12.7.

DILUTE SULPHURIC ACID TEST

ctTake a small guantity of the salt in a test-tube and add 1-2 ml of dilute sulphuric acid
Identify the gas and draw inferences from Table 12.7.
Table 12.7. Dilute Sulphuric Acid Test
Inference
Observations
Gas Radica!

A. Colourless, odourless gas with brisk effervescence, Co, co,2

turns lime water milky.
Colourless gas, pungent smell, turns acidified SO.?
potassium dichromate paper or solution green.
Colourless gas with smeil like that of rotten eggs, H,S
turns lead acetate paper black.
Reddish brown gas, pungent smell,turns ferrous
sulphate solution black. NO, NO,
ANo gas is evolved.
co,,

NO, absent
 l2.9. CONCENTRATED SULPHURIC ACID TEST

performed by treating small guantity of salt with conc. sulphuric acid (2-3 ml
This test is
Draw inferences fron
in a test tube. Identify the gas evolved in cold and then on heating.
Table 12.9.

Table 12.9. Conc. Sulphuric Acid Test

Inference
Observations
Gas Radical

Colourless gas with pungent smell, white fumes with aqueous HCI CI
RTS ammonia (NH, OH),white ppt. with AgNO, solution.
Reddish brown vapours with pungent smell, turns starch Br, Br
paper yellow. It does not turn FeSO, solution black.
8. Deep violet vapours with pungent smell, turns starch I, vapours I
paper blue. A sublimate is formed on the sides of the tube.
Reddish brown gas with pungent smell, turns FeSO,
solution black. NO, NO,
. Colourless vapours, vinegar smell, turns blue litmus red.
CH,COOH CH,CO0
8 A colourless gas wich turns lime water milky and also vapours,
a
gas which burns with pale-bluish flame CO, + CO C,0,
No gas/vapours evolved.
|CI, Br -, I, NO,
CH,CO0- absent
 12.10. PESTSFOR INDEPENDENT RADICALS (so, AND PO)
As-already discussed these radicals are not detected by dilute or concentrated H,SO,.
They are tested individuatly.
Sulphate (S0,) HNOg
Boil a small amount of salt with dilute HCI in a test tube. Filter the contents, and to the
iltrate add few drops of BaCl, solution. A white ppt. insoluble in conc. HCl indicates presence
of sulphate.

PPhosphate (PO,)
Add conc. HNO, to the salt ina test tube. Boil the contents and add excess of ammonium
holybdate solution. Ayellow precipitate indicates presence of phosphate.
 wJATIVE
ANAL
YSIS
Conformation 2

Confirmationof Soluble Carbonate

Cucbonate coa in 179

saltdissolves,
f the soluble carbonate is Confirmation of Insoluble Carbonate
If the snlt
remains
/ndicated. insoluble carbonateinsoluble, the
is indicated. presence
of
DitHCltest
portion of the solution, add dil. HCI. "To the salt add dil.
one
To HCL.
and
Brisk
effervescence
dioxide
evolution of
which turns lime water Brisk effervescence and evolution of car
Carbon bon dioxide which turns lime
confirms the presence of soluble car- water milky
milky confirms the presence of insoluble
honate.
Aagnesium sulphate test carbonate.
fthe
nd is To another portion of tthe solution, add mag-
nesium sulphate solution.
aken
Barmation of white precipitate in the cold
ter of
confirms the presence soluble
carbonate.

she :
wb not use sodium carbonate extract for performing the tests of carbonates because it contains
dum carbonate.
/Perform magnesium sulphate test only in case of soluble carbonates.
ater
Confirmation of Sulphite, So
(indicated in dilute acid test by the evolution of hydrogen sulphide).
Observations
Experiment

Barium chloride test

Take a portion of aqueous solution (0r A white ppt. is formed.
act. sodiun carbonate extract and dil. acetic acid
and boil off CO,). Add barium chloride
npo solution to it. Filter.
evolution of
and The ppt. dissolves with the
uble To a portion of the above ppt. add dil. HCI. sulphur dioxide.
VKMnO, test The pink colour is discharged.
10a second part of the ppt. from (1) add a
lew drops of acidified potassium permanga
hich naje solution.
ied
for VK,To Car,portion
0, test of aqueous solution or sodium A green colour obtained.

