CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium...

24
C Y O T I L S L E R G E E V I M N U A - N E G R A P L S U A R K I U V VIKAS PRE-UNIVERSITY COLLEGE CHEMISTRY PRACTICAL 2 www.vikascollege.com LAB MANUAL

Transcript of CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium...

Page 1: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

CY OTI LS LER GE EVI MNU A- NE GR

AP LS UA RKI U

V

VIKAS PRE-UNIVERSITY COLLEGE

CHEMISTRY PRACTICAL 2

www.vikascollege.com

LAB MANUAL

Page 2: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

VIKAS PRE-UNIVERSITY COLLEGE

CHEMISTRY PRACTICAL 2

LAB MANUAL

Index

Experiment No - 1 To prepare a standard ferrous ammonium sulphate solution (Mohr's salt solution) and determine the strength of the given potassium permanganate solution. 03

Experiment No - 2To prepare a standard solution of oxalic acid and determine the strength of given potassium permanganate solution. 05

Experiment No - 3 Preparation of pure sample of potash alum 07

Experiment No - 4Preparation of pure sample of Ferrous ammonium sulphate (FAS/Mohr's salt) 08

Experiment No - 5 Systematic semi-micro qualitative analysis of a simple inorganic salt. 09

Experiment No - 6 Test for the functional group present in organic compounds 14

Experiment No - 7Preparation of Acetanilide from aniline 17

Experiment No - 8Preparation of iodoform crystals 18

Experiment No - 9Preparation of Lyophilic and Lyophobic sol 19

Experiment No - 10 To study the role of emulsifying agent in stabilising the emulsions of different oils 20

Experiment No - 11Determination of heat of neutralization of Hydrochloric acid with Sodium hydroxide 21

www.vikascollege.com

Page 3: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Aim: To prepare a standard ferrous ammonium su lphate solution (Mohr’s salt solution) and

determine the strength of the given potassium permanganate solution.

Principle: Potassium permanganate is a powerful oxidising agent. It oxidizes ferrous sulphate

to ferric sulphate in the presence of dil.H2SO4.

Reactions:

Reduction half reaction: 2KMnO4 +3H2SO4-----→K2SO4+2MnSO4+3H2O+5[O]

Oxidation half reaction: [2FeSO4 +H2SO4+[O] -----→Fe2(SO4)3 + H2O] ×5

Overall reaction: 2KMnO4 +10FeSO4+8H2SO4 -----→ K2SO4 +2MnSO4 + Fe2(SO4)3 +8 H2O

Preparation of 100mL of 0.05M Mohr’s salt solution:

Molecular mass of Mohr’s salt crystal is 392.1g

Molarity =Mass × 1000/Molar mass × volume required

0.05 = Mass×1000/392.1×100

Mass =0.05×392.1/10

=1.96g

a)Preparation of 0.05M Mohr’s salt solution:

Weigh exactly 1.96g of ferrous ammonium sulphate in a weighing bottle and transfer the same

into a 100ml standard flask containing 5ml of dil.H2SO4.Small amount of distilled water is added

and shaken well until it dissolves. The solution is made up to the mark using distilled water.

Stopper the flask and shake well for the uniform concentration of ferrous ammonium sulphate.

b)Estimation of molarity of KMnO4 Solution :

Procedure: Pipette out exactly 10ml of 0.05M Mohr’s salt solution into a clean conical flask.

Add one test tube full of dil.H 2SO4 .it is titrated against potassium permanganate solution taken

in the burette until a pale pink color is obtained.

The titration is repeated until concordant values are obtained.

Result: Strength of KMnO4 solution…………..M

Experiment No - 1

CHEMISTRY PRACTICAL 2

LAB MANUAL

3

Estimation of potassium permanganate using standard Mohr’s salt solution

Page 4: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Tabulation and calculation:

Titration of 10ml of 0.05 M FAS against KMnO4 Solution

In burette : KMnO4 solution

In Conical flask: 10ml 0.05 M FAS solution + one test tube full of Dil.H2SO4

Indicator : KMnO4 (Self Indicator)

End point :Colorless to pale pink

Agreeing volume of KMnO 4 =V1=………cm3

Where a1 and a2 are stoichiometric co-efficient of KMnO4 and FAS in the balanced chemical

equation (a1=5 and a2=1)

Trial Numbers 1 2 3

4

Initial burette readingFinal Burette reading

3Volume of KMnO used in cm4

www.vikascollege.com

(KMn0 )4 (FAS)

a M V1 1 1 = a M V2 2 2

Strength of KMn0 (M )4 1 = a M V2 2 2

a V1 1

= 1 x 0.005 x 105 x v1

= ________ M

VIKAS PRE-UNIVERSITY COLLEGE

Page 5: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

AIM: To prepare a standard solution of oxalic acid and determine the strength of given

potassium permanganate solution.

