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Lab Manual 2019-20 Chemistry I Semester-1 (Corrected One)
Lab Manual 2019-20 Chemistry I Semester-1 (Corrected One)
Lab Manual 2019-20 Chemistry I Semester-1 (Corrected One)
2019 - 2020
Compiled by
Dr. P.Manivel
Dr. N. Kalaivasan
Mr.C.Raveendiran
Name :
Discipline : Batch :
Contents
TITRATION – I
TITRATION – II
HARD WATER Vs EDTA
Indicator: EBT
Volume of Burette reading
Volume of Concordant
S.No. HARD WATER
EDTA (mL) Value
(mL) Initial Final
40 0
1.
40 0
2.
40 0
3.
2. 40 0
AIM:
To estimate the temporary, permanent and total hardness of the given sample
of water by EDTA method.
PRINCIPLE:
using disodium salt of EDTA. Erichrom Black – T (EBT) is used as an indicator. The
hardness producing metal ions form a wine red coloured weak complex with EBT
N-CH2-CH2-N
Ca2+ Ca2+
Ions pH=9-10
+ EBT + EBT Weak Complex
2+ Indicator 2+
Mg Mg
Ca2+ Ca2+
pH=9-10
+ EBT Complex+ EDTA + EDTA Complex + EBT
2+ 2+
Mg Mg
Weak Complex -wine red colour Stable (colorless) - Steel blue colour
When EDTA solution is added, the indicator is replaced by this EDTA and a
stable complex is formed. The colour of the solution will be steel blue due to the
release of EBT indicator. In the EDTA method at first the total hardness is estimated.
5
CALCULATION:
V2 mL of EDTA = 20 x V2 mg of CaCO3
V1
40 mL of hard water sample =20 x V2 mg of CaCO3
V1
1000 mL hard water sample =20x (V2/V1) x (1000/40) ppm
A known volume of the same sample is boiled for 15-20 minutes to destroy the
temporary hardness. The water is then cooled, filtered and after proper volume
correction a known volume of water is used for determining permanent hardness.
Temporary hardness is the difference between the total and permanent hardness.
TITRATION – I PROCEDURE:
Pipette out 20 mL of standard calcium solution (Std. hard water) into a clean
conical flask. Add 5 ml of Ammonia (NH4OH – NH4Cl) buffer and two drops of EBT
indicator and titrate the solution against EDTA taken in the burette. The end point is
change of colour from wine red to steel blue. The titration is repeated to get
concordant value. Let V1 be the volume of EDTA consumed.
a. TOTAL HARDNESS:
40mL of the sample water is pipetted into a conical flask. 5mL of buffer solution
and a small amount of EBT indicator is added and titrated with O.O1M of EDTA
solution until the colour is changed to steel blue from wine red. The experiment is
repeated to get concordant value. Let V2 be the volume of EDTA consumed.
b. PERMANENT HARDNESS:
250mL of the water sample is boiled for 15 minutes. Then it is cooled and
filtered in a flask. The filtrate is made to 250mL. 40mL of filtrate is titrated as given
above. The titration is repeated to get concordant value. Let V2 be the volume of EDTA
consumed.
RESULT:
TITRATION – I
7
1.
I
2.
1.
II 2.
If data satisfies the condition P< ½ M. The types of alkalinity present in the
DATE:
AIM:
To determine the type and amount of alkalinity present in the given water
PRINCIPLE:
OH- + H+ → H2O
CO32- + H+ → HCO3-
TITRATION – II
1.
I
2.
1.
II 2.
If data satisfies the condition P< ½ M. The types of alkalinity present in the
From the two titrated value, the different alkaliniteis are calculated
When,
P = 0 bicarbonate alkalinity
P = M, hydroxide alkalinity
2P = M, carbonate alkalinity
carbonate equivalent.
PROCEDURE:
The burette is washed and rinsed with the given HCl. Then the burette is
filled with 0.05N HCl. 20mL of water sample is pipetted out into a clean conical
This solution is titrated against the standard acid until pink colour is
CALCULATION:
If P> ½ M.
(i) volume of acid consumed for OH- ion = (2P – M) mL = ---------------
=---------mL
(ii) volume of acid consumed for C032-ion = 2(M - P) mL = ----------------
=--------- mL
If P< ½ M
(i) volume of acid consumed for C032- ion = 2P mL = ----------------
=--------- mL
(ii) volume of acid consumed for HC03- ion= M - 2P mL = ----------------
=---------mL
1000mL of IN HCl = 1g equivalent of CaCO3
= 50g of CaCO3
= 50,000 mg of CaCO3
אmL of 0.05N HCl = 50000x 0.05 א/ 1000 mg of CaCO3
20 ml of water sample =[ 50000x 0.05 א/ 1000]
1000mL of water sample = [50000x 0.05 אx 1000] / [1000x20]
= 125 א ppm
If P> ½ M.
