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ANIONS
I. Experiment Title : Analysis of Cations and Anions
II. Experiment Date : October 18th, 2014 at 07.00 am
III. End of The Experiment : October 18th, 2014 at 10.40 am
IV. Experiment Purpose :
1. To determine the cation which can be found in the analite
2. To determine the anion which can be found in the analite
V. Basic Theory
A. Qualitative Analysis
Cations are divided into five groups. A specific reagent for each group is used
for their separation from the solution. This separation is done in a particular se-
quence because some ions of prior groups can also react with the reagent of later
groups.
The obtained filtrate after first group analysis is used for the test of se-
cond group. Usually Pb2+ is also included in the 2nd analytical group because
the solubility of PbCl2 is more than the chlorides of other two ions.
Confirmation Test
Lead (Pb2+) Silver (Ag+) Mercury (Hg2+)
Pb2+ + 2KI → PbI2 + 2 K+ Ag+ + KI → AgI + K+ Hg22++ 2KI → Hg2I2 + 2K+
Pb2+ + K2CrO4 → PbCrO4 + 2Ag+ + K2CrO4 → 2Hg22+ + 2NaOH → 2Hg2O
2K+ Ag2CrO4 + 2K+ + 2Na+ + H2O
2. Group II Cations
Cations: Cd2+, Bi3+, Cu2+, As3+, As5+, Sb3+, Sb5+, Sn2+, Sn4+ and Hg2+
The group reagent is H2S (at 0.2 - 0.3 M) which gives S2− ions in solutions.
The tests are conducted in presence of dilute HCl to keep the S2- ion concen-
tration at a minimum level. This round of tests helps only in second 2nd gro-
up cations precipitation. The cations precipitation of the 4th group if present
The precipitate colour and the presence of the respective ions are shown
in the table below.
Precipitate Colour Presence of Cation
Reddish brown or black precipitate Bi3+, Cu2+, Hg2+ or Pb2+
Yellow precipitate Cd2+ or Sn4
Brown precipitate Sn2+
Red orange Sb3+
Cations: Fe2+, Fe 3+, Al3+, Cr3+, Cr4+, Co2+, Mn2+, Mn4+, Zn2+
Cations of this group do not react either with dilute hydrochloric acid or
with hydrogen sulphide in dilute mineral acid medium. However they form
precipitates with ammonium sulphides (NH4)2S in neutral or ammonical
medium. The reaction is:
Co2++S2-⟶CoS↓ Fe3++3NH3+3H2O⟶Fe(OH)3↓+3NH4+
Ni2++S2-⟶NiS↓ Al3++3NH3+3H2O⟶Al(OH)3↓+3NH4+
Mn2++S2-⟶MnS↓ Cr3++3NH3+3H2O⟶Cr(OH)3↓+3NH4+
Zn2++S2-⟶ZnS↓
The result of experiment and the presence of the respective ions are
shown in the table below.
Result of Experiment Presence of Cation
Yellow precipitate Ba2+
Red flame Sr2+
Red-brick flame Ca2+
White crystal Ag+
Magnesium:
MgCl5.6H2O + Magnusson 1 → Blue precipitate
MgCl5.6H2O + oxine → Mg(C9H6NO)2+ 4H2O
(yellow)
The methods available for the detection of anions are not as systematic as
those which have been described above for cations. No really satisfactory scheme
has yet been proposed which permits the separation of the common anions into
major groups, and the subsequent unequivocal separation of each group into its
independent constituents; however, it is possible to detect anions individually in
most cases, after perhaps a 1-2 stage separation. It is advantageous to remove all
heavy metals from the sample by extracting the anions through boiling with sodium
carbonate solution; heavy metal ions are precipitated out in the form of carbonates,
while the anions remain in solution accompanied by sodium ions.
The following scheme of classification of anions has been found to work well in
practice; anions are divided into four groups on the basis of their reactions with di-
lute hydrochloric acid and of the differences of solubilities of their barium and sil-
ver salts.
1. Group 1 Anions
2. Group II Anions
Original Substances
Original Substances
Residue Filtrate
Brown Ring
A. NH4+ Cation Test Sample: color- Sample+ Na2CO3 2NO3-+4H2SO4+6Fe2+ Anion which contain
less crystals → Colorless solu- ⟶ 6Fe3++2NO↑+ 4SO42- in the sample no 2 is
Original Substances tion
Na2CO3: color- +4H2O NO3-, it can be pro-
Heated with Na2CO3 After heated:
less solution white precipitate Fe2++NO↑⟶ Fe(NO)]2+ ven by forming brown
Residue Filtrate H2SO4: color- formed Brown ring ring
Filtrate+ H2SO4→
-Added concentrated H2SO4 less solution
colorless solution
-added saturated FeSO4
FeSO4: yellow Filtrate + H2SO4 +
little by little through the
tube wall solution FeSO4→ brown
ring formed
Brown Ring
In this experiment we got sample number two which has form colourless crystal
through random selection. First of all we are dividing the sample into three with ratio 2:2:1.
