Flow injection potentiometric determination of amitriptyline hydrochloride

New plastic membrane electrodes for amitriptyline hydrochloride (AmCl) based on amitriptylinium phosphotungstate (Am-PTA); amitriptylinium phosphomolybdate (Am-PMA) and a mixture of both (Am-PTA/PMA) were prepared. The electrodes were fully characterized in terms of their composition, life span, pH and temperature and then were applied to the potentiometric determination of the amitriptylinium ion in its pure state and pharmaceutical preparations and flow injection conditions. The selectivity of the electrodes towards many inorganic cations, sugars and amino acids was also tested.     

Flow injection potentiometric determination of clobutinol hydrochloride

New clobutinol (Clob) ion-selective polyvinyl chloride (PVC) membrane electrodes, based on the ion-associates of Clob with phosphotungstic acid or phosphomolybdic acid were prepared using dibutyl phthalate as plasticizing solvent. The electrodes were characterized in terms of membrane composition, temperature and pH. The sensors showed a near-Nernstian response over the concentration ranges (6.31 × 10⁻⁶)-(1.00 × 10⁻²) and (5.01 × 10⁻⁵)-(1.00 × 10⁻²) M in the case of clobutinol-phosphotungstate ((Clob)₃-PT) applying batch and flow injection (FI) analysis, respectively, and (1.58 × 10⁻⁵)-(1.00 × 10⁻²) and (5.01 × 10⁻⁵)-(1.00 × 10⁻²) M in case of clobutinol-phosphomolybdate ((Clob)₃-PM) for batch and FI analysis systems, respectively. The electrodes were successfully applied for the potentiometric determination of ClobCl in pharmaceutical preparation and urine in steady state and flow injection conditions. The electrodes exhibit good selectivity for Clob with respect to a large number of inorganic cations, sugars and amino acids.     

Flow injection potentiometric determination of pipazethate hydrochloride

New plastic membrane electrodes for pipazethate hydrochloride based on pipazethatium phosphotungstate, pipazethatium phosphomolybdate and a mixture of the two were prepared. The electrodes were fully characterized in terms of composition, life span, pH and temperature and were then applied to the potentiometric determination of the pipazethate ion in its pure state and pharmaceutical preparations under batch and flow injection conditions. The selectivity of the electrodes towards many inorganic cations, sugars and amino acids was also tested.     

Flow injection potentiometric sensor for determination of phenylpropanolamine hydrochloride

A new polymeric membrane electrode has been constructed for the determination of phenylpropanolamine hydrochloride. The electrode was prepared by solubilizing the phenylpropanolamine-phosphomolybdate ion associate into a polyvinyl chloride matrix plasticized by dibutylphthalate as a solvent mediator. The electrode showed near-Nernstian response over the concentration range of 1 × 10^?5–1 × 10^?2 M with low detection limit of 6.3 × 10^?6 M. The electrode displays a good selectivity for phenylpropanolamine with respect to a number of common inorganic and organic species. The electrode was successfully applied to the potentiometric determination of phenylpropanolamine ion in its pure state and its pharmaceutical preparation in batch and flow injection conditions.     

Potentiometric determination of saccharin in dietary products using mercurous nitrate as titrant

A rapid, precise and low cost method for saccharin determination in dietary products is proposed. Saccharin in several samples is potentiometrically titrated with mercurous nitrate solution using a silver wire coated with a metallic mercury film as the working electrode, and the end point was found using a Gran's plot. The detection limit of sodium saccharin was 0.5 mg/ml and the best pH range was from 2.0 to 3.5. Sucrose, glucose, aspartame, sodium cyclamate, sorbitol, fructose, benzoic acid, salicylic acid and lactose do not interfere even in significant amounts. The interference due to the presence of chloride and/or phosphate ions can be eliminated by previous solvent extraction of this sweetener. Recovery of saccharin from various dietary products gave from 95.2 to 103.2% of the label claim.     

A simple turbidimetric flow injection system for saccharin determination in sweetener products

A new method for saccharin determination in liquid sweetener products was developed. The method is based on the precipitation reaction of Ag(I) ions with saccharin in aqueous medium (pH 3.0), using a flow injection analysis system with merging zones, the suspension was stabilized with 5 g L⁻¹ Triton X-100. All experimental parameters influencing the flow injection system were optimized by means of chemometric approaches. The linear analytical curve was built from 2.4 g L⁻¹ up to 9.64 g L⁻¹ (r = 0.9968) with a quantification limit of 2.40 g L⁻¹. The precision assessed as relative standard deviation (n = 10) was found to be 1.75 % for the saccharin concentration of 7.20 g L⁻¹. Based on interference studies performed with the substances commonly found in liquid sweeteners, such as sodium cyclamate, methylparaben, sodium aspartame, and benzoic and citric acids, at the analyte to interferent mole ratio of up to 1: 10, no interference with the saccharin determination was observed. The presence of chloride ions interferes with the method, but a preceding liquid-liquid saccharin extraction with ethyl acetate was successfully employed to overcome this drawback. Accuracy of the method in sweetener products was evaluated by a comparison with the HPLC method.     

