Volumetric studies in oxidation-reduction reactions: Reduction with ferrous ethylenediamine sulphate ceric sulphate method

Ferrous ethylenediamine sulphate has been used as a reducing agent in acid medium for the indirect volumetric estimations of potassium chlorate, potassium bromate, potassium metaperiodate, potassium dichromate, potassium ferricyanide, potassium permanganate, potassium persulphate, hydrogen peroxide and ceric sulphate. The excess of ferrous ethylenediamine sulphate added to each of the substances in acid medium was titrated with standard ceric sulphate solution using ferroin as an indicator.     

Sodium hypochlorite as volumetric reagent

Summary In presence of 5 N to 6 N hydrochloric acid, ferrous ethylenediamine sulphate was used as a reducing agent to determine indirectly potassium chlorate, potassium bromate, potassium metaperiodate, potassium dichromate, potassium ferricyanide, potassium permanganate, potassium persulphate, hydrogen peroxide, ceric sulphate and chloramine-T. An excess of ferrous ethylenediamine sulphate added to each of the substances in the acid medium was titrated with a standard solution of sodium hypochlorite. Iodine monochloride was used as catalyst and preoxidizer and chloroform was used as an indicator. Chloroform was coloured violet owing to the liberation of iodine during the titration and became very pale yellow at the end-point because of the formation of iodine monochloride.Part I: See Z. analyt. Chem. 160, 429 (1958).     

Potentiometric studies in oxidation-reduction reactions: Reduction with ferrous ethylenediamine sulphate indirect determinations

Ferrous ethylenediamine sulphate has been used as a reducing agent to determine indirectly potassium dichromate, hydrogen peroxide, potassium permanganate, potassium persulphate, potassium chlorate, potassium bromate, and ceric sulphate by a potentiometric method. An excess of ferrous ethylenediamine sulphate added to each of the substances in an acid medium is titrated with a standard solution of potassium permanganate, using platinum foil as an oxidation-reduction electrode coupled with a saturated calomel electrode through an agar-agar potassium chloride bridge.     

Potentiometric studies in oxidation-reduction reactions: Reduction with ferrous ethylenediamine sulphate ceric sulphate method

Ferrous ethylenediamine sulphate has been used as a reducing agent to determine indirectly potassium permanganate, ceric sulphate, potassium chlorate, hydrogen peroxide, potassium persulphate, potassium dichromate and potassium bromate by a potentiometric method. An excess of ferrous ethylenediamine sulphate added to each of the substances in acid medium was titrated with a standard solution of ceric sulphate, using platinum foil as an oxidation-reduction electrode coupled with a saturated calomel electrode through an agar-agar potassium chloride bridge.     

Diethylenetetra-ammonium sulphatocerate as volumetric reagent: Iodine monochloride method. Indirect determinations

In presence of 4N to N hydrochloric acid, diethylenetetra-ammnonium sulphatocerate was used as a volumetric reagent to determine indirectly potassium iodate, potassium metaperiodate, potassium dichromate, potassium bromate, ceric sulphate, hydrogen peroxide, lead dioxide and chloramine-B by the iodine monochloride method. An excess of potassium iodide added to each of the substances in the acid medium was, titrated back with a standard solution of diethylene-tetra-ammonium suphatocerate. Chloroform was used as an indicator. It was coloured violet owing to the liberation of iodine during the titralion and became very pale yellow at the end-point because of the formation of iodine monochloride.     

Potentiometric studies in oxidation-reduction reactions: Oxidation with chloramine-b. indirect determinations

Chloramine-B has been used as an oxidising agent to determine indirectly potassium iodate, potassium metaperiodate, potassium, bromate, potassium dichromate, hydrogen peroxide, chloramine-T and potassium permanganate by a potentiometric method. An excess of potassium iodide added to each of the substances in an acid medium is titrated back with a standard solution of chloramine-B, using platinum foil as an oxidation-reduction electrode coupled with a saturated calomel electrode through an agar-agar potassium chloride bridge.     

