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EXERIMENT NO – 3 (A) 2.

Weigh the exact amount of clean and dried watch glass and record its
weight in the notebook.
Aim: To prepare the standard solution M/10 of oxalic acids. 3. Weigh correctly on the watch glass 3.15 g of oxalic acid and record this
weight in the notebook.
Theory: Hydrated oxalic acid = C H O .2H O
2 2 4 2
4. Using a funnel, transfer oxalic acid softly and carefully from the watch
glass into a clean and dry measuring flask.
Molecular mass of Oxalic Acid = 126. 5. Wash the watch glass with distilled water to move the particles that stick
to it into the foam with the assistance of a wash bottle.
12.6 g of oxalic acid per litre of the solution should be dissolved to prepare M/10 6. For this purpose, the volume of distilled water should not exceed 50 ml.
oxalic acid solution. 7. Wash funnels several times with distilled water to move the sticking
On the other hand, 12.6 /4 = 3.15 g of crystals of oxalic acid should be particles into the measuring flask using a wash bottle. Add water in tiny
dissolved in water and precisely 250 ml of the solution should be produced. quantities while washing the funnel. The distilled water quantity used for
this purpose should not exceed 50 mL.
8. Using a wash bottle, wash the funnel carefully with distilled water to pass
Materials Required: Chemical balance ,Watch glass ,Weight box, the solution attached to the funnel into the measuring flask
250ml beaker, Glass rod 250ml measuring flask , Wash bottle, Weighing tube, 9. Turn the flask of measurement until the oxalic acid dissolves.
Oxalic acid, Funnel Funnel stand , Distilled water 10. Using a wash bottle, thoroughly add enough distilled water to the
measuring flask just below the etched mark on it.
11. Add the last few mL of distilled water drop into the measuring flask until
Apparatus Setup: the reduced meniscus level just touches the mark.
12. Put the stopper on the mouth of the flask and shake softly to make the
entire solution uniform. Calculate it as a solution of oxalic acid M/10.

Observation:
Weight of the watch glass W1g

Weight of the watch glass + Oxalic acid W1 + 3.15g

Weight of Oxalic acid 3.150g

Volume of distilled water 250cm3

Results: 250cm 3 of decimolar or (M/10) solution of oxalic acid is prepared.


Precautions:
1. Weighing of oxalic acid crystals need weights of 2g + 1g + 100mg + 5mg.
2. Wash the watch glass carefully so that even a single crystal of oxalic acid
is not left on the watch glass.
3. Last few drops should be added using a pipette to avoid extra addition of
Step by Step Laboratory Preparation of Standard Solution of Oxalic Acid distilled water above the mark on the neck of the measuring cylinder.
4. If it is necessary to titrate oxalic acid or oxalate, add the required dilute
Procedure: H2SO4 amount and heat the flask to 60 °-70 ° C.

