Preparation and application of a new glucose sensor based on iodide ion selective electrode

An electrode for glucose has been prepared by using an iodide selective electrode with the glucose oxidase enzyme. The iodide selective electrode used was prepared from 10% TDMAI and PVC according our previous study. The enzyme was immobilized on the iodide electrode by holding it at pH 7 phosphate buffer for 10 min at room temperature. The H₂O₂ formed from the reaction of glucose was determined from the decrease of iodide concentration that was present in the reaction cell. The iodide concentration was followed from the change of potential of iodide selective electrode. The potential change was linear in the 4×10⁻⁴ to 4×10⁻³ M glucose concentration (75-650 mg glucose/100ml blood) range. The slope of the linear portion was about 79 mV per decade change in glucose concentration. Glucose contents of some blood samples were determined with the new electrode and consistency was obtained with a colorimetric method. The effects of pH, iodide concentration, the amount of enzyme immobilized and the operating temperature were studied. No interference of ascorbic acid, uric acid, iron(III) and Cu(II) was observed. Since the iodide electrode used was not an AgI-Ag₂S electrode, there was no interference of common ions such as chloride present in biological fluids. The slope of the electrode did not change for about 65 days when used 3 times a day.     

Stripping voltammetry of bromide and iodide ions at a renewal silver electrode

The behavior of bromide and iodide ions at a silver electrode renewed by cutting off a thin 0.5-μm surface layer was studied. The advantage of this method of electrode renewal over some variants of mechanical renewal was demonstrated. It was shown that bromide and iodide ions can be determined in concentration ranges from 10^-6 to 10^-3 M and from 10^-7 to 10^-3 M, respectively. Deceased.     

New method for determining small concentrations of chloride ion

A new method has been devised for the determination of concentrations of chloride ion from approximately 10^-6 to 2·10^-4 M. The test solution is equilibrated with solid silver chloride, the silver ion concentration is determined by potentiometric titration with iodide ion, and the chloride concentration is calculated by the solubility product principle. Chloride concentrations near 10^-6 M can be determined with an accuracy of about ±5%, and at 10^-5 M the error is within ±0.5%. Chloride concentrations above 2-3· 10^-4 M cannot be accurately determined because of the formation of AgCl₂^-.     

Indirect atomic absorption spectrometric determination of mixtures of chloride and iodide by precipitation in an unsegmented flow system

Chloride and iodide are injected into a carrier silver nitrate and the precipitates formed are retained on a stainless-steel filter, so that total chloride and iodide can be determined by the decrease in the atomic absorption signal for silver. The silver chloride precipitate is subsequently dissolved with ammonia and chloride only is determined. Iodide is determined by difference. Mixtures of these anions at μg ml^?1 levels can be determined for chloride/iodide ratios from 7.5:1 to 1:60, with a sampling frequency of ca. 10 h^?1. Applications to the determination of chloride in foodstuffs and wines are described. Up to 10 samples per hour can be handled and 50–100 samples can be run before the filter must be cleaned.     

Kinetic study of the iodate—iodide and chlorate—iodide reactions in acidic solutions,and a method for the microdetermination of bromide

The iodate—iodide and chlorate—iodide reactions were studied spectrophotometrically in acidic solutions by stopped-flow techniques. Intermediate products(I⁺)were followed; reaction rate constants and activation energies of the reactions were determined. A method of determining bromide was developed on the basis of its accelerating effect on the iodate—iodide reaction ; microamounts of bromide in the range 16–320 μg (10^-4–2 × 10^-3M) were determined with relative errors and relative standard deviation of about 2%.bl]     

Electrolytic determination of traces of iodide in solution with a piezoelectric quartz crystal

The frequency of a piezoelectric quartz crystal is decreased when iodide is electrodeposited on the silver electrode of the crystal at—0.05 V vs. Ag/AgCl. From 3 × lO^-7 M to 1 × 10^-5 M iodide can be determined with few interferences, and a procedure for removal of interfering species is given. Iodide is removed from the electrode by electrolysis at —0.4 V after each determination.     

Determination of trace iodide in iodised table salt on silver sulfate-modified carbon paste electrode by differential pulse voltammetry with electrochemical solid phase nano-extraction

Electrochemical solid phase nano-extraction, a novel sample preparation technique, was used for the determination of trace iodide in iodised table salt based on the silver sulfate nanoparticle-modified carbon paste electrode. Electrochemical solid phase nano-extraction was realized in the exchange between the sulfate anion in nanoparticles and an iodide anion from aqueous solution. The released silver cation serves as the electrochemical probe for the determination of iodide. The extraction follows a Freundlich adsorption isotherm, and can be used in the detection of iodide in the concentration range 5.0 × 10⁻¹²-4.0 × 10⁻⁹ M. The amount of iodide in iodised table salt was determined as 0.875 ± 0.002 μg/g, which is about 2.5% of the addition amount of iodate with a relative deviation of 5.92% and a standard addition recovery of 90-110%. The large amounts of chloride and iodate did not interfere with the detection.     