Volumetric estimation of potassium permanganate and potassium dichromate in mixtures with oxalic acid

1. A simple method has now been developed for the volumetric estimation of potassium permanganate and potassium dichromate in mixtures The method consists in taking an aliquot volume of the mixture in an Erlenmeyer flask, adding sufficient quantities of sulphuric acid and manganous sulphate (catalyst) and titrating with a standard solution of sodium oxalate or oxalic acid run in from the burette, until the colour changes from orange-red to yellow. The oxalic acid run ingives a measure of the permanganate present in the mixture Then the mixture in the flask is titrated with a standard solution of Mohr's salt using diphenylbenzidine as indicator. The volume of Fe⁺² solution run in the second stage gives a measure of the dichromate present in the original mixture. 2. The reverse titration does not give accurate results, because it is affected by the induced reaction between oxalic acid and dichromate which is induced by the reaction between oxalic acid and permanganate during the first stage of the reaction. This induced reaction has been studied in some detail.     

Volumetric Studies In Oxidation-Reduction Reactions: Oxidation with ceric sulphate ferrous ethylenediamine sulphate method

Ceric sulphate has been used as an oxidizing agent in acid medium for the indirect volumetric determinations of ferrous ammonium sulphate, cuprous chloride, potassium thiocyanate, sodium thiosulpliate, sodiuin nitrite, hydrogen peroxide, sodium oxalate, hydroquinone and pyruvic acid. The excess of ceric sulphate added to each of the substances in acid medium was titrated with standard ferrous ethylenediamine sulphate solution using ferroin as an indicator.     

Oxidimetric methods for the volumetric estimation of sulphite

1. The use of permanganate, ceric sulphate, and dichromate for the estimation of sulphite has been reinvestigated, although these reagents have heen discarded as useless by earlier investigators. By using catalysts under controlled acid concentration, we have been able to develop conditions for the quantitative oxidation of sulphite to sulphate at room temperature by any one of these oxidizing agents, avoiding the formation of dithionate. Copper sulphate and iodine monochlonde have been found useful as catalysts with potassium permanganate and dichromate; but only iodine monochloride with ceric sulphate. 2. Sodium sulphite is also oxidized quantitatively to sulphate at room temperature, when added to excess of sodium vanadate solution containing 5 to 6N hydrochloric acid and iodine monochloride as catalyst.     

Studies in bivalent chromium salts

Summary It has been shown that chromous solution can be standardised with the help of potassium dichromate, sulphatocerate, potassium iodate, bromate and periodate solutions. N-phenylanthranilic acid, ferroin and diphenylbenzidine serve as reversible indicators for the titrations of potassium dichromate and ceric sulphate against chromous solution.The authors are indebted to Dr. R. N. Singh, Professor of Chemistry, B. R. College, Agra, for his kind encouragement and for providing laboratory facilities.Part II: See Z. anal. Chem. 158, 189 (1957).     

Mercurous nitrate as a reductimetric reagent : The titration of various oxidising agents

It has been found that when excess of a solution containing ferrous ions is added to certain oxidising agents, the equivalent amount of ferric iron produced can be titrated accurately with mercurous nitrate, enabling the original oxidant to be assessed. Oxidising agents which have been determined in this way are potassium permanganate, potassium persulphate, ceric sulphate, sodium vanadate, potassium chlorate, hydrogen peroxide and potassium dichromate. The last substance provides a convenient primary standard for the standardisation of mercurous nitrate solutions.     

The use of 2,6-dichlorophenol-indophenol as indicator in iodometric titrations with ascorbic acid

2,6-Dichlorophenol-indophenol can be used as an indicator in iodometric methods, provided that near the end-point the solutions can be buffered with potassium hydrogen carbonate, so that ascorbic acid can be used as the titrant. Procedures for the determination of iodine, chlorine, bromine, hypochlorite, Chloramine T, bromate, iodate, permanganate, dichromate, copper(II), hydrogen peroxide, peroxydisulphate, thiosulphate, sulphite, sulphide, hydrazine and formaldehyde are described.     

