FACULTY OF APPLIED SCIENCES

LABORATORY REPORT

ANALYTICAL CHEMISTRY
(CHM 421)

Title Analysis Of An Unknown Vinegar Sample

No Experiment 2

Name Nur Qistina Sofia Binti Zakaria

Student Id Number 2019268758
Lecturer’s Name Sir Mohd Hafiz Yaakob

Date Of Experiment 30th September 2019

Submission Date 14th October 2019

ABSTRACT

The purpose of this experiment is to prepare the standard solution pf sodium hydroxide.
Firstly, we need to determine the volume of NaOH that we need to use throughout the
experiment by using the formula M1V1 = M2V2. From this we obtained the volume needed
which is 11.82 mL. 800 mL distilled water followed by 11.82 mL of NaOH was added to
plastic bottle. The standard solution that had been prepared was used for the next
experiment.

To standardise the base against the potassium hydrogen we need to use the titration
method in order to determine the molarity of sodium hydroxide solution. Firstly, the
amount of KHP required was weighed and transfer to the conical flask. Then, dissolve the
KHP by adding 35 mL of distilled water to the flask and swirl it. Record the initial and final
volume of NaOH used. The molarity of NaOH obtained from this section was 0.16 M.

The last purpose of this experiment was to analyse the unknown in vinegar sample.
Pipetted 10.00 mL of vinegar sample into conical flask followed by 25 mL distilled water. The
phenolphthalein indicator was added to the flask and the titration process begin. Record the
volume of NaOH used for the solution to change its colour. The percentage of acetic acid in
vinegar was determined which is 2.73%.

OBJECTIVES

1) To prepare the sodium hydroxide solution.

2) To standardise the base against potassium hydrogen phthalate.
3) To analyse the unknown vinegar sample.
INTRODUCTION

Standardisation is the condition in which a standard has been successfully established

(Based on WordNet 3.0, Farlex clipart collection. © 2003-2012 Princeton University, Farlex
Inc.). Another definition of standardisation is to bring to or make of an established standard
size, weight, quality and strength (Based on Thesaurus.com). A standard solution is solution
of accurately known concentration prepared from a primary standard that is weighed
accurately and made up to a fixed volume. Primary standard is a reagent that can be
obtained in a very pure, stable and easily weighed form. A weighed primary standard is
dissolved in the desired solvent and diluted to known final volume in a volumetric flask. The
volumetric flask is inverted a few times to obtain homogeneous solution.

Firstly, you need to prepare the sodium hydroxide solution. Sodium hydroxide is not
a primary standard because it is hygroscopic. The definition of hygroscopic is it absorbs
moisture rapidly when exposed to air. Thus, it can determined by standardising the solution
against a very pour potassium hydrogen phthalate (KHP) in a series of titrations.
Standardization of sodium hydroxide is used to determine the acetic content acid of a
vinegar sample.

The secondary standard is used when the primary standard form cannot be obtained
by preparing the concentration of the solution of reagent. Then using standardisation
process to determine its true concentration. By titrating the prepared solution against a
measured mass of a suitable primary standard the standardisation can be achieved.

We can use potassium hydrogen phthalate as the primary standard to prepare a

secondary standard solution of sodium hydroxide. The standardised solution of sodium
hydroxide is then used to analyse the content of acetic acid in a vinegar sample.
PROCEDURES

A. Preparation of the Sodium Hydroxide Solution

A800mL of approximately 0.25M sodium hydroxide solution was prepared by diluting a

laboratory prepared stock solution of approximately 50% (w/w) NaOH. The rough density of
the prepared 50% NaOH was determined by measuring the mass of 10mL solution. a dry and
empty 50mL beaker was weighed. 10mL of the NaOH solution was measured in a cylinder
and transferred to the pre-weighed beaker. The beaker was reweighed. The weight of 10mL
50% NaOH prepared in this laboratory obtained by the difference in weight given. The
volume of the stock solution required to prepare 600mL of approximate 0.25mL sodium
hydroxide solution was calculated using the density of the prepared 50% NaOH.

About 300mL of distilled water was placed into a clean plastic bottle. The calculated volume
of the stock NaOH solution required was measured into a graduated cylinder by using a
dropper. The contents of the cylinder was poured carefully into the partially filled plastic
bottle. The cylinder was rinsed a few times with fresh distilled water and added all the rinses
content into the plastic bottle. The cap on the plastic bottle was screwed and the contents
was mixed thoroughly by vigorously inverting the bottle and swirling it repeatedly. The
remaining volume of water in three 100mL batches finally added, the contents in the bottle
was mixed thoroughly each time. The bottle was shaken at least 20 times after the last
addition.

