S.No.

Experiment Observation Inference

Pb2 absent.
1. To the salt/mixture solution, add dil. HC1. No ppt.
2. To the above solution, pass H,S gas. No ppt. Pb Cu,2+ Cd A3+ ions
may be absent.

QUALITATIVE INORGANIC ANALYSIS 125

 3 Boil off H,Sfrom the above solution completely. Cool and then Reddish brown ppt. Fe may be present.
add few drops of conc. H,SO, and heat. Cool and then add
NH,CI(s) and NH,OH in excess. Filter the ppt. and keep the
filtrate for group IV.
4 Dissolve the ppt. in dil HCl and divide into three parts:
Fe3t confirmed.
() To the first part, add potassium ferrocyanide solution. Prussian blue colour or ppt.
(i) To the second part, add potassium ferricyanide solution. Green colouration. Fet confirmed.
(iii) To the third portion, add potassium thiocyanate solution. Blood red colouration. Fe3+ confirmed.

ChemicalReactions:
Fe+3OH’ Fe(OH)3
(Reddish brown ppt.)
Fe(OH); + 3HCI ’ FeCl, + 3H,0
4FeCl, + 3K4[Fe(CN)%] ’ Fe4[Fe(CN)%l3 + 12KCI
Potassium Ferric ferrocyanide or Iron (I) hexacyanoferrate (II)
ferrocyanide (Prussian blue)
FeCl, + K,[Fe(CN),] ’ Fe[Fe(CN)%] + 3KCI
Pot. ferricyanide Ferric ferricyanide or Iron (II) hexacyanoferrate (I)
(green colouration)
FeCl; + 3NaSCN ’ Fe(SCN); + 3NaCl
Sodium Ferric thiocyanate
thiocyanate (Blood red colouration)
RESULT
The given salt/mixture contains Fe" ions.
 S.No.
Observation Inference
Experiment 2 2

To the pinch of salt, add dil. H,SO4

No gas evolved. CO; , SO s, NO, absent.
2 No gas evolved. CI, Br , I, NO, absent.
To the fresh pinch of salt, add conc. H,SO4 (1 ml). 2
3. Awhite ppt. is formed. SO4 may be present.
To the salt solution, add 1-2 ml of BaCh solution.
4. The ppt. is insoluble. SO2 confirmed.
To the above ppt., add conc. HCI or conc. HNO3.
5. A white ppt. is formed. SO42 may be present.
To the salt solution,add Lead acetate solution. 2
6. The ppt. dissolved. SO confirmed.
To the above ppt., add Ammonium acetate solution in excess.
Chemical Reactions:
So,2 + BaCl, ’ BaSO4+ 2C1
(white ppt insoluble in conc. HCland conc. HNO3)
so + Pb(COOCH;)2 ’ PbSO4 + 2CH,CO0
Lead acetate White ppt.
PbSO4 + 2CH;COONH4 ’ Pb(COOCH;); + (NH),SO4
RESULT
2
The given salt contains SO4 (sulphate ions).
 EXPERIMENT NO. 10.1(B)
OBJECTIVE

To prepare standard solution of oxalic acid and Mohr's salt.

MATERIALS REQUIRED

Eunnel, measuring flask (250ml), chemical balance, weight box and weighing tube, oxalic acid (Analytical reagent, A.R),
Mohr's salt (A.R).
PROCEDURE

(a) Preparation of a standard solution M/40 of oxalic acid:

1 Weigh an empty watch glass by using a chemical balance.
Weigh 0.7875 g of oxalic acid by using chemical balance on a watch glass.
1 Takea measuring flask (250 ml). Transfer the oxalic acid from the watch glass into the measuring flask with the help
of a funnel.
4 Wash the funnel several times with distilled water using wash botle without removing the funnel from the fiask.
5. Swirl the flask till solid oxalic acid is dissolved completely.
6. Make the solution up to the marked point with distilled water and shake it by closing the stopper of the flask.

