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The Extraction of Tin From Its Ores and The Preparation and Behavior of Certain Pmesaltsoftin
The Extraction of Tin From Its Ores and The Preparation and Behavior of Certain Pmesaltsoftin
by
Harry Borden M a r s h a l l
CHEMISTRY
The U n i v e r s i t y of B r i t i s h Columbia
A p r i l - 1931.
TABLE OF CONTENTS
INTRODUCTION.
1. P r e p a r a t i o n of Stannic C h l o r i d e .
2. P r e p a r a t i o n o f Caesiian 0hloride.
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3. Method.
INTRODUCTION.
The existence of isotopes has explained a great many-
d i s c r e p a n c i e s i n the theory of atomic s t r u c t u r e . I t has also
d e f i n i t e l y s e t t l e d the v a l i d i t y o f the whole number r u l e f o r
the atomic weights of the elements. Henee any experimental
work whieh w i l l corroborate the existence o f i s o t o p e s , w i l l
be o f great importance i n strengthening the proof of the
atomic Theory.
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F. W. Aston, by u s i n g the p o s i t i v e ray spectograph, and
p l a t e s of i n c r e a s e d s e n s i t i v i t y to p o s i t i v e rays, has found
i t p o s s i b l e t o d e f i n i t e l y prove that a group of eight l i n e s ,
corresponding approximately t o atomic weights of 116, 117,
118, 119, 120, 121, 122, 124, was due t o T i n . I t i s extremely
l i k e l y that these eight i s o t o p e s do e x i s t i n the case of t i n ,
but as y e t no d i r e c t chemical evidence has proven t h e i r
existence.
One method of a t t a c k i n g t h i s problem i s t o determine the
atomic weight of t i n i n i t s d i f f e r e n t ores. Due to extremely
d i f f e r e n t g e o l o g i c a l formation there may be wide v a r i a t i o n s
i n the concentration of the isotopes i n these d i f f e r e n t ores.
Such a v a r i a t i o n might be detected by separate atomic weight
determinations of the t i n i n the d i f f e r e n t samples.
T h i s was the o r i g i n a l problem attempted. However, the
e x t r a c t i o n of t i n from i t s ores proved to c o n s t i t u t e a
problem i n i t s e l f , and t h i s t h e s i s w i l l deal l a r g e l y w i t h
t h i s p a r t of the work, together w i t h the preparation of pure
t i n from the m a t e r i a l e x t r a c t e d .
3. The D i s i n t e g r a t i o n of Stannite.
Very l i t t l e study has been made of the d i s i n t e g r a t i o n
of s t a n n i t e ores. A c c o r d i n g l y those methods which are
s u c c e s s f u l i n f u s i n g C a s s i t e r i t e , were also t r i e d w i t h stannite
with varied results.
5. The P u r i f i c a t i o n of Stannite T i n .
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gave a value f o r the atomic weight of t i n whieh was much too
high, i n d i c a t i n g that the weight of the p r e c i p i t a t e was
correspondingly low. Moreover, on evaporating the f i l t r a t e
and wash water a number of c r y s t a l s s e t t l e d out. As the
f i l t r a t e should contain nothing but a s l i g h t concentration of
caesium c h l o r i d e , i t was concluded that the low r e s u l t s could
be a t t r i b u t e d to the s o l u b i l i t y o f caesium ehlorostannate.
Two more determinations were made taking greater
precaution to decrease an e r r o r due to s o l u b i l i t y and more
accurate values were obtained. This j u s t i f i e s the assumption
that the e r r o r i s due at l e a s t i n part to s o l u b i l i t y .
As very l i t t l e work has been done on t h i s compound i t
was considered necessary to obtain more d e f i n i t e information
on i t s s o l u b i l i t y i n v a r i o u s concentrations of h y d r o c h l o r i c
a c i d and caesium c h l o r i d e . Such information would enable us
to s t a t e more d e f i n i t e l y whether t h i s method i s s u i t a b l e or
not f o r atomic weight determinations, and i f so, the most
s u i t a b l e concentration f o r p r e c i p i t a t i o n . Accordingly, t h i s
has c o n s t i t u t e d another phase of the i n v e s t i g a t i o n .
Apparatus.
I n order to a g i t a t e the s o l u t i o n s at a constant
temperature u n t i l the e q u i l i b r i u m of s a t u r a t i o n was obtained,
a g r a n i t e k e t t l e of f o r t y l i t r e s capacity was nearly f i l l e d
w i t h water and covered w i t h a t h i c k l a y e r of f e l t to prevent
radiation. The water was maintained at constant temperature
by a tungsten lamp which was c o n t r o l l e d by a thermostat and
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relay. The temperature remained w i t h i n .05 of SO with t h i s
apparatus. Pyrex t e s t tubes of twenty-five c c . capacity
were used and rubber stoppers which had been p r e v i o u s l y b o i l e d
f o r s e v e r a l hours w i t h ammonium hydroxide.
Method of Determination.
To the tubes were added twenty-five c c . of s o l u t i o n , and
somewhat more of the caesium chlorostannate than would
d i s s o l v e i n that p a r t i c u l a r concentration. The s a l t was
prepared as i n the determinations above. The rubber stoppers
were then wired i n and the tubes attached to the s t i r r i n g
apparatus and rotated f o r twenty-four hours.
In order to determine how much of the s a l t had d i s s o l v e d ,
the t e s t tube was placed i n the bath so that the top just
stood above the water. A f t e r the excess s o l i d had s e t t l e d
to the bottom, the l i q u i d was drawn up i n t o the c a l i b r a t e d
p i p e t t e and two t e n c.e. p o r t i o n s withdrawn. The t i p of the
p i p e t t e was prepared by t y i n g a f i l t e r paper around i t w i t h
a small piece of s i l k thread. I n t h i s manner the p o s s i b i l i t y
of s o l i d p a r t i c l e s being drawn o f f was e l i m i n a t e d .
The twenty c.e. p o r t i o n s of l i q u i d were c a r e f u l l y
evaporated i n small p o r c e l a i n c r u c i b l e s , and the amount
d i s s o l v e d taken as the weight of the residue obtained on
evaporation.