Flow injection potentiometric determination of paraquat in formulations and biological samples

A flow injection potentiometric method for the rapid determination of paraquat in herbicide formulations and biological samples is described. It is based on the utilization of a flow-through potentiometric detector containing polyvinyl chloride-immobilised octamethylcyclotetrasiloxane, a lipophilic plasticizer (tetra-n-undecyl 3,3′,4,4′-benzophenone tetracarboxylate) and membrane additive potassium tetrakis(4-chlorophenyl)borate. The detector was minimally interfered by the presence of constituents such as Na⁺, K⁺, Ca²⁺, Mg²⁺, glucose, urea, lactic and citric acids at physiological levels, respectively. Good correlation between results of the proposed method and HPLC for the formulation samples was found, while results for the determination of paraquat in biological samples such as urine, vomitus and stomach washout was less satisfactory.     

Flow injection differential potentiometric determination of lysine by using a lysine biosensor

This paper describes a method for the determination of lysine based on a flow injection (FI) differential potentiometry system. The flow injection manifold is composed of a support electrolyte solution channel and a water channel acting as a carrier into which the sample solution is injected. The lysine biosensor was consisted of lysine oxidase chemically immobilized on a nylon membrane and attached to an all-solid-state ammonium electrode. A circular ammonium electrode was used as a reference. Hence, the possible interference of endogenous ammonium can be partly corrected by differential potentiometry. In order to increase the sensitivity of the response, the reaction was kinetically developed following a stopped-flow method. As a result, the sensitivity increased from 20 to 40 mV per decade when comparing the FI and the stopped-flow values. Furthermore, the peak-to-peak stopped-flow signals generated can be used as a more selective analytical response for lysine. The quantification of lysine in mixture samples containing small amounts of ammonium can be achieved with an acceptable accuracy, with prediction errors lower than 4%. However, when the ammonium concentration exceeded the lysine concentration, multivariate calibration with non-linear partial least squares (PLS) regression was needed to improve the lysine quantification, with an overall prediction error around 10%.     

Flow injection potentiometric stripping analysis and potentiometric stripping coulometry

Summary Potentiometric Stripping Analysis is used as a detection method for Flow Injection Analysis. A wall-jet glassy carbon disc electrode is applied for the determination of zinc, cadmium, and lead. Microliter samples are sufficient for high-speed determination in the ng-range. The sample throughout is up to 180 per hour depending on the metal ion concentration. The influence of various parameters on the stripping time is investigated.In addition the new concept of Potentiometric Stripping Coulometry is presented. Based on Faraday's law the measured stripping time can be used to calculate the mass of deposited metal. Provided that the deposition is complete the value found is identical to the mass totally present in the sample. Using lead as an example the accuracy of the determination is demonstrated for the wall-jet electrode. The application of a porous carbon felt electrode increases the speed of deposition. Optimum parameters are given for exhaustive depletion.

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Fließinjektion zur potentiometrischen Stripping-Analyse und potentiometrischen Stripping-Coulometrie

Zusammenfassung Die potentiometrische Stripping-Analyse wird zur Detektion in der Fließinjektionsanalyse eingesetzt. Zur Bestimmung von Zink, Cadmium und Blei wird eine Wall-Jet Scheibenelektrode aus Glaskohlenstoff verwendet. Bei Injektion vonl-Mengen sind Schnellbestimmungen im ng-Bereich möglich. Je nach Metallionenkonzentration läßt sich ein Probendurchsatz von bis zu 180 pro Stunde erreichen. Der Einfluß verschiedener Parameter auf die Strippingzeit wird untersucht. Weiterhin wird das neue Konzept der potentiometrischen Stripping-Coulometrie vorgestellt. Die abgeschiedene Metallmasse kann aus der gemessenen Strippingzeit und dem zu berechnenden Oxydationsstrom ermittelt werden. Nach vollständiger Abscheidung ist diese Masse der gesamten in der Probe enthaltenen Masse gleich. Am Beispiel einer Bleibestimmung mit der Wall-Jet-Elektrode wird die Richtigkeit dieser Methode belegt. Durch die Verwendung einer Carbonfilzelektrode wird die Geschwindigkeit der vollständigen Abscheidung erhöht. Der Einfluß von Flußrate und injizierter Menge wird untersucht.