PRINCIPLE: Potassium permanganate is a powerful oxiding agent .It oxidises oxalic acid in the

presence of Dil.H2SO4 to CO2 and H2O.Potassium permanganate acts as a self indicator.

REACTION:

Reduction half reaction: 2KMnO4 +3H2SO4-----→K2SO4+2MnSO4+3H2O+5[O]

Oxidation half reaction:[H2C2O4 +[O] -----→H2O +2CO2] ×5

Over all reaction: 2KMnO4 +3H2SO4+5H2C2O4 -----→ K2SO4 +2MnSO4 + 8 H2O +10CO2

Preparation of 100ml 0.05M oxalic acid:

Molecular mass of oxalic acid =126

Molarity =Mass × 1000/Molar mass × volume required

0.05 = Mass×1000/126×100

Mass = 126×100 ×0.05/1000

=0.63g

Mass required to prepare 100ml of oxalic acid solution is 0.63g.

a)Preparation of 0.05M oxalic acid:

Weigh exactly 0.63g of oxalic acid crystals and transfer the same into a 100ml standard flask. It

is dissolved in small amount of distilled water. The solution is then made up to the mark using

distilled water. stoper the flask and shake well for uniform concentration of oxalic acid.

b)Estimation of molarity of KMnO Solution: 4

Procedure: pipette out exactly 10ml of 0.05M oxalic acid solution into a clean conical flask.

Add one test tube full of dil.H2SO4 to prevent the formation of manganese dioxide.The mixture

is heated near to boiling. The hot solution is titrated against potassium permanganate solution

taken in a burette until a pale pink is obtained. The titration is repeated until concordant values

are obtained.

Result: Strength of the KMnO4 Solution= ………M

Experiment No - 2

CHEMISTRY PRACTICAL 2

LAB MANUAL

5

Estimation of potassium permanganate using standard oxalic acid solution

Page 6: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Tabulation and calculation:

Titration of 10ml of 0.05 M oxalic acid against KMnO4 Solution

In burette : KMnO4 solution

In Conical flask: 10ml 0.05 M oxalic acid solution + one test tube full of Dil.H2SO4

Indicator : KMnO4 (Self Indicator)

End point :Colourless to pale pink

Agreeing volume of KMnO4 =V1=………cm3

Where a1 and a2 are stoichiometric co-efficient of KMnO4 and Oxalic acid in the balanced

chemical equation (a1=5 and a2=2)

6

Trial Numbers 1 2 3

Initial burette readingFinal Burette reading

3Volume of KMnO used in cm4

www.vikascollege.com

(KMn0 )4 (oxalicacid)

a M V1 1 1 = a M V2 2 2

Strength of KMno (M )4 1 = a m v2 2 2

a M1 1

= 1 x 0.005 x 105 x v1

= ________ M

VIKAS PRE-UNIVERSITY COLLEGE

Page 7: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

AIM: Preparation of pure sample of potash alum

PRINCIPLE: When a mixture of potassium sulphate and aluminum sulphate are saturated and

cooled, crystals of Potash alum is formed.

K2SO4+Al2(SO4)3 +24H2O ------→K2SO4 .Al (SO2 4) 3 24H2O

PROCEDURE: Dissolve in potassium sulphate (2.0g) and aluminium sulphate (8.0g) separately

in 10 mL of water.(since aluminum sulphate is less soluble in water add 3 to 4 drops of

conc.H2SO4 and warm)Mix the two solutions in china dish, it is heated to a small volume and

cooled. Colourless crystals of potash alum are formed.

Report: Yield of potash alum=……….g

Experiment No - 3

CHEMISTRY PRACTICAL 2

LAB MANUAL

7

Page 8: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Aim: Preparation of pure sample of Ferrous ammonium sulphate(FAS/Mohr’s salt)

Principle: When equimolar solutions of ferrous sulphate and ammonium sulphate are

mixed,subsequently evaporating the solution to crystallizations, the double salt seperates out.

