electrode based on a charge transfer complex of iodine and Bis(2-hydroxyacetophenone)butane-2,3-dihydrazone (ICT), as a membrane carrier was prepared. The electrode has a linear dynamic range between 1.0 ${\times}$ $10^{-2}$ and 5.0 ${\times}$ $10^{-7}$ M, with a Nernstian slope of 58. 99 ${\pm}$ 0.3 mV $decade^{-1}$ and detection limit of 3.0 ${\times}$ $10 ^{-7}$ M. The potentiometric response of the proposed sensor is independent of the pH of the solution in the pH range of 3.0-10.0. The electrode possesses the advantages of short conditioning time, fast response time, and especially, very good selectivity over a large number of common organic and inorganic anions. The electrode can be used for at least 6 months without any considerable divergences in the potentials. It was used as an indicator electrode in potentiometric titration of triiodide ion with thiosulfate.

Salphen H2 as a Neutral Carrier for the Uranyl Ion-Selective PVC Membrane Sensor

  • Kim, Dong-Wan;Park, Kyeong-Won;Yang, Mi-Hyi;Kim, Jin-eun;Lee, Shim-Sung;Kim, Jae-Sang
    • Bulletin of the Korean Chemical Society
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    • 제27권6호
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    • pp.899-902
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    • 2006
  • The complexation of N,N'-4,5-(ethylenedioxy)benzenebis(salicylideneimine), (salphen$H_2$) with uranyl ion was studied in acetonitrile solution spectrophtometrically, and the formation constant of the resulting 1 : 1 complex was evaluated. The salphen$H_2$ ligand was used as an ionophore in plasticized poly(vinyl chloride) (PVC) matrix membrane sensor for uranyl ion. The prepared sensors exhibited a near Nernstian response, 28.0-30.9 mV/decade for uranyl ion over the concentration range $1.0\;{\times}\;10^{-2}$ to $1.0\;{\times}\;10^{-6}$M with a limit of detection of $3.2\;{\times}\;10^{-7}$ M. The proposed electrode could be used at a working pH range of 1.5 - 4.0.

Novel Tm(III) Membrane Sensor Based on 2,2'-Dianiline Disulfide and Its Application for the Fluoride Monitoring of Mouth Wash Preparations

  • Ganjali, Mohammad Reza;Norouzi, Parviz;Tamaddon, Atefeh;Husain, Syed Waqif
    • Bulletin of the Korean Chemical Society
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    • 제27권9호
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    • pp.1418-1422
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    • 2006
  • In this work the construction of a novel poly(vinyl chloride) membrane sensor based on 2,2'-dianiline disulfide (DADS) as a neutral carrier, o-nitrophenyloctyl ether (NPOE) as a plasticizer and sodium tetraphenyl borate (NaTPB) as an anionic site with unique selectivity towards Tm(III) ions is reported. The electrode has a linear dynamic range between $1.0\;{\times}\;10^{-6}$ and $1.0\;{\times}\;10^{-2}$ M, with a nice Nernstian slope of 19.5 ${\pm}$ 0.3 mV per decade and a detection limit of $4.0\;{\times}\;10^{-7}$ M at the pH range of 4.8-8.5. It has a very fast response time (<15 s) in the whole concentration range, and can be used for at least 4 weeks without any considerable divergence in the electrode potentials. The proposed sensor revealed comparatively good selectivity with respect to most common metal ions, and especially lanthanide ions. It was used as an indicator electrode in the potentiometric titration of Tm(III) ions with EDTA and in direct determination of concentration of Tm(III) ions in binary mixtures. It was also applied in determination of fluoride ions in mouth wash preparations.

Copper(II) Selective PVC Membrane Electrodes Based on Schiff base 1,2-Bis (E-2-hydroxy benzylidene amino)anthracene-9,10-dione Complex as an Ionophore

  • Jeong, Eun-Seon;Lee, Hyo-Kyoung;Ahmed, Mohammad Shamsuddin;Seo, Hyung-Ran;Jeon, Seung-Won
    • Bulletin of the Korean Chemical Society
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    • 제31권2호
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    • pp.401-405
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    • 2010
  • The Schiff base 1,2-bis(E-2-hydroxy benzylidene amino)anthracene-9,10-dione has been synthesized and explored as ionophore for preparing PVC-based membrane sensors selective to the copper ($Cu^{2+}$) ion. Potentiometric investigations indicate high affinity of these receptors for copper ion. The best performance was shown by the membrane of composition (w/w) of ionophore: 1 mg, PVC: 33 mg, DOP: 66 mg and KTpClPB as additive were added 50 mol % relative to the ionophore in 1 ml THF. The proposed sensor's detection limit is $2.8{\times}10^{-7}$ M over pH 5 at room temperature (Nernstian slope 31.76 mV/dec.) with a response time of 15 seconds and showed good selectivity to copper ion over a number of interfering cations.

Potentially Multidentate Tripodal Amine Catechol Ligands as Chelators for Ga(III) and In(III)

  • Sahoo, Suban K.;Baral, Minati;Bera, Rati Kanta;Kanungo, B. K.
    • Bulletin of the Korean Chemical Society
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    • 제30권9호
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    • pp.1956-1962
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    • 2009
  • The binding abilities of two multidentate tripodal amine catechol ligands, cis,cis-1,3,5-tris[(2,3-dihydroxybenzylamino) aminomethyl]cyclohexane (TMACHCAT, $L^1)\;and\;N^1,N^3,N^5$-tris(2-(2,3-dihydroxybenzylamino) ethyl)cyclohexane-1,3,5-tricarboxamide (CYCOENCAT, $L^2$) with Ga(III) and In(III) have been investigated by potentiometric and spectrophotometric methods in an aqueous medium of 0.1 M KCl at 25 ${\pm}\;1\;{^{\circ}C}.$ The ligands $L^1\;and\;L^2$ formed various monomeric species $MLH_3,\;MLH_2$, MLH and ML (M = $Ga^{+3}\;and\;In^{+3}$) and showed potential to form strong encapsulated tris(catechol) type complexes. The coordination modes, binding ability and selectivity of the ligands towards Ga(III) and In(III) have been discussed with the help of experimental evidences, and supported with molecular modeling calculations.