LAB REPORT CHM 421

LECTURERS NAME : PUAN SITI NOORASHIKIN JAMAL

EXPERIMENT NO : 2
TITLE : ANALYSIS OF UNKNOWN ACETIC ACID SOLUTION

DATE OF SUBMISSION:

EXPERIMENT
SOLUTION

2 :

ANALYSIS

OF AN

UNKNOWN

ACETIC ACID

Abstract :
This experiment were carry out to analysis the unknown acetic acid
solution. In order to further the experiment, it is important to prepare the
sodium hydroxide, NaOH solution. In this part, we had to prepared 1 litre
of approximately 0.25 M NaOH solution by diluting a prepared stock
solution of approximately 50% NaOH by mass. Experiment also asked
about to standardise the NaOH as a base against Potassium Hydrogen
Phthalate(KHP). In this part, we have learned about a weighing technique
called weighing by difference. It is important to get accurate weigh of KHP.
Then, the main part for this experiment is to analysis the unknown acetic
acid solution. In this experiment, we need to find the density of vinegar
sample first. The phenolphthalein indicator is used for titration with
standardized NaOH solution.
Objectives

1. To prepare the Sodium Hydroxide Solution

2. To Standardise the Base against Potassium Hydrogen Phthalate
3. To Analysis the Unknown Acetic Acid Solution
Introduction :
In this experiment we will learned about primary standard,
standardisation and standard solution. Primary standard is a solute
which can be obtained in a very pure, stable, weighable form. Sodium
Hydroxide, NaOH is not a primary standard because it is hygroscopic
meaning that it absorbs moisture rapidly when expose to air. Thus its
accurate concentration can only be determined by standardising the
solution against a very pure potassium hydrogen phthalate, KHC 8H404
(KHP) in a series of replicate titrations. This process is called
standardisation. While, standard solution is a solution whose solute
concentration is accurately known.

Method :
(A) Preparation of the Sodium Hydroxide Solution
1. The density of the prepared 50% NaOH is determined by measuring
the mass of 10 mL solution. A dry and empty 50 mL beaker is weighed. 10
mL of the NaOH solution is pipetted and transferred to the pre weighed

beaker. The beaker is reweighed. The difference in weight gives the

weight of 10 mL 50% NaOH prepared in this laboratory. The density of the
prepared 50% NaOH is used, the appreciate volume of the stock solution
is calculated, preparation of 1L of approximately 0.25 M Sodium
Hydroxide, NaOH solution is required.
2. 400 mL of distilled water is placed into a clean plastic bottle. The
calculated volume of the stock NaOH solution is obtained using graduated
cylinder. Polyethylene dropper is used to dispensed this volume. Then, the
content is poured into the partially filled plastic bottle. The cylinder is
rinsed out a few times with fresh distilled water and all the rinses is added
into the contents of the plastic bottle. The cap on the plastic bottle is
screwed and the contents is mixed by carefully and the bottle is inverted
vigorously and swirling it repeatedly. The remaining 600 mL of water is
added in three 200 mL batches, the contents is mixed in the bottle each
time. The bottle is shakes at least 20 times after the last addition.

(B) Standardisation of the Base against Potassium Hydrogen Phthalate

1. 1 g sample of dry primary-standard grade potassium hydrogen
phthalate(KHP) is weighed on to a weighing boat. The KHP has been dried
earlier, in an oven at 110 C for 2 hours and stored in a desiccator prior to
use.
2. The appearance of the above 1 g sample is used as a guide to
accurately weigh two more such samples by difference. Quantitatively,
the first sample is transferred from the weighing boat into a 250 mL
conical flask. All the sample is made sure has been transferred by rising
the boat with a small amount of water from your wash bottle. Then, 35 mL
of water is added to each flask and swirled solution is rinsed on the side
walls of the flask with distilled water.
3. A 50 mL burette is rinsed and filled with the NaOH solution that
wished to standardize. Be very carefully with air bubbles especially at the
tip of the burette. The air bubbles is removed before adjusting the initial
volume and did the titration process. One quick stroke downward is made
beginning at the stopcock and ending in the air beyond the burette tip in
order to remove the air bubble. Did not waste time trying to hit 0.00 with
the meniscus for the starting point. Rather, went a few drops below the
zero mark and read and the actual starting volume is recorded to the
nearest 0.002 mL. Any adhering solution is wiped at the sides and tip of
the burette with the laboratory tissue before begun the titration.