     

Flow injection analysis of fluoride in electroplating baths with potentiometric detection

A high dispersion FIA system with a fluoride selective and a double junction reference electrode in cascade arrangement was developed for the determination of the fluoride content in chromium electroplating baths. The analyses of seven synthetic baths prepared in the laboratory and two samples provided by the industry gave results with a mean recovery value of 100.5%, and a mean variation coefficient of 1.6%. These data were better than those obtained by the EDTA complexometric titration, the reference technique, with a mean recovery of 94.0% and a mean variation coefficient of 7.5%. The sampling rate for the FIA manifold was 20 samples per hour.     

Flow injection analysis of fluoride in electroplating baths with potentiometric detection

A high dispersion FIA system with a fluoride selective and a double junction reference electrode in cascade arrangement was developed for the determination of the fluoride content in chromium electroplating baths. The analyses of seven synthetic baths prepared in the laboratory and two samples provided by the industry gave results with a mean recovery value of 100.5%, and a mean variation coefficient of 1.6%. These data were better than those obtained by the EDTA complexometric titration, the reference technique, with a mean recovery of 94.0% and a mean variation coefficient of 7.5%. The sampling rate for the FIA manifold was 20 samples per hour. Received: 27 November 1997 / Revised: 24 February 1998 / Accepted: 1 March 1998     

Flow injection determination of anisidine value in palm oil samples using a triiodide potentiometric detector

A flow injection analysis (FIA) procedure for the determination of anisidine value (AV) in palm olein using a triiodide detector is described. Undiluted oil sample and chloramine-T reagent were added to a reaction chamber, and reaction was accelerated by applying a short vortex action (typically for 30 s). After allowing the emulsified oil phase to be separated from the aqueous phase (bottom layer), an aliquot of the aqueous phase (containing unreacted chloramine-T) was aspirated into a carrier stream that contained I⁻ where the chloramine-T oxidized the I⁻ to form I₃⁻ which was finally detected by a flow-through triiodide potentiometric detector. Variables that affect the FIA signals such as size of the reaction chamber, oil and reagent flow rates, chloramine-T concentration, vortex time, time for phase separation, carrier stream pH and injected volume were studied. The optimized FIA procedure is linear over 1.0-23.0 AV. The method exhibits good repeatabililty (R.S.D. of ±3.16% (n = 4) for the determination of 5.0 AV) and a sampling rate of 40 samples per hour was achieved. Good correlation (r² = 0.996 (n = 4)) between the proposed method and the manual American Oil Chemists’ Society procedure was found when applied to the determination of twenty different types of palm olein samples.     

Flow injection potentiometric determination of pancuronium bromide in pharmaceutical preparation and urine samples using modified carbon paste electrodes

Carbon paste electrodes for pancuronium bromide was prepared based on ion association complexes of pancuronium bromide with sodium tetraphenylborate (NaTPB) or ammonium reineckate using dibutyl phthalate as solvent mediator and tetradodecylammonium tetrakis-(4-chlorophenyl)borate (ETH 500) as lipophilic additive. The sensors showed a near-Nernstian slope of 28.1 mV concentration decade(-1) at 25°C within the concentration range 6.31×10(-6)-1.00×10(-2) M in case of pancuronium-tetraphenylborate electrode and 26.6 mV concentration decade(-1) in the concentration range 5.66×10(-5)-1.00×10(-2) M in case of pancuronium-reineckate electrode. The sensors were successfully applied for the potentiometric determination of pancuronium bromide in pharmaceutical preparation and biological fluids in batch and flow injection conditions.     

Flow injection determination of hydrazine with fluorimetric detection

A spectrophotometric flow injection system is described for the determination of hydrazine, involving oxidation of hydrazine by thallium(III) with concomitant formation of thallium(I). The optimum analytical conditions have been established. The linear range for hydrazine is 25-500 ng ml(-1) with a detection limit of 20 ng ml(-1). The sampling frequency is 40+/-5 samples h(-1). The relative standard deviation for 100, 250 and 500 ng ml(-1) is 3.5, 2.6 and 1.8%, respectively. The method has been applied to the determination of hydrazine in water.     

Sequential injection with lab-at-valve (LAV) approach for potentiometric determination of chloride

Sequential injection with “Lab-at-Valve (LAV)” approach is demonstrated for potentiometric determination of chloride. The LAV flow-through electrode system consists of two Ag/AgCl electrodes: one as a reference electrode, silver chloride activated surface-silver wire soaked in a constant-concentration chloride ion solution in a small tube covered with a polymer-membrane, another as a working electrode (a similar silver chloride activated surface-silver wire) placed in a flow channel. The electrode system is attached at one port of a 10 port multiposition valve. A modified autoburette was used as a propelling device. Using SI operation via a program written in-house, based on LabVIEW^®, a standard/sample is inserted, via the selection valve, in potassium nitrate as an electrolyte and water is used as a carrier. The zones are transported from the holding coil to the flow cell to monitor the difference in potential due to concentration cell behavior. The potential difference is then recorded as a peak. Peak height is proportional to logarithm of chloride concentration. The SI-LAV for chloride determination is very simple, fast, precise, accurate, automatic and economical. Applications to mineral drinking water and surface water have been made. The results agree with those of IC and titrimetric methods.     

