Controlled potential lodometric determination of nitrate after reduction to nitrite by coppered cadmium

A controlled-potential coulometric iodometric method previously developed for the accurate determination of small amounts of nitrite has been extended for the determination of nitrate after its reduction on a coppered cadmium reductor. The conditions for quantitative reduction have been investigated with respect to type of reductor and pH. Nitrate-nitrogen in the range 0.01-100 mug ml may be determined with high accuracy in less than 10 min, including the reduction step. The method has been applied with good results to a large variety of samples such as meat products, juices and waste waters.     

Flow-injection analysis of nitrate by reduction to nitrite and gas-phase molecular absorption spectrometry

Two flow-injection manifolds have been investigated for the determination of nitrate. These manifolds are based on the reduction of nitrate to nitrite and determination of nitrite by gas-phase molecular absorption spectrophotometry. Nitrate sample solution (300 microL) which is injected to the flow line, is reduced to nitrite by reaction with hydrazine or passage through the on-line copperized cadmium (Cd-Cu) reduction column. The nitrite produced reacts with a stream of hydrochloric acid and the evolved gases are purged into the stream of O2 carrier gas. The gaseous phase is separated from the liquid phase using a gas-liquid separator and then swept into a flow-through cell which has been positioned in the cell compartment of an UV-visible spectrophotometer. The absorbance of the gaseous phase is measured at 204.7 nm. A linear relationship was obtained between the intensity of absorption signals and concentration of nitrate when Cd-Cu reduction method was used, but a logarithmic relationship was obtained when the hydrazine reduction method was used. By use of the Cd-Cu reduction method, up to 330 microg of nitrate was determined. The limit of detection was 2.97 microg nitrate and the relative standard deviations for the determination of 12.0, 30.0 and 150 microg nitrate were 3.32, 3.87 and 3.6%, respectively. Maximum sampling rate was approximately 30 samples per hour. The Cd-Cu reduction method was applied to the determination of nitrate and the simultaneous determination of nitrate and nitrite in meat products, vegetables, urine, and a water sample.     

Réduction et dosage des arséniates en présence de catalyseurs,en particulier le rhénium

The reduction of arsenates to arsenites is normally slow, but is accelerated in the presence of catalysts the use of alkali perrhenate or iodide permits a quantitative reduction by stannous chloride. A method of determination using the latter reducing agent has been developed.     

Titrimetric determination of chloramine-T and some aldoses by amplification reactions

A titrimetric method with amplification has been worked out for the determination of chloramine-T and certain aldoses. It is based on Leipert determination of iodide produced in the case of chloramine-T by reduction of the determinand with excess of iodide, and extraction and subsequent reduction of the iodine liberated. In the other case, the aldoses are oxidized with iodine, the surplus oxidant is extracted, and the residual iodide is determined. The method is applicable to chloramine-T in the range 0.01-3 mg, with a relative error between -3.0 and -0.4% and a relative standard deviation of 0.6-0.8%, depending on the amount present, and to 0.05-1 mg of glucose, galactose or arabinose, or 0.1-2 mg of lactose or maltose, with a relative standard deviation of 1.4% for > 0.5 mg of aldose.     

Reduction and determination of dixanthogens

A convenient method for the reduction and determination of dixaathogen has been developed. It is based on the quantitative reaction of dixanthogen with zinc amalgam to form xanthate; the latter can be determined by iodine titration, potentiometric titration with silver nitrate or by spectrophotometry at 310 mmu. Dixanthogen can be determined in mixtures containing xanthate, by titration of aliquots with and without reduction. Higher dixanthogens can also be determined, and flotation liquors analysed.     

Electrochemical behaviour of triphenylgermanium bromide

The electrochemical behaviour of triphenylgermanium bromide has been thoroughly investigated using various electrochemical techniques including polarography, cyclic voltammetry and controlled potential coulometry. It has been found that in non-aqueous solvents triphenylgermanium bromide gives only one small drawn-out wave, while in aqueous-organic media two reduction waves are observed. The first wave has been ascribed to adsorption of the products of the reduction step II. The triphenylgermanium free radicals have been postulated to combine rapidly with protons in acidic media or to abstract hydrogen from water in alkaline media. The protonated species has been found to be reduced at potentials at which normal reduction of triphenylgermanium bromide takes place giving rise to a superimposed catalytic proton-discharge wave. A mechanism of reduction of triphneylgermanium bromide at the DME has been postulated and analytical methods for the determination of triphenylgermanium compounds at the formulation and trace analysis levels have been developed.     

