Time: Session: Date:

Student's duties:

 Students prepare prelab before the experiment day.

 Submit the report of the old lesson before doing the new one.
 Students cannot be absent.
 Students go to practice at the prescribed time (Morning: 7am; Afternoon:
13h00).
 Attitude to practice experiments seriously, carefully and honestly.
 Missing a practice test (absence, not fully prepared, not fully prepared) will
disqualify the exam.
 EXPERIMENT REPORT LESSON 3
ACID – BASE TITRATION METHOD
PREPARING OXALIC ACID STANDARD SOLUTION
DETERMINATING THE CONCENTRATION OF NaOH SOLUTION AND
H3PO 4 SOLUTION

II. Testing result

Experiment 1. Prepare standard solution H2C2O4 0.1N from H2C2O4.2H2O
crystal.

- Number of grams of H2C2O4.2H2O (stock) required to make 100.0 mL of H2C2O4

solution 0,1000N.
𝑀 126.07
𝐶𝑁 × 𝑧 ×𝑉 0.1000× 2
×100
mtheo = = ≈ 0.63 (𝑔)
10×𝑝 10×99.5

- Accurate weighing of H2C2O4.2H2O, mrel = 0.63 (g)

- True concentration of H2C2O4 (confidence interval ±ɛ0.95%):
𝑚𝑟𝑒𝑙 0.63
𝐾= = =1
𝑚𝑡ℎ𝑒𝑜 0.63

𝐶𝑁𝐻2𝐶2𝑂4 𝑟𝑒𝑙 = 𝐶𝑁𝐻2𝐶2𝑂4 𝑡ℎ𝑒𝑜 × 𝐾 = 0.1 × 1 = 0.1 (N)

𝑎 2
0.05 2 𝑎𝑣𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑎𝑠𝑘 2
𝜀𝐻2 𝐶2 𝑂4 = 𝐶𝑁𝐻2𝐶2𝑂4 𝑟𝑒𝑙 × √( 𝑏𝑎𝑙𝑎𝑛𝑐𝑒 ) + ( ) +( )
𝑚×√3 𝑝×√3 𝑉×√6

0.01 2 0.05 2 0.1 2

→ 𝜀𝐻2 𝐶2 𝑂4 = 0.1 × √( ) + (99.5× 3) + (100× 6) = 0.00092
0.63×√ 3 √ √

𝜇𝐶𝐻2𝐶2𝑂4 = 𝐶𝐻2 𝐶2𝑂4 ± 𝜀𝐻2 𝐶2𝑂4 = 0.10000 ± 0.00092 (𝑁)

2
Results and discussion
The real concentration of NaOH is quite desirable because it is equal to the
theory, with the K value is 1. But there is still some error come from system which
are balance, volumetric flask. But again, the concentration value is good.
Experiment 2. Prepare an approximate 0.1N NaOH solution. Determine the
concentration
Experiment 2.1. Prepare NaOH solution
Dilute the 1M NaOH solution to 500 mL NaOH 0.1N:
𝐶𝑀𝑁𝑎𝑂𝐻 = 1𝑀 → 𝐶𝑁𝑁𝑎𝑂𝐻 = 𝐶𝑀𝑁𝑎𝑂𝐻 × 𝑧 = 1 × 1 = 1

𝐶1 × 𝑉1 = 𝐶2 × 𝑉2 → 1 × 𝑉1 = 0.1 × 500 → 𝑉1 = 50 𝑚𝐿

Thus, we will take 50 mL 1M NaOH solution dissolve with distilled water, diluted
it into volumetric flask 500 mL, fill up until reaching 500 mL line.
Experiment 2.2. Determine the concentration of NaOH solution

NaOH H2C2O 4
Apparatus Burette 25mL Pipette 10mL
σ ±0.03 ±0.05
Measure 1 09.85 mL 09.95 mL
Measure 2 09.90 mL 10.00 mL
Measure 3 10.10 mL 10.05 mL
Average 09.95 mL 10.00 mL