1. Take a watch glass, wash it with distilled water and dry it.
EXERIMENT NO – 3 (B) 11. Add the last few mL of distilled water drop into the measuring flask until
the reduced meniscus level just touches the mark.
12. Put the stopper on the mouth of the flask and shake softly to make the
Aim - To determine the strength of a given solution of sodium hydroxide entire solution uniform. Calculate it as a solution of oxalic acid M/10.
solution by titrating it against a standard solution of oxalic acid.
Theory - This estimation involves titration of a weak acid that is oxalic (b) Titration of Sodium Hydroxide and Oxalic Acid
acid against a strong base sodium hydroxide and phenolphthalein is the
indicator of choice. The reaction between oxalic acid and sodium hydroxide Solution
is (COOH)2 + 2NaOH → (COONa)2 + 2H2O
1. Rinse the burette with the standard oxalic acid solution.
Since sodium hydroxide is not a primary standard a standard solution of oxalic 2. Take 10cm3 of oxalic acid solution in a titration flask. Fill the burette with
acid is prepared and used for standardisation of sodium hydroxide. sodium hydroxide solution.
In acid-base titration at the end point the amount of acid becomes chemically 3. Remove the air gap if any, from the burette by running the solution
equivalent to the amount of base present. In case of strong acid and strong base forcefully from the burette nozzle and note the initial reading
titration at the end point of solution the solution becomes neutral. 4. Pipette out 20ml of NaOH solution is a conical flask. Add 2-3 drops of
phenolphthalein indicator to it.
Materials Required – Burette, Pipette , Conical flask, Burette stand, 5. Titrate the base with oxalic acid solution until the pink colour disappears.
Funnel, Stirrer, White glazed tile, Measuring flask , Oxalic acid (solid), Oxalic acid 6. Repeat the titration till three concordant readings are obtained.
(as per needed), Sodium hydroxide solution (as per needed), Phenolphthalein
indicator (as per needed)
Observations
Apparatus Setup – Directed by TEACHER 1. Molarity of oxalic acid solution=M10
2. Molarity of sodium hydroxide solution = x
Procedure 3. Volume of oxalic acid solution = 10cm3
4. Indicator = Phenolphthalein
5. End point = Light pink colour
(a) Preparation of 0.1M Standard Oxalic Acid Solution
1. Take a watch glass, wash it with distilled water and dry it. S.No Initial Reading Final Reading Volume of Concordant
2. Weigh the exact amount of clean and dried watch glass and record its of the Burette of the Burette NaOH solution Reading
weight in the notebook. used
3. Weigh 3.15 g of oxalic acid on the watch glass correctly and record this
weight in the notebook.
4. Using a funnel, transfer oxalic acid softly and carefully from the watch
1 a cm3 b cm3 (b-a) cm3 V cm3
glass into a clean and dry measuring flask.
5. Wash the watch glass with distilled water to move the particles that stick
to it into the foam with the assistance of a wash bottle.
6. For this purpose, the volume of distilled water should not exceed 50 ml. 2 b cm3 c cm3 (c-b) cm3 V cm3
7. Wash the funnel several times with distilled water to move the sticking
particles into the measuring flask using a wash bottle. Add water in tiny
quantities while washing the funnel. The distilled water quantity used for 3 c cm3 d cm3 (d-c) cm3 V cm3
this purpose should not exceed 50 mL.
8. Using a wash bottle, wash the funnel carefully with distilled water to pass
the solution attached to the funnel into the measuring flask
9. Turn the flask of measurement until the oxalic acid dissolves.
10. Using a wash bottle, thoroughly add enough distilled water to the
measuring flask just below the etched mark on it.
Calculations
Mass of oxalic acid dissolved in 100ml of standard solution = y g
Strength of oxalicacid=y×10g/L

Normality(N) of standard oxalic acid=Strength/Eq.wt=y×1063.04=N

Normality (N1) of sodium hydroxide solution


N1×V1=N×V

Therefore,
N1=N×VV1

Normality (N2) of given oxalic acid solution


N2×V2=N1×V1

N2=N1×V1V2

Strength of given oxalic acid = N2 x 63.04 g/L

Results and Discussion


The strength of the given sodium hydroxide solution is _______ g/L.

Precautions
1. Weighing of oxalic acid crystals need weights of 2g + 1g + 100mg +
50mg.
2. While weighing, do not spill the substance on the balance pan.
3. Rotate the knob of balance gently.
4. Keep the weights in the weights box at the proper places after weighing
5. Wash the watch glass carefully so that even a single crystal is not left on
the watch glass.
6. Bring the watch glass close to the funnel while transferring weighed
substance and transfer it gently. Wash it repeatedly with distilled water.
7. Wash the burette with water after titration is over.
8. The last few drops should be added using a pipette to avoid extra addition
of distilled water above the mark on the neck of the measuring cylinder.
EXERIMENT NO – 3 (C) Observations
Aim- To prepare the 250 cm 3
of N/10 standard solution of sodium Weight of the watch glass
carbonate.

Theory- Sodium carbonate is essentially insoluble in nearly saturated Weight of the watch glass + Sodium carbonate
sodium hydroxide. The insoluble sodium carbonate will settle to the bottom
of the container after the saturated NaOH has equilibrated for a couple of
days. The supernatant can be withdrawn carefully to prepare a diluted Weight of Sodium carbonate
NaOH solution free of sodium carbonate. The water for preparing NaOH
standard solution should be boiled to remove any dissolved CO 2, because
dissolved CO2 can cause a titration error. To prepare the standard solution Volume of distilled water
of sodium carbonate, The equivalent weight of sodium carbonate =
Molecular weight2=1062=53

1000cm3 of normal sodium carbonate solution requires 53g of sodium carbonate. Results and Discussion
Therefore, 250cm3 of 250cm3 of decimolar or N/10 standard solution of sodium carbonate is prepared.
N10, sodium carbonate requires

