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B.Sc.-I Mannual PDF
B.Sc.-I Mannual PDF
Record File
Department Of Chemistry
KHANDELWAL COLLEGE OF
MANAGEMENT SCIENCE &
TECHNOLOGY
Bareilly
B.Sc. – I
Name of Student ...................................... ..........
Roll. Number: -
Session: 2018-19
Note: - This lab manual will be treated as practical record file in the final university exam.
1
INDEX
Sl.
Name of the experiment Page No.
No.
GENERAL- EXPERIMENT
1 4-5
To analyze the given inorganic mixture and identify two acid and two basic
2 6-7
radicals
To analyze the given inorganic mixture and identify two acid and two basic
3
radicals
To analyze the given inorganic mixture and identify two acid and two basic
4
radicals
To analyze the given inorganic mixture and identify two acid and two basic
5
radicals
To analyze the given inorganic mixture and identify two acid and two basic
6
radicals
preparation of sodium extract, identification of functional groups and odour
7
of different compounds
To identify the given organic compound
8
2
Instructions/Working hints
1. Maintain the silence in the lab.
2. Attend the lab session in time.
3. Don’t forget to bring Lab manual and lab coat.
4. Cleaning of apparatus: - It is essential to keep all apparatus scrupulously clean if trustworthy
results are to be obtained. All apparatus must be thoroughly cleaned with chromosulphuric acid
(concentrated sulphuric acid containing about 100g of potassium dichromate per litre) or with a brush
and cleaning powder. The cleaning agent is highly corrosive. The apparatus is then rinsed several
times with tap water, and repeatedly with distilled water. All apparatus should have been cleaned
during the previous laboratory period.
5. Upon commencing work, arrange the more common and frequently used apparatus in an orderly
manner on your bench. Each item of apparatus should have a definite place so that it can be found
readily when required.
6. Return each reagent bottle to its proper place immediately after use.
7. Reagent bottles and their stoppers should not be put upon the bench. They should be returned to
their correct places upon the shelves immediately after use. If a reagent bottle is empty, it should be
returned to the store-room for filling.
8. Do not waste gas or chemicals. The size of the Bunsen flame should be no longer than is absolutely
necessary. It should be extinguished when no longer required.
9. Never dip your own dropper into a reagent. Pour a little of the reagent into a small clean vessel
(test-tube, crucible, beaker etc) and introduce your dropper into this. Never return the reagent to the
bottle. It is better to waste a little of the reagent than to take the risk of contaminating the whole
supply.
10. Do not introduce your spatula into a reagent bottle to remove a little solid. Pour a little of the solid
on to a clean, dry watch glass, and use this. Do not return the solid reagent to the stock bottle. 11. Try
to estimate your requirements and pour out only the amount necessary.
12. Record your observations briefly in your note-book in ink immediately after each operation has
been completed.
.
Declaration by Student
I have read and understand these rules and procedures. I agree to abide by these rules and
procedure at all time during the lab. I understand that failure to follow these rules and procedure will result
in my immediate dismissal from the laboratory and additional disciplinary action may be taken.
3
GENERAL- EXPERIMENT
Aim: - To analyze the given inorganic mixture and identify two acid and two basic radicals.
Apparatus: Test tubes, Test tube holder, Test tube stands, beaker etc.
ACID RADICALS
4
GROUP TEST FOR
BASIC RADICALS
Group Test : - boil
1. Mixture + 1 ml. NaOH smell of
Ammonia observe Zero group present
2. Aqueous solution of mixture + 1 ml. dil. HCL
Appearance of white ppt. I group present
3. Acidic solution of mixture + pass H2S gas Coloured ppt. appears
II group present
4. Acidic solution of mixture (or) Filtrate of II-Group boil with 1ml. conc. HNO3
Add small amount of NH4Cl and excess of NH4OH Gelatinous ppt. appears III-
Group present.
5. Filtrate of III-Group – boil till the removal of NH4Cl + NH4OH and pass H2S
Coloured ppt. appears – IV group present
6. Evaporate the filtrate of IV – group till the removal of H2S +
heat
NH4OH (excess) add (NH4)2CO3 in excess If ppt. appears within
5 minutes V-group present.