Perform CN of NaOH with ε0.95

𝑪𝑵𝑯 𝑪 𝑶 (𝑵)×𝑽𝑯𝟐 𝑪𝟐𝑶𝟒 (𝒎𝑳) 𝟎.𝟏 (𝑵)×𝟏𝟎 (𝒎𝑳)

𝟐 𝟐 𝟒
𝑪𝑵𝑵𝒂𝑶𝑯 = = = 𝟎. 𝟏𝟎𝟎𝟓𝟎 (𝑵)
𝑽𝑵𝒂𝑶𝑯 (𝒎𝑳) 𝟗.𝟗𝟓 (𝒎𝑳)

3
 𝟐 𝟐
𝜺𝑯𝟐 𝑪𝟐 𝑶𝟒 𝟒.𝟑×𝒔𝑽𝑯 𝑪 𝑶 𝒂𝒑𝒊𝒑𝒆𝒕𝒕𝒆 𝟒.𝟑×𝒔𝑽𝑵𝒂𝑶𝑯 𝟐
𝒂𝒃𝒖𝒓𝒆𝒕𝒕𝒆
𝜺𝟎.𝟗𝟓 = 𝑪𝑵𝑵𝒂𝑶𝑯 √( ) + ( 𝑽 𝟐 𝟐 𝟒
+ ) +( + )
𝑪 𝑵𝑯 𝑪 𝑶 𝑯𝟐𝑪𝟐 𝑶𝟒 √𝒏 √𝟔 𝑽𝑵𝒂𝑶𝑯 √𝒏 √𝟔
𝟐 𝟐 𝟒

𝟎.𝟎𝟎𝟎𝟗𝟐 𝟐 𝟒.𝟑×𝟎.𝟎𝟓 𝟎.𝟎𝟓 𝟐 𝟒.𝟑×𝟎.𝟏𝟑 𝟎.𝟎𝟑 𝟐

→ 𝜺𝟎.𝟗𝟓 = 𝟎. 𝟏𝟎𝟎𝟓𝟎 × √( ) +( + ) +( + ) = 𝟎. 𝟎𝟎𝟓𝟔𝟓
𝟎.𝟏 𝟏𝟎√𝟑 √𝟔 𝟗.𝟗𝟓√𝟑 √𝟔

𝝁 = 𝑪𝑵𝒂𝑶𝑯 ± 𝜺𝑵𝒂𝑶𝑯 = 𝟎. 𝟏𝟎𝟎𝟓𝟎 ± 𝟎. 𝟎𝟎𝟓𝟔𝟓 (𝑵)

Accuracy of the titration:

𝜀0.95 0.00565
(1 − ) × 100 = (1 − ) × 100 = 94.38%
𝑪𝑴𝑵𝒂𝑶𝑯 0.10050

Perform the concentration of NaOH as: CM, TNaOH, TH2C2O4/NaOH

𝐶𝑁𝑁𝑎𝑂𝐻 𝟎.𝟏𝟎𝟎𝟎𝟓
𝐶𝑀𝑁𝑎𝑂𝐻 = = = 0.10050 (M)
𝑧 1

𝑚𝑁𝑎𝑂𝐻 (𝑔) 𝐶𝑀𝑁𝑎𝑂𝐻 ×𝑉𝑁𝑎𝑂𝐻 (𝐿)×𝑀𝑁𝑎𝑂𝐻 0.10050×500×10−3 ×40 𝑔

𝑇𝑁𝑎𝑂𝐻 = = = = 0.00402 ( )
𝑉𝑁𝑎𝑂𝐻 (𝑚𝐿) 𝑉𝑁𝑎𝑂𝐻 (𝑚𝐿) 500 𝑚𝐿

40
𝑁𝐻2 𝐶2 𝑂4 ×𝐸𝑁𝑎𝑂𝐻 0.1×
1
𝑇𝐻2 𝐶2 𝑂4⁄𝑁𝑎𝑂𝐻 = = = 0.00400
1000 1000

Results and discussion

Phenomenon: The H2C2O4 solution in the Erlenmeyer flask change its color,
from no color to light pink.

