Full name :.................................................

Student ID : ..............................................
Group:.........................................................
Numberï :...................................................

Experiment 1: Gravimetric determination of Ba2+

Principle: Ba2+ is precipitated as barium sulfate with sulfuric acid. After the filtering with
filter paper, the paper is charred off, and the precipitate is ignited to constant weight. The
Ba2+ content is calculated from the weight of BaSO4.

Equation:
Ba2  SO24  BaSO4  pKsp (BaSO4) = 9.97
Chemicals required:
Provided: 0.2 M H2SO4

Procedure

Precipitation
Take V (mL) of sample solution from a pipet to a 100-mL beaker, add approximately 70
mL of hot distilled water. Slowly add 10 mL of hot 0.2 M H2SO4 (stirring). Let the
precipitate settle and stand for approximately 15-20 minutes (digestion) before filtration.

Filtration and washing of the precipitate:

Filtering is performed by folding the filter paper into a cone, which is placed in a long-
stem funnel. A seal between the filter cone and the funnel is formed by dampening the
paper with water and pressing the paper to the wall of the funnel.
Decant the solution in the beaker through the filter paper (pouring the solution down a
stirring rod). The precipitate should be disturbed as little as possible. Add approximately
25 mL of the washing solution (hot distilled water), stir well, let the precipitate settle, and
decant the solution through the filter paper. Repeat the washing by decantation four times,
and finally bring the precipitate onto the filter paper, use small portions of the wash
solution for transfer. Remove any solid particles adhering to the beaker. Continue washing
the precipitate in the filter paper with the wash solution until the last portions of washing
give a negative test with silver ion.

Drying and weighing of the precipitate:

Folding and place the filter paper containing the precipitates in a porcelain crucible. Heat
the porcelain crucible until the paper is completely charred (no traces of smoke) and place
the porcelain crucible in the oven for 1 hour at 800 0C (until constant weight). Cool the
crucible in the desiccator and weigh accurately.
Results:

 Sample number (Ba2+):……………………

 Volume of the sample (pipet number……………) : V =

 Weight of the porcelain crucible : m0 =

 Weight of the porcelain crucible + the precipitate : m1 =

 The precipitate : m =

Calculations: (You must show all works to receive full credit)

 The concentration of Ba2+ (g/L) in the sample is:

 The concentration of Ba3(PO4)2 (M = 601.9) (g/L) in the sample is:

 The concentration of BaCl2.2H2O (M = 244.31) (g/L) in the sample is:

Full name : .........................................
Student ID : .........................................
Class/Group: ..........................................
Number :..........................................

Experiment 2: Acid - Base Titrations

I. Titration of NaOH with HCl:

Principle: An unknown concentration solution of NaOH is titrated with a standard HCl

solution. This is a titration of a strong acid with a strong base. The unknown concentration
of the basic solution is determined by equivalent equation: Cacid. Vacid = Cbase. Vbase

Equation:
NaOH + HCl NaCl + H2O

Chemicals required:

Provided. Sample solution: NaOH

Standard solution: 0.050N HCl
Indicator: 0.1% phenolphthalein solution in 60% ethanol
Procedure:

Rinse the burette with three small portions of your NaOH sample solution, fill, and adjust
to zero. Transfer V (mL) of 0.050 N HCl from a pipet to a 250-mL conical flask, add 2-3
drops of phenolphthalein indicator solution and titrate with the unknown NaOH solution to
a light pink end point. Stop the titration and report the volume of NaOH solution. Perform
the procedure three times.

Bromothymol blue or methyl red can be used as the indicator.

Result:
 Sample Number (NaOH solution):………………………
 The volume of HCl solution : V = (pipet number:…………)
C = 0.050 N
 The volume of NaOH solution:
V1 =
V2 = V' =
V3 =
Calculation: (You must show all work to receive full credit)
The molarity (CM), the normality (CN) and C (g/L) of NaOH (M = 40) in the sample
solution:

CN =
CM =
Cg/L =
II. Titration of H3PO4 with NaOH:

Principle:
This is a titration of polyprotic acid with a strong base. Unknown H3PO4 solution (pKa1 =
2.12, pKa2 = 7.21 and pKa3 = 12.38) is titrated with a standard NaOH solution, of which
the concentration has just determined in the above experiment.
If the Ka(s) of a polyprotic acid are more than 10-10 and the pKa(s) differ by about 4 or
more, then distinctive BREAKS are observed in a titration curve. Thus, in principle,
THREE breaks will be observed in the titration of H3PO4 solution with NaOH solution.
However, the last acid step is so WEAK that it is difficult to observe.
The two endpoints are detected by bromocresol green and phenolphthalein, respectively.

