Section-B Proper use of Bench Chemicals

Object: Standardization and analysis of some very basic bench

chemicals in a lab.

Experiment-1 Preparation and standardization of Hydrochloric acid

(HCl) with anhydrous Sodium carbonate (Na2CO3)

Procedure:
1. Wash all the glass ware with tap water and then rinse with distilled water.
2. Prepare an approximately (0.2 to 0.5M) known strength of HCl solution. (For 0.4M,
500mL HCl, 20ml of 34% HCl measured by measuring cylinder having specific
gravity 1.19 )
(Always measure the concentrated acid with measuring cylinder)
3. In a weighing bottle, weigh accurately about 0.2g of pure dried sodium carbonate.
4. Transfer it to a conical flask with the help of distilled water. Add a drop of methyl
orange and add distilled water till a light yellow color obtain. Titrate against HCl
solution. (Note: if the reading is less than 5.0ml then increase the amount in next
titration).
5. Calculate the ratio of W/V (weight of Na2CO3 / volume of HCl used).
6. Repeat the steps 3 and 4 until you get concordant ratio.
7. Calculate the molarity of HCl by dividing the concordant ratio by factor of Na2CO3
with HCl (0.053). #NOTE: The factor of Na2CO3 is the amount of base
required for 1 ml of 1M HCl.

B: Find out the percent purity of commercial sodium carbonate.

8. Repeat the step 3 and 4 with commercial sample of Na2CO3.

9. Calculate the percent purity of commercial sodium carbonate by using formula;
Amount of Na2CO3 = MHCl x VHCl x 0.053

% purity = calculated amount x 100

amount taken

CAUTION Always add acid into water (AAA rule)

While diluting the concentrated acid, pour the acid slowly
and carefully into the water, with constant stirring to
dissipate the heat of solution that can cause the solution to
boil and splatter.

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Observations:
A. Standardization of HCl
Weight of
Initial volume Final volume Difference W/V ratio
S# Na2CO3
(Vi), mL (Vf), mL (V=Vf-Vi), mL g/mL
(g)
1. __________ __________ __________ __________
2. __________ __________ __________ __________ __________
3. __________ __________ __________ __________

B. Est the percent purity of commercial

1. Weight of commercial Na2CO3 = ______________g.

2. Molarity of Standard HCl = ______________M.
3. Volume of Standard HCl = ______________mL.
4. Factor b/w Na2CO3/HCl = 0.053.

Calculations:
A. Molarity of HCl;

Amount of (Na2CO3) = Molarity (HCl) x Volume (HCl) x Factor

Molarity (HCl) = Amount of (Na2CO3)

Volume (HCl) x Factor

Molarity (HCl) = W/V ratio / Factor

Molarity (HCl) = _______ / 0.053

Molarity (HCl) = _______ M.

B. Percentage of Commercial Na2CO3;

Amount of (Na2CO3) calculated = Molarity (HCl) x Volume (HCl) x Factor

Amount of (Na2CO3) calculated = _______ (M) x _____ (mL) x 0.053

Amount of (Na2CO3) calculated = _______ g.

% Purity of Na2CO3 = Amount of (Na2CO3) calculated x 100

weight of commercial (Na2CO3) taken

The Purity of Na2CO3 = ___________%.

Result
a) The molarity of HCl was found to be _________M.
b) Purity of Na2CO3 = ___________%.

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Experiment-2 Back Titration by adding excess HCl

Object-A: Find out the percent purity of Calcium carbonate (CaCO3)

Procedure:
1. Wash all the glass ware with tap water and then rinse with distilled water.
2. In a weighing bottle weigh accurately about 0.2g of calcium carbonate.
3. Transfer it to a conical flask with the help of distilled water. Add one or two
drops of phenolphthalein.
4. Add 20.0ml of standard HCl (concentration found out in previous experiment
i.e. experiment No. 1 of proper use of bench chemicals), if pink color appears
add 10.0ml more HCl this total amount will be Vt.
5. Boil the solution of the flask for few minutes to remove CO2 till clear solution
is obtained.
6. During this heating standardize the roughly prepared NaOH (usually this step
is performed at first to save the time).
7. Cool and titrate the flask content with standard NaOH solution until pink color
appears. (Note; if the reading is less than 5.0ml add more HCl accurately
measured in a same flask and continue titration, remember that Vt will be
increased).
8. Convert the burette reading into VCorr.
9. VCorr = M NaOH x V NaOH / MHCl
10. Calculate the used volume of HCl for calcium carbonate in the given sample
by using subtracting VCorr from Vt.
11. VUsed = Vt – VCorr
12. Calculate the percentage of Calcium carbonate in the given sample by using
the factor of calcium carbonate (0.05).

