CHM421 LAB REPORT

NAME : AZAMUDDIN BIN AHMAD TAZLAN

MATRIX NO : 2022611616

EXPERIMENT : ANALYSIS OF AN UNKNOWN VINEGAR SAMPLE

LECTURER’S NAME : DR. NURULFAZLINA EDAYAH BINTI RASOL

DATE : 17 OCTOBER 2023

GROUP MEMBER :

NAME STUDENT ID
AHMAD ZULHAIRIE BIN BEDDU 2022495572
IKMAL HAFIZ BIN ZAM SHAHRANY 2022835938

MUHAMMAD ADAM BIN JOHARI 2022605112

MUHAMMAD IRFAN BIN MUHD SABRI 2022464732
 Experiment 2: ANALYSIS OF AN UNKNOWN VINEGAR SAMPLE

ABSTRACT:
This experiment was conducted to achieve the three objectives which are to prepare the sodium
hydroxide solution, to standardize the base against potassium hydrogen phthalate and to analyze
the unknown vinegar sample.The first thing that I do was determining the density of sodium
hydroxide before preparing 1000 ml solution with molarity 0.25 M.Then, the second objective
which is standardizing the base against potassium hydrogen phthalate, resulting in an average
concentration of 0.18 M . Next, analyzing the unknown vinegar with the percentage of acetic
acid in vinegar (w/w) is 5.25% .In this experiment, the prepared sodium hydroxide solution that
had been diluted become as standard solution will be titrated to the next two last objectives of
this experiment. Phenolphthalein was used as the indicator for titration. The experiment will be
successed when the endpoint is achieved which is from colourless solution to pale pink colour of
the solution after the titration.

OBJECTIVES:
1) To prepare the sodium hydroxide solution
2) To standardize the base against potassium hydrogen phthalate
3) To analyze the unknown vinegar sample

INTRODUCTION:
There are three approaches that must be followed in this experiment. First, prepare the Sodium
Hydroxide (NaOH). Second, the base's standardisation against Potassium Hydrogen Phthalate.
Third, an unknown vinegar sample was studied. By doing this experiment, the concept that I
applied is standardizing a solution by titration method using a burette until the endpoint is reached.
A standard solution is one whose concentration has been determined precisely. Standard solutions
are made from highly pure substances, and their precise concentration is determined by a process
known as standardisation. A primary standard is a highly pure substance that is accessible for the
standardisation of a solution.There are several steps to prepare standard solution of sodium
hydroxide.Firstly,calculating the number of mole of sodium hydroxide so that the mass of sodium
hydroxide needed can be determined.Then, weighing by difference method is applied due to
hygroshcopic of sodium hydroxide means that weight of weighing boat with sodium hydroxide,
substracted with weight of weighing boat only.Next, dissolve it with distilled water and pour into
1000 ml of volumetric flask.The solution will be diluted until reach the calibrated mark of
volumetric flask then swirl it gently become even.Other than that, standardisation is a technique
for determining the exact concentration of a solution. Titration is the most common method for
standardising a solution. As a reference in the standardisation process, a standard answer is
necessary. There are two kinds of standard solutions: primary standard solutions and secondary
standard solutions. For exact standardisation, we typically use primary standard solutions. These
solutions are extremely pure (99.9% correct).The ultimate concentration of a solution made from
a solid chemical material can vary based on a number of factors, including technical mistakes,
compound purity, human error, and others.There are severals steps to standardise the base against
potassium hydrogen phthalate. Firstly, weighing potassium hydrogen phthalate (KHP) by using
weighing by difference. Then, use the standard solution of sodium hydroxide to titrate KHP that
is dissolved with distilled water and the indicator is added in KHP solution.The result is occurred
when the solution must change from colourless solution into pale pink solution which is the
endpoint is achieved.

PROCEDURES:
A. Preparation Of The Sodium Hydroxide Solution

1)The number of mole of sodium hydroxide (NaOH) and also the mass of sodium hydroxide is
calculated respectively.
2)The weighing boat only was weighed first and the mass was recorded.
3)Then, the weighing boat was reweighed again which is including the solid of sodium hydroxide.
Then, the mass was recorded.
4)The solid of sodium hydroxide was poured into a 50 mL beaker and dissolved with distilled
water.
5)The sodium hydroxide solution was poured into 1000 mL volumetric flask. The wall of beaker
was rinsed with distilled water and the balance solution was poured again into volumetric flask.
6) The sodium hydroxide was diluted until the calibrated mark was reached.
7) Then, the solution in the volumetric flask was swirled gently until the solution become even.

B.Standardisation Of The Base Against Potassium Hydrogen Phthalate

1)1 g sample of dry primary-standard grade potassium hydrogen phthalate(KHP) was weighed
accurately on to a weighing boat.The KHP had been dried earlier, in an oven at 110°C for 2 hours
and stored in a dessicator prior to use.
2)The appearance of the above 1 g sample as a guide was used and weighed accurately for two
more such samples by difference.Each sample from the weighing boat was transferred quantitively
into a 250 mL conical flask.All the sample had been transferred by rinsing the boat with a small
amount of water from the was bottle.35 mL of water was added to each flask and the flask was
swirled gently until all the solids was dissolved.Any drops of the sample solution was rinsed on
the side walls of the flask with distilled water.
3)A 50 mL burette was rinsed and filled with the standard sodium hydroxide(NaOH) solution.Air
bubbles was removed before adjusting the initial volume and doing titration process.The stopcock
was turned quickly 360° a few times until all bubbles were removed.Then, the initial volume was
adjusted.Instead the meniscus was placed at our eye level.
4)Three drops of phenolphthalein indicator were put into the first conical flask.The flask was
placed under the burette and the burette tip was lowered well into it.Thief titration was included in
first trial.A piece of white tile was placed under the flask, the flask was held with our right hand
or left handed , others hand was controlled the stopcock of the burette and titration was started by
carefully turning the stopcock to let a gentle and steady stremaed of the titrant flow(without
splashing) into the acid solution. The solution was swirled gently in the flask.The base could be
added rapidly at first, but concentrated on the colour change.The pink colour initially was
disappeared as it was formed but with time , this colour was began to linger as we swirled the
flask.At this point, the flow rate of titrant was reduced from the burette.The first permanent faint
pink colour that persists for at least 20 seconds was the end point.