FeSO4+( NH4)2SO4 +6H2O------→ FeSO4( NH4)2SO4 .6H2O

Procedure: In a 250mL beaker dissolves ferrous sulphate (7.0g) and ammonium sulphate

(3.5g) in 10mL of water containing 2-3mL of dil.H2SO4 to prevent the hydrolysis of ferrous

sulphate. Boil the solutions for 2-3 minutes and allow the beaker to cool slowly. Pale green

crystals of Mohr’s salt separates out. Filter and dry between the folds of the filter paper.

Report: Yield of Ferrous ammonium sulphate (Mohr’s salt) = ………..g

Experiment No - 4

8www.vikascollege.com

VIKAS PRE-UNIVERSITY COLLEGE

Page 9: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Inorganic salt analysis Aim: Systematic semi-micro qualitative analysis of a simple inorganic salt.

Experiment Observation Inference 1. The given salt is observed in the presence of light.

White crystalline Cu2+,Fe3+,Mn2+,Co2+,Ni2+,may be absent in salt.

Light pink crystalline Mn2+ salts may be present.

White amorphous CO32-,HCO3

-,or S2- may be present

2.Solubility in water: A pinch of salt+ 10 drops of water and shaken.

Soluble No inference possible Insoluble Salts of Na+,K+ or NH4

+ may be absent.

DETECTION OF ACID RADICALS: (ANION)

DETECTION OF FIRST GROUP ACID RADICS: (CO 32-)

A pinch of salt +dil.H2SO4

The gas liberated is passed into the test tube containing lime water.

Brisk effervescence I group acid radicals are present

Lime water turns milky Carbonate is present and confirmed

No brisk effervescence I group acid radicals are absent

DETECTION OF SECOND GROUP ACID RADICALS (Cl-,Br-,NO3-)

A pinch of salt+Conc.H2SO4 Colourless fuming gas is evolved, which gives dense white fumes with a glass rod dipped in NH4OH

II group acid radicals is present Chloride may be present

Reddish brown fumes and the solution turns brown

II group acid radical is present Bromide may be present

No characteristic observation

Chloride and Bromide are absent

Above solution + Copper turnings. Heated strongly.

Reddish brown fumes and the solution turns blue No reddish brown gas

II group acid radicals is present Nitrate may be present Nitrate is absent II group acid radicals absent.

CHEMISTRY PRACTICAL 2

LAB MANUAL

9

Experiment No - 5

Page 10: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

DETECTION OF THIRD GROUP ACID RADICAL(SO42-)

a)Barium Chloride test: Clear solution of the salt in dil.HCl+2drops of Barium chloride solution.

A white precipitate insoluble in excess of dil.HCl

III group acid radical is present Sulphate is present and confirmed

b)Lead acetate test: Clear solution of the salt in water+Acetic acid+Lead acetate solution.

A white precipitate soluble in ammonium acetate solution

Sulphate is present and confirmed.

CONFIRMATORY TEST FOR CHLORIDE (Cl-)

1.Silver Nitrate test: Clear salt solution in dilute Nitric acid+3 drops of silver nitrate solution

A curdy white precipitate soluble in excess of ammonium hydroxide

Chloride is confirmed.

2.Chromyl Chloride test: A pinch of salt +potassium dichromate crystals +few drops of conc.H2SO4,mixture is heated The vapours are dissolved in water. To the yellow solution+3 drops of NH4OH+3 drops of acetic acid+2 drops of lead acetate solution

Reddish brown vapours of Chromyl Chloride are evolved

Yellow solution. Yellow precipitate

Chloride is confirmed.

CONFIRMATORY TEST FOR BROMIDE (Br-)

1.Silver Nitrate test: Clear salt solution in dilute nitric acid boil & cool +3 drops of silver nitrate solution.

A pale yellow precipitate partially soluble in excess of ammonium hydroxide

Bromide is confirmed

2.Orange globule test: Clear salt solution in water+3 drops of carbon tetrachloride+Chlorine water,shaken well.

