Beruflich Dokumente
Kultur Dokumente
+ 3OH
2Bi+ 3Sn(OH)
6
2-
CuS, Bi
2
S
3
+ NO
3
-
Cu
2+
, Bi
3+
+ S+ NO
Separating the
Arsenic Subgroup
Soln 2-6
SnCl
6
2-
, SbCl
4
Discard
Residue
SbTest Sn test
Sb
2
S
3(s)
(orange)
Soln 2-2 (arsenic subgroup)
SbS
3
3-
, SbO
3
3-
, SnS
3
2-
, SnS
2
OH
(aq)
SnCl
6
2-
+3H
2
C
2
O
4
Sn(C
2
O
4
)
3
2-
(stable)
SbCl
4
-
+ H
2
S Sb
2
S
3
(orange)
Sn
2+
+2HgCl
2
Hg
2
Cl
2(s)
+Sn
4+
+2Cl
-
8
Procedure 1: Separating Copper and
Arsenic Subgroups
Add 13%TA
Warm in hot water
Produce sulfide ppt
Centrifuge
Balance diagonally
Separate ppt and
liquids by decantation
1) 1 d 6 M NH
4
Cl/20 d H
2
O to
wash ppt, then cfg.
2) 10 d 0.5 M KOH to ppt
3) Heat in boiling water bath
4) Cfg.
Sulfide ppt
Ppt 2-2
Copper subgroup
CuS, Bi
2
S
3
Soln 2-2
Arsenic subgroup
Contains Sn
4+
, Sb
3+
9
Separating Copper Subgroup:
Using HNO
3
to dissolve CuS, Bi
2
S
3
3(CuS, Bi
2
S
3
)
(s)
+ 2NO
3
-
(aq)
+ 8H
+
(aq)
3(Cu
2+
Bi
3+
)
(aq)
+ 2NO
(g)
+ 3S+ 4H
2
O
The water bath should be at boiling
Mix the HNO
3
and ppt thoroughly
Heat to the black sulfides disappear, and the solution appears to be
off-white for elemental sulfur forms
Heat till reaction starts
(starts to bubble)
Ppt is dissolved and appears
white and milky
Add 5 d water and 6 M HNO
3
Heat in boiling water bath
Ppt 2-2
Copper
subgroup
CuS, Bi
2
S
3
1 d 0.2 M NH
4
NO
3
/
20 dH
2
O to wash ppt, cfg.
10
Separating and Identifying:
Cu
2+
and Bi
3+
Centrifuge
Cfg. and
take
supernatant
Contains
Cu
2+
, Bi
3+
Sodium stannite reagent: freshly prepared, NaSn(OH)
3
Do not add more NaOH when dissolved. (Approx. 3 d)
3(aq)
NaOH
2(s)
NaOH
2(aq)
Sn(OH) Sn(OH) SnCl
(aq) (aq)
Add conc.
ammonia to
basic
Cu(NH
3
)
4
2+
Bi
Add sodium
stannite reagent
(confirm with litmus test)
11
Separating and Identifying:
Sn
4+
and Sb
3+
in Arsenic Subgroup
SbS
3
3-
+ SbO
3
3-
+ 6H
+
Sb
2
S
3(s)
(orange) + 3H
2
O
SnS
2
OH
-
+ H
+
SnS
2(s)
(yellow) + H
2
O
Copper
subgroup
Arsenic
subgroup
Soln 2-2
Contains
Sn
4+
, Sb
3+
Add conc.
HCl slowly
Evaporate
Dissolves when
heated
Excess conc.
HCl
1/4small spatula H
2
C
2
O
4(s)
2 d 13%TA
Heat
Small Al strips / HCl
Heat till dissolve, cfg.
