CHM 421

ANALYTICAL CHEMISTRY

EXPERIMENT 2 :

ANALYSIS OF AN UNKNOWN VINEGAR SAMPLE

NAME : OMMY MADINA BINTI ABDUL HALIM

STUDENT NUMBER : 2019295426

GROUP NUMBER : RAS2451A

LECTURER’S NAME : MOHD HAFIZ BIN YAAKOB

DATE EXPERIMENT : 30 SEPTEMBER 2019

DATELINE EXPERIMENT : 14 OCTOBER 2019

Abstract :

The first step of the experiment is to prepare the sodium hydroxide solution which is
important to the next part of the experiment.It will prepare 800 mL of approximately of 0.25M
NaOH by diluting a prepared stock solution of approximately 50% (w/w) NaOH by mass.Next
,the experiment is to standardise the base against potassium hydrogen phthalene using the
technique weighing by difference.The most important things is to make sure that the accurate
weight of KHP.The last objective is to analyse the unknown vinegar sample.10.0 mL vinegar was
pipetted into a dry pre-weighed 50 mL beaker.The beaker was reweighed. 10.0 mL vinegar
sample was pipette from the beaker into a clean 250 mL conical flask. Three drops of
phenolphthalein indicator was added into one of the titration vessels and the contents was
titrated to endpoint with the standardized NaOH solution.The percentage of acetic acid is
3.02%.
Objectives:
1.To Prepare the Sodium Hydroxide solution.

2.To Standardise the base against Potassioum Hydrogen Phthalane.

3.To Analyse the Unknown Vinegar Sample.

Introduction:
Standard solution is a solution that can know the exact concentration in the experiment
while primary standard is a solute that have weighable and high purity.An accurately weighed
primary standard is dissolved in the desired solvent and diluted to an accurately known final
volume in a volumetric flask and the volumetric flask will inverted a few times so that the
solution become homogeneous solution.

Firstly,this experiment will prepare the approximate concentration of sodium hydroxide

solution.Sodium hydroxide can absorbs moisture and rapidly exposed to the air.So it only can
determined by standardising the solution against potassium hydrogen phthalene (KHP).The
standardized sodium hydroxide solution is to determined the acetic acid content of a vinegar
sample.

Secondary standard solution is an approximate concentration of the solution that get

from the reagent of first prepared which is the to determined the true
concentration.Standardisation is can obtained by titrating the prepared solution against a
measured of primary standard substance or direct analysis for the reagent that interest by some
non-volumetric method.
Method:

A. Preparation of the Sodium Hydroxide Solution.

In this Preparation of the Sodium Hydroxide solution part,approximately 0.25 M will

prepared 800 mL of sodium hydroxide by diluting a laboratory prepared solution of
approximately 50% (w/w) NaOH.The density of the commercially prepared stock solution of
50%(w/w) NaOH is 1.525 g/ mL .The density of the 50% (w/w) NaOH prepared in the laboratory
may be slightly different.

The rough density of the prepared 50% NaOH was determined by measuring the mass 10
mL solution.A dry and empty 50 mL beaker was weighed.10 mL of the NaOH solution was
measured in cylinder and was transferred it to the pre-weighed beaker.The beaker was
reweighed.The difference in weight gives the weight of 10 mL 50% NaOH prepared in this
laboratory.Using the density of the prepared 50% NaOH,the volume of the stock solution
required was calculated to prepare 800 mL of approximately 0.25 M sodium hydroxide solution.

About 400 mL of distilled water was placed into a clean plastic bottle.Using the
dropper,was measured into the graduated cylinder, the volume of the stock NaOH solution
required was calculated.Then carefully the contents of the cylinder was poured into the partially
filled plastic bottle.The cylinder was rinsed out a fe times with the fresh distilled water and all
rinse into the contents of the plastic bottle.The cap on the plastic bottle was screwed and the
contents was mixed thoroughly by carefully and vigorously inverting the bottle and swirling it
repeatly.Finally,the remaining volume of water was added in three batches,the contents in the
bottle was mixed thoroughly each time.The bottle should be shaken at least 20 times after last
addition.
B. Standardisation of the Base against Pottasium Hydrogen Phthalene.

Firstly, the container containing the primary standard was weighed.Then,some of the
solute was removed and was placed it in a container.The original container and the residual
content was reweighed.The difference between the two values gives the mass of the solute
removed.If the weight of the solute removed has not yet reached the desired weight,repeat the
process.

Accurately,about 1g sample of dry primary-standard grade potassium hydrogen

phthalate (KHP) was weighed on to a weighing boat.The KHP has been dried earlier in oven at
110⁰C for 2 hours and stored in a desicator prior to use.

Use the appearance of the above,1g of sample as guide to accurately weigh two more
such sample by difference.Quantitatively,each sample from the weighing boat was transferred
into a 250 mL conical flask.Then,35 mL of water was added to each flask and the flask was
swirled gently until the solid dissolve.Any drops of the sample solution was rinsed on the side
walls of the flask with distilled water.