far. carbonate extractcadd potassium dichromate

Solution acidifed with dil. H,SO,
-hol
enylaminetest Y 180
,Lead
acetate
test
drops
ine.of To potassium
prepared
solution.
starchStarch-iodide dil. To mium carbonate
drops Totest sulphate
Ferrous
test (Undicated Cadmium
carbonate acid)
Totestcarbonate Tosolution.
a nitroprusside
Take test
add dium Sodium
a acetic a a a
portion portion portion onfirmatiòn portion add
of carbonate portion a
Conforation
carbonate a
acid few portion
iodide dil. extract) lead
Experimnent extraçt
of of and of in of of drops Experiment
aqueous H,SO, acetate
solution aqueous aqueous dilute aqueous
in aqueous
ferrous of water. add extract) of
acidified of
aqueous
and Nitrite,
acid a solution. soxdium
solution, solution,
followed solution sulphate solution
suspension solution in
a test with a
solution of
few test
NO,
by (or
nitroprusside
(or
add drops
by add solution. add dil. tube
freshly the sodiumof sodium (or
sulphide
a a some acetic
few few evolution cad and
of so

A A
obtained. A of A
deep blue dark brown yellow black A Purple ion
blue solution brown ppt. or
vapours ppt. S
violet2-PRACTICAL
uration Observations is is Observations
is or formed. obtained.
black of colouration
obtained.
nitrogen
is colouration CHEMISTRY--XI
obtained. is
peroxide obtained.

is )
 CHEMISTRY
182
Confomation of chlode ion, C|in:PhHACTICAL
Observations
Experiment
Silver nitrate test
A white ppt. is formed which is soluble i
Acidify a portion of aqueous solution (or ammonium hydroxide.
sodium carbonate extract) with dil. HNO,.
Boil for some time, cool and add AgNO,
solution.
Manganese dioxide test
Evolution of greenish yellow gas having a
Heat a pinch of the salt with a small quantity pungent irritating smell. It turns moist
of MnO, and conc. H,S0, starch-iodide paper blue.

Chromyl chloride test

Mix a smallquantity of the salt with a small A yellow ppt. is formed.
amount of powdered potassium dichromate.
Take the mixture ina test tube and add conc.
H,So,
Heat the tube and pass the red vapours
evolved into the gas detector containing
NaOH solution. To the yellow solution thus
obtained, add dil. CH,COOH and lead
acetate solution.

Cønfirmation of Bromide, Br
Noaction with dilute H,SO, but decomposed by conc. H,SO, with the evolution of bromine
vapours).

Experiment Observations

Silver nitrate test

Acidify a portion of aqueous solution (or so Alight yellow ppt. is obtained which is par
dium carbonate extract) with dil. HNO,. Boil, tially soluble in NH,OH.
cool and add AgNO, solution.
Manganese dioxide test
Heat a small quantity of the salt with solid Evolution of yellowish brown vapours ot
MnO, and conc. H,SO, bromine which turn starch paper yellow.
Chlorine water test
Acidify a portion of aqueous solution (or s0 Carbon disulphide layer acquires orange
dium carbonate extract) with dil. HCl and cokouration.
add 1-2 ml of carbon disulphide and then
chlorine water. Shake vigorously and allow
to stand.

Xote.Chlorine water is preparedby adding dropwise conc. HCl to asmall volume ofKMn O, solution
till the pink colour is just discharged, the resulting solution is chlorine water.
 AVE
ANALYSIS
183
Aafirmationof lodide, I-
oationuithdilute H,S0,but decomposed by conc. H,S0, with the evolution of vapours

Byperiment Observations
ernitratetest

portion of aqueous solution (or A yellow ppt. is ormed which is insoluble

Aodili
carbonate extract) with dil. HNO, in NH,OH.
stum add
cooland AgNO, solution.
Manganese
Rul, dioxide test
lquantity of the salt with alittle
small Evolution ofviolet vapours of iodine which
Heata
conc. H,SO,.
St

and turn starch paper blue.