Orange brown globule separates out

Bromide is confirmed

10www.vikascollege.com

VIKAS PRE-UNIVERSITY COLLEGE

Page 11: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

CONFIRMATORY TEST FOR NITRATE(NO3-):

Brown ring test: 3 drops of clear salt solution in dil.H2SO4+3 drops of freshly saturated solution of Mohr’s salt+conc.H2SO4 is added carefully along the sides of the test tube

A brown ring is formed at the junction of two liquids

Nitrate is confirmed

DETECTION OF BASIC RADICALS (CATIONS):

TEST FOR AMMONIUM (NH4+) RADICAL: (ZERO GROUP ANALYSIS)

Action of NaOH: A pinch of the salt is heated with 5 drops of sodium hydroxide

A Pungent smell of ammonia which gives dense white fumes with a glass rod dipped in conc.HCl

NH4

+ may be present

No pungent smell of ammonia

NH4+ is absent

CONFIRMATORY TEST FOR AMMONIUM (NH4+) RADICAL:

Nessler’s reagent test: One drop of salt solution in water+3 drops of Nessler’s reagent

Brown precipitate is formed

NH4

+ is confirmed

PREPARATION OF ORIGINAL SOLUTION:

The given salt is taken in a test tube and it is dissolved in minimum amount of water or dil.HCl.

CHEMISTRY PRACTICAL 2

LAB MANUAL

11

Page 12: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

DETECTION OF GROUP OF CATIONS:

Group 1: 1cm3 of OS + 1cm3 of dil.HCl in a test tube

No precipitate I group cations are absent

Group II: 1cm3 of OS + 1cm3 of dil.HCl+H2S solution is added

No precipitate II group cations are absent

Group III: 1cm3 of OS +2cm 3 of NH4Cl solution +NH4OH solution in excess

A Gelatinous white precipitate Al3+ may be present

No precipitate III group cations are absent

GroupIV: 1cm3 of OS +2cm 3 of NH4Cl solution +NH4OH solution in excess+H2S solution is added

A flesh coloured precipitate Mn2+ may be present

No precipitate IVgroup cations are absent

GroupV: 1cm3 of OS +2cm 3 of NH4Cl solution +NH4OH solution in excess +(NH4)2CO3 Solution

A white precipitate Ba2+,Sr2+,or ca2+ may be present

No precipitate V group cations are absent

Confirmatory test for Aluminium(Al3+)

a)Sodium hydroxide test: 1Cm3 of original solution+NaOH solution dropwise Above solution is treated with NH4Cl solution.

Gelatinous white precipitate soluble in excess of NaOH White gelatinous precipitate reappears

Al3+ is confirmed

b)Lake test: Original solution+blue litmus solution +NH4OH drop wise along the sides of the test tube

Blue precipitate floating in the colourless solution

Al3+ is confirmed

Confirmatory test for Manganous (Mn2+)

a)Sodium hydroxide test: 1cm 3 of original solution+NaOH solution dropwise.

White precipitate formed is insoluble in excess of NaOH and turns brown on exposure to air.

Mn2+ is confirmed

b) Lead dioxide test: 1cm 3 of OS +conc.HNO3+a pinch of lead dioxide,heated strongly and diluted with water.

Supernatant layer is pink in colour.

Mn2+ is confirmed

12www.vikascollege.com

VIKAS PRE-UNIVERSITY COLLEGE

Page 13: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Confirmatory test for V group cations:

a)Potassium chromate test: 1cm3 of original solution+acetic acid + potassium chromate solution

Yellow precipitate Ba 2+ is confirmed

No yellow precipitate Ba2+ is absent

b)Ammonium sulphate test: 1cm 3 of original solution+ammonium sulphate solution,warm.

White precipitate Sr2+ is confirmed

No white precipitate Sr2+ is absent

c)Ammonium oxalate test: 1Cm3 of original solution+5 drops of NH4OH +Ammonium oxalate solution.

White precipitate Ca2+ is confirmed

Flame test: A pinch of salt +few drops conc.HCl and made into a paste. The paste is held to the flame with the help of a platinum wire.

a)Apple green colour is imparted to the flame b)Crimson red colour is imparted to the flame c)Brick red colour is imparted to the flame

Ba2+ is confirmed Sr2+ is confirmed Ca2+ is confirmed

Analysis of VI group basic radical:

Confirmatory test for Magnesium (Mg2+) 1)Disodium hydrogen phosphate test: 1cm 3 of original solution+2cm3 of NH4OH+5 drops of disodium hydrogen phosphate.The side of the test tube is scratched with glass rod.

White crystalline precipitate

Mg2+ is confirmed.