Equation:

H3PO4 + OH-  H2PO4- + H2O , pH (eq 1) ≈ ½ (pKa1 + pKa2) ≈ 4.7

H2PO4- + OH-  HPO42- + H2O , pH (eq 2) ≈ ½ (pKa2 + pKa3) ≈ 9.8
HPO42- + OH-  PO43- + H2O

Chemicals required:

Provided. Sample solution: H3PO4

Standard solution: NaOH (calculated from the above experiment)
Indicator: 0.1% bromocresol green solution in 20% ethanol and 0.1%
phenolphthalein solution in 60% ethanol

Procedure:

Burette: your NaOH solution

Transfer V (mL) of your unknown H3PO4 sample from a pipet to a 250-mL conical flask,
add 2-3 drops of bromocresol green and 2-3 drops of phenolphthalein indicator, titrate
with the NaOH solution. The color changes at the equivalent points from yellow to green
(the first end point) and from blue to purple (the second end point), respectively. Record
the volumes of NaOH solution at individual end points. Perform the procedure three
times.

Methyl orange can be used as the indicator for the first end point.

Result:
 Sample number (H3PO4 solution):…………………………
 The volume of H3PO4 solution: V = (Pipet Number:………)
 The volume of NaOH solution:
o Used to neutralize only the first proton:
V’1 =
V’2 = V' =
V’3 =
 o Used to neutralize two protons:
V’’1 =
V’’2 = V'' =
V’’3 =

Calculation: (You must show all works to receive full credit)

The molarity (CM), C (g/L) and the normalities of H3PO4 solution (M = 98) in the sample
solution:

CM =
Cg/L =
C’N =
(C’N: the normality of H3PO4 of the reaction in which only the first proton is
neutralized by NaOH.)
C’’N =
(C’’N: the normality of H3PO4 of the reaction in which two protons of the acid are
neutralized by NaOH.)
Full Name : ...............................................
Student ID : ..............................................
Class/Group: ...............................................
Number : ...............................................

Experiment 3: Reduction-Oxidation Titrations

I. Titration of KMnO4 with H2C2O4 (acid oxalic) (direct titration):
Principle: An unknown concentration KMnO4 in a solution is titrated with a standard
H2C2O4 solution.
Equation:
2MnO4- + 5C2O42- + 16 H+ 2Mn2+ + 10CO2 + 8H2O

Eo(MnO4-+ 8H+/Mn2+ + 4H2O) = 1.51 V; Eo(2CO2/C2O42-) = 0.49 V

Chemicals required:
Provided. H2SO4 (1:5, v/v) solution
Standard 0.0200 N H2C2O4 solution
Procedure:
Rinse the burette with three small portions of your KMnO4 sample solution, fill, and adjust
to zero. Transfer V (mL) of standard 0.0200 N H2C2O4 solution from a pipet to a 250-mL
conical flask, add approximately 40 mL of hot distilled water (70-80 oC) and 5 mL of
H2SO4 (1:1, v/v). Titrate with unknown KMnO4 until the light pink end point (stable
approximately 2 minutes). Perform the titration three times.

Result:
 Sample Number (KMnO4 solution):………………………
 The volume of H2C2O4 solution: V1 = (pipet number:……………………)
C = 0.0200 N
 The volume of KMnO4 solution:
V1 =
V2 = V =
V3 =
Calculation: (You must show all works to receive full credit)
The molarity (CM), the normality (CN) and C (g/L) of KMnO4 (M = 158.04) in the
sample solution are:

CN =
CM =
Cg/L =
II. Titration of Na2S2O3 with KIO3 (indirect titration):
Principle: the standard KIO3 is reacted with excess KI (in acidic environment) to produce
an equivalent amount of I2 (I3-), which is titrated with unknown Na2S2O3 solution, using a
starch indicator.

Equation: 2IO3- + 10I- + 12H+ 6I2 + 6H2O

2-
I2 + 2S2O3 2I- + S4O62-
Eo (2IO3- + 12H+/I2 + 6H2O) = 1.19 V; Eo (I2/2I-) = 0.621 V;
Eo (S4O6 2-/2S2O32-) = 0.09 V

Chemicals required:

Provided. 0.050 N KIO3 solution

KI (10% in water) solution
H2SO4 (1:5, v/v) solution or HCl (1:1, v/v) solution
Starch (indicator)
Procedure:
Rinse the burette with three small portions of your Na2S2O3 sample solution, fill, and
adjust to zero.
Transfer V (mL) of standard 0.050 N KIO3 solution from a pipet to a 250-mL conical flask,
add approximately 30 mL of distilled water, add 5 mL of 10% KI solution (KI in excess)
and add 5 mL of HCl (1:1, v/v) solution. Titrate I2 (produced in the conical flask – brown
color solution) with the unknown NaS2O3 solution to light yellow color, add 2-3 drops of
starch (the solution turns blue) and continue to titrate with NaS2O3 until the blue color
disappear (the end point). Record the volume of Na2S2O3 at the end point. Perform the
titration three times.

