LABORATORY REPORT

CHM421

(ANALYTICAL CHEMISTRY)

NAME: 1. SITI AISYAH BINTI RAMDAN ( 2022861662 )

2. NUR AZRINA HAFIZAH BINTI AZIZAN ( 2022471074 )
3. MUHAMMAD SYAHIN BIN MOHD SAHARUDIN ( 2022663344 )
4. AIMAN IMAN BIN SHAIFUDDIN ( 2022478888 )
5. MUHAMMAD AIMAN BIN AHMAD SALLEH ( 2022484412 )

GROUP: AS222 2A1

EXPERIMENT NO: 2

EXPERIMENT ANALYSIS OF UNKNOWN VINEGAR SAMPLE

TITLE.:
DATE OF 12 APRIL 2023
EXPERIMENT:
DATE OF REPORT 3 MAY 2023
SUBMISSION:
NAME OF DR NUR SOFIAH ABU KASSIM
LECTURER:
 EXPERIMENT 2: ANALYSIS OF UNKNOWN VINEGAR SAMPLE

Objectives
1. To prepare the Sodium Hydroxide solution.
2. To standardize the Base against Potassium Hydrogen Phthalate.
3. To analyses an unknown vinegar sample.

Introduction
In this experiment, it involved the standard solution, primary solution and standardization.
Firstly, a standard solution is actually a solution of accurately known concentration that
prepared from a primary standard that is weighed accurately and made up to a fixed volume.
The compound is actually stable, high purity, highly soluble in water and high molar mass to
allow for accurate weighing. (Royal Society of Chemistry, 2023).
Next, to prepare standard solution is from a primary standard. Primary standard solutions
were prepared by dissolving a substance of high purity (primary standard) of known exact
weight in a solution of precisely known volume. However, if the titrant is not pure enough, it
needs to be standardized with a primary standard. (Dianingsi et al. 2021). A process
standardization can be defined as the process standardizing the solution against a very pure
potassium hydrogen phthalate in a series of replicate titrations.
The title of the experiment is the analysis of an unknown vinegar sample. Vinegar is
actually produced from a raw material containing starch or sugar via sequential ethanol and
acetic acid fermentations and it is used in a variety of food applications. Other than that, vinegar
has two main ingredients which are acetic acid and water. (Fermented Foods in Health and
Disease Prevention, 2017). Therefore, based on this experiment, an acid and base reaction
was performed by adding NaOH to vinegar to determine its acetic acid substances.
Procedure
A. Preparation of the Sodium Hydroxide Solution

1. 41.67 mL of 3.0 M NaOH was added into a 500 mL volumetric flask.

2. Distilled water was added into the volumetric flask. The volumetric flask was
swirled to mix the solution thoroughly.

B. Standardization of the Base against Potassium Hydrogen Phthalate.

1. 1 g sample of dry primary-standard grade potassium hydrogen phthalate (KHP) was

weighed on to a weighing boat.
2. The appearance of the above 1 g sample was used as a guide to accurately weigh
two more such samples by difference.
3. Each sample from the weighing boat was transferred into a 250 mL conical flask.
The boat was rinsed with a small amount of water from the wash bottle to make
sure all the samples had been transferred.
4. 35 mL of water was added to each flask and the flask was swirled gently until all
the solids dissolved. Any drops of the sample solution were rinsed on the side walls
of the flask with distilled water.
5. A 50 mL burette was rinsed and filled with the NaOH solution. The air bubbles were
removed before adjusting the initial volume and doing titration process. The
stopcock was turned quickly 360° a few times until all bubbles were removed.
6. The initial volume was adjusted. 3 drops of phenolphthalein indicator were added
into the first conical flask.
7. The flask was placed under the burette and lowered the burette tip well into it. A
piece of a white tile was placed under the flask, the flask was holden with right hand
and the stopcock of the burette was controlled with left hand and the titration was
started. The solution in the flask was swirled gently.
8. The titration was stopped when the solution reached a pale pink solution in the flask.
The volume of NaOH was recorded.

C. Analysis of the Unknown Vinegar Sample.

1. The density of the vinegar sample was determined. 10 mL vinegar was pipette
into a dry pre-weighed 50 mL beaker. The beaker was reweighed. The weight
for 10 mL vinegar samples was given by the difference. More vinegar was taken
into the 50 mL beaker for titration.
2. 10 mL vinegar sample was pipette from the beaker into a clean 250 mL conical
flask. Two more such samples were prepared. The sides of each flask were
washed down with 25 mL water from wash bottle.
3. Three drops of phenolphthalein indicator were added into one of the titration
vessels and the contents were titrated to endpoint with the standardized NaOH
solution from Part B. The process was repeated for the other two samples
Results
A. Preparation of the Sodium Hydroxide Solution.

