Fabrication Of Potentiometric Sensors For The Determination Of Certain Metal Ions

In this study Fabrication of Potentiometric sensors for the determination of certain metal ions, presents the synthesis and characterization of seven ionophores, their use in the fabrication of potentiometric sensors and the results and discussion of fourteen sensors developed for the determination of five transition metal ions. As part of the present investigations a total of fourteen potentiometric sensors have been developed and fabricated. A three fold approach has been taken in developing he sensors, PVC plasticized membrane sensor, carbon paste electrode and chemically modified carbon paste electrode. All the sensors are highly useful in the determination of metal ions such as manganese, nickel, copper, mercury and lead. A through analytical study has been carried out with respect to each other developed. Based on these studies, optimum conditions have been developed for the quantitative determinations of the selected metal ions using the sensors. Systematic application studies have also been carried out for all the developed sensors and the results revealed that the presently developed sensors are far superior than most of the sensors reported.

A Novel Potentiometric Sensor for the Determination of Nimesulide

A novel electrochemical sensor has been developed for the determination of nimesulide. The sensor is based on the NIM- molybdophosphoric acid (MPA) as the electroactive material in PVC matrix in presence of bis(2-ethyl hexyl) phthalate (BEP) as a plasticizer. The sensor showed a fast, stable, near Nernstian response for 1 × 10-2 –1 × 10-6 M NIM over the pH range 5 – 8 with a slope 55.6 ±0.5m V/decade and the response time is < 45 s. Selectivity coefficient data for some common ions show negligible interferences. The sensor was successfully applied for the determination of NIM in tablet and the results obtained are in good agreement with those obtained by the official method.

A Chloride Ion-Selective Potentiometric Sensor Based on a Polymeric Schiff Base Complex

This paper describes the fabrication of an ion-selective electrode in which a polymeric Schiff base complex of cobalt(II) is used as the ionophore.The main advantage of the electrode is that it is mechanically stable upto 3 months..The electrode shows a linear response in the range of 2.5 × 10-5-0.5 × 10-1 mol dm-3. The response time of the electrode is 30 s.The pH range at which the electrode works is 3.8 to 6.8. The electrode was found to be selective towards chloride ion in the presence of ions like Na+, Ca2+, Mn2+, ,Fe3+, Co2+, Ni2+, Cu2+, Zn2+, CH3COO-, NO3-, SO42- ,Br- and NO2-.

PVC Supported Liquid Membrane and Carbon Paste Potentiometric Sensors Incorporating a Mn(III)-Porphyrin for the Direct Determination of Undissociated Paracetamol

PVC supported liquid membrane and carbon paste potentiometric sensors incorporating an Mn(III)-porphyrin complex as a neutral host molecule were developed for the determination of paracetamol. The measurements were carried out in solution at pH 5.5. Under such conditions paracetamol exists as a neutral molecule. The mechanism of molecular recognition between the Mn(III)-porphyrin and paracetamol, leading to potentiometric signal generation, is discussed.The sensitivity and selectivity toward paracetamol of carbon paste and polymeric liquid membrane electrodes incorporating an Mn(III)-porphyrin host were compared. The applicability of these sensors to the direct determination of paracetamol was checked by performing a recovery test in human plasma.

Fabrication of Potentiometric Sensors for the Selective Determination of Ketoconazole

The fabrication and analytical applications of two types of potentiometric sensors for the determination of ketoconazole (KET) are described. The sensors are based on the use of KET-molybdophosphoric acid (MPA) ion pair as electroactive material. The fabricated sensors include both polymer membrane and carbon paste electrodes. Both sensors showed a linear, stable and near Nernstian slope of 57.8mV=decade and 55.2mV=decade for PVC membrane and carbon paste sensors respectively over a relatively wide range of KET concentration (1×10-2-5×10-5 and 1×10-2-1×10-6). The sensors showed a fast response time of <30 sec and <45 sec. A useful pH range of 3–6 was obtained for both types of sensors. A detection limit of 2.96 10 5M was obtained for PVC membrane sensor and 6.91 10 6M was obtained for carbon paste sensor. The proposed sensors proved to have a good selectivity for KET with respect to a large number of ions. The proposed sensors were successfully applied for the determination of KET in pharmaceutical formulations. The results obtained are in good agreement with the values obtained by the standard method.

