Chemistry Practical (MIC) Ramakrishna Mission Vivekananda Cemenary College

Day-I Date:
Experiment 1Detection of special elements (N, S, CI, Br, I) in organic compounds
(Lassaigne's Test).
Take a small piece of sodium in a fusion tube and melt it by gentle heating, Add a
small amount organicsample to the fuscd sodium so that no substance is adhered to the side
of fusion tube. Now heat the mixture first gentle and then strongly until the fusion tube
becomes red hot. After that quickly plunged the fusion tube into 20 mL. of distilled water
taken in a mortar.Ground the mixture thorougihly with the help of a pestle and then finally
filter the mixture through a filter paper. Collect the filtrate. This filtrate is called sodium
extract. Now, perform the following experiments using this sodium extract.
Here, a small piece of Na metal is heated in a fusion tube with the organic
compound. The principle is that, in doing so, Na converts all the elements present
nto ionicform.
Na + C+N’NaCN
2Na + S’NaS
Na + X NaX( X=Cl, Br, orl)

Experiment Observation Inference

(a) Test for N Prussian blue Nitrogen
Add few drops of freshlyprepared FeSQi:s0lution colour. present.
to a part of 2 mL sodium extract. First boil the
mixture and then cool under tap watet, Finally
acidified the resultant solution with cond HSO4
(check with blue litmus paper)
NaCN +FeSO4’ Na4Fe(ÇN)6] NazSO4
(sodium ferrocyanid:
H,SO, + O
FeSO4 Fe,(SO)a
Na[Fe(CN)el:+ Fea(SOs)s-Fe[Fe(CN)s +12NaCI
Ferrosoferric cyanide
(Prussian Blue)
(b) Test for S Black Sulphur
Acidify 2 mL of sodiüm'extract with 2 mL of acetic precipitation present
acid and then add 0:5 mL of lead acetate in to it. (ppt).
H+
Na,S + (CH,cOO),Pb PbS+ 2CH,COONa
Black
(C) Boil2 m of sodium extract with 1 mL of conc. White ppt. This
HNO, acid. Cool down the solution and add few ppt. is soluble in
drops of AgNO, solution into it. NH, but
NaCl + AgNO, HNO, reappears when
AgCl + NaNO, acidified with
White
Conc. HNO,.

Samples: (i) Aniline hydrochloride, (i) Sulfanilic acid

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Chemistry Practical (MI) Ramakrishna Mission Vivekananda Centenary College

Day-2 Date:
Experiment 2: Test for aromatic primary amine group (Ar-NH).
Experiment Observation Inference
Dissolve 0.1 g of the supplied organic sample in Red or orange- Ar-NH2
to 5 mL of dil. HClacid and kept it in an ice bath. red dye. present.
Then add 1 mL of ice cold dilute solution of
NaNO2 to this solution. Finally,add the resultant
solution to an ice-cold alkaline solution of 10% B
naphthol.
NaNO,+ HCI
-NHa -GENCI
Benzene Diazonium Chloride

OH

-GENCr

B-Naphtho!

HO

B-Naphthol azo-dye (Scarlet red)

Sarmple: (1) Para toluidine

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Chemistry Practical (MIC) Ramakrishna Mission Vivekananda Centenary College

Day-3 Date:
Experiment 3: Test for -NO2 group. Inference
Observation
Experiment
(a) Mulliken-Barker's test:
Dissolve 0.1 g of supplied organic sample into 5 mL
of 50% alcohol. Small amount of Zn dust and little
amount of solid NHCI add to it and then boil the
stand
mixture for few minutes. Cool tlhe mixture and
for 5 minutes. Finally filter the fixture and collect the
filtrate. Perform the following tests with this filtrate.
() To a small part of filtrate, add few drops offreshly A silver -NO2 group
preparedTollen's reagent and then warmed in water
bath. mirtor or present.
black or grey
PhNO, +4}HPhNHOH+H,0 Ppt.