531000×25010=1.325g
Precautions
1. While weighing do not spill the substance on the balance pan
Materials Required - Chemical balance, Watch glass, Weight box, 2. While preparing the laboratory reagent apron should be used.
250ml beaker, Glass rod. 250ml measuring flask, Wash bottle, Weighing 3. Bases are highly corrosive so they should be handled with extreme care.
tube, Sodium Carbonate, Funnel, Funnel stand, Distilled water 4. Watch glass must be dry.
5. Funnel should be washed thoroughly several times.
6. Shaking of solution should be done thoroughly so that it may become
Apparatus Setup- As set up in experiment 3 (A) uniform.
7. While making the solution the solvent should be added such that the
Procedure lower meniscus of the solvent must be on the mark of the measuring
flask.
1. Weigh the exact amount of clean and dried watch glass and record its
8. Last few drops should be added using a pipette to avoid extra addition of
weight in the notebook.
distilled water above the mark on the neck of the measuring cylinder.
2. Weigh correctly on the watch glass with 1.325 g of sodium carbonate
Using a funnel, transfer sodium carbonate softly and carefully from the
watch glass into a clean and dry measuring flask.
3. Wash the watch glass with distilled water to move the particles that stick
to it into the foam with the assistance of a wash bottle.
4. Wash funnels several times with distilled water to move the sticking
particles into the measuring flask using a wash bottle. Add water in tiny
quantities while washing the funnel. The distilled water quantity used for
this purpose should not exceed 50 mL.
5. Add the last few mL of distilled water drop into the measuring flask until
the reduced meniscus level just touches the mark.
6. Put the stopper on the mouth of the flask and shake softly to make the
entire solution uniform. Calculate it as a solution of sodium carbonate
N/10.
EXERIMENT NO – 3 (D) Observations
Aim - Determination of strength of a given solution of dilute Hydrochloric Volume of HCl solution = 10cm3
acid by titrating it against standard solution of Sodium Carbonate solution
(M/10). Volume of sodium carbonate solution used = V cm3

Theory - Hydrochloric acid solution may be titrated against sodium S.No Initial reading of Final reading of Volume of Sodium
carbonate solution using methyl orange indicator. When weak base is the burette the burette carbonate solution used.
titrated with a strong acid, solution will be slightly acidic at end point. If a
weak acid is titrated with a strong base the solution is slightly basic
because the salt formed will be hydrolysed to a certain extent. 1
The chemical reactions involved in this titration are given below.
Na2CO3(aq) + 2HCl(aq) → 2NaCl(aq) + CO2(g) + H2O(l) 2
CO (aq) + 2H (aq) → CO2(g) + H2O(l)
3
2- +

In acid base titrations at the end point the amount of the acid becomes chemically 3
equivalent to the amount of base present. In case of a strong acid and a strong
base titration at the end point of solution the solution becomes neutral.
Materials Required – Burette, Pipette , Conical flask, Burette stand,
Funnel, Measuring flask, Hydrochloric acid,Sodium carbonate, Methyl orange Calculations
Procedure

