Exp 2.

Traditional acid-alkali titration

Panghung Wen

Introduction
This experiment is going to determine the number of moles of water of crystallization

in solid crystals of ethane-1,2-dioic acid (oxalic acid) which has the formula

(COOH)2·xH2O. Theoretically, the number of moles of water is 2, through this

experiment, we can know also know the difference between reality and theoretic.

We’re going to use the traditional method of titration, in which the main concept is

neutralization happens between hydrogen ions and hydroxide ions in the solution, the

reaction shown in equation 1.

𝐻! 𝑂" (𝑎𝑞) + 𝑂𝐻# (𝑎𝑞) ⇌ 2𝐻$ 𝑂 𝑜𝑟 𝐻" (𝑎𝑞) + 𝑂𝐻# (𝑎𝑞) ⇌ 𝐻$ 𝑂 (1)

In order to know whether the neutralization has been accomplished or not, it’s highly

recommended to add a suitable indicator, the indicator will change color depending

on the pH value, also through the color of the indicator, we can know its

corresponding pH value. In this experiment, we use Phenolphthalein to be the

indicator, Phenolphthalein has no color when it’s in an acid solution, and it has color

in red when it’s in a base solution. However, when the Phenolphthalein indicator is

under a strong base solution, it will change color rapidly from red to transparent color,

and it will also change color under a strong acid. The Phenolphthalein indicator

overdose will make the solution become white and turbid because the Phenolphthalein

indicator is composed of Phenolphthalein and alcohol, alcohol is soluble in water, but

Phenolphthalein is hard to soluble in water, which causes Phenolphthalein precipitate.

In the experiment, we’ll use volumetric flasks, pipettes, and burettes, because we have

to discuss the data under the volumes that we get, so it has strongly dependent on the

1
reading of relatively large volumes. The reaction of oxalic acid and sodium hydroxide

is shown in equation 2.
𝐻! 𝐶! 𝑂" (𝑎𝑞) + 2𝑁𝑎𝑂𝐻 → 𝑁𝑎! 𝐶! 𝑂" (𝑎𝑞) + 2𝐻! 𝑂(𝑎𝑞) (2)

Experiment
Chemical

The ethane-1,2-dioic acid (oxalic acid), sodium hydroxide, phenolphthalein indicator,

and potassium hydrogen phthalate (KHP) were used in this experiment.

Apparatus

The conical flasks are used to contain KHP and oxalic acid and transfer the NaOH

into a glass plastic burette to titrate KHP solution in a conical flask.

Procedure

First of all, in order to know the molar concentration of NaOH, we use the KHP to

standardize, approximately 200mg of KHP are dissolved into 20cm3 water in a

conical flask, add one drop of phenolphthalein indicator, and start to drop NaOH from

the burette to the flask, until the indicator changes its color, and record the data.

Repeat the steps until getting at least 3 groups of data.

Second, replace KHP with oxalic acid with the weight 120mg, and repeat the

procedure again.

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Result and discussion
Experimental data

Table 1. Standardization of the alkali solution

NaOH burette reading/cm3 NaOH [NaOH]
No. KHP/mg
Initial Final volume cm3 mol dm3
1. 215 37.3 49.8 12.5 0.0842
2. 258 9.8 24.3 14.5 0.101
3. 252 24.3 38.3 14 0.0987

average 0.0947

Table 2. Titration of the oxalic acid

Oxalic acid NaOH burette reading/cm3 NaOH Oxalic acid
No.
crystal/mg Initial Final volume cm3 mmol
1. 138 0 25.5 25.5 1.53

2. 95 25.5 43.1 17.6 1.06

3. 48 38 46.7 8.7 0.533

average 1.041

From table 1, we can know that the molar concentration of NaOH, through this data,

calculates the mole of hydroxide ion, and hydrogen ion, and calculate the mass

difference between the Oxalic acid crystal and the result.

For data 1, NaOH has a volume of 25.5 cm3, which means it contains 0.00242 mole of

hydroxide ion, and it can react with 0.00121 mole of oxalic acid, which has a mass of

109 mg, so the mass of water of crystallization is 29 mg, so it has 1.63 of water of

crystallization.
0.138 − 0.0947 × 0.0255 × 0.5
𝑊𝑎𝑡𝑒𝑟 𝑜𝑓 𝑐𝑟𝑦𝑠𝑡𝑎𝑙𝑙𝑖𝑧𝑎𝑡𝑖𝑜𝑛 ∶ = 1.63
18
For data 2, NaOH has a volume of 17.6 cm3, which means it contains 0.00167 mole of

hydroxide ion, and it can react with 0.000833 mole of oxalic acid, which has a mass

3
of 75 mg, so the mass of water of crystallization is 20 mg, so it has 1.11 of water of

crystallization.
0.095 − 0.0947 × 0.0176 × 0.5
𝑊𝑎𝑡𝑒𝑟 𝑜𝑓 𝑐𝑟𝑦𝑠𝑡𝑎𝑙𝑙𝑖𝑧𝑎𝑡𝑖𝑜𝑛 ∶ = 1.11
18
For data 3, NaOH has a volume of 8.7 cm3, which means it contains 0.000824 mole of

hydroxide ion, and it can react with 0.000412 mole of oxalic acid, which has a mass

of 37 mg, so the mass of water of crystallization is 10 mg, so it has 0.606 of water of

crystallization.
0.048 − 0.0947 × 0.0087 × 0.5
𝑊𝑎𝑡𝑒𝑟 𝑜𝑓 𝑐𝑟𝑦𝑠𝑡𝑎𝑙𝑙𝑖𝑧𝑎𝑡𝑖𝑜𝑛 ∶ = 0.606
18
The average has a value of 1.112.
1.63 + 1.11 + 0.606
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 ∶ = 1.12
3
Furthermore, the standard deviation of water of crystallization is 0.418 and the

percentage relative standard deviation of water of crystallization is 37.3%

𝜎 0.418
𝑊𝑎𝑡𝑒𝑟 𝑜𝑓 𝑐𝑟𝑦𝑠𝑡𝑎𝑙𝑙𝑖𝑧𝑎𝑡𝑖𝑜𝑛 ∶ = × 100% = = 37.3%
Χ 1.12

To detect the accuracy of the experiment, the number of moles of water is 2,

theoretically. In this experiment, we have a percentage error of 44%, which is a very

huge error, from the data, data 1 is the closest, because during the titration, we have to

wait until the phenolphthalein indicator change its color, and it to be pale pink, the

data 1 is the most accurate in this experiment, it’s color is closest to pale color, other’s

color is more like hot pink, that means we put too many OH ion into the conical flask,

so the volume we got is not the correct one, that causes the error of the experiment.
|1.12 − 2|
𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑒𝑟𝑟𝑜𝑟 = × 100% = 44%
2

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Conclusion
In this experiment, we have done the titration of oxalic acid, determined the number

of moles of water of crystallization, and compared it to the theoretical one, from the

result we get, it has a percentage error of 44%, that’s a huge error, but it’s more like

the human error because we can’t let every set get the same color.

Reference

歐惠郡, & 張祖辛 (Eds.). (2009, September 21). 酸鹼指示劑. 科學 Online.

Bylikin S., Horner G., Murphy B., & Tarcy D. (2014). Chemistry course companion
(2014 ed.). Oxford University Press.