Mass beaker: 36.6028 g

Volume of NaOH taken from the 50% stock solution: 41.67 ml

B. Standardization of the Base against Potassium Hydrogen Phthalate.

Rough 1 2 3
Weight of KHP 1.0170 g 1.0627 g 1.0055 g 1.07839 g
Final reading 45.3 ml 29.8 ml 22.8 ml 30.0 ml
NaOH
Initial reading 5.0 ml 5.3 ml 1.6 ml 8.0 ml
NaOH
Volume NaOH 40.3 ml 24.5 ml 21.2 ml 22.0 ml
used
Ratio volume 39.62 ml 23.0544 ml 21.0840 ml 20.4008 ml
NaOH / weight
of KHP

C. Analysis of the Unknown Vinegar Sample.

Rough 1 2 3
Volume of
unknown 10 ml 10 ml 10 ml 10 ml
vinegar
Final reading 50.0 ml + 50.0 ml + 50.0 ml + 50.0 ml +
standard NaOH 35.1 ml 12.4 ml 20.9 ml 18.6 ml
Initial reading 2.0 ml + 2.0 ml + 9.2 ml + 12.4 ml +
standard NaOH 31.9 ml 6.0 ml 8.5 ml 1.0 ml
Volume
standard NaOH 51.2 ml 54.4 ml 53.2 ml 55.2 ml
used

Rough 1 2 3
Mass pre 36.928 g 31.5433 g 31.9347 g 32.4297 g
weight beaker
Beaker + 47.2218 g 41.6178 g 42.0340 g 42.5103 g
vinegar
Actual weight 10.2938 g 10.0745 g 10.0993 g 10.0806 g
vinegar
 Calculation
A. Preparation of the Sodium Hydroxide Solution
M1V1= M2V2
(3) (V1) = (0.25) (500m𝑙)
V1= 41.67 m𝑙
𝑙
B. Standardization of the Base against Potassium Hydrogen Phthalate
Equation:
KHC8H4O4 + NaOH → KNaC8 H4O4 + H2O
Molar mass KHP: 204.22 g/mol
Based on the equation, 1 mole of KHP react with 1 mole of NaOH to produce 1 mole of
KNaC8 H4O4 and H2O
It is used to find the molarity of NaOH
1. Rough
Molarity KHP Molarity NaOH
1.0170 𝑔
204.23𝑔/𝑚𝑜𝑙
= 0.0049 mol KHP 0.0049 mol KHP (
1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻
)= 0.0049 mol NaOH
1 𝑚𝑜𝑙 𝐾𝐻𝑃
0.0049 𝑚𝑜𝑙
0.035 𝑙
= 1.4 M KHP 0.0049 𝑚𝑜𝑙
= 0.12 M NaOH
0.0403 𝑙

2. Titrant 1
Molarity KHP Molarity NaOH
1.0627𝑔 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻
(204.23𝑔/𝑚𝑜𝑙) = 0.0052 mol KHP 0.0052 mol KHP (
1 𝑚𝑜𝑙 𝐾𝐻𝑃
) = 0.0052 mol NaOH
0.0052 𝑚𝑜𝑙
0.0052 𝑚𝑜𝑙
= 0.15 M KHP 0.0245 𝑙
= 0.21 M NaOH
0.035 𝑙
 3. Titrant 2
Molarity KHP Molarity NaOH
(
1.0055𝑔
204.23 𝑔/𝑚𝑜𝑙
) = 0.0049 mol KHP 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻
0.0049 mol KHP ( 1 𝑚𝑜𝑙 𝐾𝐻𝑃 ) = 0.0049 mol NaOH

0.0049 𝑚𝑜𝑙
0.035 𝑙
= 0.14 M KHP
0.0049 𝑚𝑜𝑙
0.0212 𝑙
= 0.23 M NaOH

4. Titrant 3
Molarity KHP Molarity NaOH
1.07839𝑔
(204.23𝑔/𝑚𝑜𝑙) = 0.0053 mol KHP 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻
0.0053 mol KHP ( 1 𝑚𝑜𝑙 𝐾𝐻𝑃 ) = 0.0053 mol NaOH

