1.

0 ABSTRACT :-

This experiment was carried out first to prepare the sodium hydroxide solution , second
to standardise the base against potassium hydrogen phthalate and lastly to analyse the
unknown vinegar sample. The sodium hydroxide solution was very important as in this
experiment, we prepared 900 L of approximately 0.25 M NaOH by diluting a stock
solution of approximately 50 % ( w/w ) NaOH by mass. Besides , in this experiment
also need us to standardise the NaOH as a base against potassium hydrogen phthalate ,
KHP. For this part , it show us about weighing technique called weighing by difference
as we can get accurate weight for the KHP. Next was to analyse the unknown vinegar
sample which this was the main part of this experiment. For this part , it tech us how to
find the density of vinegar sample first as phenolphthalein indicator was used for
titration with standardized NaOH solution.

2.0 OBJECTIVE : -

i) To prepare the sodium hydroxide solution , NaOH.

ii) To standardise the base against potassium hydrogen phthalate , KHP.
iii) To analyse the unknown vinegar sample.

3.0 INTRODUCTION : -

Diagram 1

As shown in Diagram 1, it is molecular structure of a acetic acid. Vinegar which consist

of acetic acid has a molecular formula of CH3COOH.
 Vinegar is a liquid that is produced from the fermentation of ethanol into acetic acid as
this fermentation process is carried out by bacteria. Vinegar consist of acetic acid and water.
In this experiment, the titration technique was been done as to determine the concentration
of acetic acid in vinegar by adding base , NaOH to the solution as this is an acid/base
reaction. Besides , titration technique is a common laboratory method of quantitative
chemical analysis that used to determine the unknown concentration of an identified
analyte.

Next, a reagent or also known as titrant is prepared as a standard solution. A known

concentration and volume titrant will react with the solution of an analyte to determine the
concentration. The accurate concentration can be obtain by standardized it with potassium
hydrogen phthalate, KHP. The KHP is used to determine acetic acid contain in an unknown
vinegar sample by titration technique as the colour changes occur.

4.0 PROCEDURE :-

A. Preparation of the Sodium Hydroxide Solution

i) The 50 mL of an clean and empty beaker being weight.

ii) 12 mL of NaOH solution was poured into the 50 mL beaker and being
weight again.
iii) Then, poured 890 mL of distilled water into a clean plastic bottle using a
pipette.
iv) After that , poured the 12 mL of NaOH into the plastic bottle containing 890
mL of distilled water.
v) The total volume of the solution containing NaOH and distilled water was
900 mL.
vi) The bottle was closed with the lid and carefully mix vigorously the solution.
B. Standardisation of the base against Potassium hydrogen phthalate , KHP.

i) For this step, first the potassium hydrogen phthalate, KHP was weight about
1 g of sample. Prepared four times.
ii) Then, poured the KHP into each of the 250 mL of conical flask.
iii) Add 35 mL of distilled water into each of the 250 mL conical flask
containing the KHP.
iv) Each of the 250 mL conical flask containing distilled water and KHP were
added with 3 drop phenolphthalein indicator.
v) Next, poured diluted NaOH that been prepared earlier into the 50 mL burette
and make sure there was no bubbles at the tip of the burette.
vi) Begin the titration for each of the conical flask until it changes the colour to
pink. But for the first conical flask , do a rough titration.
vii) Repeat the process for the other sample.

C. Analysis of the unknown vinegar sample

i) For this part, first 50 mL of clean and empty beaker was being weight.
ii) Then , 10 mL of unknown vinegar was being pipette into the 50 mL beaker and
being weight again.
iii) The difference of the weight was a weight of the 10 mL unknown vinegar as it
can be used to calculate the density of vinegar sample.
iv) Prepared for four time and poured the 10 mL of unknown vinegar into each of
250 mL conical flask and then added 3 drops of phenolphthalein.
v) Then added NaOH that being prepared earlier into the 50 mL burette.
vi) Next, begin the titration as the first one begin with a rough titration.
vii) Repeat the process for the other sample until there was changes in colour.
5.0 RESULT and CALCULATION :-

A. Preparation of the Sodium Hydroxide Solution

Table 1 : Volume NaOH from 50% ( w/w ) , 0.25 M

Volume of NaOH taken from the 50% stock solution 12 mL

Calculations :-

Preparation of NaOH from 50% ( w/w ) stock solution , 0.25 M , density = 1.525 g/mL

