ANALYTICAL CHEMISTRY

PRACTICAL 4:

Determination of the Acetic

acid of Vinegar Titration

Supervisor: Dr. Wan Hazman Bin Danial

Group Members:

NAME MATRIC NO

AMIR AZNAN BIN ALI RAHMAN 2017839

AHMAD ZAIDI BIN ZAKARIA 2013765

Date of Submission: 06/04/2021

1.0 Introduction

Volumetric glassware is a basic tool of operation in analytical chemistry that is used to

measure the volume of a liquid. There are three main types of volumetric glassware which are

volumetric flask, pipette and burette. Volumetric flask is used for the dilution of solutions to a

certain volume. This flask is marked with “TC” to indicate “to contain” as it is designed to

contain an accurate volume at the specified temperature when the bottom of the meniscus

touches the graduation mark. Meanwhile pipet is used to transfer a particular volume of solution.

Pipette is marked with “TD” to indicate “to deliver” since it is designed to deliver a specified

volume at a given temperature. On the other hand, burette is used for the accurate delivery of a

variable amount of solution. It is usually used in titration whereby a standard solution is added to

the sample solution until the equivalence point is reached.

In this experiment, acetic acid is used as the titrant which is the unknown molarity

meanwhile NaOH solution is used as the standard solution (also known as the analyte).

Essentially, there are four main objectives for this experiment that we should be able to perform

after this lab session is conducted which are:

● To demonstrate proper techniques for using pipette, burette and volumetric flask.

● To assess the random error in the volume delivered from the pipette and a burette

● To accurately dilute a sample

● To use a suitable titration to determine the concentration of ethanoic acid in vinegar

2.0 Apparatus and Methodology

Apparatus Chemicals
1. 50 mL burette 1. Vinegar

2. 10 mL Serological pipette 2. Distilled water

3. Pipette bulb 3. 0.05 M NaOH

4. 25 mL Graduated measuring cylinder 4. Phenolphthalein

5. Clamp stand

6. Volumetric flask

7. Erlenmeyer flask

8. Dropper

9. Funnel

10. Stirring rod

11. Beaker

12. Wash bottle

Methodology

1. The acetic acid was diluted by transferring 5 cm3 of acetic acid into a 100 cm3 volumetric

flask using a pipette.

2. Distilled water was added until the graduation mark reached.

3. The mixture in the volumetric flask was thoroughly mixed by inverting the flask at least

10 times.

4. 10 mL of diluted vinegar was pipetted into a 100 cm3 of conical flask and few drops of

phenolphthalein was added.

5. The 50 mL burette was filled with the 0.05 M NaOH standard solution.

6. The diluted acetic solution was titrated against NaOH solution

7. The titration was repeated three times and the observation was recorded.
3.0 Results

CH₃COOH

Trial 1 Trial 2 Trial 3

Initial buret reading 0.4 11.75 23.25

(mL)

Final buret reading 11.75 23.25 34.50

(mL)

Volume of NaOH 11.35 11.50 11.25

used (mL) Too pink*

Molarity of NaOH 0.05 0.05 0.05

used (M)

Volume of diluted 10 10 10
acid sample (mL)

Molarity of diluted 0.06 0.06 0.06

acid sample (M)
Table 1

Class Results Vinegar (CH₃COOH)

11.35

Volume of NaOH used (mL) 11.50

11.25

Mean (mL) 11.37

Standard Deviation 0.18

Table 2
4.0 Calculation

Sample calculation for no. of mol of NaOH:

n = MV

11.35
n = 0.05 x ( 1000
)

n = 5.675 x 10-4 mol of NaOH

Calculate the concentration of the diluted acetic acid in your sample of vinegar
𝑛
M=
𝑣

−4
5.675 𝑥 10
M=
(10/1000)

M = 0.6 M

Sample calculation of mean of volume of NaOH used:

𝑉𝑜𝑙𝑢𝑚𝑒 𝑡𝑟𝑖𝑎𝑙 1 + 𝑉𝑜𝑙𝑢𝑚𝑒 𝑡𝑟𝑖𝑎𝑙 2 + 𝑉𝑜𝑙𝑢𝑚𝑒 𝑡𝑟𝑖𝑎𝑙 3

Mean = 𝑇𝑜𝑡𝑎𝑙 𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑑𝑎𝑡𝑎

11.35 + 11.50 + 11.25

Mean = 3

Mean = 11.37

Sample calculation of standard deviation of volume of NaOH used:

∑( 𝑥𝑖 − 𝑀𝑒𝑎𝑛 𝑜𝑓 𝑁𝑎𝑂𝐻 𝑣𝑜𝑙𝑢𝑚𝑒)²

Standard deviation =
𝑁−1

( 11.35 − 11.37 )² + (11.50 − 11.37)² + (11.25 − 11.37)²

Standard deviation =
2

Standard deviation = 0.18

Estimate the error in your pipette and volumetric flask volumes
According to J.S. Fritz & G. H. Schenk (1974),

0.08
Error in 100 mL volumetric flask ( ± 0.08 cm3) = x 100 = 0.08%
100

0.02
Error in 10 mL pipette ( ± 0.02) = x 100 = 0.2 %
10

Estimate the error in each burette reading

Result table shows:

Initial buret reading 0.4 11.75 23.25

(mL) ± 0.02 cm3

Final buret reading 11.75 23.25 34.50

(mL) ± 0.02 cm3

Volume of NaOH 11.35 11.50 11.25

used (mL) Too pink*

Minimum reading Maximum reading

Formula Min Final - Max Initial Max Final - Min Initial

Trial 1 (11.75-0.02) - (0.4+0.02) = 11.31 (11.75+0.02) - (0.4-0.02) = 11.39

Trial 2 (23.25-0.02) - (11.75+0.02) = 11.46 (23.25+0.02) - (11.75-0.02) = 11.54

Trial 3 (34.50-0.02) - (23.25+0.02) = 11.21 (34.50+0.02) - (23.25-0.02) = 11.29

Comparing each burette reading to their minimum and maximum reading to get the error

Error Minimum Error Maximum

Trial 1 11.35 - 11.31 = 0.04 11.35 - 11.39 = -0.04

Trial 2 11.50-11.46 = 0.04 11.50 - 11.54 = -0.04

 Trial 3 11.25 - 11.21 = 0.04 11.25 - 11.29 = -0.04

Calculate the error in each titration volume and the error in the average titration volume

Errors Minimum Value Maximum Value

Trial 1 (11.75 - 0.4) ± 0.04 = 11.35 ± 0.04 11.31 11.39

Trial 2 (23.25 - 11.75) ± 0.04 = 11.50 ± 0.04 11.46 11.54

Trial 3 (34.50 - 23.25) ± 0.04 = 11.25 ± 0.04 11.21 11.29

Average 11.37 ± 0.04 11.33 11.41

(a) the molar concentration of acetic acid in the original sample of vinegar

M1V1 = M2V2

M1(5) = (0.06)(10)

M1 = 0.12 M

(b) what is the the mass of acetic acid per 100 g of solution (the density of acetic acid
solution is 1.01 g/cm3 )

CH3COOH
Molar mass: 60.052 g/mol
1 𝑐𝑚3
Volume of solution = 100 g x = 99.01 cm3
1.01 𝑔

n = 0.12 x ( 99.01/1000)
n = 0.0119 mol
Mass = no. of mol x molar mass
= 0.0119 mol x 60.052 g/mol
= 0.72 g
5.0 Discussion

In this lab session, we are focusing on using the volumetric glassware such as burette, pipette

and volumetric flask. For this experiment, we are using the serological pipette to transfer acetic

acid into the volumetric flask, which is then diluted using distilled water. We are also using the

pipette to transfer the diluted acetic acid into the conical flask. For the titration process, we used

10 mL of diluted acetic acid as the titrant and 0.05 M NaOH solution becomes the analyte.

Before starting the experiment, every equipment that we will be using during the experiment

was cleaned with distilled water thoroughly to avoid contamination from any pollutant or

leftover chemicals. This is because it might affect the result of the experiment, especially when

dealing with concentration in which any pollutants can disrupt our reactions. This can be caused

if our titrant or analyte reacted with the leftover chemicals in the equipment. Titration concerns

the accuracy of the delivery so the cleaning process is very important.

After the cleaning process, we pipetted the acetic acid into the volumetric flask and carefully

added distilled water until the mixture reached the 100 mL graduation mark. Overfilling the flask

will have an affect on the concentration of the acid sample. The solution was then mixed

consistently by inverting the flask to ensure it is properly mixed and diluted. Then for the burette,

we filled it with the standard solution of 0.05 M NaOH above the zero mark using a stirring rod

and a funnel. Next, we checked for the presence of any bubbles at the tip of the burette and

discharged some of the excess NaOH until the bubbles disappeared.

Before the titration process begins, a few drops of phenolphthalein were added into the
diluted acetic acid solution to act as an indicator for determining the endpoint for the titration.