Flow-injection analysis for l-glutamate using immobilized l-glutamate oxidase: comparison of an enzyme reactor and enzyme electrode

An enzyme electrode and enzyme based on immobilized l-glutamate oxidase are used for the determination of l-glutamate in a flow-injection system. The hydrogen peroxide produced is monitored amperometrically. The enzyme reactor system surpasses the enzyme electrode system with regard to sensitivity and analytical speed. For both systems, the peak current is linearly related to the l-glutamate concentration in the range 5 × 10^?6-1 × 10^?3 M. l-Glutamate in seasoning can be determined very selectively with < 0.7% r.s.d.     

An amperometric monoamine oxidase biosensor for determining some antidepressants

An amperometric biosensor based on a platinum screen-printed electrode and immobilized monoamine oxidase is developed to determine antidepressants of different classes. Petylyl, pyrazidol, and flu-oxetine can be determined with determination limits of 8 × 10^?9, 8 × 10^?7, and 8 × 10^?10 M, respectively. A procedure is proposed for determining fluoxetine in tablets. It is shown that petylyl can be selectively determined by an immunochemical technique using the developed biosensor and immobilized antibodies in the concentration range from 1 × 10^?4 to 1 × 10^?8 M.     

Spectrophotometric determination of trace amounts of iodide-ions in form of ionic associate with brilliant green using electrochemical oxidation

A combined method involving electrochemical oxidation of iodide to iodate at a platinum electrode followed by extraction in CCl₄ of ionic associates of iodine-iodide complexes with brilliant green, formed in excess of iodide, was developed for the spectrophotometric quantification of iodide. The slope of the calibration curve yields a molar extinction coefficient of ɛ = 3·10⁵ L mol⁻¹cm⁻¹. This method can be used for the quantification of iodide in the concentration range of 3·10⁻⁷ − 3·10⁻⁶ mol L⁻¹ with a detection limit of 5·10⁻⁸ mol L⁻¹. The interfering effect of other ions on the determination of the iodide concentration was also investigated. The method was successfully applied for the determination of iodide in real samples of NaCl and spring water. Relative standard deviation is 1–2%.     

Copper(I)-bathocuproine complex as carrier in iodide-selective electrode

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.     

Analytical use of a biochemical luminous membrane

Luminous membranes were prepared by immobilizing peroxidase (POD) to collagen matrix. The POD luminous membrane generated luninescence in the presence of luminol and H₂O₂, and the peroxide was determined in the concentration range 10-⁶-10-³ M by following luminescence emitted from the membrane. Glucose was determined using a luminous membrane in which POD and glucose oxidase (GOD) were coimmobilized. The luminous membranes appear to be feasible for the determination of enzyme substrates and enzyme activity.     

Construction of a guanine enzyme electrode and determination of guanase in human blood serum with an ammonia gas sensor

The guanine electrode is based on guanase used with an ammonia gas-sensing membrane electrode; immobilization of the enzyme is optimized. Guanine in the range 10^-4–10^-2 M gives a linear potential vs. log(concentration) plot with a response time of 4–1.5 min over the range specified. Guanase (0.12–12 I.U. I^-1) is determined in serum by adding guanine to the sample, and measuring the ammonia evolved with the gas-sensing electrode. Results compare favourably with the xanthine oxidase method.     

Alternating current polarographic determination of microgram amounts of iodide ion by means of the catalytic oxidation of 1-amino-2-naphthol-4-sulfonic acid

The catalytic oxidation of 1-amino-2-naphthol-4-sulfonic, acid proceeds quickly with microgram amounts of iodide in the presence of sodium chlorate at pH between 1.3 and 2.0. The oxidation product shows a sensitive tensammetric wave at potentials of about +0.03 V vs. SCE (pH 1.75), so that the catalytic reaction was applied for the determination of microgram amounts of iodide ion. The most suitable conditions of the pH range, the concentration of ANS and sodium chlorate, reaction temperature and standing are 1.3–2.0, 3 × 10^?4M, 0.05 M, 50° C and 1 h respectively. Using the recommended procedure, iodide ion can be determined precisely in the concentration range 0.4–6.5 ng ml^?1 with a relative error of about 3%. Interference of foreign species and the application to the determination of total iodine in river and sea water are described.     