PANHOH + 2[Ag(NH,)2J0H’PhNO +2H,0+4NH, +2Ag

grey black

(Mulliken Barker test is used for the detection of the

mono nitro group in our compound. NO is reduced
to -NHOH i.e. hydroxylamine group by a neutral
reducing agent. Thus formed hydroxylamine reduces
the Tollerns reagent and oxidised it to a nitroso
compound.)
(ü) Add little amount of Fehling's solutiön to asmall Red ppt. NO2 group
portion of filtrate and warm it in to water bath. present.
Sample: (1) Meta dinitrobenzene
Tollen's reageDt:
This reagent is not commercially, available due to its short life, so it must be freshly
prepared in the laboratory Comnonpreparation involves two steps.
First a few drops. of dilute sodium hydroxide are added to some aqueous
'0.1M silver nitrate: The OH ions convert the silver aquo-complex form into
silver(1) oxide(Ag.0) which precipitates from the solution as a brown solid:
2AgNO, + 2NaOH Ag,0 +t 2NaN0, + H,0
Silver nítrate Sodium Silver oxlde Sodium Water
hydroxlde (brown ppt.) nitrate
> In the next step, sufficient aqueous ammonia is added until the brown
silver() oxide dissolves completely. The resulting solution contains
the
[Ag(NH3)2]* complexes in the mixture, which is the main component of
Tollens' reagent.
Ag,0 + 4NH,
H,o 2[Ag(NH,),) oH
Silver oxlde Ammonla Water
diaminesilver() hydroxide
(Tollens' reagent)

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Chemistry Practical (MIC) Ramakrishna Mission Vivekananda Centenary College

Fehling's Solution
Fehling's test consists of a solution that is usually prepared fresh in laboratories.
Initially, the solution exists in the form of two scparate solutions which are labelled
as Fehling's A and Fehling's B.
Fehling's Ais a solution containing copper(l) sulphate, which is blue. Fehlings Bis
a clear liquid consisting of potassium sodium tartrate (Rochelle salt) and a strong
alkali, usually sodium hydroxide. During the test solutions A and B are prepared
individually and stored.The two solutions are mixed in equal volumes to get the
final Fehling's solution which is deep blue. The deep blue ingredient is
bis(tartrate) complex of Cu2+. The tartrate tetra-anions serve as a chelating the
the solution. agent in
A B
Cuso,Solution Alkallne solution of sodium GH-CH - C0Di0
potassium tartarate
CuSO, + 2Na0H OH-cH-COGK
Cu(oH, +ta,S0, Rochetle salt
CuoH;

Cu

Deep blue colour comptex

Daep be coleur
(Fehling's solution)
Ca,C + RCOOH
(Cu} Redet

Precaution: Fehling's solutionäs môstly corrosive in nature. Therefore, it is always

good to wear protective gear like goggles and gloves.

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Chemistry Practical (MIC) Ramalrishna Mission Vivekananda Centenary College

Day-4 Dale:
Experiment 4: Test for aromatic -NO group in absence of aromaticamine.
Inference
Experiment Observation

Warm amixture of 0.1 g organic sample, few Red or orange-|present.

Ar-NO2
pieces of granulated tin and 3 mL of conc. HCI, red dye.
and thern cool the mixture at 0oC-5oC in an ice
bath. Then add 1 mL of ice cold dilute solution of
NaNO2 to this solution. Finally, add the resultant
solution to an ice-cold allkaline solution of 10% B
naphthol.
NO2 NH2
Sn, HCI

NaNO, +HCI -ÄENCT

-NH

Benzene Diazonium Chloride

OH

-NNC

B-Naphthol

HO

B-Naphthol azo-dye (Scarlet red)

Samples: {i) Meta dinitrobenzene, (ii) Para nitrotoluine

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Chemist1ry Practical (MI) Ramakrishna Mission Vivekananda Centenary Colege

Day-5 Date:
Experiment 5: Testfor -COOH, -coORand phenolic -OH groups. Inference
Experinent Observation
(i) Test for -COOH (carboxylic acid) group Effervescence -COOH
Add small amount of solid organic sample to the due to thegroup
saturated aqueous solution of NaHCO3. evolution of present.
CO2.
+ NaHCO3

Hz0 + cog (9
R

(iü) Test for -COOR(ester) group

Add two drops of phenolphthalein and one Fading. of -COOR
NaOH solution to a solution of 0.2g organic drop of disappearance group
mL alcohol. Then warm the mixture in sample in 2 of pink present.
a hot water.bath. colour.
Base-Catalyzed
Base. H0
R Acid Work-Up R ON Rg-OH