Alkalinity due to OH-ion =125 אppm (= א2P-M) =
= -----------ppm
Alkalinity due to CO32-ion = 125 אppm (= א2(M-P) =
= -----------ppm
If P< ½ M
Alkalinity due to ion CO32- =125 אppm (= א2P) =
= -----------ppm
Alkalinity due to HCO3-ion = 125 אppm (( = אM-2P)=
= -----------ppm
12
Few drops of methyl orange indicator is added to the same titration after
the phenolphthalein end point. The titration is continued until the solution
becomes red orange. The titer value is noted (M). The titration is repeated for
concordant value.
RESULT:
Sample : I
Sample : II
TITRATION – I
2. 20 mL
3. 20 mL
CALCULATION :
V1N1 = V2N2
V1N1
=
V2
Strength of Na2S2O3 (N2) = -------- N
14
DATE :
AIM:
by Wlinkler’s method.
PRINCIPLE:
Conc.H2SO4).
TITRATION – II
Indicator: Starch
Volume of Burette reading Volume of
Concordant
S.No. water sample Na2S2O3
Value
mL Initial Final (mL)
1. 20 mL
2. 20 mL
3. 20 mL
CALCULATION :
ESTIMATION:
Amount of dissolved oxygen in one
litre of the tap water Normality of Equ. Wt. of
= water sample × Oxygen
= N3 x 8 x 1000 mg/ L
= --------------mg/L
16
PROCEDURE:
TITRATION – I
The burette is washed and rinsed with sodium thiosulphate solution. Then
the burette is filled with the given Na2S2O3 solution 20mL of standard K2Cr2O7
solution is pipetted out into a clean conical flask. To this 5 mL of 4N H2SO4 and
5mL of 5% KI are added. This is titrated against Na2S2O3 solution. When the
solution becomes straw yellow colour, starch indicator is added and the titration
TITRATION – II
manganese sulphate and 2mL of alkali iodide are added. The stopper is
replaced and the flask is inverted and shaked several times for the rough mixing
of reagents. The flask is kept aside for some time. When half of the precipitate
The stopper is replaced and the flask is inverted several times for complete
against the standardised Na2S2O3 solution. Starch indicator is added when the
solution becomes light yellow. The titration is continued until the blue colour
disappears. From the titer value the strength of dissolved oxygen is calculated
and hence the amount of dissolved oxygen in the water sample is calculated.
RESULT:
TITRATION-1
1. 10 mL
2. 10 mL
3. 10 mL
CALCULATION :
= (10 x 0.01) / V2
=……………..N
DATE:
20
AIM:
To determine the amount of chloride present in water sample by
Argentometric method.
THEORY:
Chlorides are present in water usually as NaCl, MgCl2 and CaCl2.
Although chlorides are not harmful as such, their concentrations above 250 ppm
impart a peculiar taste to the water, thus rendering the water unacceptable for
drinking purposes from aesthetic point of view. Further, existence of unusually
high concentrations of chloride in a water sample indicates pollution from
domestic sewage or from industrial waster-waters. Presence of chlorides is also
undesirable in boiler feed water. Salts like MgCl2 may undergo hydrolysis under
the high pressure and temperature prevailing in the boiler, generating
hydrochloric acid which causes corrosion in boiler parts.
PRINCIPLE:
TITRATION :2
SILVER NITRATE VS WATER SAMPLE
21
1. 10 mL
2. 10 mL
3. 10 mL
Calculation:
Volume of silver nitrate solution (V4) =
Strength of silver nitrate solution (N2) =
Volume of water sample (V3) =
Strength of water sample (N3) = ?
= v4 x N2 / V3
=
Amount of chloride in water sample
= Strength of water sample x 35.46 x 1000 mg
= x 35.46 x 1000 mg
PROCEDURE:
22
TITRATION-1:
TITRATION-2:
RESULT :
The amount of chloride present in the water sample = ------------- mg/Lit
V 1 N1
N2 =
V2
20 x
= ………
…
Strength of sodium thiosulphate N2 = ---------------- N
AIM
To estimate the amount of copper present in the given solution by
iodometric titration. You are provided with standard ……………. N K 2Cr2O7
solution.