(a) Preparation of standard solution of sodium


carbonate
1. Molecular weight of sodium carbonate = 106
2. Amount of sodium carbonate required to prepare solution of 250ml = 1.325g
3. Dissolve 1.325g of sodium carbonate in distilled water and prepare the
standard solution in 250ml of measuring flask by adding the required amount Results and Discussion
of water.
The strength of hydrochloric acid solution is ________ g/L.
(b) Titration of HCl and sodium carbonate solution
Precautions-
1. Wash, rinse and fill the burette with M/10 Na2CO3 solution. Note the initial
reading. 1. While weighing do not spill the substance on balance pan.
2. Take 10cm3 of HCl solution with the help of a pipette and transfer it into a clean 2. Rotate the knob of balance gently.
washed titration flask. 3. Keep the weights in weights box at proper places after weighing
3. Add 2 drops of methyl orange into the titration flask. 4. Wash the watch glass carefully so that even a single crystal is not left on the
4. 4. Add M/10 sodium carbonate solution to the titration flask till the colour watch glass.
changes to the light pink. 5. Bring the watch glass close to funnel while transferring weighed substance and
5. transfer it gently. Wash it repeatedly with distilled water.
6. Note the final reading and find out the volume of sodium carbonate solution 6. Wash the burette with water after titration is over.
used to neutralize HCl solution. 7. Last few drops should be added using pipette to avoid extra addition of distilled
7. Repeat the experiment till you get concordant readings. water above the mark on the neck of the measuring cylinder.
EXERIMENT NO – 4 (A) EXERIMENT NO – 4 (B)
Experiment No 08 AIM- To detect one cation and one anion radical from given AIM- To detect one cation and one anion radical from given salt.
salt. A.. PHYSICAL EXAMINATION
A.. PHYSICAL EXAMINATION COLOUR- WHITE AND CRYSTALLINE – Cu++,Ni++,Fe+++, Fe++, Mn++, Co++ Ni++ absent
COLOUR- WHITE AND CRYSTALLINE – Cu ,Ni ,Fe , Fe , Mn , Co Ni absent
++ ++ +++ ++ ++ ++ ++ Odour- characterstic pungent smell- NH4+ may be present
Odour- characterstic pungent smell- NH4+ may be present Solubility- soluble in water
Solubility- soluble in water Soluble in Dil. HCl
Soluble in Dil. HCl Dry Heating Test-
Dry Heating Test- S.N. EXPERIMENT OBSERVATION INFERENCE
S.N. EXPERIMENT OBSERVATION INFERENCE 1 Heat a pinch of salt in dry No redish brown gas NO3- absent
1 Heat a pinch of salt in No redish brown gas NO3- absent test tube Sublimation not occurs Halide may be absent
dry test tube Sublimation occurs Halide may be present No crackling sound Pb(NO3)2 may be absent
No crackling sound Pb(NO3)2 may be absent
B. TEST FOR ACIDIC RADICAL
B. TEST FOR ACIDIC RADICAL S.N. EXPERIMENT OBSERVATION INFERENCE
S.N. EXPERIMENT OBSERVATION INFERENCE 1. Dil H2SO4 test No effervasence of CO2 CO32- absent
1. Dil H2SO4 test No effervasence of CO2 CO32- absent Take a pinch of salt in No rotten egg smell of H2S s2- absent
a test tube add Dil No S02 gas ( turn K2Cr2O7 green) so32- absent
Take a pinch of salt in No rotten egg smell of H2S s2- absent
No S02 gas ( turn K2Cr2O7 green) H2SO4 No reddish Brown gas make NO2- absent
a test tube add Dil so32- absent FeSO4 solution black
H2SO4 No reddish Brown gas make NO2- absent
FeSO4 solution black 2. Conc. H2SO4 test Colorless odourless gas (CO2) C2O42-(oxalate)
2. Conc. H2SO4 test HCl gas (suffocating smell) Cl- may be Take a pinch of salt in a may be present
Take a pinch of salt in a test tube add Conc
Give white PPT with AgNO3 present
H2SO4
test tube add Conc (soluble in NH4OH)
H2SO4 3. CONFIRMATORY TEST White PPT C2O42-(oxalate)
CONFIRMATORY TEST White PPT – soluble in NH4OH Cl- Confirm a. To the salt solution Confirm
3.
a. To the salt solution add acetic acid and
add conc HNO3 and calcium chloride
AgNO3 solution C2O42-(oxalate)
b. To the salt solution Pink colour of KMnO4 discharged Confirm
b. To the salt add MnO2 add Dil H2SO4 and warm