7. Mixture + 1 ml. NaOH Smell of Ammonia does not observe Zero group
absent Evaporate the filtrate of V- group to one third ,add little quantity of (NH4)2SO4 and
(NH4)2C2O4 if ppt. appears filter and discard the residue, use the filtrate for the identification of
Mg2+
8. Aqueous solution of mixture + dil. HCL No ppt. appears I-group absent
9. Acidic solution of mixture + H2S No. ppt. appears II-group absent
10. Acidic solution of mixture boil with 1 ml. conc. HNO3 add small amount of NH4Cl and excess
of NH4OH No ppt. appears III-group absent
11. Filtrate of III-group + small quantity of NH4Cl + NH4OH and pass H2S
(Excess)
5
EXPERIMENTAL No. 1
Aim :- To analyse the given inorganic mixture and identify three acid and two basic
radicals.
Apparatus : Test tubes, Test tube holder, Test tube stands, beaker etc.
6
GROUP TEST FOR
BASIC RADICALS
boil
1. Mixture + 1 ml. NaOH smell of Ammonia observe Zero group present
White ppt of I- group boil whit ppt. dissolve. Pb2+ may be present.
2 water
Add KI in solution Yellow colour appear Pb2+ confirmed.
7
EXPERIMENTAL No. 2
Aim :- To analyse the given inorganic mixture and identify three acid and two basic
radicals.
Apparatus : Test tubes, Test tube holder, Test tube stands, beaker etc.
Mixture + dil. HCL heat to boil Appearance of white ppt. SO42- may be present
and fitter
2ml. Filtrate + 2 ml. BaCl2 Ppt. does not dissolve SO42- confirmed
3
Add conc. HNO3 to the ppt.
8
GROUP TEST FOR
BASIC RADICALS
1. Mixture + 1 ml. NaOH Smell of Ammonia does not observe Zero group absent.
3. Acidic solution of mixture + pass H2S gas Coloured ppt. appear II group
present
9
Experiment No-3
Aim: - To analyses the given inorganic mixture and identify three acid and two basic
radicals.
Apparatus: Test tubes, Test tube holder, Test tube stands, beaker etc.
2ml. Filtrate + 2 ml. BaCl2 Appearance of white ppt. SO42- may be present
SO42- confirmed
Add conc. HNO3 to the ppt. Ppt. does not dissolve
10
GROUP TEST FOR
BASIC RADICALS
1. Mixture + 1 ml. NaOH Smell of Ammonia does not observe
Zero group absent
2.Aqueous solution of mixture + dil. HCl
No ppt. appears I-group absent
3.Acidic solution of mixture + H2S
No. ppt. appears II-group absent
4.Acidic solution of mixture (or) Filterate of II-Group boil with 1ml. conc. HNO3
Add small amount of NH4Cl and excess of NH4OH Gelatinous ppt. appears
III-Group present.
5. Filterate of III-Group – boil till the removal of NH4Cl + NH4OH and pass H2S
Coloured ppt. appears – IV group present
ppt of IIIrd group boil with Residue observe Fe3+ may be present
NaOH
Residue desolve in conc. Blue colour appears Fe3+ confirms
HNO3 and add
1 K4[Fe(CN)6]
Shake the ppt of IVth group Residue form Co3+, Ni2+ may be
and filter present
11
Experiment No-4
Aim: - To analyses the given inorganic mixture and identify three acid and two basic
radicals.
Apparatus: Test tubes, Test tube holder, Test tube stands, beaker etc.
2ml. Filtrate + 2 ml. BaCl2 Appearance of white ppt. SO42- may be present
SO42- confirmed
Add conc. HNO3 to the ppt. Ppt. does not dissolve
12
GROUP TEST FOR
BASIC RADICALS
1. Mixture + 1 ml. NaOH Smell of Ammonia does not observe
Zero group absent
2.Aqueous solution of mixture + dil. HCl
No ppt. appears I-group absent
3.Acidic solution of mixture + H2S
No. ppt. appears II-group absent
4.Acidic solution of mixture (or) Filterate of II-Group boil with 1ml. conc. HNO3
Add small amount of NH4Cl and excess of NH4OH Gelatinous ppt. appears
III-Group present.