Analytical applications of the photochemical action of light: Determination of ferric iron by photochemical reduction in the presence of citric and mandelic acids

A new method has been developed for the determination of ferric sulphate through its photochemical reduction with citric and mandelic acids in sunlight. The method consists in irradiating with sunlight a measured volume of the ferric sulphate solution together with an excess of citric or mandelic acid in a quartz or pyrex glass beaker until reduction is complete. The ferrous salt formed is determined by titration with a standard solution of sodium vanadate in the presence of the proper concentration of sulphuric and phosphoric acids, employing diphenylbenzidine or diphenylamine sulphonate as internal indicators. The photoreduction is greatly retarded by sulphuric acid.     

A FIA-system for As(III)/As(V)-determination with electrochemical hydride generation and AAS-detection

A flow-injection system with electrochemical hydride generation and atomic absorption detection for As(III)/As(V) determination is described. A simple electrolytic flow-through cell has been developed and optimized. Several cathode materials like Pt, Ag, Cu, C and Pb have been tested. The influence of the electrolysis current, concentration of sulfuric acid, carrier stream, flow rate, sample volume and interferences by other metals on the arsenichydride generation have been studied. For the determination of total inorganic arsenic, As(V) is reduced to As(III) on-line by postassium iodide or L-cysteine at 95 degrees C. The influence of the temperature and the reduction medium on this pre-reduction step has been tested. The calibration curve is linear in the range of 5 to 50 microg/L for As(III) and total inorganic arsenic and shows a higher sensitivity than in case of reduction with sodium tetrahydroborate. The detection limit is 0.4 microg/L for As(III) and 0.5 microg/L for total inorganic arsenic at a sample volume of 1 mL.     

A rapid and mercury pollution-free redoximetry determination of total iron in copper ore

A rapid and mercury pollution-free method for the determination of total iron in the presence of copper is described. The sample was decomposed either by an acid attack of hydrochloric acid-nitric acid (1 + 2) or by fusion with sodium peroxide. The ferric ion in the sample solution was amenable to direct reduction to ferrous ion with potassium borohydride in sulphuric acid medium under the catalysis of cupric ion, followed by titration with potassium dichromate using sodium diphenylaminesulfonate as an indicator. After reduction, the iron (II) in the solution was stable for 300 min. The proposed method is free of interference from copper and has been successfully used for the large-scale routine determination of total iron in copper ores showing the same or better degree of precision and accuracy as those obtained by the classic standard stannous chloride-mercuric chloride method with the separation of iron from copper.     

Controlled-potential iodometric titration of nitrite. Application to the determination of nitrite in meat products

A controlled-potential coulometric method using iodine as an intermediate has been devised for the determination of nitrite. Nitrite is reduced by iodide and the iodine formed is then reduced coulometrically. The reduction of nitrite in the pH range 0-6 has been studied and the optimum conditions for an accurate determination are stated. The time of analysis for a determination in the range 0.005-5 mg of nitrite is about 2-5 min and the error +/- 0.1%. The method is applied to the determination of nitrite in some meat products.     

A new method for the titrimetric determination of perchlorate

A new method for the titrimetric determination of perchlorate has been developed, based on its reduction to chloride by iron(II) in a strong sulphuric acid medium at high temperature. The effect of variables, such as the sulphuric acid concentration, the temperature and the period of heating, on the extent of reduction has been studied and the optimal conditions for analytical determination of perehlorate derived.     

Extractive separation and spectrophotometric determination of palladium and platinum with dithizone in the presence of stannous chloride

The conditions [acid used, presence of chloride and tin(II)] for the extractive separation and spectrophotometric determination of palladium and platinum as the dithizonates Pd(HDz)(2) and Pt(HDz)(2) have been examined. In the absence of stannous chloride platinum does not undergo extraction. Conditions for the separation and determination of these metals in the presence of mercury, gold and copper, which are also extracted with dithizone into carbon tetrachloride or chloroform under the conditions suitable for palladium (1M sulphuric acid/0.1M hydrochloric acid), have been defined. The mercury and gold dithizonates are formed quickly and can be removed before the palladium and platinum compounds have had time to form. They can be decomposed with iodide. Copper dithizonate is decomposed by reduction with tin(II). The proposed procedure has been applied to the determination of palladium in technical platinum metal.     

Experimental study of radon and thoron diffusion through barriers

The radon chamber and radon calibration set have been modified for investigation of the diffusion coefficients of the barriers for reduction of radon exposure in the dwellings and for application as filters to separate radon and thoron. The volume radon activities have been measured by continuous monitors with scintillation cell or ionisation chamber. The theory on which the experimental determination of a barrier diffusion coefficient is based, is presented. The diffusion ability of radon has been studied for different materials and the results of the measurements are presented and discussed.     