2) Sodium hydroxide test: 1cm 3 of original solution+NaOH Solution.

White precipitate insoluble in NaOH solution

Mg2+ is confirmed.

Report: The given inorganic salt contains,

Anion is ……………………(……..).It belongs to group……….

Cation is…………………….(…….).It belongs to group……….

Hence the given salt is…………………………(……….)

CHEMISTRY PRACTICAL 2

LAB MANUAL

13

Page 14: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Aim: Test for the functional group present in organic compounds

1)Test for unsaturation:

Experiment Observation Inference a)Baeyer’s test: Organic compound is dissolved in water or acetone+a few drops of 1%alkaline KMnO4 Solution. b)Bromine water test: Organic compound is dissolved in CCl4 +2% Solution of bromine in CCl4 dropwise.

Pink colour of KMnO4

Orange red colour of bromine discharges

The given organic compound is unsaturated

The given organic compound is unsaturated.

2) Test for Alcoholic (R-OH) group:

a) Ceric ammonium nitrate test: Organic compound+few drops of Ceric ammonium nitrate solution.Shaken well. b)Esterification : Organic compound+acetic acid+2 drops of conc.H2SO4 keep it in boiling water bath for 5 minutes.Pour the mixture in Na2CO3 solution

A pink colour or red colour appears.

A fruity smell

Alcoholic (-OH)group present

Alcoholic (-OH)group present

3) Test for Phenolic (Ar-OH) group:

a)Neutral FeCl3 test: Organic compound in a test tube +a few drops of neutral FeCl3 solution.

A violet colour

The given organic compound contains a phenolic group.

b) Phthalein test: Organic compound +phthalic anhydride +conc.H2SO4,heated and added to NaOH

A pink colour

The given organic compound contains a phenolic group.

Experiment No - 6

14www.vikascollege.com

VIKAS PRE-UNIVERSITY COLLEGE

Page 15: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

4) Test for Aldehydic (-CHO)group:

a)2,4-DNP test: Organic compound in a test tube +2,4-Dinitrophenyl hydrazine solution. b)Schiff’s test: Organic compound in a test tube+Schiff’s reagent. c)Tollen’s test: Organic compound in a test tube +Tollen’s reagent keep in a boiling water bath d) Benedict’s /Fehling’s test: Organic compound + Benedict’s /Fehling’s solution and heated.

Orange yellow crystalline precipitate is formed. A pink colour is obtained A black precipitate or silver mirror is formed A brick red precipitate is obtained

The given organic compound contains aldehydic or a ketonic group. The given organic compound contains aldehydic group. The given organic compound confirms the presence of an aldehydic group The given organic compound contains aldehydic group.

5)Test for Ketonic (-CO-)group:

a)m-dinitrobenzene test: Organic compound in a test tube+m-dinitrobenzene(s)+dil.NaOH solution and shake well.

A violet colour which slowly fades

The given organic compound contains Ketonic group.

b) Sodium nitroprusside test: Organic compound in a test tube +Sodium nitroprusside solution +NaOH solution

A wine red colour is obtained

The given organic compound confirms the presence of a ketonic group.

CHEMISTRY PRACTICAL 2

LAB MANUAL

15

Page 16: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

6)Test for carboxylic (-COOH-)group:

a)Litmus test: Organic compound in a test tube+blue litmus paper. b) Sodium Bicarbonate test: Organic compound in a test tube +NaHCO3 solution. c)Esterification: Organic compound in a test tube +ethyl alcohol+2 drops of conc.H SO ,keep it in a 2 4

boiling water bath for 5 minutes and cool,pour into Na2CO3.

Blue litmus paper turns red. Brisk effervescence of CO2

A fruity smell

The given organic compound contains a carboxylic group The given organic compound contains a carboxylic group. The given organic compound confirms the presence of carboxylic group.

7) Test for Amino group(-NH 2) group:

a) Carbylamine test: Organic compound in a test tube +a few drops of chloroform +alcoholic potash.Warm. d)Diazotisation (test for aromatic primary amine) Organic compound dissolved in dil.HCl and cooled in ice .+ice cooled NaNO2 solution +ice cooled solution of β-naphthol in NaOH.

An intolerable smell of isocyanide. A red or orange dye is obtained

The given organic compound is a primary amine and confirms the presence of amino group. Primary aromatic amino group is present.

