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/SC

Chemlstry Lab Manual XIl


6 To 2 ml of
followed by glfewyceroldrops
, addof about 1 ml of |23]
6 To about 1 ml of NaOH copper
solution. sulphate solutionA blue colouration is produced.
drops of
aqueOus lycerol, add 2 ml of water and, 4-5|A white
2 ml of conc. solution of
ml of ethanol. HaSO4. Shake well andpyrogallol followed by
residue is formed.
boil. Cool and add 10
7 Take about 2 ml of
glycerol and heat the
Tollen's reagent. Now add
5
minutes without content by keeping it in boiling2-3 water
drops of Shining silver miror is formed on standing.
disturbing it. tor

sts for Formaldehyde FORMALDEHYDE (HCHO)


S. No.
Experiment Observation
lo I ml of
of formaldehyde, add freshly prepared strong
solution A white precipitate is
pyrogallol containing excess of hydrochloric acid. formed which readily
turns pink and then deep red.
2 1ml of 1% phenyl hydrazine solution is mixed with 1 ml ofA
treshly prepared solution of sodium nitroprusside. This deep blue colour appears which turns
is now added to 5 ml of mixturegreen to brown and finally red on standing.
formaldehyde finally the contents
are made alkaline by adding
and
excess NaOH solution.
Treat 2 ml of formaldehyde with equal volume of
solution A and B. Shake and heat. Fehling| Ared precipitate of Cu,0 is formed.
4 Add 5 ml of Schiff's reagent to 3 ml of formalin.
The pink colour is discharged.
5. To 2 ml of 1% solution of phenyl hydrazine add about 1 ml ofA rose
red colour appears.
formalin and 1 ml of 5% solution of potassium ferricyanide.
Now add few drops of conc. HCI.
b.4 To 1 mlof formaldehyde, add a crystal of resorcinol and shake. YA red ring is formed at the junction of
Then add about 1 ml conc.H2S04 slowly by the side of test two liquids but white ppt. is formed in
tube. aqueous layer.
7 Add 2 ml of Tollen's reagent to 2 ml of formalin..Warm the Shiny silver mirror forms at the walls of
Contents. the test tube.
Nootan./SC
Chemistry Lab Manual XI
(251

Tests for Aniline ANILINE (CH;NH2)}


S. No.
Experiment Observation
1. Tane dbout 1 ml of aniline solution and add
1ml of red aboutColour of litmus solution changes trom reo
litmus solution. to blue.
2 lake about 1 ml of the original substance and add
1 ml of Pinkish ppt. is formed.
bromine water.
3.lake about 5 ml of aqueous solution of aniline, Add 2-3 dropsPurple colouration is obtained which turris
of sodium hypochlorite solution with constant shaking. Nowto rose red on addition of (NHalzs0A
add few drops of (NH),SOA solution to it. solution toit.
About 1 ml of original substance is mixed with l ml of conc.A white ppt. is obtained which turrs to
HCI in a test tube. To this mixture, add few drops of ferric pale green colour.
chloride solution. Shake and dilute with water.
colouration is produced
5. lo an aqueous solution of aniline, add few drops of solutionA purpleviolet
changes to green or brown
of bleaching powder and shake welI. Now dilute it with waterwhich readily
away.
and adda few drops of ammonium sulphide (NHal,S solution. and then fades
H,SOAA/deep red colour is produced which
Mix about 1 ml of original substance with 3 ml of dilute
solution. Shakechanges to deep blue or black.
in a test tube. Now add few drops of K5Cr50,
the mixture well.
[64] Nootan /SC Chemistry Lab Manual Y
Procedure
Identificatlon of anion
Preparation of Sodium Carbonate Extract : Mix the given salt (C-16) with solid NazC0, in
1:3 ratio and add about 20 mi of distilled water to it. Boil for some time and filter. The filtrate is
sodium carbonate extract.
S. No. Observation Inference
Experiment
NO SUspected
Heat a pinch of salt with conc. H,SO4.Light brown fumes are evolved
with pungent odour.
2. NO3 confirmed
Add copper turnings to the above test The brown fumes become more
tube. dense.
NO3 confirmed
3. Neutralize 5 ml of sodium carbonate A brown ring appears at the
extract with dil. HCI and add to it junction of two liquids.
freshly prepared equal volume of FeSO4
solution. Now add conc. HaSO, from
the side of test tube.