Determination of micromolar concentrations of iodide by electrothermal atomic absorption spectrometry

When a solution (at pH 3.4–4.8) containing iodide and mercury(II) nitrate in a graphite tube is heated by increasing the temperature at a uniform rate, two mercury absorption peaks appear because the decomposition temperature of mercury(II) iodide is higher than that of mercury(II) nitrate. Measurement of the second peak allows 1 × 10^-6–5 × 10^-5 M iodide to be determined with good reproducibility. Equimolar concentrations of cyanide, sulfide and thiosulfate interfered, but these anions could be destroyed with hydrogen peroxide. Interfering cations were removed by extraction of 8-quinolinol complexes.     

Bestimmung von jodid auf grund seiner katalytischen wirkung mittels der jodat-arsenit-reaktion

The catalytic action of iodide on the iodate-arsenite reaction can lie used to detect 0.5 μg of iodide at a dilution limit of 1:10⁷. The reaction time is inversely proportional to the iodide concentration so that a chronometric estimation of iodide is possible; the “simultaneous comparison” method is advantageous, being independent of temperature variations. The relative errors are ± 10% in the range 1–10 μg 1-, and ± 5% in the range 10–50 μg 1-. Silver and mercury ions interfere.     

Reverse flow injection spectrophotometric determination of iodate and iodide in table salt

A very simple and sensitive reverse flow injection method is described for the determination of iodate and iodide. The iodate reacts with excess iodide in acidic medium to form tri-iodide, which can be spectrophotometrically monitored at 351 nm, and the absorbance is directly related to the concentration of iodate in the sample. The determination of iodide is based on oxidizing iodide to iodate. The calibration curve is linear in the range of 0.02-3.0 μg ml⁻¹ I with r²=0.9998, and the limit of detection is 0.008 μg ml⁻¹ I. The chemical and flow injection variables were studied and optimized to make the procedure suitable for quantitating iodate and iodide in table salts. It is shown that the reverse flow injection analysis could greatly improve the sensitivity and precision for determination of iodate with a relative standard deviation of 0.9%. A complete analysis, including sampling and washing, could be performed in 35 s. The procedure was applied successfully to the determination of iodate and iodide in table salts, and the results were statistically compared with results determined by standard iodometry method.     

Determination of low concentrations of chlorite and chlorate ions by using a flow-injection system

A flow-injection method is reported for the determination of chlorite ion and chlorite and chlorate ions in mixtures at the submilligram per liter level in drinking water. The chlorite ion concentration is selectively determined by using its reaction with iodide ion at pH 2, which liberates iodine. Both species react with iodide ion in6 M HCl to produce iodine, the concentration of which is measured spectrophotmetricaly at 370 nm. The individual species are determined using multiplel regression. The method exhibits a linear range from 2 to 150 μM (0.1–10.1 mg l^-1) for chlorite ion and from 2 to μM (0.1–8.3 mg l^-1 for chlorate ion, with relative standard deviations of 0.4 and 1.2%, respectively.     

Construction of a N-Acetyl-L-methionine Electrode and Determination of Acylase with an Ammonia Gas Sensor

Abstract

The N-acetyl-L-methionine electrode is based on a coupled enzymatic system consisting of acylase and L-amino acid oxidase with an ammonia gas sensor; conditions of imobilization are optimized. N-acetyl-L-methionine in the range 4×10^?5–2×10^?3M gives a linear potential vs. log(concentration) plot with a response time of 2–5 min over the range specified. This electrode combined with an L-methionine electrode, based only on L-amino acid oxidase and an ammonia gas sensor, can be used for the determination of both substrates in mixtures, thus extending the feasibility of the method. Acylase (0.1–2.00) is determined in aqueous solutions by adding N-acetyl-L-methionine to the sample, and measuring the ammonia evolved with the gas-sensing electrode.     

Kinetic determination of adrenaline,l-dopa and their mixtures with a stopped-flow spectrophotometric technique

Catecholamines (adrenaline and L-Dopa) can be determined by a stopped-flow spectrophotometric technique. For individual determinations, catecholamines are oxidized to the corresponding o-benzoquinones by hexachloroiridate(IV). Concentrations in the range 2·10^-4–2·10^-3 M can be determined with errors of about 2 %. For evaluation of mixtures, aminochromes are formed. The method allows a catecholamine concentration of about 5·10^-6 M to be determined in the presence of a ten-fold amount of another catecholamine, with a maximum error of about 10 %.