共查询到20条相似文献,搜索用时 31 毫秒
1.
M. M. Antonijević R. P. Mihajlović B. V. Vukanović 《Journal of Solid State Electrochemistry》2001,5(1):29-35
The results obtained in potentiometric titrations of copper(II), mercury(II) and iron(III) with standard EDTA solutions are
presented. The titration of copper(II) at pH values in the range from 8.11 to 10.99 (ammonia buffer) and the titration of
mercury(II) and iron(III) at pH values from 3.59 to 5.65 (acetate buffer) were performed. The titration end-point (TEP) was
detected with an indicator electrode made from natural crystalline pyrite as an electrochemical sensor. The results obtained
in potentiometric titration with the pyrite electrode were compared with those obtained using a platinum electrode (Fe3+), a Cu ion selective electrode (Cu2+) and a Hg electrode (Hg2+). Accurate and reproducible results with good agreement were obtained, but higher potential changes at the TEP were obtained
using the pyrite electrode. In the course of the titration the potential was established within less than 1 min, whereas at
the TEP it was within about 2–3 min. The potential changes at the TEP were in the range from 60 to 200 mV per 0.1 ml EDTA,
according to the stability constant of the complex formed. The highest potential changes, ranging from 160 to 200 mV, were
obtained in the titration of iron(III) at pH 3.59. Reverse titration was also performed and accurate and reproducible results
were obtained. Moreover, titration of halogenide and thiocyanate with standard mercury(II) solutions, as well as cyanide with
silver(I) solution, were performed and accurate and reproducible results were again obtained.
Received: 20 February 1998 / Accepted: 19 November 1999 相似文献
2.
A micro extraction – spectrophotometric procedure is developed for the determination of bismuth in pharmaceutical formulations.
The procedure is based on the extraction of tetraiodobismuthate(III) ion paired with benzyltributylammonium cation into chloroform.
The application of Nile Blue as internal standard (IS) enabled good analytical performance for micro-scale analysis. The ratio
between the absorbances measured at 491 nm (bismuth complex) and at 632 nm (IS) was taken as the analytical signal. The procedure
was carried out in Eppendorf tubes, lowering significantly the use of reagents and the volume of organic solvent. In the calibration
range up to 60 mgċl−1, the linear regression coefficient was 0.9999, the CV for 15 mgċl−1 and for 50 mgċl−1 Bi were 1.6% and 0.7% respectively. The results obtained in the analysis of pharmaceutical formulations were in good agreement
with the results of EDTA titration method.
Received November 25, 1999. Revision February 14, 2000. 相似文献
3.
A New Approach for Titration Calorimetric Data Analysis on the Binding of Magnesium Ion with Myelin Basic Protein 总被引:1,自引:0,他引:1
G. Rezaei Behbehani A. A. Saboury A. Fallah Baghery 《Journal of solution chemistry》2008,37(8):1127-1135
The interaction of the myelin basic protein (MBP) from the bovine central nervous system with divalent magnesium ion was studied
by isothermal titration calorimetry at 27 °C in aqueous solution. A simple rapid method for determination of the dissociation
binding constants for Mg2+-MBP interaction was introduced using the isothermal titration calometric data. The binding isotherm for Mg2+-MBP interaction is easily obtained by carrying out a titration calorimetric experiment using only one set of concentrations
of MBP. There are two identical independent intrinsic association constants equal to 0.021 μmol⋅L−1 in the first- and second-binding sites, respectively. 相似文献
4.
Sayed S. Badawy Yousry M. Issa Waheed F. El-Hawary Manal S. Ashour 《Mikrochimica acta》2001,136(1-2):1-7
A PVC membrane electrode selective for cetyldimethylethylammonium (CDEA) ion was prepared. The active element is a plasticized
poly vinyl chloride membrane containing a dissolved ion associate complex of CDEA with phosphotungstic acid (PTA). The electrode
showed a near-Nernstian response within the CDEA+ concentration range 2.34 × 10−6 to 1.96 × 10−4 M at 25 ± 1^C, good selectivity, and is usable within the pH range 3.5–9.0. The isothermal temperature coefficient of the electrode amounted
to −0.00012 V/°C. The electrode has been used for the direct determination of cetyldimethylethylammonium bromide either by
the standard addition method or by potentiometric titration against PTA.
Received January 1, 1998. Revision June 13, 2000. 相似文献
5.
An interdigitated microelectrode array (IDA) biamperometric titration is presented for the microdetermination of formaldehyde.
