SALT ANALYSIS
Anions are divided into 3 Groups:
i) Dil. H2SO4 Group: CO32-, SO32-, NO2-, S2-
ii) Conc. H2SO4 Group: Cl-, Br -, I -, NO3-, CH3-COO –
iii) Not identified by i) & ii) (Special group): SO42-, C2O42-, PO43-
Detection of Anion: Two types of tests are to be done in order to detect anion: Dry Tests and Wet Tests.
1. Preliminary observations:
a. Colour:
b. Structure:
2. Dry Tests for Anion
Experiment Observation Inference
i) Action of dil. HCl a. Colourless, odourless gas evolved with brisk Gas evolved is CO2.
Add 2 c.c of dil. HCl to effervescence. CO32-confirmed.
the salt(0.1gm) taken b. Turns blue litmus red
in a clean and dry test c. Burning splinter is extinguished
tube. d. Lime water turns milky.
a. Colourless gas is evolved with rotten egg Gas evolved is H2S.
smell b. Lead acetate paper turns black. S2- may be present.
a. Colourless gas is evolved with suffocating Gas evolved is SO2.
odour. b. Acidified K2Cr2O7 paper turns green SO32- may be present
c. Acidified KMnO4 paper turns colourless.
a. Light brown gas is evolved with pungent odour Gas evolved is NO2.
b. Pass the gas through ferrous sulphate solution, NO2 – may be present
it turns brown
ii) Action with conc.
H2SO4.
2 cc of conc. Sulphuric a. Colourless gas is evolved with pungent 1st Gas evolved is HCl.
acid is added to a odour. b. Turns blue litmus red;
small amount of salt c. Dense white fumes obtained when a glass rod
taken in a clean and dipped in NH4OH is brought near the gas.
dry test tube and
heated (do not boil)
the contents gently.
Greenish yellow coloured gas is obtained, which 2nd Gas evolved is
A pinch of MnO2 is turns starch iodide paper blue black. Cl2 Cl – may be
added to the above present.
solution and heated.
a. Reddish brown gas with pungent odour. More Gas evolved may
reddish-brown fumes of bromine are evolved be HBr.
when MnO2 is added to the solution and heated. b. Br –may be present.
Turns moist starch paper yellow
a. Violet vapours of iodine are evolved with Gas evolved may be
pungent odour. More violet vapours are HI I – may be
obtained, when MnO2 is added to the solution present.
and heated.
b. Turns moist starch paper blue
Salt analysis
a. Light brown gas with pungent odour. Gas evolved is NO2
b. Add Cu-turnings and heat. Formation of brown NO3–may be present.
gas increases.
c. Turns starch iodide paper blue.
iii) Action with conc. Gas with vinegar smell. Acetate may be
Sulphuric acid and A strong Fruity odour of ethyl acetate is obtained. present. CH3COO
ethanol. –
confirmed.
Few ml of conc.
Sulphuric acid is added
to a small amount of
salt. Now a few ml of
ethanol is added to it
and then heated.
3) Wet Tests for Anion: Wet tests are done with Na2CO3 extract (Soda Extract).
i) Preparation of Soda Extract: 1 part of salt is mixed with 3 parts of Na2CO3 in a test tube and about 10 -15 ml
of distilled water is added. It is then boiled for 5 minutes taking care that the contents do not boil over. It is
then cooled, filtered and the filtrate is called Soda Extract.
ii) Confirmatory tests for anion:
Experiment Observation Inference
Test for S2- A purple or violet colour is formed. S2- confirmed
• Add 1 mL of sodium
nitro-prusside S2-confirmed
solution to 1 ml soda Black ppt. formed.
extract.
• Add 1 mL of lead
acetate solution to 1
ml soda extract.
Test for NO2- Yellow ppt. is obtained NO2-is
Acidify soda extract with confirmed.
acetic acid and add
concentrated solution of
cobalt chloride. Then add
KCl solution. Warm the
contents and wait for
some time.
Test for Cl White ppt soluble in cold NH4OH. Cl–confirmed
1 ml soda extract is
acidified with dil. HNO3,
and then add 1 mL of
AgNO3 solution to it.
Test for Br Pale yellow ppt is obtained partially soluble in Br–confirmed.
1 ml soda extract is NH4OH. CS2 test:
acidified with dil. HNO3, Acidify about 2 ml of S.E. with dilute hydrochloric acid.
and then add 1 mL of Add to it 1 ml of chlorine water (or KMnO4 and conc.