and Conc H2SO4 and Cl2 gas evolves Cl- Confirm
add 2-3 drops of KMnO4
heat . solution
c. Salt + solid K2Cr2O7 + Red vapours- add NaOH ( yellow
solution obtained) add acetic acid Cl- Confirm
Conc H2SO4 & heat C. TEST FOR BASIC RADICAL
& lead acetate - Yellow PPT 1. To the salt solution add Smell of ammonia NH4+ may be
C. TEST FOR BASIC RADICAL NaOH solution and heat present
1. To the salt solution add Smell of ammonia NH4+ may be 2. Bring a glass rod dipped White fumes appears NH4+ may be
NaOH solution and heat present in Dil HCl over the test present
2. Bring a glass rod dipped White fumes appears NH4+ may be tube
in Dil HCl over the test present 3. Add Nessler’s reagent Brown PPT formed NH4+ confirm
tube Result- The given salt has NH4+ is cation and C2O42- as anion radical
3. Add Nessler’s reagent Brown PPT formed NH4+ confirm
By – Hasin Ahmed Dekho seekho jano 9425761832
Result- The given salt is NH4 Cl in which NH4+ is cation and Cl- as anion radical
EXERIMENT NO – 4 (C) EXERIMENT NO – 4 (D)
AIM- To detect one cation and one anion radical from given salt. AIM- To detect one cation and one anion radical from given salt.
A.. PHYSICAL EXAMINATION A.. PHYSICAL EXAMINATION
COLOUR- WHITE AND CRYSTALLINE – Cu++,Ni++,Fe+++, Fe++, Mn++, Co++ Ni++ absent COLOUR- WHITE AND CRYSTALLINE – Cu++,Ni++,Fe+++, Fe++, Mn++, Co++ Ni++ absent
Odour- NO characterstic pungent smell- NH4+ may be absent Odour- characterstic pungent smell- CH3COO- may be present
Solubility- soluble in water Solubility- soluble in water
Soluble in Dil. HCl Soluble in Dil. HCl
Dry Heating Test- Dry Heating Test-
S.N. EXPERIMENT OBSERVATION INFERENCE S.N. EXPERIMENT OBSERVATION INFERENCE
1 Heat a pinch of salt in Reddish brown gas NO3- may be present 1 Heat a pinch of salt in No redish brown gas NO3- absent
dry test tube NO Sublimation occurs Halide may be absent dry test tube Sublimation not occurs Halide may be absent
Crackling sound Pb(NO3)2 may be present No crackling sound Pb(NO3)2 may be
absent
B. TEST FOR ACIDIC RADICAL
B. TEST FOR ACIDIC RADICAL
S.N. EXPERIMENT OBSERVATION INFERENCE
S.N. EXPERIMENT OBSERVATION INFERENCE
1. Dil H2SO4 test No effervasence of CO2 CO32- absent
1. Dil H2SO4 test No effervasence of CO2 CO32- absent
Take a pinch of salt in a No rotten egg smell of H2S s2- absent
No S02 gas ( turn K2Cr2O7 green) Take a pinch of salt in No rotten egg smell of H2S s2- absent
test tube add Dil H2SO4 so32- absent
No reddish Brown gas make a test tube add Dil No S02 gas ( turn K2Cr2O7 green) so32- absent
NO2- absent No reddish Brown gas make
FeSO4 solution black H2SO4 NO2- absent
FeSO4 solution black
2. Conc. H2SO4 test NO2 gas (reddish brown)- NO3- may be
Take a pinch of salt in a 2. Conc. H2SO4 test Colorless vapours of vinegar CH3COO-
turn FeSO4 solution black present
test tube add Conc H2SO4 Take a pinch of salt in a smell (acetate)
test tube add Conc H2SO4 may be
3. CONFIRMATORY TEST Reddish brown gas NO3- Confirm
a. To the salt solution add present
conc H2SO4 and Cu chipps 3. CONFIRMATORY TEST Vinegar smell CH3COO-
then heat. a. To the solid salt add (acetate)
oxalic acid and 2-3 drops Confirm
b. To the salt solution add Dark brown ring NO3- Confirm of water- Rub with finger
FeSO4 soln and Conc
b. ESTER TESST- To the CH3COO-
H2SO4 by the side of test Fruity smell of ester
salt solution add ethanol (acetate)
tube .
and Conc H2SO4 and heat Confirm
C. TEST FOR BASIC RADICAL
1. To the salt solution add No Smell of ammonia Zero group NH4+ C. TEST FOR BASIC RADICAL
NaOH solution and heat absent 1. To the salt solution add No Smell of ammonia Zero group
2. To the salt add dil HCl White PPT Pb++ may be present NaOH solution and heat NH4+ absent
3. CONFIRMATORY TEST 2. To the salt add dil HCl White PPT Pb++ may be
To the above solution Yellow PPT formed Pb++ confirm present
I.add KI soln (one part) 3. CONFIRMATORY TEST
ii. add K2CrO4 soln Yellow PPT formed Pb++ confirm To the above solution Yellow PPT formed Pb++ confirm