PRINCIPLE
Copper ion occurs naturally in drinking water and is a micronutrient
required for the metabolism of living beings. But the presence of copper in water,
in quantities more than 1.3 mg/l, will cause stomach ache, intestinal distress
and digestive problems. High concentration of copper will also impart a metallic
bitter taste to water. Occurrence of copper ions in drinking water may be due to
corrosion in plumbing materials and faulty water treatment processes. Copper
is also known to cause toxicity to aquatic organism.
Titrimetric estimation of copper is done through a redox reaction in which
stoichiometric quantity of iodine is liberated on reaction with potassium iodide.
The liberated iodine can be titrated against standardized sodium thiosulphate
solution.
When KI is added the copper ion solution, copper ions react with KI and
liberates I2.
2CuSO4 + 4KI --------> 2K2SO4 + 2CuI + I2
The liberated I2 is titrated against sodium thiosulphate, using starch indicatore.
2Na2S2O3 + I2 -----------> 2NaI + Na2S4O6
Sodium tetrathionate
2Cu2+ I2 2Na2S2O3
Starch
CALCULATION
Volume of sodium thiosulphate solution (V1) =………. ml
Strength of sodium thiosulphate solution (N1) = ……… N
Volume of the given copper ion solution (V2) = 20 ml
/ Stength of the given copper ion solution (N2) = ?
According to the law of volumetric analysis,
V1N1 = V2N2
V1 N1
N2 =
V2
……. x
N2 = …….
20
TITRATION I
Standardisation of sodium thiosulphate
TITRATION II
Estimation of copper ion content of the given solution
20 ml of the given copper ion solution is pipette out into a clean conical
flask. About 5 ml of dil. H2SO4 and 5 ml of 5% KI solutions are added to this
solution and the liberated iodine is titrated against standardized sodium
thiosulphate taken in the burette. When the solution turns pale yellow, about 1
ml of freshly prepared starch indicator is added and the titration is continued.
The disappearance of blue colour is the end poin. The titration is repeated for
concordant values.
RESULT
1. Strength of the given copper ion solution = ………. N
2. The amount of copper in the given copper ion solution = …………… g/lit.
S.No. pH
27
Volume of
NaOH mL
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
Burette
NaOH
Glass
electrode Beaker
Reference HCl
electrode
28
AIM:
To determine the strength of given HCl by pH metry, a standard solution
of NaOH 0.1 is provided.
PRINCIPLE:
The increases in pH takes place until the all the H+ ions are completely
neutralized (upto the end point). After the end point, further addition of NaOH
increases pH sharply as there is an excess of fast moving OH- ions.
MATERIALS REQUIRED:
PROCEDURE:
The burette is filled with std. NaOH solution. Given unknown acid solution
transferred into 100 ml standard flask, and then diluted upto the mark using
distilled water. Exactly 10 ml of the given HCl solution is pipetted out into a clean
beaker. It is then diluted to 30 ml by adding distilled water. The glass electrode
is dipped in it and connected with a pH meter.
29
pH / v
PH
Volume of NaOH
Volume of NaOH ------→
25
Now NaOH solution is gradually added from the burette to the HCl solution
taken in the beaker and pH of the solution is noted for each addition. This
process is continued until atleast 5 readings are taken after the end point. The
observed pH values are plotted against the volume of NaOH added. From the
graph the end point is noted.
RESULT:
N2 =
= ---------------------------
31
AIM:
PRINCIPLE:
When a solution of NaOH is titrated with HCl, the fast moving hydrogen ions are
progressively replaced by slow moving sodium ions. As a result conductance of the
solution is decreases. This decreases in conductance will take place until the end
point is reached. Further addition of alkali raises the conductance sharply as there is
an excess of hydrogen ions.
A graph is drawn between volume of HCl added and the conductance of
solution. The exact end point is intersection of the two curves.
METERIALS REQUIRED:
(i) Conductivity meter
(ii) Conductivity cell
(iii) Beaker
(iv) Standard N/10 HCl
(v) Approximately N/10 NaOH
(vi) Burette, pipette, glass rod etc.,
33
Determination of conductance
34
PROCEDURE:
The burette is filled with std. NaOH solution. Given unknown acid
solution transferred into 100 ml standard flask, and then diluted upto the mark
using distilled water. Exactly 10 ml of the given HCl solution is pipetted out into
a clean 100 ml beaker. It is diluted 30 ml of distilled water. The conductivity cell
is placed in it. So that the electrodes are well immersed in the solution. The two
terminals of the cell are connected with a conductivity meter.
The graph is plotted by taking volume of NaOH in the X-axis and conductance
in Y-axis. The end point is noted from the graph and the amount of HCl present
in the given solution is calculated.
RESULT:
N2 =
= ---------------------------