Volumetric studies in oxidation-reduction reactions: Oxidation with chloramine-t. indirect determinations

Chloramine-T has been used as an oxidizing agent in hydrochloric acid medium for the indirect volumetric determination of hydrogen peroxide, lead dioxide, selenium dioxide, sodium formate, potassium meta-periodate, potassium permanganate and potassium dichromate using iodine monochloride as a catalyst, prcoxidizer and an indicator. Chloroform is coloured pink owing to the liberation of iodine during the titration and becomes very pale yellow at the end-point because of the formation of iodine monochloride.     

Oxidation of sulphides with alkaline potassium permanganate

Summary Sulphides are oxidised with potassium permanganate in alkaline medium to give dithionate. A method based upon this reaction is proposed for the determination of sulphides. The method consists in mixing the sulphide solution with an excess of permanganate in presence 1–2 M NaOH and 0.2 g telluric acid. The excess permanganate is then treated with ferrous ammonium sulphate in acid medium and the excess ferrous titrated with permanganate.     

Standardization of titanous chloride and sulphate solutions

It is confirmed that the presence of iron as impurity in titanous chloride and sulphate solutions invalidates the use of potassium dichromate as a standard substance. Methods of overcoming this interference and of preparing iron-free titanous salt solutions are discussed and reasons are given for preferring titanous chloride to titanous sulphate for most purposes.     

Micro and semi-micro determination of organic nitrogen by use of potassium bromate

After Kjeldahl digestion of an organic compound, nitrogen is determined by oxidation of the resultant ammonium sulphate with hypobromite produced in situ by the addition of an excess of potassium bromate and bromide in a special flask. The unreacted potassium bromate is determined iodometrically.     

Volumetric determination of small amounts of uranium : Chromous chloride as reducing agent

A volumetric method is proposed for the rapid determination of small amounts of uranium. The hexavalent uranium is reduced to the quadrivalent state by chromous chloride, the excess of which is destroyed by air oxidation. A low potential redox indicator is used to follow the reduction and air oxidation. Ferric sulphate is added to the solution and the resulting ferrous ion titrated with dichromate solution.     

Thiourea as reductimetric standard: Standardisation of cerium(IV), dichromate,bromate, chloramine-T,and N-bromosuccinimide solutions

Summary The use of 0.01N thiourea as a reductimetric standard has been described for the standardisation of Ce(IV), potassium dichromate, potassium bromate, chloramine-T andN-bromosuccinimide solutions.

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Zusammenfassung Die Anwendung von 0,01N Thioharnstofflösung als reduzierende Standardlösung für Ce(IV), Bichromat, Bromat, Chloramin-T und N-Bromsuccinimid wurde beschrieben.

     

Rapid estimation of metallization in reduced iron oxide ores

A simple and accurate method is described for the determination of degree of metallization in reduced iron oxide ores. Both metallic iron and total iron are determined in a single sample. The metallic iron is selectively dissolved in copper sulphate solution and the oxides are filtered off. The filtrate is titrated with potassium dichromate solution. The residue is dissolved in dilute sulphuric acid in presence of excess of copper powder and after filtration is titrated with the same dichromate solution. The first value gives the metallic iron content and the second value gives the iron content of the oxide residue. From these two values, the degree of metallization is computed.     

The determination of periodate by infrared spectroscopy

An infrared method has been developed to determine periodate on the microgram scale. Periodate is precipitated in slightly acid solution with tetraphenylarsonium chloride and in presence of perchlorate as carrier. The precipitate is mixed with powdered potassium bromide and pressed into a disc. The base-line absorbance of the periodate band at 11.68 μ is calculated in order to find the concentration of periodate from a calibration curve. No interference is caused by perchlorate, permanganate, perrhenate, chlorate, iodate or bromate.