Equation: CaCO3 + 2HCl  CaCl2 + CO2 + H2O

Observations:
Standardization of NaOH
Molarity of HCl = (MHCl ) = ___________M.
Volume of HCl = 10.0mL.
Indicator used = Phenolphthalein.
Volume of NaOH used against standard HCl solution
S# Initial reading Initial reading Difference Concordant reading
(Vi), (mL) (Vf), mL (V=Vf-Vi), mL mL
1. __________ __________ __________
2. __________ __________ __________ V2
3. __________ __________ __________

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Estimation of Sample Solution
1. Weight of CaCO3 taken = ___________g.
2. Indicator used = Phenolphthalein.
3. Excess volume of Standard HCl solution added in CaCO3 = (Vt) = _____mL.
4. Volume of Standard NaOH solution used for sample titration = (Vr) == _____mL.

Calculations:
A-Standardization of NaOH
HCl : NaOH

M1.V1 = M2.V2

NaOH = MHCl x 10.0mL

V2

MNaOH = __________M.

B-Volume Correction

VCorr = MNaOH x VNaOH / MHCl

VCorr = MNaOH x Vr / MHCl

VCorr = _____M x _____mL / _____M

VCorr = mL.

C-Volume Used,

VUsed = Vt – VCorr

VUsed = ___mL – ___mL.

Vused = mL.

D-Amount of Sample Calculated

Amount of CaCO3 = MHCl x Vused (HCl) x Factor (CaCO3/HCl)

Amount of CaCO3 = _____M x _____mL x 0.05

Amount of CaCO3 = _____g.

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E-Percentage of CaCO3 in the given sample
% of CaCO3 = Amount of CaCO3 x 100
Weight of CaCO3 taken
% of CaCO3 = _________g x 100
..………g

% of CaCO3 = ________%

Result:
The percentage purity of CaCO3 was found to be _____%.

Object-B: Find out the percentage of NH3 in NH4HCO3.

Procedure
1. Do all steps mentioned in part-A, with ammonium bicarbonate. Finally calculate
the percentage of ammonia by using the factor of ammonia (0.017).

Equation: 2NH4Cl + CaCO3  2NH3 + CaCl2 + H2O + CO2

Note: All the calculations for part-B are same except the factor which is 0.017 for
NH3.

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Experiment-3 Back Titration by adding excess NaOH

Object: Find out the percentage of NH3 in ammonium salt.

Procedure:
1. Wash all the glass ware with tap water and then rinse with distilled water.
2. In a weighing bottle weigh accurately about 0.2g of ammonium salt.
3. Transfer it to a conical flask with the help of distilled water. Add two or
three drops of phenolphthalein.
4. Add 20.0ml of standard NaOH solution, if no pink color appears add
10.0ml more NaOH. This amount will be Vt..
5. Boil the solution of the flask for few minutes to remove NH3 completely
(check by red litmus paper or by rod dipped in HCl).
6. During this heating standardize the roughly prepared NaOH. In this
process HCl should be filled in burette.
7. Cool, add BaCl2 and titrate the flask contents with standard HCl solution
until solution becomes colorless. (Note; if reading is less than 5.0mL
add more NaOH accurately measured in same flask and continue
titration).
8. Convert the Vt into be Vcorr.

9. VCorr = M NaOH x V t NaOH / MHCl.

10. Calculate the used volume of HCl for ammonium carbonate (if this is the
salt provided) by subtracting burette reading from VCorr.