B. Standardisation of the Base against Potassium Hydrogen Phthalate

1 g sample of dry primary-standard grade potassium hydrogen phthalate (KHP) was weighed
on to a weighing boat. The KHP have been dried earlier to use. By using the appearance of
the above 1 g sample as a guide to accurately weigh two more such samples by difference.
Each sample was transferred quantitatively from weighing boat into a 250mL conical flask.
The boat was rinsed with a small amount of water from wash bottle to make sure all the
sample have been transferred. 35mL of water was added to each flask and was swirled
gently until all the solids dissolve. The side wall of conical flask was rinsed using the distilled
water.
 50 mL burette was rinsed using distilled water and was filled with NaOH stock
solution that we had prepared. The air bubbles was removed before adjusting the initial
volume and doing the titration process. The stopcock was turned quickly 360° a few times
until all the air bubbles removed. The initial volume adjusted. The meniscus was placed at
eye level. The actual starting volume was read and record to the nearest 0.02 mL. Any
adhering solution was wiped out at the sides and the tip of the burette before the titration
begin.

Three drops of phenolphthalein indicator was added into the first conical flask. The
conical flask was place under the burette and lower the tip well into it. Start the titration.
The stopcock was control gently and steady stream of the titrant flow into the acid solution.
The solution was gently swirled and the first permanent pink colour disappears. Reduce the
flow rate of the titrant form burette. The experiment was repeated three times and the
result was recorded.

C. Analysis of the Unknown Vinegar Sample

The density of vinegar sample was determined. 10.0mL vinegar was pipetted into dry pre-
weigh 50mL beaker and the beaker was reweigh back. More vinegar sample was took into
the 50m mL beaker for titration.

10.00 mL vinegar sample was pipetted from the beaker into a clean 250 mL conical
flask. Two more samples was prepared. The sides of each flask wash washed down with 25
mL water from the bottle.

Three drops of phenolphthalein indicator was added into one of the titration vessels
and the contents was titrated to endpoint with the standardised NaOH solution from part B.
The process was repeated for two samples
DATA AND RESULTS

Experiment 2: Analysis of an Unknown Vinegar Sample

A) Preparation of the Sodium Hydroxide Solution

Volume of NaOH taken from the 50% stock solution = 11.82 mL

B) Standardisation of the base against Potassium Hydrogen Phthalate

Rough 1 2
Weight of KHP 1.0223 g 1.0054 g 1.0068 g

Final reading of NaOH 31.00 mL 30.50 mL 30.00 mL

Initial reading of NaOH 0.00 mL 0.00 mL 0.00 mL
Volume of Naoh(mL) used 31.00 mL 30.50 mL 30.00 mL
Ratio volume of NaOH/Weigh 1:1 1:1 1:1
of KHP
Table 1: Data and observation from first titration

C) Analysis of the Unknown Vinegar Sample

Density of vinegar sample = 1.08306 g/mL

Rough 1 2
Volume of unknown 10.0 mL 10.0 mL 10.0 mL
vinegar (mL)
Final reading of 13.5 mL 13.0 mL 14.0 mL
standard NaOH
Initial reading of 0.0 mL 0.0 mL 0.0 mL
standard NaOH
Volume of standard 13.5 mL 13.0 mL 14.0 mL
NaOH used
Table 2: Data and observation from second titration

CALCULATION

A) Preparation of the Sodium Hydroxide Solution

Mass of empty measuring cylinder 31.0672 g
 Mass of measuring cylinder + NaOH 44.6072 g
Mass of NaOH 44.6072 g – 31.0672 g
= 13.54 g
Table 3: Data of weighing by difference

By using formula density:

Density = mass/volume

Density = 13.54 g / 10.00 mL

= 1.354 gmL-1

Molarity Naoh = (1.354 g/1 mL) x (1000 mL/1 L) x (1 mol NaOH/40 g/mol) x (50%/100%)
=16.925 M

By using formula M1V1 = M2V2

(16.925M)(V1) = (0.25M)(800mL)
16.925V1 = 200
V1 = 200/16.925
V1 = 11.82 mL

B) Standardisation of the base against Potassium Hydrogen Phthalate

The chemical equation
KHC8H4O4 (aq) + NaOH(aq)KNaC8H4O4 (aq) + H2O(l)
Molar mass KHP = 204.23 g/mol
At balance equation: 1 mol of KHP is equal to 1 mole NaOH

1) Rough
Calculating molarity of KHP:
(1.0023 g KHP/204.23g/mol) = 0.00491 mole KHP

Calculating molarity of NaOH:

= 0.00491 mol KHP/31.0 mL) x (1000mL/1L) x (1 mol NaOH/1 mol KHP)
= 0.16 M NaOH

2) Titration 1
Calculating molarity of KHP:
(1.0054 g KHP/204.23g/mol) = 0.00492 mole KHP

Calculating molarity of NaOH:

= 0.00492 mol KHP/31.0 mL) x (1000mL/1L) x (1 mol NaOH/1 mol KHP)
= 0.16 M NaOH

3) Titration 2
Calculating molarity of KHP:
(1.0068 g KHP/204.23g/mol) = 0.00493 mole KHP