4
 Figure 1. H2C2O4 solution before titration

Figure 2. H2C2O4 solution after titration

Explanation and discussion: Because H2C2O4 is an acid so when we add some
drops of phenolphthalein in H2C2O4 solution, it has no color. And every single time
we add a NaOH drop to the H2C2O4 solution, the pink color appears but then

5
disappear very quick. However, after continuously adding NaOH to the H2C2O4
solution until the volume of NaOH come close to 10 mL, the color turns light pink
and lasts for 30 seconds, this is due to the fact that the indicator – phenolphthalein
changes its color from no color in acid condition to pink in base condition. At this
point, we record the result and depend on this we can calculate the normality of
NaOH, based on the equation: C1.V1 = C2.V2. According to theory, the normality of
NaOH must be 𝟎. 𝟏 ± 𝟎. 𝟎𝟎𝟎𝟗𝟐 (𝑵). In addition, from our experiment, we can see
that the normality of NaOH is 𝟎. 𝟏𝟎𝟎𝟓𝟎 ± 𝟎. 𝟎𝟎𝟓𝟔𝟓 (𝑵). This real value is within
the acceptable range and is close to the theory.
Nevertheless, there is still a distinction in the concentration of NaOH between
the reality and theory since:
- Error from concentration of H2C2O4 lead to the error of NaOH concentration.
- The losses of NaOH, H2C2O4 during pouring, filling.
- The systematic error of the balance pipet and burette.
- Stop the valve of burette at wrong time which led to a little unnecessary
NaOH.
- The titration errors.

Experiment 3. Determine the concentration of H3PO4 solution

Prepare 500 mL 0.1 M H3PO4 solution from H3PO4 solution 1M
𝐶1 × 𝑉1 = 𝐶2 × 𝑉2 → 1 × 𝑉1 = 0.1 × 500 → 𝑉1 = 50 𝑚𝐿
Thus, we will take 50 mL 1M H3PO4 solution dissolve with distilled water, diluted
it into volumetric flask 500 mL, fill up until reaching 500 mL line.
Note: 0.1 M is just theory concentration of 500mL H3PO4 when diluted from H3PO4
solution 1M. Because H3PO4 solution is not standard solution, it must be determined
by NaOH which has been known exactly concentration.

6
Experiment 3.1. Titrate with methyl orange indicator
NaOH H3PO4
Apparatus Biuret 25mL Pipet 10mL
σ ±0.03 ±0.05
Measure 1 09.95 mL 10.05 mL
Measure 2 10.00 mL 10.00 mL
Measure 2 09.80 mL 09.95 mL
Average 09.92 mL 10.00 mL

Perform CM of H3PO 4 with ε0.95

𝑪𝑵𝑯 𝑷𝑶
𝟑 𝟒
𝑪𝑴𝑯 = , z = 1 because the reaction completes at reaction (1)
𝟑 𝑷𝑶𝟒 𝒛

(1): NaOH+H3PO4 → NaH2PO4 + H2O

̅ 𝑁𝑎𝑂𝐻
𝑪𝑵𝑵𝒂𝑶𝑯 ×𝑉 0.10050×9.92
Where 𝑪𝑴𝑯 = = = 𝟎. 𝟎𝟗𝟗𝟔𝟗𝟔 (𝑴)
𝟑 𝑷𝑶𝟒 𝑽𝑯𝟑 𝑷𝑶𝟒 ×z 10×1