ldentification of cation
Preparation of Original Solution (0.S.) :The O.S. is prepared in distilled water.
Observation Inference
S. No. Experiment
1 0.S. dil. HCI. White ppt. is formed. Group I present
2 Filter the contents. Dissolve the
precipitate in hot water and divide the
solution into two parts : Pb* confirmed
(a) To the first part, add potassium Yellow ppt. is formed.
chromate (KzCrO4) solution.
Pb* confirmed
(b) To the second part, add KI solution. Yellow ppt. is formed.
Result
The salt (C-16) contains :
Anion : Nitrate (NO3)
Cation: Lead (Pb*)

ExPERIMENT 4
Object
Analyse qualitatively the salt (C-18) containing one cation and one anion applying formal group
analysis.
Nootan ISC Chemistry
Lab Mana
ExPERIMENT
Object
You are provided with two solutions as follows :
1. A10 is a solutiou prepared by dissolving 1.85 g of potassium manganate (VIl) (KMno) be
litre,
2A-11 is a solution prepared by dissolving 22gof hydrated ammonium iron (1) sulphaz
erystals, (NH)SO, FeSO4 xH,0 per litre.
Procedure
Rinse and fill the burette with the given solution A-10 of potassium manganate (VI). Pipette ou
20 ml or 25 ml of the solution, A-11 of ammonium iron (I) sulphate solution into a clean conica
flask. To this add 20 ml of A-12 solution of dilute H,SO4 specially provided for titration.
Titrate the solution by running solution A-10 from the burette till one drop of this solution gives
a permanent light pink colour to the solution C-11 in the conical flask. The pink colour should no,
disappear on shaking the contents of the conical flask.
Repeat the above procedure to get at least two concordant readings. Tabulate your readings.
State

(a) The capacity of the pipette used.


(b) The titre value which you use in your calculations.
The equations for the reactions mnay be written as follows.
2KMnO4 +8H,S04 +10(NH, ),SO4 · FeSO4 xtH,0
K,sO4 + 2MnSO, +10(NH,),SO4 +SFe,(SO4)3 +8H,0 +10xH,0
or

2MnO, + 10Fe* + 16H* 2Mn* +10Fe"+ 8H,0


Relative atomic masses :
K=39, Fe = 56, S= 32,N = 14,H = 1, Mn = 55, 0= 16
Calculate the following
1. The molarity of potassium manganate (VI) solution A-10.
2. The molarity of hydrated ammonium iron (II) sulphate solution A-11.
3. The molecular mass of hydrated ammonium iron () sulphate, deduced from the
experimental data.
4. The numerical value of x, ie., the number of molecules of water of crystallization in
(NH), SO4 FeSO4 xH,0.
Note: Calculate the molarity of the solutions at least upto 4decimal places.
Mootan lSC Ghemistry Lab Manual XII
Observation Table
S. No. Burette reading (ml)
Initial
1. 0.0 Final Volume of KMnOa Used (ml) End point or titre value (ml)
2 0.0 23.5
23.5
3 0.0
23.6 23.6 23.6 ml
23.6
Capacity of pipette used = 25 ml 23.6