AIR
AIR
FUNNEL
STAND

Fig. 10.8 Transferring solution to Fig. 10.9 Washing of watch glass to transfer Fig.10.10 Transferring last traces of
measuring flask sticking particles to beaker solution to measuring flask

Fig. 10.11 Fig. 10.12 Fig. 10.13

VOLUMETRIC ANALYSIS (REDOX TITRATION) 93

(6) Preparationof standardsolution of Mohr's salt FeSO, (NH), S0,-6H,0
Molar mass of Mohr's salt = 392 g mol
M 392
1000 ml of solution of Mohr's salt requires =9,80 g of Mohr's salt
20 40
M 9.80
250 ml of solution of Mohr's salt requires -x250 = 2.45 g of Mohr's salt.
20 1000
Weigh 2.45 g of Mohr's salt in the same manner as above and dissolve in water. Add few drops of dil. H s while
preparing its solution and make the volume up to 250 ml.
PRECAUTIONS
1. While weighing, the substance should not be spilled on the pan.
2. The knob of the balance should be rotated gently.
3. After weighing, weights should be kept in the weight box at their appropriate places.
4. While transferring the substance into the funnel, weighing tube should be brought very close to the cdge of the funnel
and the substance should be transferred gently.
5. Watch glass must be dry.
6. Funnel should be washed thoroughly several times.
7. Shaking of solution should be done thoroughly so that it may become uniform.
8. While making the solution,the solvent should be added such that the lower meniscus of the solvent must be on the mark
of the measuring flask.
 (E) To test the presence of carboxylic group.
THEORY
causing effervescence.
Carboxylic acid turns blue litmus red and react with NaHCO, to give CO, gas
MATERIALS REQUIRED
Blue litmus paper, alcohol, NaHCO, solution.
S.No. Observation Inference
Experiment
1 To the drop of liquid compound or a solution of given It changes to red. Carboxylic acid group may
compound, add blue litmus paper or blue litmus solution. be present.
2. To the givencompound or its aqueous solution, add solution Brisk effervescence due to CO,Carboxylic acid group
of NaHC0,. present.

3. Ester formation test. To the given organic compound, add Pleasant fruity smelling - COOH group confirmed.
ethylalcohol and few drops of conc. H,SO4. compound (ester) is formed.

Chemical Reactions:

CH,COOH +NaHCO,CH,COONa +CO, +H,0

78
SARASWATI LAB MANUAL CHEMISTRY-XI
P R E C A U T I O N S

Add cold NaHCOz Solution in small quantity to the given oroanic compound and effervescence should be nouceu
time.

2 Heatingshoula notbe done while performing NaHCO, test, because NaHCO, decompose on heating and gives CO
RESULT

The given sample of compound contains carbOxylic acid group.

(B Totest the presence of alcoholic group.
THEORY
Alcoholic compounds give pink red or wine red colour with ceric ammonium nitrate. They liberate H, gas with sodium
metal. They form Xanthate with CS,.
MATERIALS REQUIRED
Ceric ammonium nitrate, sodium metal, CS,, KOH, CH,COOH, conc. H,SO4, etc.

TEST FOR FUNCTIONAL GRUOUP IN ORGANIC COMPOUNDS 75

 Observation Inference
S.No. colouration. Alcoholic group is
Experiment
of Ceric Wine red present.
1. To the given liquid (organic compound) add few drops
1s Alcoholic groun is
ammonium nitrate solution. Yellow precipitate
compound and warm formed.
confimed
2. Add a pellet ofKOH to I ml of liquid organic shake.
of CS, and
it to dissolve KOH. Cool it and add few drops evolved. Alcoholic group 1S present.
H, gas is
3 Add sodium metal to the given organic compouna. Alcoholic group 1S confimed
drops of Pleasant fruity smelling
Add few
4. Add acetic acid to the given organic compound. ester is formed.
conc. H, SO,. Warm a little.

Chemical Reactions:
C,H,OH + KOH ’C,H,OH +H,0
SK
KOH
S=C=S+ C,H,0K S=-OC,H,
Potassium ethyl xanthate (yellow ppt.)

2C,H,OH+ 2Na ’ 2C,H,ONa + H,

Conc.H,SO 4
CH,COOH +C,H,0H ’ CH,CO0C,H, + H,0
(Pleasant fruity smelling ester)
PRECAUTIONS
1. Do not dissolve organic compound in alcohol.
2. Keep organic compound away from flame.
RESULT
The given organic compound contains alcoholic group.
 1otest
the p 3I ket0 group.
)
MATERIALs REQUIRED
2 4 - D N P
(Dinitro
phenylhydrazine), NaHSO,
THEORY

Bothaaldehydes and ketones give 2, 4-DNP test.