5.Filterate of III-Group – boil till the removal of NH4Cl + NH4OH and pass H2S
Coloured ppt. appears – IV group present
ppt of IIIrd group boil with Residue observe Al3+, Cr3+ may be
NaOH present
Filtrate (solution) boil with White ppt.appears
NH4Cl Al3+ confirms
1
ppt of IVth group shake Ppt dissolve Mn2+, Zn2+ may be
with NaOH present
Aim :- To analyse the given inorganic mixture and identify three acid and two basic
radicals.
Apparatus : Test tubes, Test tube holder, Test tube stands, beaker etc.
Mixture + Conc. H2SO4 Brown colour gas appears NO3-- may be present
3 2ml. Filtrate + 2 ml. BaCl2 Ppt. does not dissolve SO42- confirmed
14
GROUP TEST FOR
BASIC RADICALS
1. Mixture + 1 ml. NaOH Smell of Ammonia does not observe Zero group absent
2. Aqueous solution of mixture + dil. HCl No ppt. appears I-group absent
3. Acidic solution of mixture + H2S No. ppt. appears II-group absent
4. Acidic solution of mixture boil with 1 ml. conc. HNO3 add small amount of NH4Cl and excess of
NH4OH No ppt. appears III-group absent
5. Filtrate of III- group + small quantity of NH4Cl + NH4OH (excess) and pass H2S No. ppt.
appears IV-group absent
6. Evaporate the filtrate of IV – group till the removal of H2S + NH4OH (excess) heat
Procedure : - Take one test tube distt. water in a porceline dish ,take sodium metal and O.S.( equal to
rice grain) in a ignition tube, heat to red hot and pour in the porceline dish repeat the same process in same
porceline dish ,boil till the volume reduce to half filter . Filtrate is called sodium extract
Detection of Nitrogen :-- take 1ml.sodium extract + 1 ml.freshly prepared FeSO4 → a dirty green colour
is observed ,add 1 ml.dill. H2SO4 → prussion blue colour observed → Nitrogen is present in the organic
compound
Na + C +N → NaCN
FeSO4 + 2NaOH → Fe(OH)2 + Na2(SO)4
Fe(OH)2 +6NaCN → Na4[Fe(CN)6] + 2NaOH
2FeSO4+H2SO4+O(Air)→Fe2(SO4)3+H2O
3 Na4[Fe(CN)6] + 2 Fe2(SO4)3 → Fe4[Fe(CN)6]3 + 6Na2SO4
Ferric-Ferrocyanid
Detection of Halogen :---
Acidify 2ml sodium extract with dil. HNO3 and add an excess of AgNO3 solution. A curdy white
precipitate indicates the presence of a halogen. Decant the mother liquor and treat the precipitate with
dil.aqueous ammonia and observe:-
The ppt is white curdy- readily dissolves in aq.ammonia – Cl-
The ppt is curdy whitish yellow – difficulty soluble in aq.ammonia –Br-
The ppt is curdy yellow – insoluble in aqueous ammonia – I-
Na + X → NaX
1. warm 1ml.organic liquid with Bromine water , Bromine water decolorized . organic liquid is
unsaturated
2. 1ml.organic liquid add 1ml.cerric ammonium nitrate appearance of red colour confirms the presence of
alcoholic group
3. 1ml.organic liquid,0.5ml.NaOH and 1ml.sodiumnitopruside appearance of wine red colour confirms the
presence of Ketonic group
4. 1ml.organic liquid add 1ml. Tolluence reagent appearance of Black colour / silver mirror confirms the
presence of Aldehydic group
5. 1ml.organic liquid add1ml.NaHCO3 evolution of brisk effervescence confirms the presence of
carboxylic group
6. 1ml.organic liquid ,2 drops of NaOH,1ml.phenolpthaline indicator.apink colour appears warm the
solution pink colour disappears it confirms the presence of ester group
16
Odour :----
Observation Inference
Odour of better almond Benzaldehyde, Benzonitrile, Nitrobenzene
Pleasant-Fruity Ester
17
Experiment No.: - 7
Preliminary Observation:
Element detection:
Detection of Nitrogen :-- take 1ml.sodium extract + 1 ml.freshly prepared FeSO4 → a dirty green colour
is observed ,add 1 ml.dill. H2SO4 → No prussion blue colour observed → Nitrogen is absent in the organic