50 𝑔 𝑁𝑎𝑂𝐻
i) 50% ( w/w ) -
100 𝑔 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛

𝑚𝑎𝑠𝑠 50 𝑔
ii) Number of mol NaOH - = = 1.25 mol NaOH
𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 40 𝑔/𝑚𝑜𝑙

𝑚𝑎𝑠𝑠 𝑚𝑎𝑠𝑠 100 𝑔

iii) Density = Volume = 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 = = 65.574 𝑚𝐿
𝑣𝑜𝑙𝑢𝑚𝑒 1.525 𝑔𝑚𝐿

iv) 65.574 mL 0.0656 L

1.25 𝑚𝑜𝑙
v) Molarity of NaOH = = 10.06 𝑀
0.0656 𝐿

vi) M₁V₁ = M₂V₂

( 0.25 M ) ( 900 mL ) = ( 19.06 M ) ( V₂ )

V₂ = 11.8 mL

V₂ ~ 12 mL
 Table 2 : Result for weight of 12 mL NaOH

Weight of empty 50 mL beaker 35.3545 g

Weight of 50 mL beaker + 12 mL NaOH 51.3804 g
Weight of 12 mL NaOH 16.0259 g

Density of 12 mL NaOH :-

𝑚𝑎𝑠𝑠 16.0259 𝑔
Density = = = 1.3355 g/ mL
𝑣𝑜𝑙𝑢𝑚𝑒 12 𝑚𝐿

B. Standardisation of the base against Potassium hydrogen phthalate , KHP.

Table 3 : Result of standardisation of the base against KHP

Rough 1 2 3
Weight of KHP 1.001 g 1.005 g 1.005 g 1.009 g
Final reading of NaOH 33.1 mL 33.0 mL 33.0 mL 33.2 mL
Initial reading of NaOH 0 0 0 0
Volume of NaOH ( mL ) used 33.10 mL 33.00 mL 33.00 mL 33.20 mL
Ratio volume of NaOH / weight of KHP 33.06 32.84 32.84 32.90

Calculations :-

Ratio volume NaOH / weight of KHP –

𝟑𝟑.𝟏𝟎 𝒎𝑳 𝟑𝟑.𝟎𝟎𝒎𝑳
Rough = = 𝟑𝟑. 𝟎𝟔 2nd = = 𝟑𝟐. 𝟖𝟒
𝟏.𝟎𝟎𝟏 𝒈 𝟏.𝟎𝟎𝟓 𝒈

𝟑𝟑.𝟎𝟎 𝒎𝑳 𝟑𝟐.𝟐𝟎 𝒎𝑳
1st = = 𝟑𝟐. 𝟖𝟒 3rd = = 𝟑𝟐. 𝟗𝟎
𝟏.𝟎𝟎𝟓 𝒈 𝟏.𝟎𝟎𝟗 𝒈
 C. Analysis of the unknown vinegar sample

Table 4 : Result for the Unknown vinegar sample

Rough 1 2 3
Volume of unknown vinegar ( mL ) 10 10 10 10
Final reading of standard NaOH 52.0 53.0 51.0 51.0
Initial reading of standard NaOH 0 0 0 0
Volume of standard NaOH ( mL ) used 52.0 53.0 51.0 51.0

Table 5 : Calculation density of unknown vinegar

Weight of empty 50 mL beaker 29.843 g

Weight of 50 mL beaker + 10 mL unknown vinegar 39.827 g
Weight of 10 mL unknown vinegar 9.984 g

Calculations :-

𝑚𝑎𝑠𝑠 9.984 𝑔
Density of unknown vinegar = = = 0.9984 𝑔/𝑚𝐿
𝑣𝑜𝑙𝑢𝑚𝑒 10 𝑚𝐿

6.0 DISCUSSION :-

In this analysis of an unknown vinegar sample experiment , the purpose were to prepare
the sodium hydroxide solution , to standardise the base against potassium hydrogen phthalate
, KHP and to analyse the unknown vinegar sample.

While doing this experiment , we have followed all the step based on the procedure given.
In this experiment in order to analysis the unknown vinegar sample , we divided into three part
which were for part A was to prepare the sodium hydroxide solution , as for part B was to
standardise the base against potassium hydrogen phthalate and for part C was where we analyse
the unknown vinegar.