Titre value = 23.6 ml


Calculations
1. Molarity of A-10 (KMnO4)
Molarity(M,) =Weight in g/litre 1.85
= 0.0117089 M
Mol.weight 158 S
2. Molarity (M) of 11 (Hydrated ammonium iron (1) sulphate) O"o1075
MVn
Where VË = Volume of A-10 solution (Titre value)
V= Volume of A-1l solution
n = Number of moles of A-10
n, = Number of moles of A-11
MË = Molarity of A-10 solution
M, = Molarity of A-11 solution
0.0117089 x 23.6 2 23"7
10
M, x 25
M, = 0.05526 M oo52495)
3. Molecular weight of A-11 Weight in g/litre
Molecular weight = Molarity (M2)
22 2OGo
0.05526
= 398.117

of xin (NH),S04·FeSO4 xH,0


4. Value Strength =Molarity (M,) xFormula weight
22 =0.05526 x (284 + 18)
398.117= 284 + 18x
x=6.33 6
ammonium iron (W) sulphate
Formula of hydrated - PeSO4 (NH),S046H,0
Nentan SC Chemistry Lab Manual XU
Size of the pipette used = 25 ml
Titre value = 23.7 ml
Calculations
1. Molarity of ferrous ammonium sulphate (M) = Strength
Mol. weight
20.5
392
=0.05229M
2. M,V (Ferrous ammonium sulphate) n
M;V,(KMnO,) n
Mi
0.05229 x 25 10
M2 x 23.7 2
M, = 0.01103 M
3. Concentration or strength = Molarity (M,) x Mol-weight
0.01103 x 158
= 1.742 g/l
Pure substance x 100
4. % Purity =
Impure sample
1.742
1.85*l00

= 96.77%

ExPERIMENT 3
Object
You are provided two solutions:
g of an impure sample of hydrated
1. C-10 is a solution which is prepared by dissolving 19.0
ammonium iron (11) sulphate per litre. ns
manganate (Vil) KMnO4:
2. C-11 is a solution containing 1.25 gof potassium
Procedure clean
burette with C-1l solution. Now pipette out 20 ml or 25 ml of C-11 solution into a
Fill the H,SO4 specially provided to you for titration
conical or titration flask. To this add 20 ml of diluteTitrate it with C-1ll solution from the burette,
cylinder.
by measuring with the help of measuring colour to the solution in the flask.
shaking the flask gradually till last drop gives a light pink
State
(a) The size of the pipette used and,
(b) The titre value you intend to use in your calculations.
LaoMar

ExPERIMENT 2
Object
You are provided with two solutions as follows:
\7
1. Solution C-10 is prepared by dissolving
(VII) KMn04 per litre of the solution. 1.80 g of impure sample of potassium mangan
2. Solution C-11 is a solution of 20.5 g of
pure hydrated ammonium iron () sulpha
(NH),S0,FeSO, 6H,0 per litre of the solution.
Procedure
Rinse and fill the burette with C-10
25 ml of the solution of potassium manganate (VI). Pipette out 20 ml o
solution C-11 of ammonium iron (I) sulphate
add 20 ml of C-12 solution of dil. solution in a
H,SO, specially provided for the titration.clean conical flask. To thi
Titrate the solution by running solution C-10 from the
a permanent light pink colour to the solution C-11 in the burette till one drop of this solution give
obtained should not disappear on shaking the contents of conical flask. The light pink colour thue
Repeat the above procedure of titration to get at least the conical flask.
two concordant readings.
State
(a) The capacity of the pipette used.
(b) The titre value which is used in
4.oheequations for the above your calculations.
reactions are as follows
2KMnO4 + 3H,S04 K,SO4 + 2MnS04 + 3H,0 + 5[0]
10FeSO4 + SH,SO, + 5[O] SFe,(SO4)3 + 5H,0
or
2MnO4 + 10Fe+2 + 16H 2Mn+2 + 10Fet3
+ 8H,0
Relative atomic masses :
K=39, Fe = 56, S =32, N= 14, H = 1, Mn = 55, O=
16
Calculate the following
1. The
molarity of hydrated ammonium iron (I) sulphate
2. The molarity of potassium solution C-11.
3. The concentration of potassium
manganatel(VII) solution C-10.
4. The percentage purity of impure
manganate (VII) solution C-10 in g/.
sample of potassium manganate (VII) C-10 solution.
Note: Calculate the molarity of the solutions at least upto 4
decimal places.
Observation Table
6.No Burette reading (ml) Volume of KMnO4 solution
Initial Final Titre value (ml)
1.
used (ml)
0.0
23.7 23.7
2 0.0
23.7 23.7
3 0.0 23.7 ml
23.8 23.8
(67]
yootan ISC Chemistry lLab Manual XII
Inference
S.No. Experiment Observation Group I absent
0.S. + dil. HCI. No ppt. is formed.
1. Group Il absent
Pass H,SS gas to this solution. No ppt. is formed.
2. Group lll present
NowA gelatinous white ppt. is formed.
3. Boil off H,S gas from the above solution.
add a pinch of NH,Cl and excess of NH,OH
solution.
filtrate for
4 Filter the contents. Retain the
subsequent groups. Dissolve the residue
and divide the
minimum amount of dil. HCI
solution into two parts: formed. A confimed
solid NH,Cl and excessA white gelatinous ppt. is
(a) To the first part, add A confimed
NH,OH solution. lake is formed.
few drops of blue A floating blue
part, add
(b) To the second NH,OH solution drop
litmus solution and
wise.