Flow injection potentiometric detection of trimethylamine in seafood using tungsten oxide electrode

A simple flow injection gas/diffusion method for the determination of trimethylamine (TMA) in seafood with potentiometric detection using tungsten oxide electrode has been developed. The method is based on the diffusion of TMA through a PTFE membrane from a sodium hydroxide donor stream to a phosphate buffer acceptor stream. The TMA in the acceptor stream passes through an electrochemical flow cell containing a tungsten oxide wire and a silver/silver chloride electrode, where TMA was sensitively detected. The parameters affecting the sensitivity of the electrode such as sodium hydroxide concentration, buffer concentration, pH, flow rate and injected volume were studied in details. The electrode response was linear in the concentration range from 1 to 10 μg ml⁻¹ TMA with a correlation coefficient (R²) of 0.991 and a detection limit of 0.05 μg ml⁻¹ TMA. The intra- and inter-days precision (R.S.D.) was found to be, respectively, 1.20 and 1.6% (n=6). The method was applied to the determination of TMA in fish tissue and recoveries of 99-100% were obtained for fish extracts. Results were in close agreement with those obtained by the existing classical official method. Common interference from those species that can diffuse through the membrane were removed by the addition of formaldehyde to the seafood extract. The method is simple, feasible with satisfactory accuracy and precision and thus, could be used for monitoring seafood quality with a sampling rate of 20±2 sample h⁻¹.     

Flow injection amperometric determination of hydrogen peroxide in household commercial products with a ruthenium oxide hexacyanoferrate modified electrode

Hydrogen peroxide was determined in oral antiseptic and bleach samples using a flow-injection system with amperometric detection. A glassy carbon electrode modified by electrochemical deposition of ruthenium oxide hexacyanoferrate was used as working electrode and a homemade Ag/AgCl (saturated KCl) electrode and a platinum wire were used as reference and counter electrodes, respectively. The electrocatalytic reduction process allowed the determination of hydrogen peroxide at 0.0 V. A linear relationship between the cathodic peak current and concentration of hydrogen peroxide was obtained in the range 10–5000 μmol L^?1 with detection and quantification limits of 1.7 (S/N?=?3) and 5.9 (S/N?=?10) μmol L^?1, respectively. The repeatability of the method was evaluated using a 500 μmol L^?1 hydrogen peroxide solution, the value obtained being 1.6% (n?=?14). A sampling rate of 112 samples h^?1 was achieved at optimised conditions. The method was employed for the quantification of hydrogen peroxide in two commercial samples and the results were in agreement with those obtained by using a recommended procedure.     

Flow injection analysis of sulfite ion with a potentiometric titanium phosphate-epoxy based membrane sensor

A novel pH sensor suitable for use in both aqueous and non-aqueous mediums is reported. The sensor is derived from polymer modified electrode obtained from electrochemical polymerisation of aniline in dry acetonitrile containing 0.5 M tetraphenyl borate at 2.0 V versus Ag/AgCl. The light yellow colour polymer modified electrode obtained under the present experimental condition has been characterised by scanning electron microscopy (SEM). The pH sensing of polymer modified electrode in both aqueous and non-aqueous mediums is examined and reported. As the typical examples, we used weak acid (acetic acid) and weak base (ammonium hydroxide) as analytes. The acetic acid is analysed in both aqueous and dry acetonitrile whereas ammonium hydroxide is analysed only in aqueous medium. The analysis in aqueous medium is conducted in 1 mM Tris-HCl buffer pH 7.0 and also in 0.1 M KCl. The slope of pH sensing is calculated from the data recorded in typical buffers and found to be approximately 86 mV per pH. The application of polymer modified electrode for the construction of urea biosensor is described based on immobilised urease within poly vinyl alcohol (PVA) matrix and also within organically modified sol-gel glass on the surface of polymer-modified electrode. The new urea sensor has shown maximum response of 160 mV at 25 degrees C with a lowest detection limit of 20 muM. The performance of new pH sensor and urea sensor has been studied and reported in this communication.     

流动注射化学发光法测定阿莫西林

在碱性介质中,铁氰化钾能够氧化阿莫西林产生微弱的化学发光,Na2SO3对该体系有较强的增敏作用,据此,结合流动注射技术,建立了测定阿莫西林的新方法.阿莫西林在5.0×10-8～2.0×10-5 g/mL范围内与化学发光强度呈良好的线性关系,检出限为3×10-8 g/mL,对2.0×10-6 g/mL的阿莫西林进行11次平行测定,相对标准偏差为1.5%.本法已用于胶囊中阿莫西林的测定,并初步探讨了该化学发光反应的机理.