compound
Acidify 2ml sodium extract with dil. HNO3 and add an excess of AgNO3 solution. No curdy precipitate
appears→ Halogen is absent in the organic compound
Functional group test: 1ml.organic liquid add 1ml.cerric ammonium nitrate appearance of red colour
confirms the presence of alcoholic group
Confirmatory test: 1ml. liquid +few crystal of salicylic acid+ 3-4drops of Conc.H2SO4 and heat gently
A smell like IODEX is observe due to the formation of Methyl
salicylate→Methylalchol confirmed
Structural Formula:
18
Experiment: - 8
Preliminary Observation:
Element detection:
Detection of Nitrogen :-- take 1ml.sodium extract + 1 ml.freshly prepared FeSO4 → a dirty green colour
is observed ,add 1 ml.dill. H2SO4 → No prussion blue colour observed → Nitrogen is absent in the organic
compound
Acidify 2ml sodium extract with dil. HNO3 and add an excess of AgNO3 solution. No curdy precipitate
appears→ Halogen is absent in the organic compound
Functional group test: 1ml.organic liquid, 0.5ml.NaOH and 1ml.sodiumnitopruside appearance of wine
red colour confirms the presence of Ketonic group
Confirmatory test: 1ml. organic liquid in a beaker + 5ml NaOH+ 2 drops of iodine solution, stirrer the
solution, appearance of yellow colour confirms the presence of acetone due to the formation of iodoform.
Structural Formula:
19
Experiment: - 9
Preliminary Observation:
Element detection:
Detection of Nitrogen :-- take 1ml.sodium extract + 1 ml.freshly prepared FeSO4 → a dirty green colour
is observed ,add 1 ml.dill. H2SO4 → No prussion blue colour observed → Nitrogen is absent in the organic
compound
Acidify 2ml sodium extract with dil. HNO3 and add an excess of AgNO3 solution. No curdy precipitate
appears→ Halogen is absent in the organic compound
Functional group test: 1ml.organic liquid add 1ml. Tolluence reagent appearance of Black colour / silver
mirror confirms the presence of Aldehydic group
Confirmatory test: 1ml.organic liquid add 1ml. Tolluence reagent appearance of Black colour / silver
mirror confirms the presence of formaldehyde.
Structural Formula:
20
Experiment: - 10
Preliminary Observation:
Element detection:
Detection of Nitrogen :-- take 1ml.sodium extract + 1 ml. freshly prepared FeSO4 → a dirty green colour
is observed ,add 1 ml.dill. H2SO4 → No prussion blue colour observed → Nitrogen is absent in the organic
compound
Acidify 2ml sodium extract with dil. HNO3 and add an excess of AgNO3 solution. No curdy precipitate
appears→ Halogen is absent in the organic compound
Functional group test: 1ml.organic liquid add1ml.NaHCO3 evolution of brisk effervescence confirms the
presence of carboxylic group
Confirmatory test: 2ml.organic liquid add 1ml. mercuric chloride + 2ml formic acid and heat white /grey
ppt obtained confirms the presence of formaldehyde.
Structural Formula:
21
Experiment: - 11
Preliminary Observation:
Element detection:
Detection of Nitrogen :-- take 1ml.sodium extract + 1 ml. freshly prepared FeSO4 → a dirty green colour
is observed ,add 1 ml.dill. H2SO4 → No prussion blue colour observed → Nitrogen is absent in the organic
compound
Acidify 2ml sodium extract with dil. HNO3 and add an excess of AgNO3 solution. No curdy precipitate
appears→ Halogen is absent in the organic compound
Functional group test: 1ml.organic liquid add1ml.NaHCO3 evolution of brisk effervescence confirms the
presence of carboxylic group
Confirmatory test: 2ml. neutral organic liquid add 2ml. dil FeCl3 Solution, red colour of ferric acetate
obtained confirms the presence of Acetic acid.