11. Vused = Vcorr - Vr.

12. Finally calculate the percentage of ammonia by using the factor of
ammonia (0.017).

Equation: (NH4)2 CO3 + 2NaOH  Na2CO3 + NH3+ H2O

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Observations:
Standardization of NaOH
1. Molarity of HCl = (MHCl ) = ___________M.
2. Volume of NaOH = 10.0mL.
3. Indicator used = Phenolphthalein.
4. Volume of standard HCl used against prepared NaOH solution
S# Initial reading Initial reading Difference Concordant reading
(Vi), (mL) (Vf), mL (V=Vf-Vi), mL mL
1. __________ __________ __________
2. __________ __________ __________ V2
3. __________ __________ __________

Estimation of Sample Solution

1. Weight of ammonium salt taken = ___________g.
2. Indicator used = Phenolphthalein.
3. Excess volume of Standard NaOH solution added in ammonium salt = (Vt) =
_____mL.
4. Volume of Standard HCl solution used for sample titration = (Vr) == _____mL.

Calculations:
A. Standardization of NaOH
HCl : NaOH

M1.V1 = M2.V2

NaOH = MHCl x V2
10.0

MNaOH = __________M.

B. Volume Correction

Vtcorr = MNaOH x VNaOH / MHCl

Vtcorr = MNaOH x Vt / MHCl

Vtcorr = _____M x _____mL / _____M

Vtcorr = mL.

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C. Volume Used,

VUsed = Vtcorr – Vr

VUsed = ___mL – ___mL.

Vused = mL.

D. Amount of Sample Calculated

Amount of NH3 = MHCl x Vused (HCl) x Factor (NH3/HCl)

Amount of NH3 = _____M x _____mL x 0.017

Amount of NH3 = _____g.

E-Percentage of NH3 in the given sample

% of NH3 = Amount of NH3 x 100
Weight of ammonium salt taken
% of NH3 = _________g x 100
..………g

% of NH3 = ________%

Result:
The percentage of NH3 in the ammonium salt, was found to be ______%.

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Experiment-4 The Bench age of NaOH

Object: Find out the percentage of Na2CO3 in NaOH

Procedure:
1. Wash all the glass ware with tap water and then rinse with distilled water.
2. Fill the burette with standard HCl solution.
3. Take 10.0ml of NaOH sample solution in conical flask and titrate with
standard HCl solution. This reading will be Vt.
4. Take the same volume again and add about 0.5g barium chloride in NaOH
sample solution and titrate the content of flask against standard HCl after
adding indicator. This reading will be V’ (volume of standard HCl
solution used for actual NaOH solution).
5. After subtracting V’ from Vt, the volume of HCl used for Na2CO3 in
NaOH will be obtained.
6. Calculate the percentage of Na2CO3 in NaOH, also calculate the percent
purity of NaOH (calculate the factor of NaOH against HCl).

Observations:
A. Estimation of NaOH without BaCl2:
1. Molarity of standard HCl solution = _________M
2. Volume of NaOH solution = 10.0ml
3. Indicator used = Phenolphthalein
4. Volume of standard HCl used against bench solution of NaOH = VTotal = _____mL.

B. Estimation of NaOH with BaCl2:

1. Molarity of standard HCl solution = _________M
2. Volume of NaOH solution = 10.0ml
3. Indicator used = Phenolphthalein
4. Volume of standard HCl used against bench solution of NaOH = VNaOH = _____mL

Calculations
VTotal = VNa2CO3 + VNaOH similarly
VNa2CO3 = VTotal ─ VNaOH
VNa2CO3 = _____mL ─ _____mL
VNa2CO3 = _____mL.

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Amount of NaOH
Amount NaOH = MHCl x VNaOH x FactorNaOH
Amount NaOH = _____M x _____mL x 0.04
Amount NaOH = _____g.

Amount of Na2CO3
Amount Na2CO3 = MHCl x VNa2CO3 x FactorNa2CO3
Amount Na2CO3 = _____M x _____mL x 0.053
Amount Na2CO3 = _____g.

% of NaOH
% NaOH = Amount NaOH x 100
(Amount NaOH + Amount Na2CO3)

% NaOH = _________________________

% NaOH = _____%.

% of Na2CO3
% Na2CO3 = Amount Na2CO3 x 100
(Amount NaOH + Amount Na2CO3)

% Na2CO3 = _________________________

% Na2CO3 = _____%.