C. Analysis Of The Unknown Vinegar Sample:

1)The density of the vinegar sample was determined. 10.0 mL was pipetted into a dry pre-weighed
50 mL beaker. The beaker was reweighed. The difference would give the weight for 10 mL vinegar
sample. More vinegar sample were taken into the 50 mL beaker for titration.
2) 10.0 mL vinegar sample was pipetted from the beaker into a clean 250 mL conical flask.Two
more such samples were prepared.The sides of each flask was washed down with 25 mL water
from the wash bottle.
3) Three drops of phenolphthalein indicator were added into one of the titration vessels and the
content was titrated to endpoint with the standardised sodium hydroxide solution from part B.
Titration theft was adopted still, at least for the first titration. The process for other two samples
were repeated.Ideally, the titration should be reproducible.

RESULT AND DISCUSSION:

 From this experiment, I have learned to prepare the standard solution of sodium hydroxide
respectively.The experiment has been done and succeeded.By calculating the number of mole of
sodium hydroxide and mass needed for the standard solution.Then, the solid of sodium hydroxide
is dissolved with distilled water and diluted to 1000 mL of volumetric flask until reach the
calibrated mark and the solution is swirled until become evenly.Due to insufficient of apparatus,
new method and calculation is occurred for part A only.The result obtained which is the mass of
sodium hydroxide is 9.9995 g .
For part B, by using the standardised NaOH solution which is diluted, the standardisation the
base against Potassium Hydrogen Phthalate (KHP) was carried out. The titration is performed
which are standard NaOH solution as titrant while the analyte is potassium hydrogen phthalate.
Phenolphthalein is used as the indicator that is added into KHP solution which is 3 drops only.
While titration is in progress, the solution will change colour from colourless to pale pink when
the reaction is accomplished. The handling of titration must be carefully, which is the swirl must
be uniform and exact. This is due to the fact that the endpoint occurs when the pale pink is only
transitory (approximately 20 seconds), and over-titration can result in a prominent pink or light
purple, which will change the concentration of Potassium Hydrogen Phthalate.The balanced
chemical equation was carried out as below:

1 KHC8H4O4 (aq) + 1 NaOH (aq) → 1 KNaC8H4O4 (aq) + 1 H2O (l)

The result is occurred for the first trial titration which is 1.0016 g with the final reading of standard
NaOH is 25.9 mL, second trial titration which is 1.0098 g with the final reading is 29.6 mL, and
third trial titration which is 0.9993 g with final reading is 28.7 mL. The concentration for the trial
I,II and III is 0.20 M, 0.17 M and 0.17 M respectively. This occurred in an average concentration
of 0.18 M.Therefore, the 90 % confidence interval for the mean molarity of NaOH

For part C, the unknown vinegar is analysed using the standard NaOH as a titrant and the
unknown vinegar solution, which is acetic acid, as an analyte. Three drops of phenolphthalein are
being used as an indicator, changing the colour of the solvent from colourless to pale pink.The
density of vinegar sample or acetic acid is occurred which is 1.01813 g/mL. The molarity for each
of trial titration(I,II and III) is 0.914 M, 0.888 M and 0.868 M respectively.Here the balanced
chemical equation for the reaction occurred below in part C:

1 NaOH (aq) + 1 HC2H3O2 (aq) → 1 NaC2H3O2 (aq) + 1 H2O (aq)

From this result, the percentage of acetic acid in vinegar (w/w) is 5.25%. Therefore, the 90 %
confidence interval for the mean molarity of NaOH

When conducting this experiment, usage of a dropper towards the end of the calibration mark can
result in a more precise reading. The eyes must have been perpendicular to the calibration mark
when the reading was obtained. Aside from that, the swirling technique must be exact, with the
other hand always at the stopcock to avoid over-titration. The titration thief might be considered
during the titration process for a more exact reading.

CONCLUSION:
The sodium hydroxide solution has been prepared with the 9.9995 g calculated from the data
provided.The base has been standardised against KHP that give the average molarity of NaOH is
0.18 M.The unknown vinegar sample have been analysed that give the average molarity of vinegar
is 0.8658 M and percentage (w/w) of vinegar is 5.1%.

REFERENCES:
1. L. (2021, September 12). 5.1: Analytical Signals. Retrieved from
https://chem.libretexts.org/Bookshelves/Analytical_Chemistry/AnalyticalChemistry2.1-
(Harvey)/05%3A_Standardizing_Analytical_Methods/5.01%3A_Analytical_Signals

2. S. M. (2015, November 10). Standardization of NaOH using KHP experiment. Retrieved

from https://www.youtube.com/watch?v=J8gDdy6y_j8
QUESTIONS:
1)Explain how weighing by difference eliminates systematic balance errors.
Since mass is determined by the difference between two readings, a systematic inaccuracy
in the absolute mass on the balance can be eliminated by subtracting the end 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?
Water is not a major concern in acid-base titration because it is not a reactant in the process.
It can be used as a solvent or to rinse the flask before titration.Because water is merely a
solvent, it has no effect on the results of titrations. Solvents do not react with the solution's
other chemical species.