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Chemistry Practicals
SPEF Chemistry
Lab Set up
Common Apparatus
Common Reagents
Special Reagents
Common Lab Rules
Chemistry Is an Experimental Science
Lab Setup
List of Common apparatus for each student for the exam
• Burette
• Pipette
• Burette stand
• White Tile
• Conical flask
• Wash bottle
• Test tube stand
• 6 test tubes
• Boiling tube
• Test tube holder
• Funnel
• Bent tube
• Small beaker (100ml)
• Measuring cylinder
• Tripod stand with Wire guaze
• Burner
• China dish
• Watch glass
• Spatula
• Filter papers
• Glass rod
• Litmus Paper
Common Reagents to be kept on shelf
Solutions 13. Ammonium carbonate
1. Dilute HCl 14. Lead acetate solution
2. Dilute HNO3
3. Dilute H2SO4
4. NH4OH
5. NaOH Solid Reagents
6. Lime Water 1. Sodium Carbonate (s)
7. Neutral Ferric Chloride 2. Ferrous sulphate (s)
8. Barium chloride solution 3. Ammonium Chloride (s)
9. Silver nitrate Solution 4. Oxalic acid
10. Potassium Chromate solution 5. Cu turnings
11. Potassium Iodide solution
Special Reagents
1. Potassium Ferrocyanide 7. Nessler’s reagent
2. Potassium ferricyanide 8. Pyrogallol
3. Disodium hydrogen phosphate 9. Sodium nitroprusside
4. Ammonium Oxalate 10. Phenolphthalein
5. Felhing’s solution 11. Borax
6. Acetic acid 12. Resorcinol
Lab Rules
Lab coat and goggles is compulsory
Keep your surroundings clean
Wash your apparatus after use
Clean your table thoroughly before you leave
Replace the reagents on the shelf
Follow instructions strictly
Precautions for observation table and titre value [4m]
1. Note down the capacity of the pipette (20 / 25 ml )
Note : different schools have different capacity of pipettes
2. Do the expt thrice before reporting it to the examiner (write in pencil first before fairing it up)
3. Ensure all pencil work is faired up in pen later
4. Observation table has to be tabulated
5. Average of titre value is NOT allowed
6. Do not report the titre value till two decimals as least count is 0.1 ml.
7. Atleast two readings have to be same (concordant)
8. If the burette reading comes in whole number, then express it till one decimal. E.g if the
burette reading is 16, express as 16.0 ml
9. Conclude the observation table by mentioning the concordant burette reading in cm3 or ml.
10. ONLY an error of only +/- 0.2 cm3 is allowed.
11. Titre value reported to the examiner ONLY has to be used for the calculation.
Systematic Analysis Of Anions
1. Dilute H2SO4 group –
A. Carbonate (CO3
2-) ,
B. Acetate CH3COO-
2. Conc. H2SO4 group –
A. Chloride (Cl-),
B. Nitrate (NO3
-)
3. Sulphate (SO4
2-)
Experiment Observation Inference
1.
Action of dil. HCl/ dil H2SO4:
About 1ml of dil. HCl is taken
in the test tube and a small
quantity of mixture added.
Brisk effervescences with
the evolution of a
colourless odourless gas
which turns moist blue
litmus red.
Gas evolved is CO2
X2CO3 + 2HCl → 2XCl + CO2 + H2O
2. Gas passed through lime
water
Lime water turns milky Carbonate confirmed.
1. Start the test in the boiling tube
2. Keep the lime water ready
3. Brisk effervescences should be observed on the surface of the liquid.
4. All Carbonates are insoluble except ammonium carbonate and sodium carbonate.
5. Lime water test should be done with sodium carbonate extract.
Experiment Observation
Inference
2.
Action of dil. HCl/ dil H2SO4:
Action of dil H2SO4:-
A little of the substance is rubbed
with dil H2SO4 and the smell
noted
Smell of vinegar
Presence of Acetate (CH3COO-)
CH3COONa+H2SO4→CH3COOH+Na2
SO4
1 Experiment Observation Inference
1.