Calculating molarity of NaOH:

= 0.00493 mol KHP/31.0 mL) x (1000mL/1L) x (1 mol NaOH/1 mol KHP)
= 0.16 M NaOH

C) Analysis of the Unknown Vinegar Sample

Mass of 50mL beaker 35.0715 g
Mass of 50mL beaker+10.0 mL vinegar 45.9021 g
Mass of 10.0 mL vinegar 10.8306 g
Table 4: Data of Analysis of the unknown vinegar sample
Density of vinegar sample : 10.8306 g / 10.00 mL
: 1.08306 g/mL
The chemical equation
CH3COOH + NaOHCH3COO- Na+ + H2O
Calculation:
Average molarity of NaOH = (0.16M+0.16M+0.16M/3)
= 0.16 M
Molar mass acetic acid = 60.02 mole NaOH

Mass acetic acid = (0.00492mole) x (60.02 g/mole)

= 0.2953

Percentage acetic acid solution % (w/w)

= (mass of acetic acid (g)/mass of vinegar sample (g)) x 100%
= (0.2953 g / 10.8306 g) x 100 %
= 2.73 %

DISCUSSION

Sodium hydroxide is a hygroscopic. Thus, it cannot be used as primary standard as it absorbs

moisture rapidly when exposed to the air. From the first experiment, in order to determine
the concentration of sodium hydroxide solution through titration we can used KHP as
primary standard. KHP is easily weighed as it is an organic solid compound. Therefore, KHP
is not a hygroscopic which is do not reacts with any other component in the laboratory.
Three drops of phenolphthalein indicator was added to the reaction to visually determine
the end point.An indicator is a chemical that changes colours. By using phenolphthalein
indicator, the colour changes to pink when the solution is base. The indicator changes
colour, when just a tiny excess of the acid or base is added beyond the completion of the
reaction. During titration, NaOH and KHP react together until reached the endpoint which is
one of the two reaction completely reacted. The total volume used from the burette at this
point is called the endpoint. This is the chemical equation for the experiment:

KHC8H4O4 (aq) + NaOH(aq) KNaC8H4O4 (aq)  +  H2O(l)

The next experiment is to analysis the unknown vinegar sample. Acetic acid, CH3COOH, is a
weak acid. The chemical equation derived from this experiment is CH 3COOH + NaOH
CH3COO- Na+ + H2O. We can determine the number of moles of acetic acid by using
stoichiometry from the above equation. From part (C) the average mass of 10.00 mL vinegar
sample titrated against sodium hydroxide is 10.7594 g. Thus, the density obtained from this
experiment was 1.0759 gmL-1. The mass of acetic acid was determined where the mass was
0.2953 g CH3COOH. The percentage of acetic acid was determine by using formula mass of
acetic acid in gram divide by mass of vinegar sample in gram time with 100%. The
percentage was 2.73%.

There were few errors that might have occurred throughout the experiment. Firstly, parallax
error while taking reading of solution in burette. Secondly, burette was not rinsed
thoroughly with the solution that was to be used might which altered the accuracy of
titration. Thirdly, air bubbles were present near the burette tip. Finally, titration was done
with the funnel still being left on top of burette.

CONCLUSION

The standard solution of sodium hydroxide has been prepared.From the second experiment
the molarity of sodium hydroxide has been determine that is 0.16M NaOH.The percentage
of acetic acid in the vinegar solution is 2.73%. Therefore, the objectives of the experiment
successfully achieved.

REFERENCES

1) Santa Monica College.(Jun 6, 2019).Experimental Determination of the Gas Constant

(Experiment)-Retrieved-from-
https://chem.libretexts.org/Ancillary_Materials/Laboratory_Experiments/Wet_Lab_Exp
eriments/General_Chemistry_Labs/Online_Chemistry_Lab_Manual/Chem_10_Experime
nts/10%3A_Experimental_Determination_of_the_Gas_Constant_(Experiment)
2) School Work Helper.(April 2018).Titration of Vinegar Lab Answers-Retrieved from-
https://schoolworkhelper.net/titration-of-vinegar-lab-answers/

QUESTIONS

1. Explain why weighing by difference eliminates systematic balance errors.

 A systemic error means that a constant error is applied to the true weight of the
object. Weighing by differencecan reduce, but noteliminate, systemic errors in an
experiment because systemic errorsdo not arise simply from errors in measurement,
but from a variety of sources.

2. Why does it not matter how much water you add when dissolving the acid (KHP) or
when carrying out the titration?

Adding water to a titrant will change the concentration of that solution. When you
add water to a solution, the number of moles of the solvent stays the same while the
volume increases. The titration equivalence point occurs when the acid present in
the sample has been exactly neutralized by the volume of base added. Additional
water added to the reaction vessel has no effect on the volume of base added.