Assignment No.
Expt. No. 11
INORGANIC QUALITATIVE ANALYSIS
1.PHYSICAL EXAMINATION:
i) Colour *
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i) State
Amorphous/Crystalline
i) Solubility Cold/hot water
Cold/ hot dil HCI
2. DRY TESTS FORACID RADICALS:
Test
Observation Inference
) Action of dil H,S0,:
To a small amount of salt
Rapid evolution of colourless Co,present.
taken in a test tube dil HSO, odourless gas which turns lime
is added and warmed
(ifrequired) water milky.
) Action of conc. H,So, (a) Rapid evolution of colourless
To a small amount ofsalt odourless gas which turns lime
taken in a test tube conc.
(a) COpresent.
water milky.
H,SO,is added and warmed. (b) Evolution ofcolourless gas with (b) CI present.
irritating smell, which forms white
fumes with a glass rod moistened
with NH,OHsolution.
(c) Evolution ofreddish brown fume (c) Br present.
with pungent smell which turns starch
iodide proper blue.
() Evolution ofviolet vapour, which (d) present
turns starch-iodidepaper blue.
) Action of conc. H,SO, and (a) Evolution of greenish yellow gas. (a) Cl present
MnO,: To asmall amount of (b) Evolution of reddish brown fume | (b) Br present
salt taken in a test tube conc. with pungent smell.
HSO,and little MnO, is (c) Evolution of violet vapour. (c) T present
added and warmed.
Inference
Test Observation
iv) Action of conc. H,SO, and Evolution ofreddish brown vapour.| NO, present
Cu-turning: To a small amount The solution in the test tube turns
of salt taken in a test tube conc. blue.
H,SO, and Cu-turnings is
added and warmed.
3. WET TESTS FORACID RADICALS:
Preparation of salt solution: As the saltis soluble in water, an aq. solution of the salt is
prepared and the following tests are performed for acid radical.
Prepation of Na,C0, extract: As the salts isinsoluble in water, to a small amount of salt
solid Na,CO,1(3-4 times of the salt) is added. The mixture is stirred well in water and boiled for 10
minutes and filtered With the filtrate (called Na,CO, extract) the following tests are performmed:
Test Observation Inference
Test for Sulphate : A little A heavy white ppt. insoluble SOpresent and
salt solution is acidified with in dil HNO, confirmed
dil HCl and BaCl, solution
i s is added.
Test for halide: A little (a) A curdy white ppt insoluble in (a) CI present and
i)
salt solution is acidified with dil HNO, but soluble in NH,OH confirmed
dil HNO, and warmed and solution.
AgNO, solution is added (b) A pale yellow ppt, partially (b) Br present.
soluble in NH,OH solution.
(c) A yellow ppt. insoluble in dil C)I present.
HNO, and NH OH solution.
Special Test for Br & T: (a) The organic layer turns reddish Br confirmed.
in)
To a little salt solution CCl, brown
(or CHC1) is added and (b) The organic layer turns violet. T confirmed.
then conc. HNO, is added
drop wise with constant
shaking
(Write this test ifpositive
result is obtained in AgNO,
test)
Test Observation Inference
iv) RingTest for Nitrate: To a A brown ring is formed at the (a) NO, present
small amount of salt solution junction ofthe two liquids and confirmed.
freshly prepared FeSO0
solution is added and cooled
under tap water and then conc.
HSO, is added slowly
down the side ofthe test tube.
4.DRY TESTS FOR BASIC RADICALS:
Test Observation Inference
Heating in a dry test tube:| (a) Smell of ammonia. (a) May be NH, salt.
A small quantity of the salt is
(b) Reddish brown fume (b) May be Pb(NO,),|
heated strongly in a test tube () Black residue on strong heating (c) May be salt of Cu
by holding it in horizontal () Yellow when hot, white when cold |(d) Zn2* Salt
position. (c) Yellow when hot or cold (e) Pb* Salt
( White sublimate ( NH, Salt
() The salt is white and shows no (8) Maybe salt of
change |AP", Ba*, Ca*, Mg*|
i) Flame test: A clean plat- a) Transient brickred flame.
(a) May be Ca salt.
inum wire is moistened with (b) Bluish green flame
(b) May be Cu salt.
conc. HCland a little ofthe ()Livid blue flame (c) May bePb
salt is taken at the tip ofthe (d) Yellowish green flame (d) May be Ba salt.
wire and then heated in the
non-luminous flame ofthe
burner
i) Charcoal reduction test: (a) No residue &smell of ammonia (a) NH,salt.
A little of the salt is mixed (b) Red flakes. (b) Cu salt.
with Na,C0, (1:2) and taken (c) White residue glows on heating (c)AP, Mg", Ca*
in a charcoal cavity & heated Ba2 salt.
with reducing flame with. (d) Grey metallic particles.
a
(d) Fe' salt.
The help of blow pipe. (e) Yellow incrustation (c) Pb salt.
( Incrustation without metal, (() Zn salt.
yellow when hot, white when cold.
Inference
Observation
Test
(a) Al salt.
iv) Cobalt Nitrate Test: (a) Blue mass (b)Zn salt.