Action of Conc.H2SO4:-
A little substance is heated
with 0.5ml of Conc.H2SO4
Evolution of a pungent gas
which turns moist blue litmus
paper red and fumes when
glass rod dipped in
NH4OH is brought to the mouth
of the test tube
Gas evolved is HCl gas
Presence of chloride
NaCl+H2SO4→NaHSO4+HCl
2. About 10mg of the salt is
warmed with 0.5 ml of
Conc.H2SO4 and copper
turnings
Evolution of a reddish
brown pungent gas
Gas is NO2.
Presence of Nitrate
NaNO3+H2SO4→NaHSO4+HNO3
Use only about 1ml of sulphuric acid for one spatula full of salt.
PREPARATION OF SODIUM CARBONATE EXTRACT :-
Sodium Carbonate extract is made by boiling 1gm of the
substance with thrice its weight of anhydrous sodium
carbonate and 20ml of water in a small beaker for about
15 minutes. It is then cooled and filtered. The filtrate is
called the sodium carbonate extract.
The confirmatory tests are done with the sodium
carbonate extract.
Experiment Observation Inference
1.
Silver Nitrate test:
(For chloride ion)
A little of the sodium carbonate
extract is neutralized with dilute
HNO3, then boiled to expel CO2
and silver nitrate solution is
added
A curdy white ppt is obtained
which is soluble in NH4OH.
Presence of Chloride is confirmed
CONFIRMATORY TESTS FOR ANIONS USING SODIUM CARBONATE EXTRACT : -
It is important to boil off CO2, because any excess sodium carbonate in the solution mat give a white ppt of
silver carbonate.
Experiment Observation Inference
2. Brown Ring test:-
(For nitrate ion)
A little of the sodium carbonate extract
is acidified with dil H2SO4 , boiled to
expel CO2 and add freshly prepared
solution of Ferrous sulphate followed
by conc H2SO4 by the side of the test
Formation of a brown
ring at the junction of
the two layers.
Presence of nitrate is
confirmed.
CONFIRMATORY TESTS FOR ANIONS USING SODIUM CARBONATE EXTRACT : -
Experiment Observation Inference
3.
Test for acetate ion :-
A little of the sodium carbonate
extract is neutralized with
dil.HNO3 (boil to expel CO2)+
neutral FeCl3 solution
Wine red
colouration
Acetate confirmed
CONFIRMATORY TESTS FOR ANIONS USING SODIUM CARBONATE EXTRACT : -
Experiment Observation Inference
4. Sodium Carbonate extract is
neutralized with dil HNO3 + BaCl2
solution
White ppt is
obtained which in
insoluble in all
mineral acids
Sulphate confirmed
CONFIRMATORY TESTS FOR ANIONS USING SODIUM CARBONATE EXTRACT : -
SYSTEMATIC ANALYSIS OF CATIONS
Preparation of Original solution :
Mixture + water -SolubleInsoluble
Mixture + Dil HCl - SolubleInsoluble
Mixutre + dilute HNO3 - Soluble
Since the salt is soluble in dilute Nitric acid, O.S is prepared by dissolving about
0.1 gm of the substance is dissolved in dilute HNO3 to get the original solution.
All Nitrates are soluble.
All Chlorides are soluble except Lead
chloride and silver chloride
All sulphates are soluble except
sulphates of Ba, Sr, Ca
All Ammonium salts are soluble
GROUP SEPARATION TABLE:--
S.N Experiment Observation Inference
1. Salt + NaOH + heat Pungent smell of
Ammonia
Presence of group Zero.
2. O.S + Dilute HCl White ppt obtained Presence of Group I (Pb2+)
3. H2S passed through the above solution Black ppt Presence of Group II (Cu2+)
4 H2S is boiled off. A few drops of conc.
HNO3 are added and boiled again and
cooled. NH4Cl crystals & excess of
NH4OH is added.
A gelatinous white ppt is
obtained
Presence of group III (Al3+)
5. H2S is passed through above solution. White ppt Presence of group IV(Zn2+)
6. H2S is boiled off and NH4Cl, NH4OH and
excess of (NH4)2CO3 is added
White ppt obtained
Presence of group V
(Ba2+, Sr2+, Ca2+)
7.