It is based on a direct titration of formaldehyde with hydroxylamine under the formation of formaldoxime. The released hydrogen
cations react with hydroxyl anions in 0.1 M NaOH. The interdigitated pair of two individually polarizable microelectrodes
serves as a biamperometric end-point indicator. Hydroxylamine together with dissolved free oxygen behave as a quasi reversible
mixed redox system, therefore a significant increase of current flowing between the IDA segments polarized by 100 mV is observed
when the first excess of titrant appears in the titrated solution. Because of the small dimension of the IDA sensor this principle
can be extended for a microanalytical variant of this method. Formaldehyde contents down to 10−3 M in small volume waste water samples could be determined by this technique. These samples usually contain carboxylic acids
which interfere in iodimetric determinations, but do not influence the titration of formaldehyde with hydroxylamine.
Received January 21, 2002; accepted August 7, 2002 相似文献
6.
A.K. Singh Puja Saxena Amit Panwar 《Journal of inclusion phenomena and macrocyclic chemistry》2006,54(3-4):299-305
Copper (II) complex of 2,4-dimethyl-1,5,9,12-tetraazacyclopentadeca-1,4-diene, [Me2(15)dieneN4] was synthesized and used in the fabrication of Cu2+ – selective ISE membrane in PVC matrix. The membrane having Cu(II) macrocyclic complex as electroactive material along with sodium tetraphenyl borate (NaTPB) as anion discriminator. Dibutyl phthalate (DBP) as plasticizer in poly(vinyl chloride) (PVC) matrix was prepared for the determination of Cu2+. The best performance was observed by the membrane having Cu(II) complex–PVC–NaTPB–DBP with composition 1:5:1:3. The sensor worked well over a concentration range 1.12 × 10−6 M–1.0 × 10−1 M between pH 2.1–6.2 and a fast response time 10±2 s and a lifetime of 6 months. Their performance in partially non-aqueous medium was found satisfactory. Electrodes exhibited excellent selectivity for Cu2+ ion over other mono-, di-, trivalent cations. It can also be used as indicator electrode in the potentiometric titration of Cu2+ against EDTA as well as in the determination of Cu2+ in real samples. 相似文献
7.
Magda M. Ayad Abdalla Shalaby Hisham E. Abdellatef Heba M. Elsaid 《Mikrochimica acta》2002,140(1-2):93-96
The construction of a plasticised PVC matrix-type promazinium cation-selective membrane electrode and its use in the potentiometric
determination of promazine hydrochloride in pharmaceutical preparations are described. It is based on the use of the ion-associate
species, formed by promazinium cation and tetraphenylborate (TPB) counter ion. The basic electrode performance characteristics
are evaluated according to IUPAC recommendations. It exhibited a linear response for 1 × 10−2−1 × 10−5 M of promazine hydrochloride solutions with a cationic Nernstian slope over the pH range 2–6. Common organic and inorganic
cations showed negligible interference. Direct potentiometric determination of 1 × 10−2−1 × 10−5 M aqueous promazine hydrochloride using this membrane electrode system showed an average recovery of 99.5% with a mean standard
deviation of 1.5%. This electrode was successfully used for monitoring the titration of promazine hydrochloride with sodium
tetraphenyl borate and for determining promazine hydrochloride in ampoules.
Received June 15, 2001 Revision November 6, 2001 相似文献
8.
Ashraf A. Mohamed 《Monatshefte für Chemie / Chemical Monthly》2001,132(8):919-928
Summary. A new selective, sensitive, and simple kinetic method is developed for the determination of trace amounts of iodide. The
method is based on the catalytic effect of iodide on the reaction of triflupromazine (TFP) with H2O2. The reaction is followed spectrophotometrically by tracing the oxidation product at 498 nm within 1 min after addition of
H2O2. The optimum reaction conditions are TFP (0.4 × 10−3
M), H2SO4 (1.0M), H3PO4 (2.0M), and H2O2 (1.6M) at 30°C. Following this procedure, iodide can be determined with a linear calibration graph up to 4.5 ng ċ cm−3 and a detection limit of 0.04 ng ċ cm−3, based on the 3 Sb criterion. The method can also be applied to the determination of iodate and periodate ions. Determination of as little as
0.2, 1.0, 2.0, and 4.0 ng ċ cm−3 of I−, IO3
-, or IO4
- in aqueous solutions gave an average recovery of 98% with relative standard deviations below 1.6% (n = 5). The method was applied to the determination of iodide in Nile river water and ground waters as well as in various food
samples after alkaline ashing treatment. The method is compared with other catalytic spectrophotometric procedures for iodide
determination.
Received January 19, 2001. Accepted (revised) March 12, 2001 相似文献
9.