We have t at 95% is t=4.3

𝟐 𝟐 𝟒.𝟑×𝒔𝑽𝑯 𝑷𝑶 𝟐
𝜺𝑵𝒂𝑶𝑯 𝟒.𝟑×𝒔𝑽𝑵𝒂𝑶𝑯 𝒂𝒃𝒖𝒓𝒆𝒕𝒕𝒆 𝒂𝒑𝒊𝒑𝒆𝒕𝒕𝒆
ε0.95 = 𝑪𝑴𝑯 √( ) +( + ) +( 𝟑 𝟒
+ )
𝟑 𝑷𝑶𝟒 𝑪 𝑴𝑵𝒂𝑶𝑯 𝑽𝑵𝒂𝑶𝑯 √𝒏 √𝟔 𝑽𝑯𝟑 𝑷𝑶𝟒 √𝒏 √𝟔

0.00565 2 4.3×0.10 0.03 2 4.3×0.05 0.05 2

→ 𝜀0.95 = 0.099696√( ) +( + ) +( + ) =0.00748
0.10050 9.92√3 √ 6 10√3 √6

μ 𝑪𝑴𝑯 = CN± ε0.95= 0.10000 ± 0.00748 (M)

𝟑 𝑷𝑶𝟒

7
Accuracy of the titration:

ε 𝟎.𝟗𝟓 0.00748
(1 − ) × 100 = (1 − ) × 100 = 92.52%
𝑪𝑴𝑯 𝑷𝑶 0.10000
𝟑 𝟒

Results and discussion

Phenomenon: When adding methyl orange solution 0.1% indicator to the H3PO 4
solution, the solution turns from no color to red. After the solution is titrated with NaOH
solution until the end point, the color changes from red to yellow.

Figure 3. H3PO 4 solution with methyl orange 0.1% before titration

8
 Figure 4. H3PO 4 solution after titration

Explanation and discussion: The change in color of the methyl orange

solution 0.1% indicator is because of the change in pH in the solution. The Methyl
orange indicator has a pH range (3.8-4.8) for changing color from orange to
yellow. Initially, when adding it to the H3PO4 - the acidic condition. In this case, the
methyl orange remains in unionized form, which is a red color. However, after
titration with the NaOH solution that has been determined concentration in the above
experiment (CMNaOH = CNNaOH = 0.10050±0.00565 M), the color changes from
red to yellow because the pH of the solution has increased to the point where it makes
the indicator change color. When the end point occurs, the titration is stopped. The
reaction between NaOH and H3PO4 is:

(1): NaOH+H3PO4 → NaH2PO4 + H2O

At the equivalence point of reaction, pH is nearly 4.68, belong to the pH range of

color’s methyl orange. Data of experiment are collected and the formular

9
C1.V1 = C2.V2 are applied to calculate concentration of H3PO4. Calculation result of
concentration of H3PO4 is 0.10000 ± 0.00748 M, which is within the acceptable
range and is close to the theory.

However, there is still a difference in the concentration of H3PO4 solution

between reality and theory because: the error in NaOH concentration leads to the
error in H3PO4 concentration, the systematic error of the balance pipet and burette,
and so on. To avoid these, practice and be more cautious during the experiment are
required.

Experiment 3.2. Titrate with phenolphthalein indicator

NaOH H3PO4
Apparatus Biuret 25mL Pipet 10mL
σ ±0.03 ±0.05
Measure 1 20.40 mL 10.05 mL
Measure 2 20.60 mL 10.00 mL
Measure 3 20.05 mL 09.95 mL
Average 20.35 mL 10.00 mL

Perform CM of H3PO4 with ε0.95

𝑪𝑵𝑯 𝑷𝑶
𝟑 𝟒
𝑪𝑴𝑯 = , z = 2 because the reaction completed at reaction (2)
𝟑 𝑷𝑶𝟒 𝒛
(1) NaOH+H3PO4 → NaH2PO4 + H2O
(2) NaOH + NaH2PO4 → Na2HPO4 + H2O