To the above solution Disodium
hydrogen phosphate is added
Crystalline white ppt is
obtained when a glass rod is
rubbed by the side of the test
tube
Presence of group VI
(Mg2+) Magnesium
confirmed
a)Salt + NaOH,heat
b) To the above expt, glass rod
dipped in HCl is brought near
to the mouth of the test tube
Colourless gas with Pungent odour
which turns moist red litmus blue
White dense fumes of NH4Cl
The gas is NH3
The gas is NH3
NH4
+ confirmed
Confirmatory test
Salt +NaOH, heat and the gas is
passed through Nessler’s
reagent
Brown colouration followed by
precipitation
The gas is NH3
NH4
+ confirmed
Salt +NaOH, heat and the gas is
passed through paper dipped
in Nessler’s reagent
Paper turns brown The gas is NH3
NH4
+ confirmed
Zero Group
Part I + KI Yellow ppt, dissolved in hot water and
reappears as golden spangles on cooling.
Pb2+ confirmed
Part II + K2CrO4 Yellow ppt Pb2+ confirmed
Group I : Pb2+
Precipitate obtained in group I dissolved in hot distilled water and divide into two
parts
Part I + NH4OH in excess Pale blue ppt which dissolves in excess to
give a deep blue solution.
Cu2+ confirmed
Part II + K4Fe(CN)6 Chocolate brown ppt Cu2+ confirmed
Group II : Cu2+
Precipitate obtained in group II dissolved in hot dilute HNO3 and divided into two parts
To the above dissolved ppt + few
drops of blue litmus solution
+ excess of NH4OH
Blue lake (pale blue floating ppt in
colourless solution)
Al3+ confirmed
Dissolve the gelatinous white ppt obtained in group III in dil. HCl
Group III : Al3+
Part 1 + Potassium ferrocyanide Bluish white ppt Zn2+ confirmed
Part 2 + NaOH White ppt soluble in excess Zn2+ confirmed
Dissolve the white ppt obtained in group IV in dil. HCl and divide the solution into two parts
Group IV : Zn2+
Part 1 + Potassium Chromate solution Yellow ppt Ba2+ confirmed
Part 2 + Ammonium sulphate solution White ppt Sr2+ confirmed
Part 3 + Ammonium oxalate White ppt Ca2+ confirmed
Dissolve the white ppt obtained in group V in warm acetic acid, boil off CO2 and divide the
solution into three parts
Group V :
Ba2+, Sr2+, Ca2+
S.No Reagent Concentration/L Special instructions
1 Dilute Hydrochloric acid 89 ml/L
Add to 500 ml water and make
upto 1 L
2 Dilute Nitric acid 63 ml/ L
Add to 500 ml water and make
upto 1 L
3 Dilute Sulphuric acid 54 ml/L
Add 54 ml of conc. Sulphuric acid
to 500 ml of water then make up to
1L
4 Dilute acetic acid 56 ml/L
Add to 500 ml water and make
upto 1 L
5 Sodium hydroxide 80 g/L
Dissolve in water and make upto 1
L
6 Ammonium hydroxide 71ml/L
Add to 500 ml water and make
upto 1 L
7 Ammonium carbonate
96g/L and 70 ml
ammonia
Dissolve in a mixture of ammonia
S.No1 Reagent Concentration/L Special instructions
9
Disodium hydrogen
phosphate
107.5 g/L Dissolve in water and make upto 1 L
10 Lead Acetate 190 g/L Dissolve in water and make upto 1 L
11 Potassium Chromate 48.5 g/L Dissolve in water and make upto 1 L
12 Potassium dichromate 24.5 g/L Dissolve in water and make upto 1 L
13 Potassium Iodide 83 g/L Dissolve in water and make upto 1 L
14 Silver nitrate 17 g/L
Dissolve in water and make upto
1 L
15 Barium Chloride 61 g/L
Dissolve in water and make upto
1 L
16 Neutral Ferric chloride 80 g/L
To the ferric chloride solution add
ammonium hydroxide gradually,
then boil to remove excess of
ammonia

