Qualitative analytical chemistry I experiments

Qualitative Analysis
of
The Group I Cations
Wimbo triono
331501!00
"niversity of #a$arta
I% &urpose
1% 'eparatin( the (roup I cations from sample
)% In*entifyin( the (roup I cations use speci+c rea(ent
3% ,no-in( chemical properties of (roup I cations
II% .asic of theory
In the classical /ualitative analysis scheme0 the +rst ion -hich
are *etermine* are A(
1
0 &b
)1
0 an* 2(
)
)1
% 3f all the commons cations0
only these form insoluble chlori*es un*er aci*ic con*itions% These
cations comprise Group I in the scheme an* are separate* from
(eneral salt solution by precipitation of their chlori*es at a p2 of
about 4ero% The chlori*e precipitate is then analy4e* the possible
presence of silver0 lea* an* mercury 5I6 on the basic of the
characteristic properties of those cations%
'ilver has only a fe- -ater soluble salts0 of -hich the nitrate is
certainly the most common% 7ost of the insoluble silver salts
*issolve in col* 8 7 293
3
0 the main exceptions bein( the silver
hali*es0 A('C9 an* A(
)
'% 'ilver ion forms many stable complexes:
of these0 the best $no-n is probably the A(592
3
6
)
1
ion% This comlex
is su;ciently stable to be pro*uce -hen A(Cl or A('C9 is treate*
-ith 8 92
3
: the reaction -hich occurs is usefull for *issolvin( those
soli*s% A(.r an* A(I are less soluble than A(Cl: A(.r -ill (o into
solution in 15 7 92
3
0 but A(I is so insoluble that it -ill not% The silver
Thiosulfate complexe ion0 A(5'
)
3
3
6
)
3<
0 is extremly stable0 an* is
important in photo(raphy0 -here it is forme* in the =+xin(> reaction
in -hich A(.r is remove* from the *evelope* ne(ative%
?ea* nitrate an* acetate are the only -ell $no-n soluble lea*
salts% ?ea* chlori*e is not nearly as insoluble in -ater as are the
chlori*es of silver an* mercury 5I60 an* becomes mo*erately soluble
if the -ater is heate*% &b'3
@
is ion of the relatively fe- insoluble
sulfates% ?ea* forms a stable hy*roxi*e complex ion an* a -ea$
chlori*e complex% Althou(h lea* or*inarily has an oxi*ation number
of 1)0 there are some &b 5IA6 compoun*s0 of -hich thenist cinnib us
&b3
)
5bro-n60 this compoun* is insoluble in most rea(ents0 but -ill
*issolve in 8 7 293
3
to -hich some 2
)
3
)
has been a**e*%
7ercury 5I6 has only one soluble salt0 the nitrate0 an* even -ith
this compoun*0 excess 293
3
must be present to $eep basic 2(5I6
salts from precipitatin(% The 2(5I6 ion0 sometimes calle* mercurous
ion0 is relatively unstable0 it -ill slo-ly oxi*i4e to 2(5II6 if expose* to
air0 an* can be re*uce* to the metal by re*ucin( cations 5e%(% 'n
)1
6%
In the presence of species that reaction to 2( 5soli*0 blac$6 an* the
2(5II6 compoun*% 7ercury5I6 chlori*e has a very characteristic
raction -ith amoniaB
2(
)
Cl
)
5s6 1 ) 92
3
5a/6 <C 2(5s6 1 2(92
)
Cl5s6 1 92
@
1
5a/6 1 Cl
<
5a/6
III% Instruments an* materials

