FREE BOOKS

Author's List




PREV.   NEXT  
|<   53   54   55   56   57   58   59   60   61   62   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   >>   >|  
n most common use are iron wire, ferrous ammonium sulphate, sodium oxalate, oxalic acid, and some other derivatives of oxalic acid. With the exception of sodium oxalate, these all contain water of crystallization which may be lost on standing. They should, therefore, be freshly prepared, and with great care. At present, sodium oxalate is considered to be one of the most satisfactory standards. !Method A! !Iron Standards! The standardization processes employed when iron or its compounds are selected as standards differ from those applicable in connection with oxalate standards. The procedure which immediately follows is that in use with iron standards. As in the case of the bichromate process, it is necessary to reduce the iron completely to the ferrous condition before titration. The reducing agents available are zinc, sulphurous acid, or sulphureted hydrogen. Stannous chloride may also be used when the titration is made in the presence of hydrochloric acid. Since the excess of both the gaseous reducing agents can only be expelled by boiling, with consequent uncertainty regarding both the removal of the excess and the reoxidation of the iron, zinc or stannous chlorides are the most satisfactory agents. For prompt and complete reduction it is essential that the iron solution should be brought into ultimate contact with the zinc. This is brought about by the use of a modified Jones reductor, as shown in Figure 1. This reductor is a standard apparatus and is used in other quantitative processes. [Illustration: Fig. 1] The tube A has an inside diameter of 18 mm. and is 300 mm. long; the small tube has an inside diameter of 6 mm. and extends 100 mm. below the stopcock. At the base of the tube A are placed some pieces of broken glass or porcelain, covered by a plug of glass wool about 8 mm. thick, and upon this is placed a thin layer of asbestos, such as is used for Gooch filters, 1 mm. thick. The tube is then filled with the amalgamated zinc (Note 1) to within 50 mm. of the top, and on the zinc is placed a plug of glass wool. If the top of the tube is not already shaped like the mouth of a thistle-tube (B), a 60 mm. funnel is fitted into the tube with a rubber stopper and the reductor is connected with a suction bottle, F. The bottle D is a safety bottle to prevent contamination of the solution by water from the pump. After preparation for use, or when left standing, the tube A should be filled with water,
PREV.   NEXT  
|<   53   54   55   56   57   58   59   60   61   62   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   >>   >|  



Top keywords:
standards
 
oxalate
 
reductor
 
agents
 

bottle

 

sodium

 

reducing

 

oxalic

 

titration

 

excess


brought

 

solution

 

ferrous

 

diameter

 

inside

 

filled

 

satisfactory

 
processes
 
standing
 

thistle


extends

 

connected

 
funnel
 

Figure

 

fitted

 

rubber

 
preparation
 

standard

 

Illustration

 
quantitative

apparatus

 
asbestos
 

prevent

 

filters

 
amalgamated
 

safety

 

stopper

 

broken

 

shaped

 

pieces


stopcock

 
porcelain
 
suction
 

covered

 

contamination

 

gaseous

 

Standards

 

standardization

 

employed

 
Method