Laboratory Methods of Inorganic Chemistry, 2nd English Ed. 1928

(singke) #1

220 COMPOUNDS OF THE RARE ELEMENTS.


water; again evaporate the solution to dryness, and dehydrate
the residue completely by heating to about 160°. Extract the
residue with absolute alcohol either in a Soxhlet apparatus or in
a simple flask with a return condenser. In the latter case, extract
eight times and distil each of the alcoholic solutions poured from
the insoluble residue, using the alcohol, thus recovered, for the
next extraction. Finally, after all of the alcohol has been dis-
tilled from the extract, dissolve the salt in a little water and
precipitate lithium carbonate by adding ammonium carbonate
and a little ammonia. From lepidolite 1 to 3 g. of pure lithium
carbonate should be obtained, from petalite a little more, and
from spodumene about twice as much. Test the purity of the
preparation by means of the spectroscope.
The insoluble salt left by the alcoholic extraction contains
rubidium, besides other of the alkali metals. Dissolve it in
water, treat the solution with about 1 c.c. of 10% chlorplatinic
acid solution, and allow it to stand over night. Next morning
filter off the insoluble chlorplatmates and ignite them in a Rose
crucible in a current of hydrogen. Dissolve the residue in a
little water and test it with the spectroscope for rubidium.

Spectroscopic Analysis.

The scale of the spectroscope, which is usually graduated arbi-
trarily, must first be standardized according to the wave lengths
of light. After the apparatus is properly set up, make the
sodium line fall upon a certain division of the scale; or, in case


the scale telescope is not movable, observe the position of this


line as accurately as possible. Then note the position of the


following lines:


Kared
Lia red
Na yellow
Tl green

768


671


589


535


Wave Length
X 10-e mm.

it
it

Src
Ha
H/3
Hv

blue
red
blue
violet

Wave Length
461 X 10-"mi
656
486
434

The hydrogen lines are very sharp and easy to observe; ready


prepared tubes filled with hydrogen under diminished pressure
can be used, and are to be excited by means of an induction coil.


Plot the scale readings as abscissas and the corresponding wave

Free download pdf