Result
given salt (C-18) contains
The CO0)
Acetate (CH
Anion : Aluminium (Al*)
Cation :
ExPERIMENT /
anion applyingformal
containingone cation and one
Object salt (G-14) in
qualitativelythegiven
Analvse
3roupanalysis.
sodium
Procedure (C-14) with solid
the given
salt The
ldentificationofanion EXtTact : Mix for some time and filter.
Deanarationof Sodium
Carbonäare distilled water to it. Boil
20 ml of
and add about Inference
in 1:3ratio extract. Observation
carbonate carbonate
sodium appear which
filtrateis Experiment
Dark brown fumes
tification of cation water
soluble in distilled
Preparation Originalof Solution (0.S.) : The salt mixture is
Inference
S.No. Experiment Observation
1. Group I absent
0.S. + dil. HCI. No ppt.
Group IIl absent
2.
Pass HzS gas to e above content. No ppt.
Group l present
3. 1O a Tresh portion of 0.S.. add few drops of Reddish brown ppt. forme0.
Conc.HNO3. Boil and cool. Add a pinch of
NH Cl and excess NH,OH solution.
4 Filter the contents. Retain the filtrate for
further group analysis. Dissolve the ppt. in
dil. HCI and divide into twO parts

(a) To the first part, add KA(Fe(CN)e]Adeep blue coloured solution. Fe* confirmed
solution.

(b) To the second part, add KCNS solution. Blood red colour.
Fe* confirmed

Result
The given salt (C-17) contains :
Anion : Nitrate (NO3)
Cation : Ferric (Fe*s
ExPERIMENT6 \wws
Object
Analyse qualitatively the salt mixture (C-18) containing one ation and one anion applying formal
group analysis.
Procedure
ldentification of anion
Preparation of Sodium Carbonate Extract: Mix the salt mixture with sodiumn carbonate in 1:3
ratio and 15 ml of distilled water in a test tube. Boil and cool. Filter the contents. The filtrate is called
sodium carbonate extract.
S.No. Experiment Observation Inference
1 Neutralize sodium carbonate extract with dil. Wine red colour is observed. CH3C00 confirmed
HCI. Now add neutral FeCl3 solution.
ldentification of cation
Preparation of Original So<ution (0.S.) : The original solution is prepared in dilute nitric acid.
Specimen Record of the
Salt Analysis 8
ExPERIMENT I NH

