Studies on Alloys 
123 
meyer flask and were treated with 15 or 20 cc. of concentrated 
sulphuric acid and 2 to 4 grams of potassium sulphate. Heat 
was applied till the melt was perfectly white, but care was taken 
not to drive off* all the sulphuric acid. The samples were then 
cooled and diluted with 50 cc. of water and 10 to 15 cc. of 
strong hydrochloric acid added. Heat was applied till all pos- 
sible had passed into solution. The flask was cooled and the con- 
tents rinsed into a 600 cc. beaker and diluted to 400 or 500 cubic 
centimeters and then titrated with the permanganate solution. 
The results of the estimation will be found at the end of this 
paper. 
The method just described involves a radical departure from 
Mr. Low’s method. Mr. Low advocates the use of hydrochloric 
acid solution for the titration of the antimony in which the con- 
tent of HCl is about 10 per cent the volume of the solution. At- 
tempts to use such a concentration ended in utter failure at lab- 
oratory temperatures, 20° to 22°. Very shortly after the per- 
manganate was added the solution turned yellow, evolved the 
odor of chlorine and threw down a brown precipitate, all of which 
showed that the permanganate was being decomposed by the 
hydrochloric acid present. The decomposition was so energetic 
that absolutely no end point could be observed. The concentra- 
tion recommended by Mr. Low is somewhat greater than that 
recommended by Fresenius and Sutton, but these authors also 
recommend the addition of Magnesium sulphate or other similar 
agent. In these experiments the volume of the acid was reduced 
to the proportions stated above. 
The solution in which the antimony had been estimated was 
poured into a round bottomed flask, was rinsed out with 50 cc. 
of strong- HCl, the rinsings being added to the contents of the 
flask. The solution at this point was made to contain one-fifth 
its volume of strong hydrochloric acid. There was then added 
about one gram of finely powdered antimony. The flask was 
shaken well and the contents digested on a water-bath till the vol- 
ume was about 300 cc. The flask was next connected with an 
apparatus for delivering a rapid stream of CO2, connection being 
made so that bubbles of the gas passed rapidly through the solu- 
tion. While the gas was passing, the flask was heated to boiling 
and maintained at the temperature for about fifteen minutes. 
This was long enough to secure the reduction of all the tin. While 