The phenolphthalein is colourless in acidic solution and turns bright pink in basic solution. Our

main target however, is to turn the solution only light pink which signifies the equivalence point.

Source: course lumen learning website

The graph above shows the progress of a titration between weak acid and strong base

similar to our titration. The axes represent the pH values and the volume of titrant (mL) added to

the solution. We can see a gradual increase to the pH level as the titrant increases because as you

increase the amount of NaOH in the solution, the solution will become more alkaline. The

exponential rise at the equivalence point indicates the nearly instantaneous transformation of the

acidic solution to become basic. This is caused by the fact the acetic acid has fully reacted with

the NaOH and any more addition of the titrant will reflect the true pH of the NaOH solution. The

equivalence point is the point just right before the endpoint which is where the solution only

consists of salt and water which is why the pH is neither very acidic or very basic. For this

particular experiment, we utilised a strong base but a weak acid so the equivalence point is
somewhat basic as the NaOH solution could not be fully neutralised in the reaction.

CH3COOH + NaOH → NaCH3COO + H2O

The balanced equation of the reaction between the acetic acid and sodium hydroxide

shows that 1 mol of acetic acid requires only 1 mol of sodium hydroxide to produce its salt

solution which means that the amount of moles for both acid and base used in the experiment

will be the same. This is why it is important that we reach the equivalence point (light pink)

rather than the endpoint (bright pink) because the accuracy of the result depends on it. This is

because if we went over the equivalence point, the NaOH added will exceed the required amount

therefore, our presumed molarity of the acid sample will be affected.

The concentration of the NaOH base used in the experiment has a big influence on the

volume necessary for the neutralisation of the acid. We used a low concentration for our NaOH

solution because it is easier to manage during the titrating to ensure that we can reach the

equivalence point. However, despite this our 2nd trial was an error because the colour is bright

pink which suggests that the solution is in excess of NaOH. However, our results are relatively

consistent because trial 1 and trial 3 observation was just light pink and we managed to reach the

equivalence point before 11.50 mL of NaOH was added.

6.0 Conclusion

To summarise, this experiment was a success as we were able to discover the molarity of

the ethanoic acid present in the vinegar which we found to be around 0.06 M. The average

NaOH solution used during the experiment was 11.37 mL which could be inaccurate because it
is affected by trial 2 result which is imprecise. During the experiment, we were able to develop

further understanding on the proper methods of using the serological pipette, pipette bulb, and

the burette. Furthermore, we learnt how to dilute a sample using the volumetric flask and how to

properly mix the solution within it. The concentration of the NaOH used was very suitable for

the titration of the acetic acid because it is relatively easier to reach the equivalence point at

lower concentration especially when using the burette. The random error of the volume delivered

by the pipette is ±0.06 mL whereas, for the burette it is ±0.04. Overall, the experiment was

conducted successfully and this practical helped us improve our titration methods with further

understanding.

7.0 Questions

1. What is the accuracy of the quantities measured using

(i) the pipette?

0.02
% Uncertainty = ± 10
x 100 = 0.2%

The accuracy of the pipette is not that accurate as the uncertainty is quite big, however typically

a pipette will have a specified optimum temperature which indicates the pipette will accurately

deliver the measured amount of water.

(ii) the burette?

0.02
% Uncertainty = ± 50
x 100 = 0.04%

The accuracy of the burette is quite accurate to the true volume as the percentage of uncertainty

is relatively low as compared to the volumetric pipette. This is important as the accuracy of the

burette has a big impact on the titration value and affects our calculation of the molarity.
8.0 References

1. Christian, GD., Dasgupta PH., Schug HA. (2014). Analytical Chemistry (7th ed.) . United

States: Petra Recter.

2. Serway, R. A., & Vuille, C. (2017). College Physics (11th ed.) Global Edition. Cengage

Learning. Conversion Factors. pg.1-20

3. Silberberg, M., & Amateis, P. (2017). Chemistry: The Molecular Nature of Matter and

Change (8th ed.). McGraw-Hill Education. Chapter 3: Stoichiometry of Formulas and

Equations. Pg.95-111.

4. Walkers, J. P. (2012). Volumetric Glassware. https://www.Webassign.Net.

https://www.webassign.net/question_assets/tccgenchem2l1/glassware/manual.html#:%7E

:text=They%20are%20manufactured%20to%20contain,of%200.5%20to%201.0%20mL.

APPENDIX

Mott, V. (n.d.). Weak Acid-Strong Base Titrations | Introduction to Chemistry. Lumen.

https://courses.lumenlearning.com/introchem/chapter/weak-acid-strong-base-titrations