Instruments D 7aterial
1% &ipete 1% 2Cl
)% .ea$er (lass )% 92@32
3% 'emimicro test tube 3% A/uare(ia
@% Centrifu(e tube
5% Eilter paper
8% funnel
IA% &roce*ure
1% To 3 ml of sample in a test tube0 a** 005 ml 8 7 2Cl% 'tir -ell an*
centrifu(e% Fecant the li/ui*0 into a test tube% To ma$e sure
precipitation of (roup I cations -as complete0 a** 1 *rop of 8 7
2Cl to the li/ui*% Wash the precipitate -ith ) ml -ater an* 3
*rops of 8 7 2Cl% 'tir -ell sentrifu(e an* *iscar* the -ash li/ui*%
Wash the precipitate a(ain -ith -ater an* 2Cl0 centrifu(e an*
*iscar* the -ash%
)% To the precipitate from step 10 -hich contains the chlori*es of the
(roup I cations0 a** about @ ml -ater% 2eat in the bolilin( -ater
bath for at least three minutes0 stirrin( constantly0 centrifu(e
/uic$ly an* *ecant the li/ui*0 -hich may contains &b
)1
0 in test
tube
3% Con+mation of the presence of lea*% To the li/ui* from step ) a**
) *rops of 8 7 acetic aci* an* 3 or @ *rops of 1 7 ,
)
Cr3
@
% The
formation of a yello- precipitate con+rms the presence of lea*%
Centrifu(in( out the soli* may help -ith the i*enti+cation0
because the li/io* phase is oran(e%
@% Con+rmation of the presence of mercury% If lea* is present0 -ash
the precipitate from step ) -ith 8 ml -ater in the boilin( -ater
bath% Centrifu(e an* test the li/ui* for &b
)1
% Continue the
-ashin(s until no positive reaction to the lea* test is obtaine*% To
the -ashe* precipitate a** ) ml 8 7 92
3
an* stir -ell% A blac$ or
*ar$ (ray precipitate estabilish the presence of the mercury 5I6
ion% Centrifu(e an* *ecant the li/ui*0 -hich may contain
A(592
3
6
)1
0 into test tube% I*enti+yin( +ltrat for A( ion%
A% Fata of experiments
sample Gxperiments result
'ample12C? A -hite precipitate
&recipitate 1 2ot -ater
Eiltrate 1 ,)Cr3@
HHHH1 9a32
2alf of precipitate solute
An yello- precipitate
&recipitate soluble
&recipitate 1 92@32
Eiltrate 1 ,I
HHHH1 9a32
HHHH1 ,)Cr3@
A (ray precipitate
A (reen precipitate
&recipitate soluble
An oran(e precipitate
&recipitate 1 A/uare(ia
Eiltrate 1 ,I
HHH%%1 9a32
A -hite precipitate
A re* precipitate
A -hite precipitate
AI% Analysis of *ata
'ample that -ill i*entifyin( compose li/ui* an* un$no-n
precipitate% 'o0 precipitate in sample have to *issolve* berfore
i*enti+cation% Assume that *issolvin( use* 2)3 -ill cause
precipitation of phosphate of (roup III0 IA cations an* ma(nesium0
*issolvin( sample use* 2933% The un$no-n precipitate ha*
*issolve*%
2Cl 8 7 a** into sample% A -hite percipitate forme* an*
establish the presence of (roup I cations% Chlori*es from other
cations -ill *issolve0 except (roup I cations% Centrifu(e an* *ecant
the li/ui* into test tube%
A(
1
1 &b
)1
1 2(
)
)1
<C A(Cl
5'6
1 &bCl
)5s6
1 2(
)
Cl
)5s6
&recipitate -hich may contains &b)
1
0 A(
1
an* 2(5I6 -ash -ith hot
-ater% &bCl
)
-hich soluble in hot -ater -ill *issolve% The -ash li/ui*
use for i*enti+cation of &b
)1
% The -ash li/ui* *ivi*e into t-o test
tube% ,
)
Cr3
@
a**e* into +rst test tube0 a yello- precipitate in*icates
the presence of &b
)1
% The secon* test tube a**e* 9a32 excess0 no
precipitate result from these because &b
)1
-ill be complex ions -ith
hi*roxi*e%
&bCl
)5s6
<C &bCl
)5A/6
&bCl
)5a/6
1 ,
)
Cr3
@
<C &bCr3
@5s6
1 ),Cl
The precipitate from separatin( &b
)1
a**e* 92
@
32 in or*er to
separate A(Cl from 2(
)
Cl
)
% A(Cl *issolve in 92
@
32 excess form ion
complex -hile 2(5I6 form precipitate of 2( an* 2(592
)
6Cl% A -hite
precipitate -hich slo-ly become (ray in*icates the presence of
2(5I6%
A(Cl 1 92
3
<C IA(592
3
6
)
J
1
1 Cl
<
2(
)
Cl
)
1 92
3
<C 2(
5s6
1 2(592
)
6Cl
5s6
1 92
@1
1 Cl
<
Centrifu(e an* *ecant the li/ui* into a test tube% To con+m the
presence of mercury0 precipitate *issolve* in a/uare(ia% The (ray
precipitate become -hite because of 2( *issolve in 293
3
but
2(592
)
6Cl not% A -hite precipitate in*icates 2(592
)
6Cl% The li/ui*
a**e* ,I to ma$e a re* precipitate0 from experiments re* precipitate
forme* an* establish the presence of mercury in the sample%
?i/ui* from separatin( A(Cl from 2(
)
Cl
)
use* to i*entify A(
1
in
sample% .ase* on experiments0 the presence of A(
1
in sample
cannot be sure because the experiments results are *iKerent -ith
theory%
AII% Tas$
Write chemical e/uations for each step

2C? 8 m
A(
1
1 &b
)1
1 2(
)
)1
<C A(Cl
5'6
1 &bCl
)5s6
1 2(
)
Cl
)5s6

2ot -ater
&bCl
)5s6
<C &bCl
)5A/6

,
)
Cr3
@
&bCl
)5a/6
1 ,
)
Cr3
@
<C &bCr3
@5s6
1 ),Cl

9a32
&bCl
)
1 )9a32 <C &b5326
)5s6
1 9aCl
%%%%%%%%%%%%%1 )9a32 excess <C 9a
)
I&b5326
@
J

92
3
A(Cl 1 92
3
<C IA(592
3
6
)
J
1
1 Cl
<
2(
)
Cl
)
1 92
3
<C 2(
5s6
1 2(592
)
6Cl
5s6
1 92
@1
1 Cl
<

293
3
82(
5s6
1 293
3
<C 2(
)
)1
1 )93 1 893
3
<
1 @2
)
3
AIII% Conclusion
1% The Group I cations is presence in the sample
)% &bCl
)
*issolve in hot -ater0 but A(Cl an* 2(
)
Cl
)
cannot
3% I*entify &b
)1
use ,
)
Cr3@ an* 9a32 establish the presence of
&b
)1
in the sample
@% I*entify 2(
)
)1
use 92
3

establish the presence of 2(
)
)1
in
sample
5% 'ample contains lea* an* mercury
IL% .iblio(raphy
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