AgNO3 solution to it. HCl) and 4- 5 drops of carbon disulphide. Shake
vigorously.
Test for I Yellow ppt. insoluble in NH4OH. I–confirmed.
1 ml soda extract is CS2 test:
acidified with dil. HNO3, Acidify about 2 ml of S.E. with dilute hydrochloric acid.
and then add 1 mL of Add to it 1 ml of chlorine and 4- 5 drops of carbon
AgNO3 solution to it. disulphide. Shake vigorously. Violet colouration is
obtained.
Test for SO42-/ SO32- White ppt is obtained, which is insoluble in dilute HCl. SO42-confirmed
2
Salt analysis
1 ml soda extract + White ppt is obtained, which is soluble in dilute HCl SO32-confirmed
acidify with dil. HCl +
BaCl2 solution.
Test for NO3- Brown ring is formed at the junction of two liquids NO3–confirmed
1 ml soda extract + 1ml
dil. Acetic acid + freshly
prepared FeSO4 sol.
+ add conc. H2SO4 along
the side of the test tube.
Test for CH3COO Wine/ blood red coloration, which turns into reddish ppt CH3 COO
1 ml soda extract on heating confirmed
neutralized with dil.
Mineral acid + neutral
ferric Chloride solution +
heat
Test for C2O42- A white precipitate is obtained. C2O42-is
• Acidify a portion of confirmed.
sodium extract
with acetic acid
and add calcium
chloride solution. Pink colour of KMnO4 is discharged.
• Filter the ppt. from
the above and
extract with dilute
sulphuric acid.
Now a few drops
of KMnO4 solution
and warm it.
Test for PO43- Yellow ppt. or colouration is obtained. PO43-confirmed
• Take about 2 ml of SE.
add to about 1 ml
of conc. HNO3 and
heat to boiling.
Now add
ammonium Yellow precipitate is obtained, which is soluble in dilute
molybdate solution nitric acid.
and heat again.
• SE is first acidified
with dilute acetic
acid and then
silver nitrate
solution is added
to it.
Cations to be detected are divided into the following groups.
Group Group Reagent Cations
Zero NaOH NH4+
Gp-1 Dil. HCl Pb2+
Gp-2 H2S in acidic medium Pb2+, Cu2+
Gp-3 NH4Cl + NH4OH Fe3+, Al3+
Gp-4 NH4Cl + NH4OH + H2S Zn2+, Mn2+
Gp-5 NH4Cl + NH4OH (excess)+ Ba2+, Sr2+, Ca2+
(NH4)2CO3
Gp-6 NH4Cl + NH4OH excess + Na2HPO4 Mg2+
3
Salt analysis
4) Preparation of ORIGINAL SOLUTION (OS): The solubility of the salt mixture should be tested in the following
order:
i) In cold water and then hot water
ii) Dil. HCl – first in cold and then in hot.
iii) Conc. HCl – first in cold and then in hot
iv) Dil. HNO3
v) Conc. HNO3
vi) Aqua Regia (3 parts conc. HCl & 1 part conc. HNO3)
A saturated solution (10 – 15 ml) is made which is called the Original Solution.
5) Group analysis and confirmatory tests for cation.
Experiment Observation Inference
Group Zero > Gas with ammonia smell Group Zero
Salt + NaOH + heating > Moist red litmus turns blue NH4+confirmed.
> Dense white fumes with conc. HCl
> Nessler’s reagent gives red ppt.
Group 1 > White ppt. is formed Group 1 (Pb2+) is
O.S + dil. HCl present.
> No White ppt. Formed Group 1 is absent
2+
Tests for Pb
Group 1 ppt is washed
with water and heated
with
water. If ppt. dissolves
then divide the solution > Yellow ppt. formed Pb2+ confirmed
into 3 parts: > Yellow ppt formed Pb2+ confirmed
Part 1 + Pot. Chromate > White ppt. formed Pb2+ confirmed
sol. Part 2 + Pot. Iodide
sol.
Part 3 + dil. H2SO4
Group 2 > Black / Brown ppt. Group 2 (Pb2+, Cu2+)
O.S + dil. HCl + pass H2S gas is present.
or to the above solution > No ppt. Group 2 is absent
pass H2S gas.