Result
1. The percentage of NaOH in sample was found to be ______%
2. The percentage of Na2CO3 in sample was found to be ______%

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Experiment-5 Impurity of HCO3- in CO32-

Object: Find out the percentage of NaHCO3 as an impurity in

Na2CO3

Procedure:
1. Wash all the glass ware with tap water and then rinse with distilled water.
2. Weigh accurately about 0.2g of sample in a weighing bottle(x g).
3. Transfer it into conical flask with the help of distilled water and titrate it
in the same way as given in experiment # 1. This burette reading will be
Vx. (1st burette reading of sample, take only one reading).

4. Weigh another accurately about 0.2g of sample (y g).

5. Transfer this amount in conical flask and titrate it in the same way as
given in experiment # 3.

6. Theoretically calculate the volume of HCl required for this (y g) from Vx

and this will be Vy.
7. Correct excess NaOH added (Vt) into Vt corr of NaOH.

8. During heating standardize your prepared NaOH solution. Remember HCl

should be in burette.
9. Now cool the content of the flask, add BaCl2 and titrate. This reading will
be Vr.(2nd burette reading).

10. Volume of HCl used for sodium bicarbonate VHCO3- will be Vt corr – Vr.
11. Volume of HCl used for sodium carbonate V CO32- will be Vy – V HCO3-
a. Amount of Na2CO3 = MHCl x VCO32- x 0.053
b. Amount of NaHCO3 = MHCl x VHCO3- x 0.084

Equation Na2CO3 + H2O + CO2  2NaHCO3

Observations:
A. Standardization of NaOH solution
1. Molarity of HCl = (MHCl ) = ___________M.
2. Volume of NaOH = 10.0mL.
3. Indicator used = Phenolphthalein.
4. Volume of standard HCl used against prepared NaOH solution
S# Initial reading Initial reading Difference Concordant reading
(Vi), (mL) (Vf), mL (V=Vf-Vi), mL mL
1. __________ __________ __________
2. __________ __________ __________ V2
3. __________ __________ __________

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B. Estimation of sample solution
1. Weight of sample (first procedure) = x g = ______g
2. Molarity of standard HCl solution = ___________M
3. Indicator used = Methyl orange
4. Volume of standard HCl solution for Na2CO3 sample = VX = ______mL
5. Weight of sample (second procedure) = y g = _______g
6. Molarity of standard HCl solution = ______________M
7. Indicator used = Phenolphthalein
8. Volume of excess NaOH= VT = ________mL
9. Volume of standard HCl solution for Na2CO3 sample = VR = _______mL

Calculations:
A. Standardization of NaOH
HCl : NaOH

M1.V1 = M2.V2

NaOH = MHCl x V2
10.0

MNaOH = __________M.

B. Volume Correction

VTcorr = MNaOH x VNaOH / MHCl

VTcorr = MNaOH x VT / MHCl

VTcorr = _____M x _____mL / _____M

VTcorr = mL.

C. Theoretical estimation of VY
VY = (First Procedure Burette reading) x (sample weight of first procedure)
sample weight of second procedure
VY = (VX mL) x (x gram)
y gram
VY = ________x _______
…………

VY = ________mL

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VHCO3- = VT corr – VR
VHCO3- = ______mL – ______mL
VHCO3- = ______mL

VCO3-2 = VY – VHCO3-
VCO3-2 = ______mL – ______mL
VCO3-2 = ______mL

Amount HCO - = MHCl x VHCO - x Factor (NaHCO )

3 3 3

Amount HCO - = ____M x ____mL x 0.084

3

Amount HCO - = ________g

3

Amount CO -2 = MHCl x VCO -2 x Factor (Na CO )

3 3 2 3

Amount CO -2 = ____M x ____mL x 0.053

3

Amount CO -2 = ________g
3

% of HCO3- = Amount HCO3- x 100

Amount of sample taken for second procedure
% of HCO3- = Amount HCO3- x 100
y(g)
% of HCO3- = _______________%.

% of CO3-2 = Amount CO3-2 x 100

Amount of sample (second procedure)
% of CO3-2 = Amount CO3-2 x 100
y(g)
% of CO3-2 = _______________%.

Result:
1. The percentage of HCO3- in sample was found to be = ________%
2. The percentage of CO32- in sample was found to be = ________%

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