The first two is for cations test, another two is for anion test and the last is for testing NH4+
cations, here is the experiments
In this experiment is analysing NH4+ cation. First, we are entering some of the sample
into reaction tube. Then, we adding 6 drops of NaOH to the tube, the sample turn its form
from colourless crystals to colourless solution. After that, we are put the red litmus paper
above the tube and enter the half part of the litmus into the tube. After a while the red lit-
mus paper changes its colour from red to blue. The reaction is:
The changing colour of the litmus indicates that in the sample number two contain
NH4+ cation.
In this experiment we analysing the contents of anion in the sample number two.
First we adding saturated Na2CO3 into the sample, the sample turn its form from colourless
crystal to colour solution. Then, we heating the solution with steam bath water for about 10
minutes until white sediment formed. Next, the heating result is filtered. We obtain colour-
less solution as the filtrate which will be used for anion test. Then, we are dividing the filt-
rate into 3 for testing anion contents.
In this experiment we authenticate anion NO3- in the sample number two. First, we
adding 2 drops of concentrate H2SO4 into the test tube which contains filtrate from prepa-
ration solution. Then, we are adding saturated FeSO4 little by little through the tube wall
until the brown ring is formed. The reaction is:
2NO3-+4H2SO4+6Fe2+⟶6Fe3++2NO↑+4SO42-+4H2O
Fe2++NO↑⟶Fe(NO)]2+
Brown ring
This experiment has purpose to determine the cation which contain in the
sample, in this case NH4+ cation. Here we using original sample because during the
course of analysis most of the group reagents are added in the form of ammonium
compound, thus by the time group V is reached, a considerable amount of
ammonium ions will be built up in the test solution.
The first thing that we have do is entering some of the sample into reaction
tube. Then, we adding 6 drops of NaOH to the tube, the sample turn its form from
colourless crystals to colourless solution. After that, we are put the red litmus paper
above the tube and enter the half part of the litmus into the tube. After a while the
red litmus paper changes its colour from red to blue because the reaction produce
ammonia (NH3) gases which is base that can be identified from its smells and
changing of litmus paper from re to blue. The reaction is:
The changing colour of the litmus indicates that in the sample number two
contain NH4+ cation.
2NO3-(aq)+4H2SO4(aq)+6Fe2+(aq)⟶6Fe3+(s)+2NO↑(g)+4SO42-(aq)+4H2O(l)
Fe2++NO↑⟶Fe(NO)]2+
Brown ring
This brown ring are caused by formation of [Fe(NO)]2+. The overall reaction is the
reduction of the nitrate ion by iron(II) which is reduced to iron(I) and formation of
a nitrosonium complex where nitric oxide is oxidized to NO1+. In this experiment
exothermic reaction are occur because existence of H2SO4 and it makes the tube
feels hot because the heat moves from system to surrounding. From this experi-
ment, we know that in the sample number two contain of NO3- anion.
XI. Conclusion
Qualitative analysis deals with the anions and cations which contain in a sample.
To analyse cations and anions have different way for each ion. To identify group I-IV
cation can be done by precipitation. For group I, HCl is used as precipitator. Then,
for group II, the precipitator is H2S. For group III, (NH4)2S is used as the precipitator
and (NH4)2CO3 is used as precipitator for Group IV. Meanwhile, for Group V is
different for each ions, it also can be done by flame test for group V. To identify
anions are different for each ion, but before done further test, the sample should be
heated with sodium carbonate to remove all heavy metals.
In this experiment we know that in the sample number two is NH4NO3 after
doing some test toward the sample. NH4+ cation can be identified by it smells and
changing colour of litmus paper from red to blue. Then, the existence of NO3- anion
can be identified by brown ring test.
6. Precipitation of sulphide salt on group II and IIIB cation analysis done in differ-
rent solution ambience. Explain!
Answer:
On group II, H2S flowed in acid solution, so the H2S gases just a little bit dissolved
and so much gas which is not absorbed in sulphide salt precipitation. It can be
done in acid ambience, because if the acidity which got from dilute HCl is too low,
so the sulphides from group IIIB will precipitate (NiS, CoS, and ZnS)
It’s different to group IIIB, H2S gas is distribute to basic solution which contain
many ammonium salt. H2S will much absorbed, it make group IIIB precipitate.
Furthermore, basic ambience also decreases the oxidation of sulphides to sul-
phate which is easy to dissolve.
7. Why the precipitations in group IV have to be done in basic ambience?
Answer:
Because in basic ambience (existence of ammonia), can prevent the precipitation
of magnesium and also to make carbonate (Ca, Sr, Ba) salts precipitate by ammo-
nium carbonate solution. It also because the difference among Mg, Ca, Sr and Ba.
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