0.0053 𝑚𝑜𝑙 0.0053 𝑚𝑜𝑙

0.035 𝑙
= 0.15 M KHP = 0.24 M NaOH
0.022 𝑙

𝑇𝑖𝑡𝑟𝑎𝑛𝑡 1 + 𝑇𝑖𝑡𝑟𝑎𝑛𝑡 2 + 𝑇𝑖𝑡𝑟𝑎𝑛𝑡 3

Average Molarity of NaOH =
3
0.21 𝑀 + 0.23 𝑀 + 0.24 𝑀
=
3
= 0.23 M

C. Analysis of the unknown vinegar sample

Equation:
CH3COOH +NaOH → CH3COO-Na+ +H2O
Molar mass vinegar/acetic acid = 60.052 g/mol
1. Rough
(M acetic acid) (10.0 ml) = (0.23 M) (51.2 ml)

M acetic acid = 1.18 M

2. Titrant 1
(M acetic acid) (10.0 ml) = (0.23 M) (51.2 ml)

M acetic acid = 1.18 M

3. Titrant 2
(M acetic acid) (10.0 ml) = (0.23 M) (53.2 ml)

M acetic acid = 1.22 M

4. Titrant 3
(M acetic acid) (10.0 ml) = (0.23 M) (55.2 ml)

M acetic acid = 1.27 M

𝑇𝑖𝑡𝑟𝑎𝑛𝑡 1 + 𝑇𝑖𝑡𝑟𝑎𝑛𝑡 2 + 𝑇𝑖𝑡𝑟𝑎𝑛𝑡 3

Average Molarity of acetic acid =
3
1.18𝑀 + 1.22 𝑀 +1.27 𝑀
=
3
= 1.22 M

𝑚𝑎𝑠𝑠 𝑣𝑖𝑛𝑒𝑔𝑎𝑟 𝑢𝑠𝑒𝑑(𝑔)

Density vinegar =
𝑣𝑜𝑙𝑢𝑚𝑒 𝑣𝑖𝑛𝑒𝑔𝑎𝑟 (𝑚𝑙)

Density Vinegar Calculation

Rough 10.2938 𝑔
= 1.0294 g/ml
10 𝑚𝑙
 Titrant 1 10.0745 𝑔
= 1.0075 g/ml
10 𝑚𝑙
Titrant 2 10.0993 𝑔
= 1.0099 g/ml
10 𝑚𝑙
Titrant 3 10.0806 𝑔
= 1.0081 g/ml
10 𝑚𝑙

