FREE BOOKS

Author's List




PREV.   NEXT  
|<   63   64   65   66   67   68   69   70   71   72   73   74   75   76   77   78   79   80   81   82   83   84   85   86   87  
88   89   90   91   92   93   94   95   96   97   98   99   100   101   102   103   104   105   106   107   108   109   110   111   112   >>   >|  
was used to liberate the iodine when it was prepared. It may be purified by sublimation after mixing it with a little potassium iodide, which reacts with the iodine chloride, forming potassium chloride and setting free the iodine. The sublimed iodine is then dried by placing it in a closed container over concentrated sulphuric acid. It may then be weighed in a stoppered weighing-tube and dissolved in a solution of potassium iodide in a stoppered flask to prevent loss of iodine by volatilization. About 18 grams of the iodide and twelve grams of iodine per liter are required for an approximately tenth-normal solution. An iodine solution made from commercial iodine may also be standardized against arsenious oxide (As_{4}O_{6}). This substance also usually requires purification by sublimation before use. The substances usually employed for the standardization of a thiosulphate solution are potassium bromate and metallic copper. The former is obtainable in pure condition or may be easily purified by re-crystallization. Copper wire of high grade is sufficiently pure to serve as a standard. Both potassium bromate and cupric salts in solution will liberate iodine from an iodide, which is then titrated with the thiosulphate solution. The reactions involved are the following: (a) KBrO_{3} + 6KI + 3H_{2}SO_{4} --> KBr + 3I_{2} + 3K_{2}SO_{4} + 3H_{2}O, (b) 3Cu + 8HNO_{3} --> 3Cu(NO_{3})_{2} + 2NO + 4H_{2}O, 2Cu(NO_{3})_{2} + 4KI --> 2CuI + 4KNO_{3} + I_{2}. Two methods for the direct standardization of the sodium thiosulphate solution are here described, and one for the direct standardization of the iodine solution. !Method A! PROCEDURE.--Weigh out into 500 cc. beakers two portions of about 0.150-0.175 gram of potassium bromate. Dissolve each of these in 50 cc. of water, and add 10 cc. of a potassium iodide solution containing 3 grams of the salt in that volume (Note 1). Add to the mixture 10 cc. of dilute sulphuric acid (1 volume of sulphuric acid with 5 volumes of water), allow the solution to stand for three minutes, and dilute to 150 cc. (Note 2). Run in thiosulphate solution from a burette until the color of the liberated iodine is nearly destroyed, and then add 1 cc. or 2 cc. of starch solution, titrate to the disappearance of the iodo-starch blue, and finally add iodine solution until the color is just restored. Make a blank test for the amount of thiosulphate solution required to react with the iodi
PREV.   NEXT  
|<   63   64   65   66   67   68   69   70   71   72   73   74   75   76   77   78   79   80   81   82   83   84   85   86   87  
88   89   90   91   92   93   94   95   96   97   98   99   100   101   102   103   104   105   106   107   108   109   110   111   112   >>   >|  



Top keywords:

solution

 
iodine
 

potassium

 
thiosulphate
 

iodide

 

sulphuric

 

standardization

 

bromate

 

dilute

 

direct


volume

 

required

 
stoppered
 

chloride

 

sublimation

 

purified

 
starch
 

liberate

 
Method
 

PROCEDURE


amount
 

beakers

 

methods

 

sodium

 

liberated

 

burette

 

volumes

 

mixture

 

minutes

 

destroyed


titrate

 

finally

 

portions

 
restored
 
Dissolve
 

disappearance

 

crystallization

 
twelve
 

volatilization

 

dissolved


prevent

 

commercial

 

standardized

 

approximately

 

normal

 
weighing
 

reacts

 
forming
 

mixing

 

prepared