Object
Analyse qualitatively the salt (C-15) containing one cation and one anion applying formal groun
analysis.
Procedure
ldentification of anion
Preparation of Sodium Carbonate Extract : Mix the given salt with solid Na,CO, in 1:3
ratio and add 20 ml of distilled water into it, in a beaker. Boil for some
time and filter. The filtrate is
sodium carbonate extract.
S. No. Experiment
1
Observation Inference
Add little amount of conc. H,SO4 to a pinch
salt and heat the contents. ofA colourless gas having a CI suspected
pungent smell evolves.
2 Bring a glass rod moistened with NHOH near the Dense white
mouth of test tube. fumes are formed. CI suspected
3. Neutralize 5 ml of sodium carbonate extract with
dil. HNO3 and add 2ml of AgNO, curdy white ppt. is formed.
solution.
4 To the above contents add
excess and shake. NH,OH solution in|The curdy white ppt. gets CI confirmed
dissolved.
ldentification of cation
S. No.
Experiment
1 To a pinch of salt, add NaOH
solution and heat.
Observation Inference
A colourless gas with
smell evolves. pungent Zero group present
2. Bring a moist red litmus paper near the gas. It turns blue.
3 A glass rod dipped in conc.
HCI is brought near Dense white NH,suspected
the mouth of the test tube. fumes evolved. NH suspected
4 Pass the evolved gas into Nessler's reagent.
It turns brown.
NHÀ confirmed
Result
The salt (C-15) contains :
Anion : Chloride (CI)
Cation : Ammonium (NH)
finalysutstarce vcution
wic Sor
m reacCEAS
SriS whicn
smel. rezur the
S formet. original
ICOCm cocing produce.
D
Observation characterstic
Cr
anc formed with formad
S Observation
elc
colGuratdn tormed warmingis
pot. of place.smell
effervescence
to an are addition
ot yellcwis is
faces crystals is crystalline takesfruity ppt.
colour
on crystals
a ppt.
C0
CH, red colour
ruby
red

have
Yellow
which
to disappears
changes
black violet Cooling.
White
on
dissolve
thisYellow
BENZOIC
ACID
(C,H;COOH) gas
Strong pleasant
CO>
coIoured
A addA A auou
A of A
sodium
solution and thesolution
cool. cool. solution
and sodium
saturated
solution change
by or conc.
a
drop solution.
sodium
bicarbonate
in
CH,
ACETONE gently till thenand Warm To acldof
of Shake
and
solution.
further
2 abouL
aci0,
NaOH solution NaOH gentlyprepared of substance ml
benzoic
Warm
gently and solution. crystals benzolc
acetone. acetone content. 2 bath.
water
boiling
of dilute Warm no ado and
Heat freshly (HgCl,)
ml prepared
while. of til original solution,of ethanol of
NH,OH ml few drop the solution solution
1 disappears.
about of add of shaking. 1
Experiment a ml Now ml of a
about chloride in
by or change Experiment
freshly
for drops by acid of
add stand 1 2 constantthen followed
dropacetone aqueous
drops aqueous
to completely.to add solution
aqueOus
of
fewand mercuric
contents. NaOH benzoic
andof iodinecolouriodine further tube
dropsto acetone, 5-10
acetone addnitroprusside add 1%
Allow with 1% solution.
FeCl,
neutral
3
of brown of acetone, bisulphite of
the of solutionthisno Acid 1% of addtest
to crystals
dissolve crystals
solution of the ofml
ml To is of ml it,
Acetone of 2 nitroprusside.. till
Tests
for ml Shake
1 there Benzoic ml 2 To Heat 2
ml by then cool. feW shakefew of sodium 1 sodium about
place.
dilute 2 dilute
cold about about
TOlowed Crystals NH,OH ml about till about tube.
2 acetate. HSO4.
lake Add and Add 1 cool. Take takes drop
To of To 4of add To
Taketest Take
for
S.No.
1. 3. 4. 5. TestsS.No.
[24] b. 2.

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