Three-phase interlines electrochemically driven into insulator compounds: a penetration model and its verification by electroreduction of solid AgCl

A dynamic three-phase interline model has been developed for the reduction of a solid insulating metal compound to the metal in a suitable electrolyte, focusing on the electrochemically driven penetration of the process (or the three-phase interlines) into the insulator. Consideration is given to the effects of electrochemical, concentration and ohmic polarizations in the reduction-generated porous metal layer on top of the solid compound. Under potentiostatic conditions, reduction in the depth direction (penetration) becomes progressively slower as a result of the rising ohmic and concentration polarizations, whilst the electrochemical polarization exerts a declining effect. The quantitative equations established here also provide simple methods for the determination of some kinetic parameters of the reduction process, including rho (total resistivity) and D(R) (diffusion coefficient). The model has been experimentally verified by electrochemical reduction of solid AgCl with two novel metal|AgCl cylinder electrodes in aqueous solutions.     

Determination of Riboflavin Using the Polarographic Reduction Wave of Its Photochemical Reaction Products

Abstract

A new, simple, and sensitive method for the determination of riboflavin based on the single-sweep polarographic reduction wave of the photolysis products of riboflavin has been developed. Under the irradiation of an iodine-tungsten lamp, the photolysis reaction of riboflavin in pH 9.3 NH₃-NH₄Cl buffer solution can be complete in about 20 min. The reaction products yield a single adsorptive reduction wave at ?0.63 V (vs. SCE) negative to the reduction wave of riboflavin by 0.18 V. The derivative wave height is linearly proportional to the concentration of riboflavin in the range of 0.01–17.5 µg/mL (correlation coefficient 0.996). The detection limit is 0.00 5µg/mL. The proposed method has been applied to the determination of multivitamin tablets with satisfactory results. In comparison with the methods directly using the reduction wave of riboflavin for the determination, this method eliminates the effect of the degradation of riboflavin on the determination accuracy and is much more sensitive. The new method could be useful in many fields.     

催化电位滴定法测定铬鞣剂中铬(Ⅲ)

报道了以氨三乙酸存在下锰(Ⅱ)催化KIO4氧化结晶紫的反应指示终点,结晶紫电极作指示电极用催化电位滴定法测定铬鞣剂中Cr(Ⅲ)的方法。该法终点灵敏、准确度高、重现性好,结果满意,用标准加入法测得的平均回收率为100.03%,RSD为0.24%。     

Catalytic Determination of Selenium in Human Hair by Polarography Using Glutathione

Abstract

A catalytic polarographic method has been proposed for the accurate determination of selenium in human hair. This method is based on the formation of Se(0)-GSH complex in alkaline medium which gives a catalytic reduction wave in polarography. The current observed is directly proportional to the amount of selenium present. The method has been applied for the determination of selenium in human hair and the recovery of added selenium from hair is found to be 97.5 to 102%. A suitable mechanism for the reduction process involving the catalytic reduction of oxidised glutathione is proposed.     

A rapid titrimetric determination of iron in copper concentrates and copper-bearing leach solutions

A titrimetric method for the determination of iron(III) in the presence of copper is presented. This method involves the reduction of iron(III) with titanous sulphate followed by titration with dichromate. It has been successfully used for the determination of iron in both leach solutions and copper concentrates with a relative error of 1%.     

硼氢化钠还原-无色散原子荧光法测定茶叶中汞

建立了汞的硼氢化钠还原－无色散原子荧光测定方法,在最佳条件下,荧光强度与汞浓度在0－25μg/L范围内呈线性关系,相关系数0．9991,检出限0．02μg/L。用拟定的方法测定了茶叶中的汞,回收率为91．6％－98．3％,变异系数不超过5．2％。     

Functional group analysis on oxidized surfaces of synthetic textile polymers

A comprehensive collection of wet-chemical analyses of functional groups on oxidatively treated surfaces of hydrophobic polymers like poly(ethylene terephthalate) or polyolefine is presented. New methods are introduced. Textiles and foils have been subjected to advanced oxidation processes and the different oxygen functions have been quantified. Analysis of surface functional groups includes radical site determination with radical scavengers like diphenylpicrylhydrazyl, reduction of peroxides determined iodometrically, cationic dyestuff adsorption, carbonyl binding to Girard reagent P and surface hydroxyl group determination by surface nitrosation and subsequent azo-dye formation photometrically determinable. Use of potential surface swelling agents has been excluded except for addition of wetting agent. Wet-chemical analyses on textile surfaces bear the benefit of integrating over (relatively) large sample areas, a point which is interesting when regarding inhomogenities of textile or other surface constructions. In addition examples for visualisation for the existence of surface groups are described.