Structural Formula:
22
Experiment: - 12
Preliminary Observation:
Element detection:
Detection of Nitrogen :-- take 1ml.sodium extract + 1 ml. freshly prepared FeSO4 → a dirty green colour
is observed ,add 1 ml.dill. H2SO4 → No prussion blue colour observed → Nitrogen is present in the
organic compound
Acidify 2ml sodium extract with dil. HNO3 and add an excess of AgNO3 solution. No curdy precipitate
appears→ Halogen is absent in the organic compound
Functional group test: Heat small quantity of given organic compound + dil NaOH evolution of
ammonia gas confirms the presence of amide group
Confirmatory test (Biuret test): 0.2gm of organic compound in a dry test tube and heat gently urea melts
and ammonia gas evolved gradually the liquid solidifies due to the formation of biuret confirms the
presence of urea. Add 2 ml dil NaOH+1ml CuSO4 → Purple colour obtains.
Structural Formula:
23
Experiment: - 13
Preliminary Observation:
Acidify 2ml sodium extract with dil. HNO3 and add an excess of AgNO3 solution. No curdy precipitate
appears→ Halogen is absent in the organic compound
Functional group test: Heat small quantity of given organic compound + dil NaOH evolution of
ammonia gas confirms the presence of amide group
Confirmatory test: Heat 0.2gm of organic compound + dil H2SO4 →Vineger smell due to the formation
of acetic acid.
Structural Formula:
24
Experiment: - 14
Preliminary Observation:
Acidify 2ml sodium extract with dil. HNO3 and add an excess of AgNO3 solution. No curdy precipitate
appears→ Halogen is absent in the organic compound
Functional group test: 1ml.organic liquid add1ml.NaHCO3 evolution of brisk effervescence confirms the
presence of carboxylic group
Confirmatory test: 200mg organic compound + dil H2SO4 Solution+ few drops of KMnO4 and warm →
decolonization confirms the presence of oxalic acid.
Structural Formula:
25
Experiment: - 15
Preliminary Observation:
Acidify 2ml sodium extract with dil. HNO3 and add an excess of AgNO3 solution. No curdy precipitate
appears→ Halogen is absent in the organic compound
Functional group test: 1ml.organic liquid add1ml.NaHCO3 evolution of brisk effervescence confirms the
presence of carboxylic group
Confirmatory test: Neutral sol. of organic compound + CaCl2 and boil → White ppt of calcium citrate
confirms the presence of Citric acid.
Structural Formula:
26
Experiment: - 16
Preliminary Observation:
Acidify 2ml sodium extract with dil. HNO3 and add an excess of AgNO3 solution. No curdy precipitate
appears→ Halogen is absent in the organic compound
Confirmatory test: boil 1ml of ester + dil alkali → acetic acid and ethyl alcohol are produced.
1ml. organic liquid in a beaker + 5ml NaOH+ 2 drops of iodine solution, stirrer the solution, appearance
of yellow colour confirms the presence of acetone due to the formation of iodoform.
Structural Formula:
Aim :- To determine the composition of given mixture of two miscible liquids of salt and
sugar by viscosity method using Ostwald’s viscometer
Theory:
Viscosity is the property of liquid & gases. It is a force between the layers of liquid which oppose
to flow. Lower layer of the liquid have the zero velocity & the upper layer liquid has maximum
velocity.
Unity of viscosity
𝐹 𝑐𝑒 𝐷𝑖 𝑎 𝑐𝑒
= x
𝑎 𝑒𝑎 𝑉𝑒𝑙 𝑐𝑖 𝑦
𝑀𝑎 x 𝑙𝑒 𝑔 ℎ x t e− e t
= x
𝑙𝑒 𝑔 ℎ e t /t e
28
Observation table:
% of sugar-------------
% of salt -----------------
29
Experiment No-18
Aim: - To determine the composition of given mixture of two miscible liquids of methyl
alcohol and water by Surface tension method using Stalagnometer
Theory:
The upper surface of the liquid is under tension & tends to contract to a small possible area.
Their fore liquid surface has to minimize the number of molecule at the surface. Due to this region
the drops of liquid in air attained the spherical shape. Which have minimum surface area their fore
surface face tension (𝛾) is defined as
The force in dynes along the surface of a liquid at right angle to any line 1 cm in length.
In SI --------------------------- N/m
30
Observation table:
5. unknown
% of CH3OH -------------
% of H2O -----------------
31