For part A which was to prepared the sodium hydroxide solution. We need to prepare 900
mL of NaOH from a stock solution of 50% ( w/w ) as its molarity was 0.25 M and its density
given was 1.525 g/mL . So, in order to determine volume that we should took from the stock
solution in order to prepare 900 mL , we can determine through the calculation. First was by
calculate number of mol of NaOH which the number of mol for NaOH was 1.25 mol. Next, as
the density of the 50 % ( w/w ) was 1.525 g/mL, we can determine the volume as the formula
for density was mass over volume. So, from the calculation the volume we got was 0.0656 L.
After that , we used molarity formula to find the concentration of the solution which the
concentration we got was 19.06 M. So that , to determine the volume of NaOH in order to
prepare 900 mL NaOH from the 50% ( w/w ) stock solution, we used dilution formula which
was M₁V₁ = M₂V₂ , and the volume we got to prepare the 900 mL solution of NaOH was 12
mL. From here , we calculate the density of the 12 mL of NaOH as the weight of the 12 mL
NaOH we can get by the difference of the 50 mL empty beaker and 50 mL beaker with 12 mL
of NaOH. The weight of the 12 mL of NaOH was 16.0259 g. So then, we calculate the density
of 12 mL of NaOH solution and the density was 1.3355 g/mL. The 12 mL of NaOH solution
was diluted with the distilled water in the clean plastic bottle.

For the next part which was for part B was to standardise the base against potassium
hydrogen phthalate , KHP. Standardization was a process to determine the exact concentration
( molarity ) of a solution. As in this experiment, titration technique was used as it was one type
of analytical procedure often used in standardization. In a titration , an exact volume of one
substances was reacted with a known amount of another substances. During the titration, the
point at which the reaction was complete in a titration was referred as endpoint. A chemical
substance known as indicator was used to indicate the endpoint as there will be the change in
colour. The type of indicator that was used in this experiment was phenolphthalein as it was
organic compound and colourless in acidic solution but pink colour in base solution. The
endpoint can be detect by the changes in the colour due to the indicator , as we can see from
the figure below :-

Figure 2 : Part B
 From the figure above , shown the appearance of pink colour shown the endpoint of the
solution. So , we can determine the volume of the NaOH used to reach the endpoint. The
volume of the NaOH used as for rough was 33.1 mL , for 1st reading was 33.0 mL , for the 2nd
reading was 33.0 mL and for the 3rd reading was 33.2 mL. Also , the weight of the KHP used
for this part also was noted as the weight for rought was 1.001 g , as for 1st reading was 1.005
g , as for 2nd reading was 1.005 g and also for the 3rd reading was 1.009 g.

Next , for part C was to analyse the unknown vinegar. For this part , the density of the
unknown vinegar was determine by using the formula density which was mass over volume.
The volume of unknown vinegar used in this experiment was 10 mL. As for the mass of the
unknown vinegar being determine by the difference weight of 50 mL empty beaker with the
weight of the 50 mL beaker contain 10 mL of unknown vinegar. From there , the weight of the
10 mL of the unknown vinegar was 9.984 g. So that, we calculate the density of the unknown
vinegar and we got the density of the unknown vinegar was 0.9984 g/mL. The result for the
titration process of the unknown vinegar can be seen below :-

Figure 3 : Part C

Lastly, every experiment there might be an error occur for an example observational error
which due to the human on how to read the reading as the eye must be perpendicular to the
instrument. Next might be source error which due to the person might record a wrong value ,
misread scale , forget a digit when reading a scale or recording a measurement. This type of
error was an outright mistake.
7.0 CONCLUSION :-

As a conclusion , 12 mL of sodium hydroxide solution was prepared and the density

of the unknown vinegar was 0.9984 g/mL.

8.0 REFERENCES :-

i) Abdullah Munir , Hamzah & Md Yunus ( 2018 ). Analytical Chemistry –

laboratory manual.
ii) Eddy, D. (n.d.). Retrieved March 18, 2019, from
http://www.chem.latech.edu/~deddy/chem104/104Standard.htm

9.0 QUESTION and ANSWER :-

i) Explain how weighing by difference eliminates systematic 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

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

Because the calculations are based on the volume of acid you put in the flask before you
dilute it, not after. You have the same moles of acid, regardless of how much water is also
present.