1.0294+1.0075+1.0099+1.0081
Average density vinegar=
4
= 1.0137 g/ml

Discussion
In this experiment for the preparation of the sodium hydroxide, 500 ml of 0.25M NaOH
solution is prepared from 3M of NaOH by the dilution method. The formula M 1V1= M2V2 is
used to determine the volume of 3M NaOH needed for diluting into 500 ml of 0.25M NaOH
solution which is V1= 41.67 ml. The 500 ml of 0.25M NaOH solution then is used for the next
experiment.
 For the experiment of the standardisation of the base against potassium hydrogen
phthalate and experiment of analyse an unknown vinegar sample, the acid-base titrations were
conducted. A solution with a known concentration, referred to as a standard solution, is
continuously added to another solution with an unknown concentration during titration until
the chemical reaction between the two solutions is complete which indicates the titration point.
We can determine the concentration of the unknown solution if we know the volumes of the
standard and unknown solutions used in the titration as well as the concentration of the standard
solution. (Chang, 2010).
For the experiment which of the standardization of the base against potassium hydrogen
phthalate, the titration between NaOH and potassium hydrogen phthalate is carried out to
determine the molarity of NaOH. Due to propensity of sodium hydroxide to absorb water from
the air and the reaction that occurs in its solution with carbon dioxide, it is difficult to obtain
solid NaOH in a pure form. Because of these factors, a sodium hydroxide solution needs to be
standardized before it can be used for precise analytical work. (Chang, 2010). Each flask with
KHP is added with phenolphthalein that turns colourless to permanent pink pale solution to
determine the equivalence point. After the titration is carried out, the molarity KHP is
determined by dividing each weigh KHP with molar mass KHP which is 204.23 g/mol to get
the mol of KHP. The mol KHP then divided with the volume of KHP which is 0.035 L to get
the molarity of KHP. Based on chemical equation, 1 mol of KHP reacts with 1 mol of NaOH
thus we can get the mol of NaOH then by dividing the mol of NaOH with the volume NaOH
used we can get molarity of NaOH. The molarity of NaOH is determined for each titration
which is for the rough titrant is 0.12M, 0.21M for titrant 1, 0.23M for titrant 2 and 0.24M for
titrant 3. The average molarity of NaOH is determined by sum of titrant 1 titrant 2 and titrant
3 than divided by 3, which is 0.23M.
For the experiment of analysis of unknown vinegar sample, the same stock of NaOH
solution is used to be titrated with the unknown vinegar sample. Vinegar sample or known as
acetic acid functioned as an acid while NaOH are the base. The titration was done, the data
were recorded, and the calculations were made to determine the molarity of acetic acid and the
density of acetic acid in each titration. For the molarity of acetic acid in each titrant, the rough
titrant was 1.18M, 1.18 M for titrant 1, 1.22 for titrant 2 and 1.27 for titrant 3. The average
molarity of acetic acid was calculated by adding the molarity of titrants 1,2 and 3 and were
divided by 3. The average molarity of acetic acid was 1.22 M. Next, the density of acetic acid
can be calculated by division between mass of acetic acid used in gram and volume of acetic
acid in milliliters. A fixed volume of 10.0 ml acetic acid was used in each titration. Density of
acetic acid for rough titrant was 1.0294 g/ml, 1.0075 g/ml for titrant 1, 1.0099 g/ml for titrant
2 and 1.0081 g/ml for titrant 3. average density of acetic acid was calculated by dividing the
density of acetic acid in titrant 1,2 and 3 and dividing it by 3. The average density of acetic
acid was 1.0137 g/ml.
In the experiment of standardization of the base against potassium hydrogen phthalate
we can see that the standard molarity of NaOH was not 0.25 M but in average, was 0.22 M.
This shows that the experiment had low accuracy with targeted molarity of 0.25 M but has high
precision based on each titration. In an experiment of analysis of unknown vinegar sample, the
presence of water during cleaning the flask containing acetic acid may affect the difference of
molarity of acetic acid in each titration. This can be avoided by using a fixed volume of water
to wash the flask containing acetic acid. When conducting both experiments involving titration,
there were errors that occurred which led to low accuracy of the experiment. The errors that
happened were human errors which can be observed by different color concentration of
phenolphthalein in each titration. Poor titrating skills lead to excess amount of base dropped
into the acid which brought to different color concentration of phenolphthalein. The right color
of phenolphthalein for the right titration point is light purple. The dark purple color indicates
that the titration had exceeded its titration point. Different students conducting each titration
also leads to errors in experimenting.

Conclusion
In conclusion, the objectives of the experiment were achieved which were preparing the
sodium hydroxide solution, standardized the base against potassium hydrogen phthalate and
analyzed an unknown vinegar sample. In standardizing the base of NaOH the result was shown
that the standardized molarity of NaOH was 0.22 M instead of 0.25 M. The calculation of this
experiment shows that it has high precision but low accuracy. In analyzing an unknown vinegar
sample, the average molarity of vinegar sample was 1.22 M, and the average density of vinegar
sample was 1.0137 g/ml. Precautions must be taken to prevent errors when conducting the
experiment such as same person must conduct each titrations for one experiment for constant
result and high skills of titrating must be taken to get precise titration point when titrating.
Fixed amount of water must be used when washing the flask to prevent the changes in
concentration of vinegar.

Questions
1. Explain why weighing by difference eliminates systematic balance errors.
-Because the mass is determined by the difference between two readings, a systematic
error in the absolute mass on the balance will be removed by subtracting the final weight
from the initial weight
2. Why does it not matter how much water you add when dissolving the acid (KHP or
when carrying out the titration?
-Adding water does not affect your results, since you are measuring the amount of acid in
solution, not the amount of water present.

Reference
1. Chang, R. (2010). Chemistry (10th ed.). Mcgraw-Hill.
2. Dianingsi Hipi, Eka Paramita Daud, & Gayatri D. Soga. (2022). Identification of
Alkalimetric Levels Using Acid-Base Reaction Principles. Journal of Health,
Technology and Science (JHTS), 2(4), 11–20. https://doi.org/10.47918/jhts.v2i4.247
3. Garcia-Parrilla, M. C., Torija, M. J., Mas, A., Cerezo, A. B., & Troncoso, A. M. (2017).
Vinegars and other fermented condiments. In Fermented foods in
health and disease prevention (pp. 577- 591). Academic Press.