M. R. Ganjali P. Norouzi S. Shirvani-Arani A. Kakanezhadifard 《Journal of Analytical Chemistry》2007,62(3):279-284
In this paper, a novel membrane triiodide sensor based on a charge-transfer complex of (1,3-diphenyldihydro-1H-imidazole)-4,5-dionedioxime
with iodine (CTCI) as a membrane carrier is introduced. The best performance was obtained with a membrane containing 30% polyvinylchloride
(PVC), 63% dibutylphthalate (DBP), 5% CTCI, and 2% hexadecyltrimethylammonium bromide (HTAB). The electrode shows a Nernstian
behavior (slope of 58.2 ± 0.3) over a very wide triiodide ion concentration range (5.0 × 10−8−1.0 × 10−2 M), and has a low detection limit (4.0 × 10−8 M). The potentiometric response of the sensor is independent of pH of the solution in the pH range 3.0–9.0. The proposed
sensor has a very low response time (<12 s) and a good selectivity relative to a wide variety of common inorganic and organic
anions, including iodide, bromide, chloride, nitrate, sulfate, thiocyanate, monohydrogen phosphate, and acetate. In fact,
the selectivity behavior of the proposed triiodide ion-selective electrode shows great improvements compared to the previously
reported electrodes for triiodide ion. The proposed membrane sensor can be used for at least 6 months without any divergence
in its potentials. The electrode was successfully applied as an indicator electrode in the titration of triiodide with thiosulfate
ion.
The text was submitted by the authors in English. 相似文献
10.
Naracham Veedu Sreekumar Ronald Aquin Nazareth Badiadka Narayana Prashant Hegde Busnur Rachotappa Manjunatha 《Mikrochimica acta》2002,140(1-2):63-67
A complexometric method for the determination of mercury in presence of other metal ions based on the selective masking ability
of potassium bromide towards mercury is described. Mercury(II) present in a given sample solution is first complexed with
a known excess of EDTA and the surplus EDTA is titrated against zinc sulfate solution at pH 5–6 using xylenol orange as the
indicator. A known excess of 10% solution of potassium bromide is then added and the EDTA released from Hg-EDTA complex is
titrated against standard zinc sulfate solution. Reproducible and accurate results are obtained for 8 mg to 250 mg of mercury(II)
with a relative error ± 0.28% and standard deviations ≤0.5 mg. The interference of various ions is studied. This method was
applied to the determination of mercury(II) in its alloys.
Received April 18, 2001 Revision October 10, 2001 相似文献
11.
A continuous flow atomic absorption spectrometric system was used to develop an efficient on-line preconcentration-elution
procedure for the determination of iodide traces. Chromium (VI) is introduced into the flow system and is reduced to chromium
(III) in acid medium proportionally to the iodide present in the sample. The Cr(III) reduced by iodide is retained on a minicolumn
packed with a poly(aminophosphonic acid) chelating resin, while unreduced Cr(VI) is not retained. Reduced Cr(III) is preconcentrated
by passing the sample containing iodide through the system during 3 min, and is then eluted with 0.5 mol L–1 hydrochloric acid and determined by flame atomic absorption spectrometry (FAAS). The detection limit (3σ) obtained is 2.5
μg L–1. Other ions typically present in waters do not interfere. The proposed method allows the determination of iodide in the range
6–220 μg L–1 with a relative standard deviation of 2.7% at a rate of 17 samples h–1. The method has been applied to the determination of iodide in tap and sea waters.
Received: 16 September 1999 / Revised: 15 November 1999 / Accepted: 19 November 1999 相似文献
12.
Determination of the structure of heparin-derived oligosaccharides by 1H NMR is challenging because resonances for all but the anomeric protons cover less than 2 ppm. By taking advantage of increased
dispersion of resonances for the anomeric H1 protons at low pD and the superior resolution of band-selective, homonuclear-decoupled (BASHD) two-dimensional 1H NMR, the primary structure of the heparin-derived octasaccharide ∆UA(2S)-[(1 → 4)-GlcNS(6S)-(1 → 4)-IdoA(2S)-]3-(1 → 4)-GlcNS(6S) has been determined, where ∆UA(2S) is 2-O-sulfated ∆4,5-unsaturated uronic acid, GlcNS(6S) is 6-O-sulfated, N-sulfated β-d-glucosamine and IdoA(2S) is 2-O-sulfated α-l-iduronic acid. The spectrum was assigned, and the sites of N- and O-sulfation and the conformation of each uronic acid residue were established, with chemical shift data obtained from BASHD-TOCSY
spectra, while the sequence of the monosaccharide residues in the octasaccharide was determined from inter-residue NOEs in
BASHD-NOESY spectra. Acid dissociation constants were determined for each carboxylic acid group of the octasaccharide, as
well as for related tetra- and hexasaccharides, from chemical shift–pD titration curves. Chemical shift–pD titration curves
were obtained for each carboxylic acid group from sub-spectra taken from BASHD-TOCSY spectra that were measured as a function
of pD. The pK
As of the carboxylic acid groups of the ∆UA(2S) residues are less than those of the IdoA(2S) residues, and the pK
As of the carboxylic acid groups of the IdoA(2S) residues for a given oligosaccharide are similar in magnitude. Relative acidities
of the carboxylic acid groups of each oligosaccharide were calculated from chemical shift data by a pH-independent method. 相似文献
13.