16www.vikascollege.com

VIKAS PRE-UNIVERSITY COLLEGE

Page 17: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Aim: Preparation of Acetanilide from aniline.

Principle: Acetanilide is prepared by the acetylation of aniline with acetic anhydride in the

presence of acetic acid.

Procedure: Take 10mL of aniline in a round bottom flask.Add 10mL of acetic anhydride and

10mL of acetic acid with constant shaking.The flask is fitted with a reflux condenser and heated

on a sand bath for 10-15 minutes.the flask is cooled and the mixture is added to ice cold water

taken in a 250mL beaker, white solid seperates out.It is filtered,the white solid is impure

acetanilide.

Recrystallisation of acetanilide :

The crude sample is recrystalised using hot water containing a small quantity of ethyl alcohol.

Report:

1.Yield of acetanilide = g

2.Melting point of acetanilide =113oC

Experiment No - 7

CHEMISTRY PRACTICAL 2

LAB MANUAL

17

Page 18: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Aim: Preparation of iodoform crystals.

Principle: Iodoform is prepared by mixing iodine in acetone and 10%Sodium hydroxide

solution.

CH3COCH3 +4I2 +6NaOH------→CHI3 +CH3COONa +5NaI

Procedure: Take 2mL of acetone in a clean conical flask add 5mL of iodine solution and 5mL

of 10%Sodium hydroxide solution to the flask slowly, shake until yellow crystals of iodoform is

formed.

The crystals are filtered, washed and dried between the folds of the filter paper.

Report:

1.Yield of iodoform= g

2.Melting point of iodoform=121oC

Experiment No - 8

18www.vikascollege.com

VIKAS PRE-UNIVERSITY COLLEGE

Page 19: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Preparation of Lyophilic and Lyophobic sol

Aim: To prepare a)Lyophilic sol and b)Lyophobic sol

a)Preparation of Lyophilic sol:

1)Egg Albumin sol: It consists of egg protein dispersed phase and water dispersion medium.

Procedure: 5g of NaCl is dissolved in 100mL H2O in a beaker to get 5%NaCl solution.Egg

Albumin is added into NaCl solution with constant shaking until a colloidal solution of egg

albumin is obtained.

2)Starch sol: In starch sol solid starch is the dispersed phase and water acts a dispersion

medium.

Procedure: A paste of 500mg of starch is prepared in hot water in a beaker.The paste of starch

is added into boiling water taken in another beaker with constant stirring for about 10 minutes

until a colloidal solution of starch is obtained.

b) Preparation of Lyophobic sol:

1.Ferric hydroxide sol: It consists of Fe(OH)3 as dispersed phase and water as dispersion

medium

Procedure: 2g of FeCl3 are dissolved in 100mL of water taken in a beaker to get 2% FeCl3

solution. The solution is added drop by drop into boiling water taken in a separate beaker with

constant stirring until a brown colloidal solution of of Fe(OH)3 is obtained.

2.Arsenous sulphide sol: It consists of As2S3 dispersed phase and water dispersion medium.

Procedure: 0.2g of arsenous oxide is dissolved in 100 mL of boiling water to get 0.2% As2O3

solution, H2S is passed into it till the solution smells H2S.The solution is gently warmed to

remove the excess of H2S and filtered to get the sol.

Experiment No - 9

CHEMISTRY PRACTICAL 2

LAB MANUAL

19

Page 20: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Study the role of emulsifying agent in stabilising the emulsions of different oils

Aim: To study the role of emulsifying agent in stabilising the emulsions of different oils

An emulsion contains liquid dispersed phase and liquid dispersion medium

Soap solution is prepared by dissolving 1g of soap powder in 10ml water.

10 drops each of mustard oil,linseed oil,castor seed oil and machine oil are taken in four

separate test tubes A,B,C and D.And 15ml of distilled water is added to each of the test

tube.

The solutions in the test tube are shaken well and left for settling to get the

emulsion . The time taken for the formation o f separate layer s in each tes t tube is

recorded using a stop clock.

The soap solution is added in drops into each test tube and shaken well for about 5 minutes.

The time taken for the formation of separate layer is recorded using a stop clock.