A 50 mL burette tip was rinsed and filled with the NaOH solution to standardise.The air
bubble was removed before adjusting the initial volume and the titration was started.The
stopcock was turned quickly 360° a few times until air bubbles are removed.Then,the initial
volume was adjusted.The actual starting volume was read and recorded to the nearest 0.02 mL.

Three drops of phenolphthalein indicator was put into the first conical flask.The flask
under burette was placed and lowered the burette tip well into it.A piece of a white tile was
placed under the flask,the flask was holded with your right hand,the stopcock of the burette
was controlled with your left hand and the titration was started by carefully turning the
stopcock to let a gentle and steady stream of titrant flow into the acid

solution.Gently,the solution was swirled in the flask.Then first permanent faint pink point colour
that persists for at least 20 seconds is the end point.
 The stopcock was closed and the contents of the ‘titration thief ’ was removed into the
flask.The pink colour should now disappear.The dropper was rinsed a few times with the
solution in the flask to ensure all KHP is removed into the flask.The dropper was taked out from
the conical flask.The dropper was rinsed and the sides of the flask with distilled water,and then
continue added the titrant drop wisely this time.The flask was swirled after each drop or ½ drop
addition of solution in the burette.When the permanent pale pink colour persists in the
solution,the titration was stopped.The final burette reading was recorded to the nearest 0.02
mL.The remaining two KHP samples was titrated.

C. Analysis of the Unknown Vinegar Sample .

Firstly,the density of the vinegar sample was determined. 10.0 mL vinegar was pipetted
into a dry pre-weighed 50 mL beaker.The beaker was reweighed.The difference will give the
weight for 10 mL vinegar sample.More vinegar was taked into 50 mL beaker for titration. 10.0
mL vinegar sample was pipette from the beaker into a clean 250 mL conical flask.Two more
such sample was prepared.The side of each flask was washed down with 25 mL water from the
wash bottle.Three drops of phenolphthalein indicator was added into one of the titration
vessels and the contents was titrated to endpoint with the standardized NaOH solution from
Part B .The process was repeated for another two sample.

Clean Up

Any remaining solution was discarded from the burette.The burette was rinsed with distilled
water.Then,the inverted burette was returned to the burette stand,leaving the stopcocock
open.All the glassware was washed and cleaned and was returned to the storage
location.Wiped oof afrom any mess and spills.
Results :

A. Preparation of the Sodium Hydroxide Solution

Volume of NaOH taken from the 50% stock solution = 13.6025 mL

B. Standardisation of the Base against Pottasium Hydrogen Phthalene.

Rough 1 2
Weight of KHP (g) 1.0304 1.0044 1.0074
Final reading of NaOH 28.50 28.70 29.10
Initial reading of NaOH 0.00 0.00 0.00
Volume of NaOH (mL) used 28.50 28.70 29.10
Ratio mol of NaOH / mol of KHP 1:1 1:1 1:1
Table 1 : Data of Standardisation of the Base against Pottasium Hydrogen
Phthalene.
C. Analysis of the Unknown Vinegar Sample

Density of Vinegar sample = 1.004 g/mL

Rough 1 2
Volume of unknown vinegar (mL) 9.9545 10.0089 10.1609
Final reading of standard NaOH 15.80 13.20 12.90
Initial reading of standard NaOH 0.00 0.00 0.00
Volume of standard NaOH (mL) used 15.80 13.20 12.90

Table 2 : Data of Analysis of the Unknown Vinegar Sample

Calculation :

A.Preparation of the Sodium Hydroxide Solution

 Mass of beaker 46.1404 g

Mass of beaker and NaOH 57.9029 g

Mass of NaOH = 57.9029 g - 46.1404 g

= 11.7625g

Table 3 : Data of weighing by difference

Density of NaOH = Mass of NaOH / Volume of NaOH

= 11.7625g / 10 mL

=1.17625 g/ mL

Molarity = 1.17625 x 1000/1 x 1 mol/ 40 x 50/100

= 14.7031 M

M1V1=M2V2

(14.7031)(V1) = (0.25)(800)

V1 = (0.25)(800)

14.7031

= 13.6025 mL

B. Standardisation of the Base against Pottasium Hydrogen Phthalene

Equation :

NaOH + KHP KNAP + H2O

Molar mass of KHP : 204.23

At balanced equation : 1 mole of KHP need to 1 mole of NaOH

ROUGH :

Number of moles = Mass

Molar Mass

= 1.0304 / 204.23

= 5.045 x 10-3 mol

At balanced Equation : 1 mol of KHP is equal to 1 mol of NaOH

Molarity = Number of moles of NaOH

Volume of NaOH

=5.045 x 10-3 mol / 28.50 X 10-3

= 0.17 M

1:

Number of moles = 1.0044 / 204.23

= 4.918 x 10-3 mol

Molarity =4.918 x 10-3 mol / 28.70 X 10-3 = 0.17 M

2:

Number of moles = 1.0074 / 204.23

= 4.9233 x 10-3 mol

Molarity =4.9233 x 10-3 mol / 29.10 X 10-3 = 0.17 M

C. Analysis of the Unknown Vinegar Sample

NaOH + CH3COOH CH3COO-Na+ + H2O

Mass of 50 mL beaker + 10 .00 mL Vinegar (g) 40.5829 40.6373 40.7893

Mass of 50 mL beaker (g) 30.6284 30.6284 30.6284
Mass of 10 .00 mL Vinegar (g) 9.9545 10.0089 10.1609

Average of Mass of 10.00 mL Vinegar (g) = 10.0414 g

Density of vinegar sample = 10.0414 g / 10.00 mL

Table 4 : Data of Analysis of the Unknown Vinegar Sample
= 1.004 g/mL

At balanced Equation :

1 mol of CH3COOH need 1 mole NaOH to produce 1 mole of CH3COO-Na+ + H2O

5.045 x 10-3 mol of CH3COOH need 5.045 x 10-3 mole NaOH to produce mole of CH3COO-Na+
+ H 2O

ROUGH :

Moles = Mass

Molar Mass

5.045 x 10-3 mol = Mass / 60.02

Mass = 0.3028 g

Percentage weight / weight = Mass of acetic acid (g)

Mass volume of Vinegar (g)
 = 0.3028 g / 10.0414

= 0.0302 x 100

= 3.02 %

Discussion:

In the Part A of this experiment,it will prepare the sodium hydroxide solution because
sodium hydroxide solution cannot prepared by primary standard because it easily to absorb
with the water and carbon dioxide from the air.Next,in this experiment will determine the exact
concentration the base against potassium hydrogen phthalene.It is because potassium
hydrogen phthalene (KHP) is easily weighed and not react with the any components.To calculate
the exact concentration it should know the mass of KHP that get during weighing by difference
method aginst the molar mass of the KHP which 204.23 g/mol.

The KHP and NaOH is reacted together until completedly dissolved make the solution
become pale pink which end point.

In the Part C of this experiment,it will analyse the unknown vinegar sample which is
vinegar is one of the actic acid that is monoprotic acid with the molar mass is 60.02 g/mol.The
data from the average molarity of NaOH solution and the density of the vinegar sample,it can
calculate the percentage w/w of acetic acid in the original unknown vinegar solution.

Briefly the possible sourse of errors in this experiment make the result does not
match with the theoretical especially during the titration.The technique of titration is
continuously repeated with the each of the sample that make the rough , 1 and 2 is 0.17 M.The
concentration should be 0.25M.The reading is not perpendicular with the burette reading which
called parallex errors.Next,the solution not fully swirled in the conical flask make the end point
less accurate.Moreover,the bubble at the tip of burette can cause the different of endpoint.

The errors may affected the result and should be avoided.There are some improvement
that can be done during the experiment.Firstly,make sure that the reading is perpendicular with
the eye’s level.Secondly,the solution must be swirled completely so that the reading of end
point is more reliable and accurate.Lastly,turn the stopcock quickly 360° a few times until all
bubble are removed then adjust the initial volume.

Conclusion :

The sodium hydroxide solution is prepared in this experiment.The standardise the base
against potassium hydrogen phthalene is 0.17 M in the Part B while in the Part C is to analyse
the unknown vinegar sample .The density of vinegar sample is 1.004 g/ mL and the percentage
weight by weight of the experiment is 3.02%.

References :

Idayu Razali (n.d) Analytic AL. Retrieved October 13,2019 from

https://www.academia.edu/7725773/Analytic_AL

Santa.M.C (June 6,2019) Titration of Vinegar .Retrieved October 13,2019 from

https://chem.libretexts.org/Ancillary_Materials/Laboratory_Experiments/Wet_Lab_Experiments
/General_Chemistry_Labs/Online_Chemistry_Lab_Manual/Chem_10_Experiments/11%3A_Titration_of_
Vinegar_(Experiment)

Sazrina.M.S (Dec 17,2011).Vinegar .Retrieved October 13,2019 from

https://www.scribd.com/doc/75915552/Lab-Report-Vinegar

Question:

1.Explain how weighing by difference eliminates systematic balance errors ?

Because the mass difference between two reading which is systematic error will obsolutely get
the true weight of the object.
2.Why does it not matter how much water you add when dissolving the acid (KHP) or when
carrying out the titration?

The weight of KHP that have been weighed can obtain the moles of KHP.Water does not
increasing or decreasing the mass of KHP present which not effect the reaction.So adding the
more water into the KHP does not effect the experiment.