The white infusible residue (b) Green mass
obtained in charcoal reduction| (c) Pink mass
(c) Mg salt
test is moistened with 1-2
drops ofcobalt nitrate solution
and then heated with
oxidisingflame
(This test is performed only
when white infusible mass
is obtained in charcoal red-
uction test)
v)Borax bead test: A little ofOxidising Elame Reducing Flame| salt
(a) Green when (a) Colourless (a) Cu
the salt is taken in a hot tran-
when hot, red
sparent borax bead made on | hot, blue when
a platinumwire loop and then | cold when cold
(b) Fe3/Fe* salt.
heated in oxidizing & reducing| (b) Yellow when (b) Green when
hot, and cold hot, and cold
flame.
(This test is performed only
when thesaltis coloured). NH, salt
|vi) Test for NHradical: The Smell ofammonia gas
salt is boiled with NaOH
solution (or solid Na,CO)
5. WETTESTS FOR BASIC RADICALS:
is taken in a beaker and
Preparation of salt solution: About 1 gram of the given salt
the solution.
dissolved in a suitable solvent (water hot/cold or dil HCI hot/cold) to prepare
With this solution group separation for basic radical is done as follows (filter whenever ppt. appears)
Inference
Test Observation
The salt solution is acidified White ppt /No ppt Gr. 1,
with dil HCl and cooled. present/absent
i The above solution (orfiltrate) Black ppt/No ppt Gr. I1,
is warmed and HS is passed present/absent
until saturated.
ËMR
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Test Observation Inference
i) HS is boiled off from the Reddish-brown/gelatinous white Gr. IIIA,
above solution (orfiltrate)
|light green ppt/ no ppt Fe AP*/Cr
cc. of conc. HNO, is added
present/absent
and boiled if Fe is
present]
Now solid NH,CI & NH,OH
solution is added to make the
solution alkaline (tested with
red litmus paper).
iv) The above solution (orfiltrate) Dirty white ppt/ no ppt
Gr. IIIB,
made alkaline with NH, OH Zn" present/ absent
solution and H,S is passed till
saturated
v) The above solution
(orfiltrate)|White ppt / no ppt Gr. TV,
is boiled to remove H,S. Now Ba, Ca present/
solid NH,CI, NH,OH solution absent
and saturated solution of
(NH,), CO,is added
vi) To the above solution (orfiltrate)| White ppt/ no ppt Gr. V,
NaHPO, solution is added. Mg* present/absent
6. TEST FOR NH,"
Test Observation Inference
To solutionofthe salt Nesslers Reddish brown ppt /no ppt. NH, present and
reagent and NaOH solution confirmed/absent
added till alkaline.
7.ANALYSIS OFGr.IPPT:
The ppt. ofGr. I is boiled with water in a test tube and divided into three portions.
) Cooled under tap water. White ppt:- Pb" confirmed.
i) Acidified with acetic acid and K,CrO, solution is added. Yellow ppt.: Pb*confirmed.
(i) Acidified and KI solution is added. Yellow ppt. soluble in excess KI solution:-Pb* confirmed.
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8.ANALYSis OFGr. II PPT:
The ppt is boiled with 1:3 HNO,. To the solution NH,OH solution is added till alkaline and
filtered
Dissolved in NaOH and acidified| Filtrate: Blue colour indicates Cu". Acetic
Residue :
with acetic acid. Divided into two portions: acid followed by potassium ferrocyanide
Yellow solution added. Reddish brown ppt.
(i) K,CrO, solution to one portion.
Ppt. confirms Pb?* confirms Cu2*
(ii) KI solution to another portion. Yellow
Ppt: confirms Pb
9.ANALYSIS OF Gr. ITl A PPT
solution and H,O,(1:1 ratio by
Theppt.of Gr. Ill A is boiled with a mixture of dil. NaOH
volume) and filtered.
Residue: The residue is dissolved in dil Filtrate: Dividedinto two parts:
HCl and divided into two parts: () To one part solid NH,Cl is added and boiled.
() To one part K_[Fe(CN)] solution is white geletinous ppt.-AP present and
added. Prussian blue colour- Fe present. | confirmed.
(i) To another part NH,SCN solution is 1i) To another part acetic acid and lead acetate
added. Blood red colour- Fe" confirmed. solution added. Yellow ppt Cr" present and
-
Confirmed.
Test for Fe* & Fe'": A fresh solution of the salt is prepared with water (or dti HC) The solution
is divided into two parts
(i) To one part K,[Fe(CN),] solution is added. Prussian blue colour or ppt. > Fe*confirmed.
Prussian blue colour or ppt. >Fe2 confirmed.
i) To one part K,[Fe(CN)] solution is added.
10. ANALYSIS OF Gr. III B PPT:
The ppt. is boiled with dil. HCI to dissolve and to remove H.S. I ml H,0, and excess
NaOH added and boiled. The solution is acidified with acetic acid and H,S passed through it. Dirty
white ppt-Zn present and confirmed
11. ANALYSIS OF Gr. IV PPT:
The ppt. is dissolved in hot dil. Acetic acid and divided into two parts
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added and filtered
() To one part ofthe above solution K,CrO, solution is
pptBa* present and confirmed by apple green flame in flame
test.
Yellow
warmed.
(i) To the filtrate/ other part (NH),C,O, solution is added and
White pptCa* present and confirmed by brick red flames in flame test.
12. ANALYSIS OF Gr. V PPT:
The ppt. is treated with dil HCI. To this solution excess NaOH solution is added
White ppt Mg" present and confirmed.
13. CONCLUSION:
The given salt contains
() . as Acid radical and
i). ..... as Basic radical
****k*
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