Result- The given salt is has Pb++ is cation and NO3 as anion radical
- I.add KI soln (one part)
ii. add K2CrO4 soln Yellow PPT formed Pb++ confirm
Result- The given salt is (CH3COO)2Pb in which Pb++ is cation and CH3COO- as anion
radical
EXERIMENT NO – 4 (E) EXERIMENT NO – 4 (F)
AIM- To detect one cation and one anion radical from given salt. AIM- To detect one cation and one anion radical from given salt.
A.. PHYSICAL EXAMINATION A.. PHYSICAL EXAMINATION
COLOUR- WHITE AND CRYSTALLINE – Cu++,Ni++,Fe+++, Fe++, Mn++, Co++ Ni++ absent COLOUR- WHITE AND CRYSTALLINE – Cu++,Ni++,Fe+++, Fe++, Mn++, Co++ Ni++ absent
Odour- characterstic pungent smell- NH4+ may be present
Odour- characterstic pungent smell- NH4+ may be present
Solubility- soluble in water
Solubility- soluble in water Soluble in Dil. HCl
Soluble in Dil. HCl
Dry Heating Test-
Dry Heating Test- S.N. EXPERIMENT OBSERVATION INFERENCE
1 Heat a pinch of salt in dry No redish brown gas NO3- absent
S.N. EXPERIMENT OBSERVATION INFERENCE test tube Sublimation not occurs Halide may be absent
1 Heat a pinch of salt in Colourless odourless gas May be CO32-- present No crackling sound Pb(NO3)2 may be absent
dry test tube which turns lime water milky
No Sublimation occurs Halide absent
B. TEST FOR ACIDIC RADICAL
No crackling sound Pb(NO3)2 may be absent
S.N. EXPERIMENT OBSERVATION INFERENCE
B. TEST FOR ACIDIC RADICAL 1. Dil H2SO4 test No effervasence of CO2 CO32- absent
Take a pinch of salt in a No rotten egg smell of H2S s2- absent
S.N. EXPERIMENT OBSERVATION INFERENCE No S02 gas ( turn K2Cr2O7 green)
test tube add Dil H2SO4 so32- absent
1. Dil H2SO4 test Effervesence of CO2, which CO32- may be No reddish Brown gas make FeSO4 NO2- absent
Take a pinch of salt in turns lime water milky present solution black
a test tube add Dil 2. Conc. H2SO4 test No Colorless odourless gas (CO2) C2O42-absent
Take a pinch of salt in a No smell of vinegar CH3COO- absent
H2SO4
test tube add Conc H2SO4 No colourless pungent smell gas Cl- absent
2. CONFIRMATORY TEST CO2 Gas evolved with brisk CO32- Confirm No brown colour gas of pungent smell Br- absent
a. To the salt solution effervescence No voilet vapour of pungent smell I- absent
add Dil HCl No reddish brown gas of pungent
smell
b. To the salt solution 3. Special group test White PPT SO42-(sulphate)
White PPT CO32- Confirm
add MgSO4 solution. a. To the salt add dil HCl and Confirm
filter. To the filtrate add BaCl2

