Sodium thiosulphate solution

Colloidal sulphur is produced by careful addition of acid to sodium thiosulphate solution. 

In what way does a solution of hydrogen peroxide react with (a) chlorine water, (b) potassium permanganate solution, (c) potassium dichromate solution, (d) hydrogen sulphide 50 cm of an aqueous solution of hydrogen peroxide were treated with an excess of potassium iodide and dilute sulphuric acid the liberated iodine was titrated with 0.1 M sodium thiosulphate solution and 20.0 cm were required. Calculate the concentration of the hydrogen peroxide solution in g 1" ... 

Required Ethanol, 30 ml. sodium, 14 g. iodine, 7 7 g. ethyl malonate, 9 ml. sodium thiosulphate solution. 

Transfer 25 ml. of this dilute solution by means of a pipette to a conical flask, and add similarly 50 ml. of Ml 10 iodine solution. Now-add 10% sodium hydroxide solution until the liquid becomes pale yeilow in colour, and allow the solution to stand, with occasional shaking, at room temperature for at least 10 minutes. Then acidify with dilute hydrochloric acid (free from chlorine) in order to liberate the remaining iodine. Titrate the latter w ith Mho sodium thiosulphate solution, using starch as an indicator in the usual way. 

Dibromobutane (from 1 4-butanediol). Use 45 g. of redistilled 1 4-butanediol, 6-84 g. of purified red phosphorus and 80 g. (26 ml.) of bromine. Heat the glycol - phosphorus mixture to 100-150° and add the bromine slowly use the apparatus of Fig. Ill, 37, 1. Continue heating at 100-150° for 1 hour after all the bromine has been introduced. Allow to cool, dilute with water, add 100 ml. of ether, and remove the excess of red phosphorus by filtration. Separate the ethereal solution of the dibromide, wash it successively with 10 per cent, sodium thiosulphate solution and water, then dry over anhydrous potassium carbonate. Remove the ether on a water bath and distil the residue under diminished pressure. Collect the 1 4-dibromobutane at 83-84°/12 mm. the yield 3 73 g. 

In a 500 ml. three-necked flask, equipped with a thermometer, a sealed Hershberg stirrer and a reflux condenser, place 32-5 g. of phosphoric oxide and add 115-5 g. (67-5 ml.) of 85 per cent, orthophosphoric acid (1). When the stirred mixture has cooled to room temperature, introduce 166 g. of potassium iodide and 22-5 g. of redistilled 1 4-butanediol (b.p. 228-230° or 133-135°/18 mm.). Heat the mixture with stirring at 100-120° for 4 hours. Cool the stirred mixture to room temperature and add 75 ml. of water and 125 ml. of ether. Separate the ethereal layer, decolourise it by shaking with 25 ml. of 10 per cent, sodium thiosulphate solution, wash with 100 ml. of cold, saturated sodium chloride solution, and dry with anhydrous magnesium sulphate. Remove the ether by flash distillation (Section 11,13 compare Fig. II, 13, 4) on a steam bath and distil the residue from a Claisen flask with fractionating side arm under diminished pressure. Collect the 1 4-diiodobutane at 110°/6 mm. the yield is 65 g. 

To determine the exact peroxide content of benzoyl peroxide (and of other organic peroxides) the following procedure may be employed. Place about 0 05 g. of the sample of peroxide in a glass-stoppered conical flask add 5-10 ml. of acetic anhydride (A.R. or other pure grade) and 1 g. of powdered sodium iodide. Swirl the mixture to dissolve the sodium iodide and allow the solution to stand for 5-20 minutes. Add 50-75 ml. of water, shake the mixture vigorously for about 30 seconds, and titrate the liberated iodine with standard sodium thiosulphate solution using starch as indicator. 

To determine the exact perbenzoic acid content of the solution, proceed as follows. Dissolve 1 -5 g. of sodium iodide in 50 ml. of water in a 250 ml. reagent bottle and add about 5 ml. of glacial acetic acid and 5 ml. of chloroform. Introduce a known weight or volume of the chloroform solution of perbenzoic acid and shake vigorously. Titrate the liberated iodine with standard O lA sodium thiosulphate solution in the usual manner. 

The m.p. is not always a safe criterion of purity. Benzoyl peroxide may be analysed as follows -. Dissolve about 0-6 g., accurately weighed, of benzoyl peroxide in Is ml. of chloroform in a 350 ml. conical flask. Cool to — 5°, and add 25 ml. of 0- IN sodium methoxide solution at once with cooling and shaking. After 5 minutes at — 5°, add 100 ml. of iced water, 5 ml. of 10 per cent, sulphuric acid, and 2 g. of potassium iodide in 20 ml. of 10 per cent, sulphuric acid in the order mentioned with vigorous stirring. Titrate the liberated iodine with standard 0-lN sodium thiosulphate solution. 

To determine the per-acid content, add 30 ml. of 20 per cent, po assium iodide solution to 2-0 ml. of the solution and, after 10 minutes, titrate the liberated iodine with standard 0-05N sodium thiosulphate solution (compare Perbemoic Acid, Section IV,198, Note 1). 