NO,
C=0+ H,NNH
C=N NH + H,0
NO, yellow ppt. of 2, 4-dinitro phenylhydrazone
2, 4-dinitro phenylhydrazine
Aliphatic aldehydes and ketones give bisulphite compound with
NaHSO,-
OH
C=0+ NaHSO,
so,Na
Ketones do not give Tollen's reagent and Fehling's solution test.
S.No. Experiment Observation Inference
1. Take 1ml of aqueous or alcoholic solution of the compound and
add I ml of a alcoholic solution of 2, 4, dinitro phenylhydrazine.
Yellow ppt. Ketone is present.
Boil the mixture and cool.
2 Prepare 2-3 ml of saturated solution of NaHSO, in water and add White ppt. Ketone is present.
to it 0.5 g of organic compound and shake the mixture.
3. To the given sample add Tollen's reagent and heat a little. No silver mirror is formed. Aldehyde group is absent.
4
Mix Iml each of Fehling solution. 'A' and 'B° in a test tube when No brick red ppt. is formed. Aldehyde group is absent.
a blue solution is obtained. Add 1 ml of the liquid compound or
solution of organic compound in water or alcohol. Boil it for two
minutes.

RESULT
Ihe given sample contains keto group.
 f test the presence of aldehydic and ketonic group
THEORY

Dath aldehydes and ketones containC=O group

and give orange
Alinhatic aldehydes and ketones give white precipitate due to their ppt. with 2, 4-dinitrophenyl hydrazine.
bisulpbite compound with sodium bisulphite.
B. Aldehydes give silver mirror with Tollen's reagent. They give pink colour with Schiff's reagent. They also give brick
red ppt.with Fehling's solution. Ketones do not give these tests.
MATERIALS REQUIRED

CAfT's reagent, Fehlings solution, alcohol, silver nitrate solution, dil. NHLOH. NaHSO., iodine solution, NaOH, 2, 4-DNP.
S.No. Experiment Observation Inference
Take 1ml of aqueous or alcoholic solution of a pinch of compound
and add 1ml of alcoholic solution of 2-4-dinitrophenyl hydrazine. Yellowish orange ppt. Aldehyde or ketone group
may be present.
Boil the mixture and cool.
2 To the aqueous solution of organic compound add 2-3 ml of White crystalline ppt. Aldehyde or Ketone group
saturated solution of sodium bisulphite in water. Shake the mixture. is present.
3 To the given organic compound add iodine solution and aqueous Yellow ppt. Aldehydes
NaOH solution.

(CH,-C H)
or Ketone having

CH,-C
group is present.

TEST FOR FUNCTIONAL GRUOUP IN ORGANIC COMPOUNDS 77

 appeared.Aldenyde group present
4. To 1 ml of the liquid compound add 3-4 drons of Schif's reagent. Pink colour is
Aldehyde group present
5
1o the given compound add Tollen's reagent (ammoniacal silver Shiny silver mirror 1s
nitrate solution). formed.
6
To the given solution add 1ml of each Fehling's solution Aand B. Brick red ppt. Aldehyde group present.
Boil the solution for two minutes.

Note: Ketones give positive 2, 4-dinitro phenyl hydrazine and negative test with Fehling's solution, Schiff s reagents and
Tollen's reagent. Therefore, these tests can be used to distinguish between aldehydes and ketones.
Chemical Reactions:

C=0+ H,N NH C=N-NHO-NO, +H,0

(yellow ppt.)
NO, NO,
-OH
C=0+ NaHSO,
sO,Na
(white ppt.)

CH,C-H+ 2[Ag(NH,),J'OH ’ CH, -C-ONH, + 2Ag + 3NH, + H,0

RCH+2Cu?t +50H ’ RCOO+ Cu,0 + 3H,0

(brick red ppt.)
Lodoform test:

CH,-C--H+31, +4NaOH ’ CHI, + CH,COONa+ 3Nal + 2H,0

RESULT
The given compound 'A' contains aldehyde group and B' contains ketone group.