C. TEST FOR BASIC RADICAL C. TEST FOR BASIC RADICAL


1. To the salt solution Smell of ammonia NH4+ may be 1. To the salt solution add No Smell of ammonia NH4+ is absent
NaOH solution and heat (group 0 absent)
add NaOH solution present
2. To the salt solution add Dil No White PPT appears Pb++ is absent
and heat HCl (group 1 absent)
2. Bring a glass rod White fumes appears NH4+ may be 3. Pass H2S gas to above No Black PPT formed or any PPT Cu++ , Pb++ absent
dipped in Dil HCl over present solution (group 2nd absent)
4. To the salt solution add White PPT formation Al+++ may be
the test tube solid NH4Cl , Con HNO3, present
3. Add Nessler’s reagent Brown PPT formed NH4+ confirm and NH4OH till smell of NH3
5 To the white PPT add dil HCl A white PPT (suspended in colourless Al+++ may be
few drops of Blue litmus + medium) called a lake, present
NH4OH soln in excess
Result- The given salt is NH4 (CO3)2 in which NH4+ is cation and CO32- as
Result- The given salt has Al2 (SO4)3 in which A+++ is cation and SO42- as anion radical
anion radical By – Hasin Ahmed Dekho seekho jano 9425761832
By – Hasin Ahmed Dekho seekho jano 9425761832
EXERIMENT NO – 4 (G) EXERIMENT NO – 4 (H)
AIM- To detect one cation and one anion radical from given salt. AIM- To detect one cation and one anion radical from given salt.
A.. PHYSICAL EXAMINATION
A.. PHYSICAL EXAMINATION
COLOUR- WHITE AND CRYSTALLINE – Cu++,Ni++,Fe+++, Fe++, Mn++, Co++ Ni++ absent
COLOUR- WHITE AND CRYSTALLINE – Cu++,Ni++,Fe+++, Fe++, Mn++, Co++ Ni++ absent
Odour- characterstic pungent smell- NH4+ may be present
Odour- characterstic pungent smell- NH4+ may be present
Solubility- soluble in water , and in Dil HCl
Solubility- soluble in water , and in Dil HCl
Dry Heating Test-
Dry Heating Test-
S.N. EXPERIMENT OBSERVATION INFERENCE
S.N. EXPERIMENT OBSERVATION INFERENCE
1 Heat a pinch of salt in dry Reddish brown gas NO3- may be present
1 Heat a pinch of salt Reddish brown gas NO3- may be present
test tube NO Sublimation occurs Halide may be absent
in dry test tube NO Sublimation occurs Halide may be absent
B. TEST FOR ACIDIC RADICAL
B. TEST FOR ACIDIC RADICAL
S.N. EXPERIMENT OBSERVATION INFERENCE
S.N. EXPERIMENT OBSERVATION INFERENCE
1. Dil H2SO4 test No effervasence of CO2 CO32- absent
Take a pinch of salt in a test No rotten egg smell of H2S s2- absent 1. Dil H2SO4 test No effervasence of CO2 CO32- absent
tube add Dil H2SO4 No S02 gas ( turn K2Cr2O7 green) so32- absent Take a pinch of salt No rotten egg smell of H2S s2- absent
No reddish Brown gas make NO2- absent in a test tube add Dil No S02 gas ( turn K2Cr2O7 green) so32- absent
FeSO4 solution black H2SO4 No reddish Brown gas make FeSO4 NO2- absent
Conc. H2SO4 test - Take a NO2 gas (reddish brown)- turn NO3- may be present solution black
2.
pinch of salt in a test tube FeSO4 solution black 2. Conc. H2SO4 test No Colorless odourless gas (CO2) C2O42-absent
add Conc H2SO4 Take a pinch of salt in a No smell of vinegar CH3COO- absent
3. CONFIRMATORY TEST test tube add Conc No colourless pungent smell gas Cl- absent
a. To the salt solution add conc Reddish brown gas NO3- Confirm H2SO4 No brown colour gas of pungent smell Br- absent
H2SO4 and Cu chipps then heat. No voilet vapour of pungent smell I- absent
No reddish brown gas of pungent smell
b. To the salt solution add FeSO4
soln and Conc H2SO4 by the side
Dark brown ring NO3- Confirm
3. Special group test
a. To the salt add dil HCl and
White PPT obtained
SO42- (sulphate)
of test tube . Confirm
filter. To the filtrate add BaCl2
C. TEST FOR BASIC RADICAL
To the salt solution add No Smell of ammonia NH4+ is absent C. TEST FOR BASIC RADICAL
1.
(group 0 absent) 1. To the salt solution add No Smell of ammonia NH4+ is absent
NaOH solution and heat
NaOH solution and heat (group 0 absent)
2. To the salt solution add Dil No White PPT appears Pb++ is absent
(group 1 absent) 2. To the salt solution add Dil No White PPT appears Pb++ is absent
HCl
HCl (group 1 absent)
3. Pass H2S gas to above No Black PPT formed or any PPT Cu++ , Pb++ etc absent
solution (group 2nd absent) 3. Pass H2S gas to above No Black PPT formed or any PPT Cu++ , Pb++ etc absent
solution (group 2nd absent)
4. To the salt solution add No change is observed (group 3nd absent)
Al+++, Fe+++ absent 4. To the salt solution add No change is observed (group 3nd absent)
NH4Cl and NH4OH in excess
NH4Cl and NH4OH in excess Al+++, Fe+++ absent
5 Pass the H2S gas to above soln No change is observed (group 4th absent)
Zn++, NI++ Co++ absent 5 Pass the H2S gas to above soln No change is observed (group 4th absent)
(group 5th present) Zn++, NI++ Co++ absent
6 To the salt solution add solid White PPT formation
Ba++, Sr++ Ca++ may be 6 To the salt solution add solid White PPT formation (group 5th present)
NH4Cl , NH4OH , (NH4)CO3
NH4Cl , NH4OH , (NH4)CO3 Ba++, Sr++ Ca++ may be
7 Dissolve the white PPT in
CH3COOH and divide it into 2 parts 7 Dissolve the white PPT in
Ba++ absent CH3COOH and divide it into 2 parts
8 PART – A + K2CrO4 soln NO change or No PPT formed
PART – B + (NH4)2SO4 solution White PPT obtained Sr ++ confirmed 8 PART – A + K2CrO4 soln YELLOW PPT formed Ba++ CONFIRMED
9
9 Performed Flame test grassy green flame Ba ++ confirmed
10 Performed Flame test Crimson red flame Sr ++ confirmed