Add HgCl
2
to liquid portion
Sb
Sn
12
Holding the Evaporating Dish
Using Crucible Tongs
13
Evaporating Dish and Crucible Tongs
14
Reagent
Cations
13 % TA HNO
3(aq)
Ammonia Sodium stannite
Bi
3+
Black-brown
ppt
2Bi
3+
+ 3S
2-
Bi
2
S
3(s)
Ppt dissolves
Bi
2
S
3(s)
+ NO
3
-
Bi
3+
+ S
(s)
+
NO
(g)
White ppt
Bi
3+
(aq)
+ OH
-
Bi(OH)
3(s)
Black ppt
2Bi(OH)
3(s)
+
3Sn(OH)
3
-
+
3OH
-
2Bi
(s)
+
3Sn(OH)
6
2-
Cu
2+
Black ppt
Cu
2+
+ S
2-
CuS
(s)
Ppt dissolves
CuS
(s)
+NO
3
-
Cu
2+
+ S
(s)
+
NO
Dark blue
solution
Cu
2+
+ 4NH
3
Cu(NH
3
)
4
2+
Theoretical Results and
Chemical Equations
15
Reagent
Cations
13 % TA KOH
(aq)
Concentrated ammonia
Sb
3+
Orange ppt
2Sb
3+
+ 3S
2-
Sb
2
S
3(s)
Ppt dissolves
Sb
2
S
3(s)
+ 6OH
-
SbS
3
3-
+ SbO
3
3-
+ 3H
2
O
Produces orange ppt first, then
disappears
SbS
3
3-
+ SbO
3
3-
+ 6H
+
Sb
2
S
3(s)
+ 3H
2
O
Sb
2
S
3(s)
+ 6H
+
+ 8Cl
-
SbCl
4
-
+ 3H
2
S
Sn
4+
Yellow ppt
Sn
4+
+ 2S
2-
SnS
2(s)
Ppt dissolves
SnS
2(s)
+ OH
-
SnS
2
OH
-
SnS
2(s)
+S
2-
SnS
3
2-
Produces yellow ppt first, then disappears
SnS
2
OH
-
+ H
+
SnS
2(s)
+ H
2
O
SnS
2(s)
+ 4H
+
+ 6Cl
-
SnCl
6
2-
+ 2H
2
S
Theoretical Results and
Chemical Equations
16
Reagent
Cations
Al + H
+
HgCl
2
H
2
C
2
O
4
+ TA
Sb
3+
Orange ppt
SnCl
6
2-
+ H
2
C
2
O
4
Sn(C
2
O
4
)
3
2-
+ 6H
+
+ 6Cl
-
(stable)
SbCl
4
-
+ 3H
2
S
Sb
2
S
3(s)
+ 6H
+
+ 8Cl
-
Sn
4+
Clear solution
Sn
4+
+ Al
Sn + Al
3+
Sn + 2H
+
Sn
2+
+ H
2
White(Hg
2
Cl
2
) black(Hg)
ppt
Sn
2+
+ 2HgCl
2
Hg
2
Cl
2(s)
+ Sn
4+
+ 2Cl
-
Sn
2+
+ Hg
2
Cl
2
2Hg
(s)
+ Sn
4+
+ 2Cl
-
Theoretical Results and
Chemical Equations
17
Cu
2+
Bi
3+
Sb
3+
Sn
4+
Expected Results
Save the
resulting
solutions for the
TA to check
18
Using the Centrifuge
Use centrifuge tubes (pointed ended), do not use normal
test tubes (round ended)
Centrifuge tubes should be placed in opposite sides to
keep balanced
The lid should be closed during use; the centrifuge should
be started from slow to check if there are unusual sounds,
then the speed can be increased
If there are unusual sounds or movement in the centrifuge,
the power should be turned off first for it to be fixed
There must be at least one person watching the centrifuge
when in use
Centrifuge for approx. 1~2 min, open lid when the
centrifuge has completely stopped
Methods for mixing solutions completely:
(1) Use stirring rod, (2) shake/flick, (3) Use Vortex mixer
Wear gloves
Always use test tube holders, test tube racks,
and crucible tongs
Do not take excess chemicals to avoid
pollution
Add reagents on top of the centrifuge tube to
avoid contamination of chemicals
Label the centrifuge tubes
Solutions must be mixed thoroughly after
adding reagents: flicking, vortex mixer, or
stirring rod
Dip solution on testing paper to determine
acidity
All heating should be done in the hood
Conc. ammonia and HCl is in hood
Recycle heavy metal waste
19
Cautions