Result:

 Sample number (S2O32- solution):………………………

 The volume of KIO3 solution: V = (Pipet Number:………)
C = 0.050 N
2-
 The volume of S2O3 solution:
V1 =
V2 = V =
V3 =

Calculation: (You must show all works to receive full credit)

The molarity (CM), the normality (CN) of S2O32- and C (g/L) of Na2S2O3.5H2O (M =
248.2) in the sample solution:

CN =
CM =
Cg/L =
Full name : .........................................
Student ID : .........................................
Class/Group: ..........................................
Number :..........................................
Experiment 4: Complexometric titrations
(Determination of Al3+ and Fe3+ in water samples)
Principle:
Solutions containing both Fe3+ and Al3+ can be selectively analyzed using EDTA at
pH of 2.5 for Fe3+ (acid salicylic indicator). Then, pH of the solution is raised to 5
and an excess EDTA added, resulting in the formation of the Al3+–EDTA complex.
The excess EDTA is back titrated using a standard solution of Cu2+ (P.A.N
indicator).
Equation:
pH 2.5
Direct titration Fe3+ + H4Y → FeY- + 3H+
The end point: FeIn + Y4- → FeY + In
(purple) (colorless) (colorless or pale yellow) (colorless)
Signal at the endpoint: purple  colorless or pale yellow
pH 5
Back titration: Al3+ + H4Y → AlY- + 3H+
Cu 2+ + H4Y (excess) → CuY2- + H+
The end point: In + Cu2+ → CuIn
(yellow) (pale blue) (purple)
Signal at the end point: yellow  purple (when only P.A.N used)
or green  purple (when P.A.N + bromocresol green indicator
are used)
Chemicals required:
Provided. 0.0100 M EDTA, 0.0100 M Cu2+
Water sample (containing Fe3+ and Al3+)
Indicator: acid salicylic (0.1% in ethanol), P.A.N (0.1% in ethanol) and
bromocresol green (0.1% in ethanol).
Buffer solution, pH 5
NH4OH (1:1, v/v)
Procedure:
Fe3+ titration:
Rinse the burette with three small portions of standard 0.0100 M EDTA solution, fill, and
adjust to zero.
Transfer V (mL) of your sample solution from a pipet to a 250-mL conical flask, add
approximately 30 mL of distilled water, add 2-3 drops of salicylic acid indicator (the color
of this solution should be purple if pH of this solution is approximately 2.5). Titrate with
the standard EDTA solution. One drop of 0.0100 M EDTA should change the titration
solution from purple to colorless or pale yellow at the end point. Record the volume of
EDTA solution at the end point. Perform the titration three times.
Keep this solution and continue to titrate Al3+ in the sample by back-titration.
Al3+ titration (back-titration):
Add 3.00 mL of 0.0100 M EDTA solution to the water sample (EDTA in excess). Increase
the pH of the water sample from 2.5 to 5 using NH4OH (1:1, v/v) drop by drop (add 1 or 2
drops of bromocresol green indicator to check the pH of 5, the color of the sample solution
changes from yellow to blue). Add 2 mL of pH 5 buffer solution and heat the water
sample (water temperature is approximately from 60 to 80 oC). Add another 2 ml of pH 5
buffer solution, 2 drops of P.A.N indicator and titrate the excessive EDTA with standard
0.0100 M Cu2+ solution. One drop of 0.0100 M Cu 2+ should change the color of the
titration solution from green to purple at the end point. Record the volume of standard
Cu2+ solution at the end point. Perform the titration three times.
Result:
 Sample number :…………………………
 The volume of the water sample: V = (Pipet Number:………)
 The concentration of EDTA: C = 0.0100 M
 The concentration of Cu2+: C = 0.0100 M
 The volume of EDTA solution for Fe3+ titration are:
V1 =

V2 = V' =
V3 =
 The volume of Cu2+ solution for Al3+ titration are :
V1 =

V2 = V' =
V3 =

Concentrations (C, mol/L) of Fe3+ and Al3+ in the water sample are:
C Fe3+ (mol/L) =
C Al3+ (mol/L) =
Concentrations (C, g/L) of FeCl3 and AlCl3 (M (FeCl3) = 162.21 and M (AlCl3) = 133.34)
in the water sample are:
C FeCl3 (g/L) =
C AlCl3 (g/L) =