Fabrication of Potentiometric Sensors for the Determination of Lanthanide Ions

In many fields such as earth science biology, environment and electronics, the knowledge about elemental distributions and chemical speciation is important. The determination of metal levels especially the toxic ones both in the environment and in biological materials are increasingly demanded by the society.Ion selective sensors have become one of the most effective ad powerful means for analytical scientists for the trace level monitoring of metal ions. The wide range of applications ,low material requirements and simplicity of analytical procedure have not only brought ion-selective electrodes in to the lime light of analytical chemistry,but have promoted their use as tools for physiologists,medical researchers,biologists,geologists,environmental protection specialists etc.Potentiometric ion-selective sensors have been developed for the determination of lanthanide ions such as La3+,Nd3+,Pr3+,Sm3+, and Gd3+.The sensors fabricated include both PVC membrane sensor and chemically modified carbon paste sensor. A set of 10 sensors have been developed. The response parameters of all the sensors have been studied and the sensors were applied as an indicator electrode in the potentiometric titration and for the determination of metal ions in real samples.

Novel potentiometric sensors for the selective determination of domperidone

The fabrication and electrochemical response characteristics of two novel potentiometric sensors for the selective determination of domperidone (DOM) are described. The two fabricated sensors incorporate DOM–PTA (phosphotungstic acid) ion pair as the electroactive material. The sensors include a PVC membrane sensor and a carbon paste sensor. The sensors showed a linear, stable, and near Nernstian slope of 56.5 and 57.8 mV/decade for PVC membrane and carbon paste sensors, respectively over a relatively wide range of DOM concentration (1.0 9 10-1–1.0 9 10-5 and 1.0 9 10-1–3.55 9 10-6 M). The response time of DOM–PTA membrane sensor was less than 25 s and that in the case of carbon paste sensor was less than 20 s.Auseful pH range of 4–6 was obtained for both types of sensors. A detection limit of 7.36 9 10-5 M was obtained for PVC membrane sensor and 1.0 9 10-6 M was obtained for carbon paste sensor. The proposed sensors showed very good selectivity toDOMin the presence of a large number of other interfering ions. The analytical application of the developed sensors in the determination of the drug in pharmaceutical formulations such as tablets was investigated. The results obtained are in good agreement with the values obtained by the standard method. The sensors were also applied for the determination ofDOMin real samples such as urine by the standard addition method.

A PVC plasticized membrane sensor for nickel ions

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 6M (limit of detection is 1.8 10 6 M) with a slope of 29.5 1.0mV 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.

A PVC Plasticized Membrane Sensor for Nickel Ions

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 6M (limit of detection is 1.8 10 6 M) with a slope of 29.5 1.0mV 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.

A PVC Plasticized Sensor for Ni(II) Ion Based on a Simple Ethylenediamine Derivative

new PVC membrane ion selective electrode which is highly selective towards Ni(II) ions was constructed using a Schiff base containing a binaphthyl moiety as the ionophore. The sensor exhibited a good Nernstian response for nickel ions over the concentration range 1.0 × 10–1 – 5.0 × 10–6 M with a lower limit of detection of 1.3 × 10–6 M. It has a fast response time and can be used for a period of 4 months with a good reproducibility. The sensor is suitable for use in aqueous solutions in a wide pH range of 3.6 – 7.4 and works satisfactorily in the presence of 25% (v/v) methanol or ethanol. The sensor shows high selectivity to nickel ions over a wide variety of cations. It has been successfully used as an indicator electrode in the potentiometric titration of nickel ions against EDTA and also for the direct determination of nickel content in real samples: effluent samples, chocolates and hydrogenated oils.