> Ppt. dissolves and colourless solution is Pb2+ is present
Gr 2 ppt is washed & formed. > Coloured solution is formed Cu2+ is present
boiled with dil. HNO3
Tests for Cu2+
Coloured sol. is divided
into 4 parts: > Pale blue ppt turns black due to CuO formation. Cu2+ is confirmed
Part 1 + NaOH sol.
>Bluish white ppt which dissolves in excess of Cu2+ is confirmed
Part 2 + NH4OH sol NH4OH
> Chocolate colored ppt. Cu2+ is confirmed
Part 3 + Pot. > Khaki coloured ppt. Cu2+ is confirmed
Ferrocyanide Part 4 +
KI sol.
Tests for Pb2+
The Colorless solution is
divided into 3 parts and
do tests as in Gp 1 for Pb2+.
4
Salt analysis
Group 3 > White gelatinous ppt. Group 3(Al3+) is
O.S. + + NH4Cl soid present
+NH4OH till alkaline. > Reddish brown ppt. Group 3 (Fe3+) is
present
> No ppt. is formed Group 3 is absent
.
Fe3+ is confirmed
Tests for Fe3+ > Deep blue coloured ppt. is obtained.
O.S + Pott. Fe3+ is confirmed
Ferrocyanide. O.S + > Deep red coloured ppt. is obtained.
Pott. Sulphocyanide.
Al3+ is confirmed
> Blue floating ppt in colourless solution. (Lake
Tests for Al3+ Test).
White gelatinous ppt is
dissolved in dil.HCl + drops
of blue litmus sol. +
NH4OH till alkaline
Group 4 > White/grey ppt. Group 4 (Zn2+) is
O.S. + NH4Cl solid +NH4OH present
till alkaline + H2S. Or to > Pink ppt. Group 4 (Mn2+)
the above solution H2S is present
passed. > Black ppt. Group 4 (Ni2+)
> No ppt formed present Group 4
absent
Tests for Zn++
White/grey ppt is washed
+ dil. HCl + boil to remove
H2S. ppt dissolves. Divide > White ppt formed dissolves in excess of NaOH.
sol. into 2 parts: pass H2S. ppt reappears. Zn2+ is confirmed.
Part 1 +NaOH drop by drop.
> White or bluish white ppt.
Zn2+ is confirmed.
Part 2 + Pott. Ferrocyanide.
> White ppt insoluble in excess & turns
++ brown. > A purple coloured solution is Mn2+ is confirmed.
Tests for Mn
formed.
Pink ppt is washed + dil. Mn2+ is confirmed.
HCl + heat. Ppt dissolves.
Divide the solution into 2
parts: Part1 + NaOH sol.
Part 2 + NaOH. Ppt formed
is filtered out and dissolve
in conc.HNO3 + lead
dioxide + boil + dilute with
water.
> Green ppt. formed
Tests for Ni 2+ and Co2+ Ni2+ is confirmed
> Scarlet red ppt formed.
Black ppt is washed and Ni2+ is confirmed.
dissolved in aqua regia.
> blue coloration is obtained.
Boil to reduce the volume Co2+ is confirmed
and divide into 3 parts:
Part 1 + NaOH sol.
Part 2 + excess
NH4OH + dimethyl
glyoxime.
Part 3 + ammonium
thiocyanate + amyl alcohol
5
Salt analysis
Group 5 White ppt is formed. Group 5 (Ba2+,
O.S. + NH4Cl solid + NH4OH Sr2+, Ca2+) is
till alkaline + (NH4)2CO3. present.
No ppt. formed.
White ppt is washed + Group 5 is absent.
dissolved in acetic acid and
divide into 3 parts. Tests
MUST be done strictly in
the following order, i.e.,
test for Sr++ is done only if
Ba++ is absent; test for
Ca++is done only if Ba++& > Yellow ppt insoluble in acetic acid
Sr++absent. Ba2+ is confirmed
Part 1 + K2CrO4 sol. > White ppt.
If Ba++ is absent then Sr2+ is confirmed
> White ppt insoluble in acetic acid
Part 2 + (NH4)2SO4 sol.
If Ba++ & Sr++ absent then Ca2+ is confirmed
> Brick red flame
Part 3 + Ammo. Oxalate
> Grass green flame Ca2+
sol.
> Blood red flame Ba2+
Flame Test Sr2+
Group 6 > White crystalline ppt. is obtained Mg2+ is confirmed.
O.S. + NH4Cl solid
+ NH4OH + Na2HPO4