Tabulation:

Test tube

Oil taken Time taken for the formation of separate layers

Without soap solution

With soap solution

A Mustard oil B Linseed oil

C Castor seed oil D Machine oil

Experiment No -10

20www.vikascollege.com

VIKAS PRE-UNIVERSITY COLLEGE

Page 21: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Determination of heat of neutralization of Hydrochloric acid with Sodium hydroxide

Aim: Determination of heat of neutralization of Hydrochloric acid with Sodium hydroxide

Principle: The heat of neutralization is the amount of heat evolved when one gram equivalent

of an acid is neutralized by 1 gram equivalent of a base.

Procedure: 100cm3 of 1N HCl and 100 cm3 of 1N NaOH are taken in separate polythene

bottles, each fitted with thermometer and a stirrer. Both the solutions are kept in a water bath

maintained at lab temperature for 15 minutes. The temperatures are noted. When both the

solutions attain the same temperature, then Sodium hydroxide is added to hydrochloric acid.

The bottle is stoppered and stirred well. The maximum temperature attained is noted.

Report: Heat of neutralization of HCl is -57.3kJ/mol

Experiment No - 11

CHEMISTRY PRACTICAL 2

LAB MANUAL

21

Page 22: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

Calculations:

Initial temperature,T10C = 25.20C+273=298.2K

Final temperature, T20C = 25.880C+273=298.88K

Rise in temperature =(T2-T1)K = 298.88-298.2 =0.682K

Volume of the solution = 100cm3 +100cm3 =200cm3

Mass of the solution 200g or 0.2kg

Specific heat of water or the solution =4200J/kg/K

Heat liberated during the reaction =mass of the solution × specific heat × rise in temperature

q = 0.2×4200 × =(T2-T1) = q J =0.2×4200×0.682

=0.573 J

1N means 1000cm3 of the solution contains 1 gram eq.mass.

Since 100cm3 of 1mol hydrochloric acid is taken,

Amount of HCl taken =1×100/1000 =0.1g eq.mass.

Amount of heat evolved when 1 gram equivalent mass of HCl is neutralized

q/0.1 =Q J = 0.573J/0.1 = 57.3kJ/eq

Heat liberated is 57.3kJ/equivalent

Heat of neutralisation of Hydrochloric acid = -57.3kJ/mol

22www.vikascollege.com

VIKAS PRE-UNIVERSITY COLLEGE

Page 23: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

CHEMISTRY PRACTICAL 2

LAB MANUAL

1. Do not enter the laboratory when an instructor/lab assistant is not present or the lab door is closed. Finish your lab work on time to clean up before the end of the scheduled lab period.

2. Perform only authorized experiments. Parents, Visitors are not permitted to be with you while you do your lab work.

3. Wear personal protective equipment (PPE) at all times in the chemistry laboratory including when cleaning up following an experiment.

4. Shoes which offer reasonable protection will be worn while in the laboratory. Shoes must cover the entire foot, including the toes, the top of the foot, and the heel.

5. Hair that is longer than shoulder-length must be tied back at all times.

6. Eating, drinking, mouth rinsing, applying cosmetics or lip balm or handling contact lenses is prohibited in the lab areas. No chewing gum is allowed.

7. Be considerate of others working in the laboratory. Do not distract others while conducting experiments or accomplishing lab activities. When finished with equipment or materials to be shared with others, make the equipment or materials available to others as quickly as possible.

8. Before leaving the lab, clean all equipment, glassware and the work area you have been using. Return equipment and glassware to their proper places in the laboratory.

9. Know the location and proper use of safety equipment in the laboratory.

10. Immediately notify the lab instructor of chemical spills, broken glass or other hazards. Do not attempt to clean up such mishaps/materials by yourself without first alerting your instructor/lab supervisor.

11. Immediately notify the instructor/lab supervisor of any accidents, injuries, or situations in which exposure to human blood or other potentially infectious materials in the laboratory has occurred, regardless of how minor they may appear to be.

12. You may be exposed to potentially hazardous materials in the process of completing your required laboratory activities. Persons with specific health concerns such as wearers of contact lenses, persons with known hypersensitivities, etc. should consult their personal physician for advisement about potential risks before continuing in the course.

SAFETY PROCEDURE IN LAB

Page 24: CHEMISTRY PRACTICAL 2 · PDF file... Dissolve in potassium sulphate (2.0g) and aluminium sulphate ... Report: Yield of Ferrous ammonium sulphate ... CHEMISTRY PRACTICAL 2 LAB MANUAL

SUCCESS GUARANTEED ONLY AT VIKAS