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1540274713-Qualitative analysis.pptx

  • 2. Lab Set up Common Apparatus Common Reagents Special Reagents Common Lab Rules Chemistry Is an Experimental Science
  • 4. List of Common apparatus for each student for the exam • Burette • Pipette • Burette stand • White Tile • Conical flask • Wash bottle • Test tube stand • 6 test tubes • Boiling tube • Test tube holder • Funnel • Bent tube • Small beaker (100ml) • Measuring cylinder • Tripod stand with Wire guaze • Burner • China dish • Watch glass • Spatula • Filter papers • Glass rod • Litmus Paper
  • 5. Common Reagents to be kept on shelf Solutions 13. Ammonium carbonate 1. Dilute HCl 14. Lead acetate solution 2. Dilute HNO3 3. Dilute H2SO4 4. NH4OH 5. NaOH Solid Reagents 6. Lime Water 1. Sodium Carbonate (s) 7. Neutral Ferric Chloride 2. Ferrous sulphate (s) 8. Barium chloride solution 3. Ammonium Chloride (s) 9. Silver nitrate Solution 4. Oxalic acid 10. Potassium Chromate solution 5. Cu turnings 11. Potassium Iodide solution
  • 6. Special Reagents 1. Potassium Ferrocyanide 7. Nessler’s reagent 2. Potassium ferricyanide 8. Pyrogallol 3. Disodium hydrogen phosphate 9. Sodium nitroprusside 4. Ammonium Oxalate 10. Phenolphthalein 5. Felhing’s solution 11. Borax 6. Acetic acid 12. Resorcinol
  • 7. Lab Rules Lab coat and goggles is compulsory Keep your surroundings clean Wash your apparatus after use Clean your table thoroughly before you leave Replace the reagents on the shelf Follow instructions strictly
  • 8. Precautions for observation table and titre value [4m] 1. Note down the capacity of the pipette (20 / 25 ml ) Note : different schools have different capacity of pipettes 2. Do the expt thrice before reporting it to the examiner (write in pencil first before fairing it up) 3. Ensure all pencil work is faired up in pen later 4. Observation table has to be tabulated 5. Average of titre value is NOT allowed 6. Do not report the titre value till two decimals as least count is 0.1 ml. 7. Atleast two readings have to be same (concordant) 8. If the burette reading comes in whole number, then express it till one decimal. E.g if the burette reading is 16, express as 16.0 ml 9. Conclude the observation table by mentioning the concordant burette reading in cm3 or ml. 10. ONLY an error of only +/- 0.2 cm3 is allowed. 11. Titre value reported to the examiner ONLY has to be used for the calculation.
  • 9.
  • 10. Systematic Analysis Of Anions 1. Dilute H2SO4 group – A. Carbonate (CO3 2-) , B. Acetate CH3COO- 2. Conc. H2SO4 group – A. Chloride (Cl-), B. Nitrate (NO3 -) 3. Sulphate (SO4 2-)
  • 11. Experiment Observation Inference 1. Action of dil. HCl/ dil H2SO4: About 1ml of dil. HCl is taken in the test tube and a small quantity of mixture added. Brisk effervescences with the evolution of a colourless odourless gas which turns moist blue litmus red. Gas evolved is CO2 X2CO3 + 2HCl → 2XCl + CO2 + H2O 2. Gas passed through lime water Lime water turns milky Carbonate confirmed. 1. Start the test in the boiling tube 2. Keep the lime water ready 3. Brisk effervescences should be observed on the surface of the liquid. 4. All Carbonates are insoluble except ammonium carbonate and sodium carbonate. 5. Lime water test should be done with sodium carbonate extract.