For the preparation of standard iodine solutions, resublimed iodine and iodate-free potassium iodide should be employed. The solution may be standardised against pure arsenic(III) oxide or with a sodium thiosulphate solution which has been recently standardised against potassium iodate. 

B) With standard sodium thiosulphate solution. Sodium thiosulphate solution, which has been recently standardised, preferably against pure potassium iodate, is employed. Transfer 25 mL of the iodine solution to a 250 mL conical flask, dilute to 100 mL and add the standard thiosulphate solution from a burette until the solution has a pale yellow colour. Add 2 mL of starch solution, and continue the addition of the thiosulphate solution slowly until the solution is just colourless. 

The liberated iodine is titrated with standard sodium thiosulphate solution. 

Measure out a 100 mL portion of the solution with a pipette and titrate the iodine with approximately Mj80 standard sodium thiosulphate solution adding 2mL of starch solution as indicator as the titration proceeds and after the titration liquid has become pale yellow in colour. 

The liberated iodine is titrated with standard sodium thiosulphate solution. The solution should not be strongly acidified with hydrochloric acid, for the little calcium chlorate which is usually present, by virtue of the decomposition of the hypochlorite, will react slowly with the potassium iodide and liberate iodine ... 

Place the prepared copper acetate solution in the beaker and add 10 mL of 20 per cent potassium iodide solution. Set the stirrer in motion and add distilled water, if necessary, until the platinum plate electrode is fully immersed. Use a saturated calomel reference electrode, and carry out the normal potentiometric titration procedure using a standard sodium thiosulphate solution as titrant. 

Reagents, ca 0.001 M Sodium thiosulphate solution, 0.1 M with respect to potassium chloride and 0.004M with respect to potassium iodide. 

Reagents required. Prepare a ca 0.001 M sodium thiosulphate solution and also a standard 0.005 M iodine solution. 

Sodium acetate (analytically pure). Potassium iodide and 0-1 N sodium thiosulphate solution. 

The Sugar Determination.—Dilute the 5 c.c. sample in a measuring flask to 25 c.c. and pour 10 c.c. of this diluted solution into 25 c.c. of 01 N-iodine solution. Then add 40 c.c. of 0-1 N-sodium hydroxide solution (free from alcohol) and leave for twenty minutes. Make faintly acid with dilute sulphuric acid and titrate back with 0-1 N-sodium thiosulphate solution. One equivalent of iodine corresponds to 0-5 mole of reducing biose, or 1 c.c. of 0-1 N-iodine solution to 17-1 mg. of maltose. What is the course of the reaction ... 

In another situation, a known excess quantity of standard iodine solution is added in the substance (a reducing agent) to be assayed and then the excess iodine may be titrated with the help of standard sodium thiosulphate solution, such as the estimation of sodium bisulphite ... 

Consequently, the equivalent amount of iodine generated by the above reaction may be conveniently assayed by titration against a standard sodium thiosulphate solution. In this context a point of caution must be observed while KI is being oxidized under a strongly acidic medium so as to avoid simultaneous oxidation of the iodide by atmospheric oxygen that may result high erroneous titer values leading to false estimations. 

In such estimations, the pharmaceutical substances can be measured either directly or back titration of excess iodine with sodium thiosulphate solution. 

Step 3 D-Penicillamine thus obtained is oxidised quantitatively by iodine to give rise to a disulphide, as expressed in the following equation whereas, the excess iodine is back titrated with 0.02 N sodium thiosulphate solution ... 

Theory Chlorinated lime reacts with acetic acid to produce a mole each of calcium acetate, hydrochloric acid and hydrochlorous acid. The two acids interact to give water and chlorine, and the latter reacts with HI to liberate iodine that can be estimated by titrating with 0.1 N sodium thiosulphate solution. The various reactions involved may be expressed as given below ... 

Procedure Weigh accurately about 0.5 g of ferric ammonium citrate and dissolve the sample in 15 ml DW. Add to it slowly 1 ml of sulphuric acid and warm gently to attain a yellow colouration so as to decompose the iron and ammonium citrate complex completely. Cool and add 0.1 N potassium permanganate solution dropwise from a burette to obtain a pink colour that persists for 5 seconds. To the resulting solution add hydrochloric acid 15 ml and potassium iodide 2.0 g, shake well and set aside for 3 minutes so that iodine may be liberated completely. Now, add 60 ml of water and titrate with 0.1 N sodium thiosulphate solution while shaking the contents continuously till a colourless end-point is achieved. 

Materials Required Thyroid gland dried 1.0 g anhydrous potassium carbonate 17.0 g bromine solution (9.6 ml of Br2 and 30 g of KBr in 100 ml DW) 7.0 ml dilute phosphoric acid (10% w/v) 42.0 ml starch iodide paper phenol solution (saturated solution of phenol in water) 5.0 ml potassium iodide solution (10% w/v in water) 0.01 N sodium thiosulphate solution starch solution. 

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