Acid-Catalyzed
Acid
R ROH # R-OH
H20
(iii) Test for PhOH (phenolic-OH) group
Add a drop of FeC3 solütionito an aqueous or alcoholic Violet colour. Phenolic
solution of organic sample (Green or blue -OH
colour may group
13 appear). present.
-3H +3HC1
Ferric chloride pieno.
Violct cofour
nplex

Samples: () Benzoic acid, (i) B-naphthol, (iii)Salicylic acid

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Chemistry Practical (MIC) Ramakrishna Mission Vivekananda Centenary College

Day-6 Date:
Experiment 6: Test for carbonyl (RaC=0)group and aldehyde (-CHO) group.
Observation Inference
Experiment Yellow or Carbonyl
(i) Test for carbonyl group(DNP test). group
Dissolve 0.1 g of organic sample in ninimum quantity of orange (may be
ethanol and then add 1 mL of 2, .4-dinitrophenyl precipitate. aldehyde
hydrazine solution (Brady's reagent) to it. Shake the tube or ketone
vigorously and scratch the inner wall of the test
tube with or both)
a glass rod. present.
NO ON CNOZ
ON R
R -H0
NHNH2
H
shinning Aldehyde
(iü) Test for aldehyde (-CHHO) group.
to 2 mL of Tollen's reagent silver mirrorgroup
Add 0.05 g organic sample for 5 minutes.
form`on the present.
and heat in a water bath inner wall of
Tollens' Reagent precipitate
the test tube
brown
to silver nitrate until a light (or grey or
Step 1: Sodium hydroxide is added
of silver oxide is formed.
brown ppt).
2AgNO, + 2NaOH Ag,o + 2NaNO, + H,o
Sodium Water
Sodium
Silver oxide
Silver nitrate nitrate
hydroxide (brown ppt.)
ammoniasoBution is added to the
silver oxide until the latter
$tep 2: Concentrated
complex.
completelydissolves forming a diaminesilver ()

Ag,0 + 4NH, H,0 2[Ag(NH,),J OH

diaminesilver() hydroxide
Silver oxide Ammonia Water
(Tollens reagent)

rreagent and aldehyde.

Step 3. Reaction between Tollen's
+ 2[Ag(NH,),)"OH + H,O
R-C-H
diaminesilver() hydroxide Water
Aldehyde

R-C-OH 2Ag 4NH, + 2H,0

Silver Ammonia Water
Carboxyllc acid

Samples: (1) Benzophenone (ii) Vanillin

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 Chemistry Practical (MIC) Ramakrishna Mission Vivekananda Centenary College

Section A: Inorganic Chemistry - Volumetric Analysis

1. Estimation of sodiumn carbonate and sodium hydrogen carbonate present in a
mixture.
2. Estimation of oxalic acid by titrating it with KMnO4.
3. Estimation of water of crystallization in Mohr's salt by titrating with KMnO4.
4. Estimation of Fe (II) ions by titrating it with KCr0; tusing internal indicator.
5. Estimation of Cu (l) ions iodometrically using Na2S,03.
Section B: Organic Chemistry
1. Detection of extra elements (N, S, CI, Br, I) in organic compounds
2. Test for the following functional groups.
Aromatic -NO2, Aromatic -NH2, -OH (phenolic),Carbonyl (aldehyde and ketone),
--COOH and olefinic unsaturation.
3. Determination of the melting point of the compound.

Reactions of Fehling's Test

In Fehling's solution the reaction between copper(Il) ions and aldehyde is
represented as;
RCHO +2 Cu2+ +5 OH- ’ RCO0-+ CupOt3 H0
When tartrate is added:

RCHO + 2 Cu(CAH4Os)22- +5OH RCOO- + Cu0 + 4 CAHO +3 H,0

Common Uses of Fehling's Test
Some common uses of Fehling's test are; it is used to determine whether a
group is an áldehyde or a ketone. Aldehydes tend to get oxidized and givecarbonyl
positive
result. Ketonès apart from alpha-hydroxy-ketones do not react.
Fehling's test is. also-used as a general test for monosaccharides
result is obtained for äldose monosaccharides and where a positive
from these, Fehlings test is used in the ketosemonosaccharides. Apart
medical field to
glucose in úrine. It helps to know whether the person is determine the presence of
diabetic or not.