  • 12. Experiment Observation Inference 2. Action of dil. HCl/ dil H2SO4: Action of dil H2SO4:- A little of the substance is rubbed with dil H2SO4 and the smell noted Smell of vinegar Presence of Acetate (CH3COO-) CH3COONa+H2SO4→CH3COOH+Na2 SO4
  • 13. 1 Experiment Observation Inference 1. Action of Conc.H2SO4:- A little substance is heated with 0.5ml of Conc.H2SO4 Evolution of a pungent gas which turns moist blue litmus paper red and fumes when glass rod dipped in NH4OH is brought to the mouth of the test tube Gas evolved is HCl gas Presence of chloride NaCl+H2SO4→NaHSO4+HCl 2. About 10mg of the salt is warmed with 0.5 ml of Conc.H2SO4 and copper turnings Evolution of a reddish brown pungent gas Gas is NO2. Presence of Nitrate NaNO3+H2SO4→NaHSO4+HNO3 Use only about 1ml of sulphuric acid for one spatula full of salt.
  • 14. PREPARATION OF SODIUM CARBONATE EXTRACT :- Sodium Carbonate extract is made by boiling 1gm of the substance with thrice its weight of anhydrous sodium carbonate and 20ml of water in a small beaker for about 15 minutes. It is then cooled and filtered. The filtrate is called the sodium carbonate extract. The confirmatory tests are done with the sodium carbonate extract.
  • 15. Experiment Observation Inference 1. Silver Nitrate test: (For chloride ion) A little of the sodium carbonate extract is neutralized with dilute HNO3, then boiled to expel CO2 and silver nitrate solution is added A curdy white ppt is obtained which is soluble in NH4OH. Presence of Chloride is confirmed CONFIRMATORY TESTS FOR ANIONS USING SODIUM CARBONATE EXTRACT : - It is important to boil off CO2, because any excess sodium carbonate in the solution mat give a white ppt of silver carbonate.
  • 16. Experiment Observation Inference 2. Brown Ring test:- (For nitrate ion) A little of the sodium carbonate extract is acidified with dil H2SO4 , boiled to expel CO2 and add freshly prepared solution of Ferrous sulphate followed by conc H2SO4 by the side of the test Formation of a brown ring at the junction of the two layers. Presence of nitrate is confirmed. CONFIRMATORY TESTS FOR ANIONS USING SODIUM CARBONATE EXTRACT : -
  • 17. Experiment Observation Inference 3. Test for acetate ion :- A little of the sodium carbonate extract is neutralized with dil.HNO3 (boil to expel CO2)+ neutral FeCl3 solution Wine red colouration Acetate confirmed CONFIRMATORY TESTS FOR ANIONS USING SODIUM CARBONATE EXTRACT : -
  • 18. Experiment Observation Inference 4. Sodium Carbonate extract is neutralized with dil HNO3 + BaCl2 solution White ppt is obtained which in insoluble in all mineral acids Sulphate confirmed CONFIRMATORY TESTS FOR ANIONS USING SODIUM CARBONATE EXTRACT : -
  • 19. SYSTEMATIC ANALYSIS OF CATIONS Preparation of Original solution : Mixture + water -SolubleInsoluble Mixture + Dil HCl - SolubleInsoluble Mixutre + dilute HNO3 - Soluble Since the salt is soluble in dilute Nitric acid, O.S is prepared by dissolving about 0.1 gm of the substance is dissolved in dilute HNO3 to get the original solution. All Nitrates are soluble. All Chlorides are soluble except Lead chloride and silver chloride All sulphates are soluble except sulphates of Ba, Sr, Ca All Ammonium salts are soluble
  • 20. GROUP SEPARATION TABLE:-- S.N Experiment Observation Inference 1. Salt + NaOH + heat Pungent smell of Ammonia Presence of group Zero. 2. O.S + Dilute HCl White ppt obtained Presence of Group I (Pb2+) 3. H2S passed through the above solution Black ppt Presence of Group II (Cu2+) 4 H2S is boiled off. A few drops of conc. HNO3 are added and boiled again and cooled. NH4Cl crystals & excess of NH4OH is added. A gelatinous white ppt is obtained Presence of group III (Al3+) 5. H2S is passed through above solution. White ppt Presence of group IV(Zn2+) 6. H2S is boiled off and NH4Cl, NH4OH and excess of (NH4)2CO3 is added White ppt obtained Presence of group V (Ba2+, Sr2+, Ca2+) 7. To the above solution Disodium hydrogen phosphate is added Crystalline white ppt is obtained when a glass rod is rubbed by the side of the test tube Presence of group VI (Mg2+) Magnesium confirmed