Development of Electrochemical Sensors for the Determination of Certain Pharmaceuticals

The quality of a drug is determined after establishing its authenticity by testing its purity and quality of the pure substance in the drug and its formulations.Ion selective sensors have become one of the most effective and powerful means for analytical scientists in the determination of drug substances and are playing an increasing role in pharmaceutical analysis.ISEs are cost effective,easy to prepare and can be rapidly manipulated . Potentiometric ion selective sensors have been developed for six drugs namely trimethoprim, ketoconazole, lamivudine, domperidon, nimesulide and Lomefloxacin. The sensors fabricated include both PVC membrane sensor as well as carbon paste sensor. A total of sixteen different sensors have been developed. The response parameters of all the sensors have been studied and the sensors were applied to the determination of the drugs in pharmaceutical formulations and also in real samples like urine.

Fabrication of Electrochemical Sensors for Pharmaceutical Analysis

Potentiometric chemical sensors,an important class of electro-chemical sensors are widely used in pharmaceutical analysis because of its inherent advantages.The present study was aimed at fabrication of potentiometric sensors for the drugs mebendazole,pefloxacin,ambroxol,sildenafil citrate,dextro-methorphan and tetracycline.A total of 18 sensors have been developed for the determination of theses drugs.The major step in the fabrication of the sensor was the preparation of the ion association.Two types of sensors viz:PVC membrane sensor and carbon paste electode (CPE) were fabricated.The response characteristics of the different sensors fabricated were studied.Various response parameters studied include response time,selectivity and the effect of pH.The developed sensors were also employed for the determination of the drugs in pharmaceutical formulations and also for the recovery of the drug from urine samples.The selectivity studies reveal that the developed sensors are highly selective to the drug even in prescence of foreign ions.

Synthesis,characterization and application studies of some polymer supported metal complexes

Polymer supports are efficient reagents,substrates and catalysts and they are extensively used for carrying out reactions at controlled rates.Tailor-made polymer supports are highly versatile which have opened an excellent area of research.Now polymer supported chemistry is being exploited at an amazing rate and it seems to join the routine world of organic synthesis.Polymer supported ligands are found to be efficient complexing agents whose high selectivity enables the analysis and removal of heavy metal ions which are toxic to all the living organisms of land and sea.polymer supported membranes function as ion selective potentiometric sensors which allow the exchange of specific ions among other ions of the same charge.In this investigation three series of polymeric schiff bases and three series of metal complexes have been prepared.An attempt is done to develop optimum conditions for the removal of heavy metal ions using polymeric schiff bases.A novel copper sensor electrode have also been prepared from polymer supported metal complex.

Development of Macrocyclics based Electrochemical Sensors

Electroanalytical techniques represent a class of powerful and versatile analytical method which is based on the electrical properties of a solution of the analyte when it is made part of an electrochemical cell. They offer high sensitivity, accuracy, precision and a large linear dynamic range. The cost of instrumentation is relatively low compared to other instrumental methods of analysis. Many solid state electrochemical sensors have been commercialised nowadays. Potentiometry is a very simple electroanalytical technique with extraordinary analytical capabilities. Since valinomycin was introduced as an ionophore for K+, Ion Selective Electrodes have become one of the best studied and understood analytical devices. It can be used for the determination of substances ranging from simple inorganic ions to complex organic molecules. It is a very attractive option owing to the wide range of applications and ease of the use of the instruments employed. They also possess the advantages of short response time, high selectivity and very low detection limits. Moreover, analysis by these electrodes is non-destructive and adaptable to small sample volumes. It has become a standard technique for medical researchers, biologists, geologists and environmental specialists. This thesis presents the synthesis and characterisation of five ionophores. Based on these ionophores, nine potentiometric sensors are fabricated for the determination of ions such as Pb2+, Mn2+, Ni2+, Cu2+ and Sal- ion (Salicylate ion). The electrochemical characterisation and analytical application studies of the developed sensors are also described. The thesis is divided into eight chapters

Synthesis, Characterization and Applications of Hybrid Nanocomposites of TiO2 With Conducting Polymers