̅ 𝑁𝑎𝑂𝐻
𝑪𝑵𝑵𝒂𝑶𝑯 ×𝑉 0.10050×20.35
Where 𝑪𝑴𝑯 = = = 𝟎. 𝟏𝟎𝟐𝟐𝟓𝟖𝟕𝟓 (𝑴)
𝟑 𝑷𝑶𝟒 𝑽𝑯𝟑 𝑷𝑶𝟒 ×z 10×2

10
 We have t at 95% is t=4.3

𝟐 𝟐 𝟒.𝟑×𝒔𝑽𝑯 𝑷𝑶 𝟐
𝟒.𝟑×𝒔𝑽𝑵𝒂𝑶𝑯 𝒂𝒑𝒊𝒑𝒆𝒕𝒕𝒆
ε0.95 = 𝑪𝑴𝑯 √( 𝜺𝑵𝒂𝑶𝑯 ) + ( +
𝒂𝒃𝒖𝒓𝒆𝒕𝒕𝒆
) +( 𝟑 𝟒
+ )
𝟑 𝑷𝑶𝟒 𝑪𝑴𝑵𝒂𝑶𝑯 𝑽𝑵𝒂𝑶𝑯 √𝒏 √𝟔 𝑽𝑯𝟑 𝑷𝑶𝟒 √𝒏 √𝟔

0.00565 2 4.3×0.28 0.03 2 4.3×0.05 0.05 2

→ 𝜀0.95 = 0.10225875√( ) + ( 20.35 + ) +( + ) = 0.00988
0.10050 √3 √ 6 10√3 √6

μ 𝑪𝑴𝑯 = CN± ε0.95= 0.10226 ± 0.00988 (M)

𝟑 𝑷𝑶𝟒

Accuracy of the titration:

ε 𝟎.𝟗𝟓 0.00988
(1 − ) × 100 = (1 − ) × 100 = 90.33%
𝑪𝑴𝑯 𝑷𝑶 0.10226
𝟑 𝟒

Results and discussion

Phenomenon: When adding phenolphthalein solution 0.1% indicator to the H3PO
4 solution, the color of the solution does not change (no color). After the solution is
titrated with NaOH solution until the end point, the color changes from no color to pink.

Figure 5. H3PO 4 solution with phenolphthalein 0.1% before titration

11
 Figure 6. H3PO 4 solution after titration

Explanation and discussion: the phenolphthalein indicator's pH range for

changing color from no color to pink is 8.0-9.6. That is why when adding it to the
acidic environment - H3PO4 solution, there is no color. When slowly dripping the
NaOH solution down from the burette, a pink color appears but quickly disappears.
However, after continuously adding NaOH to the H3PO4 solution until the volume
of NaOH reaches around 20 mL, the color turns light pink and lasts for 30 seconds.
This is the end point of the reaction, when the pH of the solution is about 9.8, which
is close to the pT=9 of phenolphthalein, so that turns the solution from having no
color to pink. In addition, there are two reactions occurring:
(1) NaOH+H3PO4 → NaH2PO4 + H2O
(2) NaOH + NaH2PO4 → Na2HPO4 + H2O
Volume of NaOH is collected and used for calculating the concentration of H3PO4.
The final calculated result of the H3PO4 solution is 0.10226 ± 0.00988 (M), which
is within the acceptable range and is close to the theory. Besides, when comparing

12
the volume of NaOH used for titrating H3PO4 solution with phenolphthalein, it is
nearly double the value used for titrating H3PO4 solution with methyl orange. This
is because two types of indicators have a different range of change color so that we
stop the titration at different volumes of NaOH.

Nevertheless, there is still a distinction in the concentration of H3PO4 solution

between reality and theory due to the fact that: the error in NaOH concentration leads
to the error in concentration of H3PO4, the systematic error of the balance pipet and
burette, stopping the valve of the burette at the wrong time, etc. To limit these, it is
necessary to practice and be more careful during the experiment.

13