Result- The given salt is Sr(NO3)2 in which Sr++ is cation and NO3- as anion radical Result- The given salt is Sr(NO3)2 in which Ba ++ is cation and SO42- as anion radical
By – Hasin Ahmed Dekho seekho jano 9425761832 By – Hasin Ahmed Dekho seekho jano 9425761832
EXERIMENT NO – 5 ( A) The procedure of crystallisation of Alum:
1. First, prepare a clear solution of alum by dissolving 1g of Alum sample in
Aim: Purification of the impure samples like Copper Sulphate, about 5 mL of water.
Alum, Benzoic Acid and Iron Sulphate by the process of 2. To this solution add 2 drops of H2SO4.
crystallisation. 3. Heat the solution for a while and filter it using a filtration unit.
4. Transfer the solution from the filtration unit to another beaker and allow it
to cool down to room temperature.
Materials Required: - 50 mL capacity Beaker, filtration unit, 5. Formation of the crystals is witnessed.
watch glass, kerosene burner and CuSO4 .5H20 6. Filter and wash these crystals and allow them to dry.
7. Weigh the crystals and report the yield.
Experimental setup:
Precautions to be taken during the experiment:
• Ensure that the crystals are washed well.
• Avoid overheating of the solution.
• The filtrate should be evaporated slowly by gentle heating of the solution.
• The solution should be cooled slowly and do not use any rapid cooling
procedures.

Observation
Weight of copper sulphate obtained

Weight of alum obtained

Weight of benzoic acid obtained

The procedure of crystallisation of copper sulphate: Weight of iron sulphate obtained

1. Prepare a clear solution of copper sulphate.


2. Dissolve 0.8 g of CuSO4.5H20 in about 8 mL of water and add 1-2 drops of
about 6 mL H2SO4 to it.
3. Heat the solution for a while and filter it using a filtration unit.
4. Transfer the solution from the filtration unit to another beaker and allow it
to cool to room temperature.
5. The crystals will appear.
6. Filter, wash these crystals and let them dry.
7. Weigh the crystals and report the yield.
This test is not given by diazonium salts as they decompose to give
Experiment 5 (B) nitrogen gas on heating.

• Lassaigne’s Test
• Test for Nitrogen Test for Sulphur
The extract is treated with sodium nitroprusside. The appearance of
• Test for Sulphur violet colour indicates the presence of sulphur.
• Test for Halogens The following reaction occurs:
S2- + [Fe(CN)5NO]2- → [Fe(CN)5NOS]4-
What is the Lassaigne’s Test?
Nitrogen, Sulphur, and halogens present in organic compounds are
detected by Lassaigne’s test. Here, a small piece of Na metal is heated Test for Halogens
in a fusion tube with the organic compound. The principle is that, in
doing so, Na converts all the elements present into ionic form. The extract is acidified with HNO3 and then treated
with AgNO3. A white precipitate soluble in NH4OH
• Na + C + N → NaCN
indicates the presence of Cl, a yellowish precipitate
• 2Na + S → Na2S
sparingly soluble in NH4OH indicates the presence of
• Na + X → NaX ( X= Cl, Br, or I)
The formed ionic salts are extracted from the fused mass by boiling it
Br, and a yellow precipitate insoluble in NH4OH
with distilled water. This is called sodium fusion extract. indicates the presence of I.
AgNO3 + NaX → AgX ↓ + NaNO3
Test for Nitrogen
The extract is boiled with FeSO4 and acidified with concentrated
H2SO4. The appearance on Prussian blue colour indicates the
presence of nitrogen.
The following reactions occur,

1. Fe2+ + 6CN– → [Fe(CN)6]4-


2. Fe2+ + H+→ Fe3+ + e–
3. [Fe(CN)6]4- + 4Fe3+ → Fe4[Fe(CN)6].H2O

The acid helps in the oxidation of ferrous ions to ferric ions. The
formation of ferriferous cyanide indicates the presence of nitrogen.
Note: This test is not given by compounds containing N but not C
atoms. For example, NH2NH2 does not answer this test despite having
an N atom. This is because both C and N are required to form CN – ion.

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