Tahereh PoursaberiMorteza Hosseini Massoud TaghizadehHooshang Pirelahi Mojtaba ShamsipurMohammad Reza Ganjali 《Microchemical Journal》2002,72(1):77-83
A highly selective electrode for iodide ion based on a thiopyrilium derivative as an excellent ionophore is described. At pH 5.5-8.0, the electrode responds to iodide ion in a linear range from 1.0×10−1 to 8.0×10−7 M with a slope of 60.2 mV per decade, and a detection limit of 2.0×10−7 M. Selectivity coefficients determined with the match potential method (MPM) indicate that the interference from inorganic and organic anions is very small. The proposed sensor shows a fast response time of approximately 15 s. It was applied as an indicator electrode in titration of iodide with Ag+. 相似文献
14.
Electrochemical properties of Meldola's Blue immobilized on silica-titania phosphate prepared by the sol-gel method 总被引:2,自引:0,他引:2
The mixed oxide phosphate (≡SiO)2Ti(O3POH)2 having a specific surface area of SBET= 595 m2 g−1 and an average pore volume of 0.43 mL g−1 was prepared by the sol-gel processing method. The material showed the following characteristics: Ti=11.6 wt% and P=10.5 wt%;
ion exchange capacity of 0.60 mmol g−1. Meldola's Blue (MLB) dye was adsorbed, by an ion exchange reaction, from an aqueous solution in a quantity of 0.62 mmol
g−1. The dye was strongly retained and was not easily leached from the matrix even in presence of 0.5 M electrolyte solution.
Changing the solution pH between 2.5 and 7.0, the midpoint potential of the dye-adsorbed (≡SiO)2 Ti(O3POMLB)2 matrix carbon paste electrode remained practically constant, i.e. about 20 mV vs. SCE. This is not the usual behaviour of
MLB since its midpoint potential changes considerably in solution phase as the pH is changed. The modified electrode has proved
to be stable and electrocatalytically active for hydrazine oxidation at pH 6.
Received: 22 June 1999 / Accepted: 7 September 1999 相似文献
15.
Binding of a cationic surfactant ion, dodecylpyridinium ion, to poly(acrylic acids) of low charge densities was examined
by potentiometry using surfactant-selective electrodes in the solutions, where the pH was kept constant by employing a pH
buffering system. The binding of the surfactant counterions was thus able to be studied at a constant pH during the binding
process. The binding took place in two steps, the first cooperative binding step and the second gradual binding step. The
critical association concentration decreased as the pH increased, indicating the predominant role of the electric interaction
in the binding. The binding isotherms obtained at different but constant pH values were analyzed by the matrix method, taking
into account the nearest-neighbor interactions among three different kinds of sites on the polymer: ionized, protonated, and
surfactant-bound. The theoretical analysis could describe only the first step but could not explain the second step. A relatively
large cooperativity parameter, u, was found for the first step and it can be between 3 × 103 and 1 × 104. When the ionic strength was decreased tenfold, the cooperativity of the binding decreased (u∼1 × 103). The binding constants of the isolated site were 5.5–6.0 × 104 kg mol−1 and slightly increased to 6.5 × 104 kg mol−1 as the ionic strength decreased. The deviation of the second step from the theoretical analysis was supposed to arise from
a change of proton dissociation constant in the nonpolar space formed by the bound surfactants.
Received: 29 November 2000/Accepted: 24 January 2001 相似文献
16.
The construction, performance characteristics and applications of a polymeric membrance electrode for lead(II) ion are reported.
The electrode was prepared by incorporating cryptand(222) as the neutral carrier into a plasticized poly(vinyl chloride) membrane.