Mn, water test
Chlorine
offtthe aqueous solution (or so- Carbon disulphide layer acquires a violet
Acidify a part extract) with dil. HCI, add
drum
carbonate
and then chlorine
colouration.
carbon disulphide
12mlof allow to stand
ater. Shake vigorously and
Cohfirmation of Nitrate, NO,
anction withperoxide).
dilute acids but decomposed by conc. H,S0, with the evolution of brown
NS of nitrogen
Experiment Observutions

Diphenylamine test
ine Add a few drops of diphenylamine to a part A deep blue colouration is obtained.
gfaqueous solution of the salt.
Copper chips test
Heat a small quantity of the original salt Dark brown fumes of nitrogen dioxide are
with concentrated sulphuric acid and a few evolved.
copper chips.
/Ring Test
Add a small quantity of freshly prepared Adark brown ring is formed at the junction
solution of ferrous sulphate to a part of the of the layers of the acid and the solution.
aqueous solution and then pour concentrated
of sulphuric acid slowly along the sides of the
test tube as shown in Fig. 12.9.

Concentrated
ion
sulphuric acid Brown
Aqueous solution of ring
SUspected nitrate
ig
Ferrous suiphale
12.9. The brown rring test for nitrates.
 PRACTICAL CHEMISTRY-XI
184

eonfirmation of Acetate, CH,CO0" conc. H,SO, with the evolution

(No action with dilute acids but decomposed by
CH,COOH vapours)
Observations
Experiment
, 1. Oxalic acid test Smell like that of vinegar.
Take a small quantity of the salt on a watch
glass. Mix it with solid oxalic acid. Prepare
paste of it with a few drops of water. Rub
the paste and smell.
A2. Ester test
Take a small quantity of the salt in a test Pleasant fruity smell of ester.
tube. Add conc. H,SO, (2 ml) and heat. Now
add ethyl alcohol (1 ml). Shake. Pour the con
tents of the tube in a beaker full of water.
Stir.
3. Ferric chloride test
Take water extract of the salt. Add neutral Reddish coloured filtrate.
ferric chloride solution. Filter. Divide the fil
trate into two portions.
(i) To one part, add dil. HCI. Reddish colour disappears.
(iü) To second part, add water and boil. Reddish brown ppt.

gonfirmation of Oxalate, C,0, (No action with dilute acids but decomposed by conc. H,S0,
with the evolution of CO, and gas)

ii go Experiment zd o Observations

1. Calcium chloride test

Take water extract (or soda extract if salt is A white ppt. is formed.
insoluble in water). Add small amount dil
acetic acid and boil off CO,. Add calcium
chloride solution.
Add dil HNO, to the white ppt and warm. The ppt.. dissolves.
2. Potassium permanganate test
Take a pinch of the salt in test tube and add The pink colour of KMnO, solution is
dil sulphuric acid. Warm to 60-70°C and add decolourized with the evolution of CO, gas.
2-3 drops of KMnO, solution.
wTATIVEANALYSIS
187
Confirmation of Sulphate, S0
Notindicatedin dilute and concentrated H,SO, acid tests).

Experiment
Observations
Barium chloride test
of the aqueous solution of the salt
To a part solution.
A white ppt. is formed which is
insoluble in
add barium chloride dil HC.
Mateh stick test
e a small amount of the salt with sodium Violet streaks are produced.
orhonate and a little powdered charcoal so
s to get a paste. Take some of this paste on
one end of a wooden splinter and heat in the
oducing flame till the mass fuses. Dip the
fused mass into sodium nitroprusside
solution taken in a china dish.
Lead acetate test
Toa part of aqueous solution of the salt add A white ppt. is formed which is soluble in
lead acetate solution. excess of hot ammonium acetate solution.

Cpirmation of Phosphate, PO,

YNot indicated in dilute and concentrated H,SO, acid test).

Experiment Observations
Ammonium molybdate test
lo the aqueous solution or sodium carbon A deep yellow ppt. or colouration is
ate extract (or the original salt) add concen obtained.
trated nitric acid and boil. Addammonium
molybdate solution in excess and again boil.
Magnesia mixture test
lake a portion of aqueous solution (or a part A white ppt. is obtained.
Of Sodium carbonate extract, add hydrochlo
nc acid to acidify it and boil off CO.,). Add
magnesia mixture prepare it, add solid
Nnlto magnesium chloride solution. Boil,
C00l and add NH.0H till a strong
smell of
ainmonia is obtained) and allow to stand.