A nanocomposite is a multiphase solid material where one of the phases has one, two or three dimensions of less than 100 nanometers (nm), or structures having nano-scale repeat distances between the different phases that make up the material. In the broadest sense this definition can include porous media, colloids, gels and copolymers, but is more usually taken to mean the solid combination of a bulk matrix and nano-dimensional phase(s) differing in properties due to dissimilarities in structure and chemistry. The mechanical, electrical, thermal, optical, electrochemical, catalytic properties of the nanocomposite will differ markedly from that of the component materials. Size limits for these effects have been proposed, <5 nm for catalytic activity, <20 nm for making a hard magnetic material soft, <50 nm for refractive index changes, and <100 nm for achieving superparamagnetism, mechanical strengthening or restricting matrix dislocation movement. Conducting polymers have attracted much attention due to high electrical conductivity, ease of preparation, good environmental stability and wide variety of applications in light-emitting, biosensor chemical sensor, separation membrane and electronic devices. The most widely studied conducting polymers are polypyrrole, polyaniline, polythiophene etc. Conducting polymers provide tremendous scope for tuning of their electrical conductivity from semiconducting to metallic region by way of doping and are organic electro chromic materials with chemically active surface. But they are chemically very sensitive and have poor mechanical properties and thus possessing a processibility problem. Nanomaterial shows the presence of more sites for surface reactivity, they possess good mechanical properties and good dispersant too. Thus nanocomposites formed by combining conducting polymers and inorganic oxide nanoparticles possess the good properties of both the constituents and thus enhanced their utility. The properties of such type of nanocomposite are strongly depending on concentration of nanomaterials to be added. Conducting polymer composites is some suitable composition of a conducting polymer with one or more inorganic nanoparticles so that their desirable properties are combined successfully. The composites of core shell metal oxide particles-conducting polymer combine the electrical properties of the polymer shell and the magnetic, optical, electrical or catalytic characteristics of the metal oxide core, which could greatly widen their applicability in the fields of catalysis, electronics and optics. Moreover nanocomposite material composed of conducting polymers & oxides have open more field of application such as drug delivery, conductive paints, rechargeable batteries, toners in photocopying, smart windows, etc.The present work is mainly focussed on the synthesis, characterization and various application studies of conducting polymer modified TiO2 nanocomposites. The conclusions of the present work are outlined below, Mesoporous TiO2 was prepared by the cationic surfactant P123 assisted hydrothermal synthesis route and conducting polymer modified TiO2 nanocomposites were also prepared via the same technique. All the prepared systems show XRD pattern corresponding to anatase phase of TiO2, which means that there is no phase change occurring even after conducting polymer modification. Raman spectroscopy gives supporting evidence for the XRD results. It also confirms the incorporation of the polymer. The mesoporous nature and surface area of the prepared samples were analysed by N2 adsorption desorption studies and the mesoporous ordering can be confirmed by low angle XRD measurementThe morphology of the prepared samples was obtained from both SEM & TEM. The elemental analysis of the samples was performed by EDX analysisThe hybrid composite formation is confirmed by FT-IR spectroscopy and X-ray photoelectron spectroscopyAll the prepared samples have been used for the photocatalytic degradation of dyes, antibiotic, endocrine disruptors and some other organic pollutants. Photocatalytic antibacterial activity studies were also performed using the prepared systemsAll the prepared samples have been used for the photocatalytic degradation of dyes, antibiotic, endocrine disruptors and some other organic pollutants. Photocatalytic antibacterial activity studies were also performed using the prepared systems Polyaniline modified TiO2 nanocomposite systems were found to have good antibacterial activity. Thermal diffusivity studies of the polyaniline modified systems were carried out using thermal lens technique. It is observed that as the amount of polyaniline in the composite increases the thermal diffusivity also increases. The prepared systems can be used as an excellent coolant in various industrial purposes. Nonlinear optical properties (3rd order nonlinearity) of the polyaniline modified systems were studied using Z scan technique. The prepared materials can be used for optical limiting Applications. Lasing studies of polyaniline modified TiO2 systems were carried out and the studies reveal that TiO2 - Polyaniline composite is a potential dye laser gain medium.