Hydrogen peroxide titration methods

Analytical Methods. The official NIOSH recommended method for determining sulfur dioxide in air consists of drawing a known prefiltered volume of air through a bubbler containing hydrogen peroxide, thus oxidising the sulfur dioxide to sulfuric acid. Isopropyl alcohol is then added to the contents in the bubbler and the pH of the sample is adjusted with dilute perchloric acid. The resultant solution is then titrated for sulfate with 0.005 M. barium perchlorate, and Thorin is used as the indicator. 

The Reich test is used to estimate sulfur dioxide content of a gas by measuring the volume of gas required to decolorize a standard iodine solution (274). Equipment has been developed commercially for continuous monitoring of stack gas by measuring the near-ultraviolet absorption bands of sulfur dioxide (275—277). The deterrnination of sulfur dioxide in food is conducted by distilling the sulfur dioxide from the acidulated sample into a solution of hydrogen peroxide, foUowed by acidimetric titration of the sulfuric acid thus produced (278). Analytical methods for sulfur dioxide have been reviewed (279). 

Analytical Methods. A classical and stiU widely employed analytical method is iodimetric titration. This is suitable for determination of sodium sulfite, for example, in boiler water. Standard potassium iodate—potassium iodide solution is commonly used as the titrant with a starch or starch-substitute indicator. Sodium bisulfite occurring as an impurity in sodium sulfite can be determined by addition of hydrogen peroxide to oxidize the bisulfite to bisulfate, followed by titration with standard sodium hydroxide (279). 

This is typically accompHshed by cooling the titration solution with ice, determining the blank, and titrating rapidly. Another method utilizes deterrnination of the total peroxide and peracid content by use of a ceric sulfate titration to measure hydrogen peroxide followed by a iodide/thiosulfate titration to measure total active oxygen (60). 

Sulfur Dioxide EPA Method 6 is the reference method for determining emissions of sulfur dioxide (SO9) from stationary sources. As the gas goes through the sampling apparatus (see Fig. 25-33), the sulfuric acid mist and sulfur trioxide are removed, the SO9 is removed by a chemical reaction with a hydrogen peroxide solution, and, finally, the sample gas volume is measured. Upon completion of the rim, the sulfuric acid mist and sulfur trioxide are discarded, and the collected material containing the SO9 is recovered for analysis at the laboratory. The concentration of SO9 in the sample is determined by a titration method. 

Satisfactory 40% peracetic acid is obtainable from Buffalo Electrochemical Corporation, Food Machinery and Chemical Corporation, Buffalo, New York. The specifications given by the manufacturer for its composition are peracetic acid, 40% hydrogen peroxide, 5% acetic acid, 39% sulfuric acid, 1% water, 15%. Its density is 1.15 g./ml. The peracetic acid concentration should be determined by titration. A method for the analysis of peracid solutions is based on the use of ceric sulfate as a titrant for the hydrogen peroxide present, followed by an iodometric determination of the peracid present.3 The checkers found that peracetic acid of a lower concentration (27.5%) may also be used without a decrease in yield. The product was found to be sufficiently pure, after only one recrystallization from 60 ml. of petroleum ether (b.p. 40-60°) and cooling overnight to —18°, to be used in the next step. 

Determination of the level of total sulfur in a rubber can give information on the type of cure system used, for example, elemental sulfur plus accelerator or sulfur donor system, etc. The ISO 6528-1 1992 method — Rubber — Determination of total sulfur content — Part 1 Oxygen combustion flask method is often employed. The principle of the method is oxidation by ignition in an atmosphere of oxygen in the presence of hydrogen peroxide, conversion of sulfur to sulfuric acid and determination of the sulfate by titration with barium perchlorate. The method is... 

Hydrogen peroxide solution and potassium bromide are two pharmaceutical substances that may be estimated by employing 0.1 N potassium permanganate solution and adopting the direct titration method. 