  • 21. a)Salt + NaOH,heat b) To the above expt, glass rod dipped in HCl is brought near to the mouth of the test tube Colourless gas with Pungent odour which turns moist red litmus blue White dense fumes of NH4Cl The gas is NH3 The gas is NH3 NH4 + confirmed Confirmatory test Salt +NaOH, heat and the gas is passed through Nessler’s reagent Brown colouration followed by precipitation The gas is NH3 NH4 + confirmed Salt +NaOH, heat and the gas is passed through paper dipped in Nessler’s reagent Paper turns brown The gas is NH3 NH4 + confirmed Zero Group
  • 22. Part I + KI Yellow ppt, dissolved in hot water and reappears as golden spangles on cooling. Pb2+ confirmed Part II + K2CrO4 Yellow ppt Pb2+ confirmed Group I : Pb2+ Precipitate obtained in group I dissolved in hot distilled water and divide into two parts
  • 23. Part I + NH4OH in excess Pale blue ppt which dissolves in excess to give a deep blue solution. Cu2+ confirmed Part II + K4Fe(CN)6 Chocolate brown ppt Cu2+ confirmed Group II : Cu2+ Precipitate obtained in group II dissolved in hot dilute HNO3 and divided into two parts
  • 24. To the above dissolved ppt + few drops of blue litmus solution + excess of NH4OH Blue lake (pale blue floating ppt in colourless solution) Al3+ confirmed Dissolve the gelatinous white ppt obtained in group III in dil. HCl Group III : Al3+
  • 25. Part 1 + Potassium ferrocyanide Bluish white ppt Zn2+ confirmed Part 2 + NaOH White ppt soluble in excess Zn2+ confirmed Dissolve the white ppt obtained in group IV in dil. HCl and divide the solution into two parts Group IV : Zn2+
  • 26. Part 1 + Potassium Chromate solution Yellow ppt Ba2+ confirmed Part 2 + Ammonium sulphate solution White ppt Sr2+ confirmed Part 3 + Ammonium oxalate White ppt Ca2+ confirmed Dissolve the white ppt obtained in group V in warm acetic acid, boil off CO2 and divide the solution into three parts Group V : Ba2+, Sr2+, Ca2+
  • 27. S.No Reagent Concentration/L Special instructions 1 Dilute Hydrochloric acid 89 ml/L Add to 500 ml water and make upto 1 L 2 Dilute Nitric acid 63 ml/ L Add to 500 ml water and make upto 1 L 3 Dilute Sulphuric acid 54 ml/L Add 54 ml of conc. Sulphuric acid to 500 ml of water then make up to 1L 4 Dilute acetic acid 56 ml/L Add to 500 ml water and make upto 1 L 5 Sodium hydroxide 80 g/L Dissolve in water and make upto 1 L 6 Ammonium hydroxide 71ml/L Add to 500 ml water and make upto 1 L 7 Ammonium carbonate 96g/L and 70 ml ammonia Dissolve in a mixture of ammonia
  • 28. S.No1 Reagent Concentration/L Special instructions 9 Disodium hydrogen phosphate 107.5 g/L Dissolve in water and make upto 1 L 10 Lead Acetate 190 g/L Dissolve in water and make upto 1 L 11 Potassium Chromate 48.5 g/L Dissolve in water and make upto 1 L 12 Potassium dichromate 24.5 g/L Dissolve in water and make upto 1 L 13 Potassium Iodide 83 g/L Dissolve in water and make upto 1 L 14 Silver nitrate 17 g/L Dissolve in water and make upto 1 L 15 Barium Chloride 61 g/L Dissolve in water and make upto 1 L 16 Neutral Ferric chloride 80 g/L To the ferric chloride solution add ammonium hydroxide gradually, then boil to remove excess of ammonia

Editor's Notes

  1. This is the question that your experiment answers
  2. Summarize your research in three to five points.
  3. Establish hypothesis before you begin the experiment. This should be your best educated guess based on your research.