The influence of membrane composition, pH and concentration of internal reference solution were investigated. The electrode
exhibits a potentiometric response for Pb2+ ion over the concentration range 10–1–10–5 M with a detection limit of 5 × 10–6 M Pb2+. It shows a relatively fast response time of about 30 s and can be used for about two months without any considerable divergence
in potential. The proposed sensor revealed good selectivities for Pb2+ in the presence of several metal ions and could be used in the pH range of 2.5 to 7.5. It was used as an indicator electrode
in the potentiometric titration of Pb2+ with EDTA.
Received: 20 November 1998 / Revised: 26 March 1999 / Accepted: 31 March 1999 相似文献
17.
The construction, performance characteristics and applications of a polymeric membrance electrode for lead(II) ion are reported.
The electrode was prepared by incorporating cryptand(222) as the neutral carrier into a plasticized poly(vinyl chloride) membrane.
The influence of membrane composition, pH and concentration of internal reference solution were investigated. The electrode
exhibits a potentiometric response for Pb2+ ion over the concentration range 10–1–10–5 M with a detection limit of 5 × 10–6 M Pb2+. It shows a relatively fast response time of about 30 s and can be used for about two months without any considerable divergence
in potential. The proposed sensor revealed good selectivities for Pb2+ in the presence of several metal ions and could be used in the pH range of 2.5 to 7.5. It was used as an indicator electrode
in the potentiometric titration of Pb2+ with EDTA.
Received: 20 November 1998 / Revised: 26 March 1999 / Accepted: 31 March 1999 相似文献
18.
Ashraf A. Mohamed 《Monatshefte für Chemie / Chemical Monthly》2001,56(2):919-928
A new selective, sensitive, and simple kinetic method is developed for the determination of trace amounts of iodide. The method is based on the catalytic effect of iodide on the reaction of triflupromazine (TFP) with H2O2. The reaction is followed spectrophotometrically by tracing the oxidation product at 498 nm within 1 min after addition of H2O2. The optimum reaction conditions are TFP (0.4 × 10−3 M), H2SO4 (1.0M), H3PO4 (2.0M), and H2O2 (1.6M) at 30°C. Following this procedure, iodide can be determined with a linear calibration graph up to 4.5 ng ċ cm−3 and a detection limit of 0.04 ng ċ cm−3, based on the 3 Sb criterion. The method can also be applied to the determination of iodate and periodate ions. Determination of as little as 0.2, 1.0, 2.0, and 4.0 ng ċ cm−3 of I−, IO3 -, or IO4 - in aqueous solutions gave an average recovery of 98% with relative standard deviations below 1.6% (n = 5). The method was applied to the determination of iodide in Nile river water and ground waters as well as in various food samples after alkaline ashing treatment. The method is compared with other catalytic spectrophotometric procedures for iodide determination. 相似文献
19.
Krishnapillai Girish Kumar Remalakshmy Poduval Sareena John Pearl Augustine 《Mikrochimica acta》2006,156(3-4):283-287
A new PVC membrane sensor, which is highly selective towards Ni (II) ions, has been developed using a thiophene-derivative
Schiff base as the ionophore. The best performance was exhibited by the membrane having the composition percentage ratio of
5:3:61:31 (ionophore:NaTPB:DBP:PVC) (w/w), where NaTPB is the anion excluder, sodium tetraphenylborate and DBP is the plasticizing
agent (dibutyl phthalate). The membrane exhibited a good Nernstian response for nickel ions over the concentration range of
1.0 × 10−1–5.0 × 10−6 M (limit of detection is 1.8 × 10−6 M) with a slope of 29.5 ± 1.0 mV per decade of activity. It has a fast response time of <20 s and can be used for a period
of 4 months with good reproducibility. The sensor is suitable for use in aqueous solutions of a wide pH range of 3.2–7.9.
The sensor shows high selectivity to nickel ions over a large number of mono-, bi- and trivalent cations. It has been successfully
used as an indicator electrode in the potentiometric titration of nickel ions against EDTA and also for direct determination
of nickel content in real samples – wastewater samples from electroplating industries and Indian chocolates. 相似文献
20.
A PVC membrane electrode for iodide ions based on Cu(I)-bathocuproine as ionophore in membrane composition is prepared. The electrode exhibits a linear response over a wide concentration range 5.0×10−6 to 2.0×10−1 mol l−1 with a detection limit 1.0×10−6 mol l−1. The proposed membrane electrode shows Nernstian behavior with a slope of −56.8 mV/decade, a fast response time 10 s and a lifetime at least 3 months. Iodide-selective electrode reveals good selectivities for iodide ion over a wide variety of the other anions and can be used in pH range of 3-9. It can also be used as an indicator electrode in potentiometric titration of iodide ion. 相似文献