Thioetherification of PECH is feasibly performed in DA-solvents as already described in the patent (20J. For example, the highest substitution was obtained by the reaction of P(ECH-EO)(1 1 copolymer of epichloro-hydrin and ethylene oxide) and equimolar thiophenoxide in HMPA at 100°C for 10 h as DS 83% for sodium and 93% for potassium salts. The DS in our nucleophilic substitution was estimated by the elemental analysis as well as the titration of liberated chloride ion with mercuric nitrate (21). In the latter method, reacted medium was pretreated with hydrogen peroxide when the reductive nucleophiles which can react with mercuric ion were used. As described before for PVC, thiolation was also achieved conveniently with iso-thiuronium salt followed by alkaline hydrolysis without the direct use of ill-smelling thiolate. The thiolated PECH obtained are rubbery solids, soluble in toluene, methylene chloride, ethyl methyl ketone and DMF and insoluble in water, acetone, dioxane and methanol. 

Classical low values for the mammalian enzyme that have appeared in the literature are the result of enzyme inactivation by hydrogen peroxide when measurements were carried out with peroxide levels in excess of 10 mM over time scales of 10 minutes or longer. The rapid sampling/titration method of Bonnichsen overcame the inactivation problem and permitted a satisfactory correlation of the overall catalytic measurements and Chance s observations on the intermediate complex (compound 1). Eventually, the introduction of the UV detector/spectrophotometer and the consequent assay based upon the UV absorbance of peroxide (35) further simplified the process by eliminating the discontinuous titrimetric assay. 

Oxidation indices, 656-72 peroxide determination, 762-3 peroxide value, 656, 657-64 colorimetry, 658-61 definition, 657 direct titration, 657 electrochemical methods, 663-4 IR spectrophotometry, 661-3 NIR spectrophotometry, 663 UV-visible spectrophotometry, 658-61 secondary oxidation products, 656, 665-72 tests for stability on storage, 664-5, 672 thermal analysis, 672 Oxidative amperometiy, hydroperoxide determination, 686 Oxidative cleavage alkenes, 1094-5 double bonds, 525-7 Oxidative couphng, hydrogen peroxide determination, 630, 635 Oxidative damage... 

A rapid volumetric method for the determination of sulphur is as follows 2 The sulphur is dissolved in a known volume of hot standard sodium hydroxide solution and after cooling is oxidised to sulphate by the addition of hydrogen peroxide the excess of alkali is then titrated with standard acid.3 The method is applicable to gases containing any common sulphur compound except thiophen (e.g. coke oven gas).4... 

Another method which is applicable also to the estimation of solutions containing sulphites and hydrogen sulphites is the addition of a known excess of acidified hydrogen peroxide to the solution of sulphurous acid. The excess of peroxide may then be titrated with standard permanganate solution. The reactions are as follows ... 

An attractive modification of this method is to treat the neutralised polythionate solution with neutral hydrogen peroxide and a known excess of standard sodium hydroxide solution on the water-bath and to determine the quantity of acid formed by the amount of standard alkali neutralised during the oxidation.3 All polythionates except the dithionates are completely oxidised to sulphate by heating in a closed tube for one hour with iodine and sodium bicarbonate by titrating the excess of iodine the total polythionate present may be estimated.4... 

The most commonly used technique for the determination of hydrogen peroxide in an industrial environment is the classical manual titration of a bath sample with potassium permanganate after acidification with sulphuric acid. In the past, numerous attempts have been made to perform the determination by means of an instrumental technique however, disadvantages were always encountered, which, up to now, have hindered the breakthrough of an alternative method. 

In a limited number of experiments, in which six different hydrogen peroxide concentrations were examined with four different pH values, the validity of the procedure used was checked by comparing the results obtained with the sensor electrode to those obtained by means of titration. The results obtained with the sensor electrode have a maximum divergence of 3% compared with the concentrations obtained by titration. The final aspect of the amperometrical detection method that was examined at laboratory scale is the stability in time of a calibrated sensor electrode. 

---