4. Three drops of phenolphthalein indicator is added to the first KHP

solution. The flask is placed under the burette and the burette tip is
lowered well into it . For the first titration, it was always advisable to suck
up with a clean polyethylene dropper a `titration thief about 1 mL of the
flask contents, the dropper is leaved in the flask. In case we overshot the
first titration having not sure of the colour at the end point, this can be
used as a precaution measure. A piece of white tile is placed under flask,
the flask is hold and tilted slightly to one sight with your right hand for us
with the right handed, the stopcock of the burette is controlled with left
hand and the titration is started by carefully turning the stopcock to let a
gentle but steady stream of base flow into the pooled acid solution. The
solution is swirled gently in the flask. The base can be added fairly quickly
at first, but on the region was concentrated where the two solutions
mixed in the flask, and the pink colour which formed there begun to linger
as we swirled the flask, the flow rate is reduced from the burette. The
solution in the conical flask was first turned into a permanent faint pink,
the stopcock is closed and the contents of the ` titration thief is removed
into the flask. Now, the pink colour is disappeared. When it does not, we
had overshot the initial base addition and the titration must be discarded.
When the solution went colourless, the dropper is rinsed with the solution
in the flask several times to make sure that you have removed all the KHP
out of it, and then it took out from the conical flask. The sides of the flask
is washed down with distilled water, and then adding of base is continued
from the burette but this time drop is added wisely. When the end point is
approached, the pink colour is disappear. The walls of the flask should be
washed down from time to time so as to recover any reagent drops from
clinging to the sides. The flask is swirled after each drop or a drop
addition of solution in the burette. A drop is added by controlling and
slowly opened the stopcock until a drop forms at the tip. This drop is
washed into the flask or the 1/2 drop is touched to the wall of the flask
and sprayed with distilled water. Adding of NaOH is stopped when the
entire flask has a faint pink colour that persists for at least 20 seconds.
When we not sure of the colour at the colour at the end point, we wished
to record the burette volume of several successive drops as we had
approached the end point. By this way, we could be sure that we are not
very far from the actual end point. The final burette reading is recorded to
the nearest 0.02 mL . The burette is refilled and titrated similarly the
remaining two KHP samples.

(C) Analysis of the Unknown Vinegar solution

1. The density of the vinegar sample is determined first. Then, 40 mL of

the unknown vinegar sample is obtained in clean, dry 50 mL beaker.
2. 10.0 mL vinegar sample is pipetted into clean 250 mL conical flask.
Two more such samples is prepared. The sides of each flask is washed
down with 25 mL water from your wash bottle.
3. Three drops of phenolphthalein is added to one of the titration vessels
and titrate the contents to end point with your standardized NaOH
solution. A titration thief would probably be advisable for at least the first
titration. The process is repeated for the other two samples. Ideally, the
range of the replicate titration volumes must be only one or two drops or
about 0.2 mL the most.

Clean-up :Any remaining solution is drained from the burette. The burette washed
with the tap water. Then, the stopcock is leaving opened, the inverted
burette is returned to the burette clamp. All the other glass wares used is
wash and clean and is placed in their storage location. Working bench off
any mess and spills is wiped.

Results :
A. Preparation of the Sodium Hydroxide Solution
Volume of NaOH taken from the stock = 15.077 mL

B. Standardisation of the Base against Potassium Hydrogen Phthalate

Weight of KHP
Final volume of
NaOH (mL)
Initial volume of
NaOH (mL)
Volume of NaOH
(mL) used
Ratio volume of
NaOH/weight of

1
1.0059
36.10

2
1.0152
36.10

3
1.0024
29.00

0.00

0.00

0.00

36.10

36.10

29.00

35.888

35.559

28.931

KHP

C. Analysis of the Unknown Acetic Acid Solution

Volume of the
Unknown Acetic
Acid (mL)
Final volume of
standard NaOH
(mL)
Initial volume of
standard NaOH
(mL)
Volume of
standard NaOH
(mL) used

1
10.00

2
10.00

3
10.00

51.00

49.30

49.00

0.00

0.00

0.00

51.00

49.30

49.00

Calculation/Analysis :
(A) Preparation of the Sodium Hydroxide Solution
Mass of empty 50 mL beaker = 52.3820 g
Mass of 50 mL beaker + 10 mL NaOH solution = 65.6435 g
Mass of 10 mL NaOH = 13.2615 g

Density of NaOH, = mass (g) / volume (mL) =13.2615 g /10 mL =

1.32615 g/mL

MNaOH = (50 g/100 g )*(1 mol NaOH/39.99 gmL -1)*(1.32615 g/1

mL)*(1000 mL/1 L)
=16.581 M

Volume of NaOH required ,

M1V1 = M2V2
16.581 M*V1 = 0.25*1000 mL
V1 = 15.077 mL
(B) Standardisation of the Base against Potassium Hydrogen Phthalate
(KHP)
MNaOH = 0.25 M
Molarity of NaOH solution
Flask 1 :
M = 4.925*10-3 mol/0.0361 L
= 0.1364 mol L-1
Flask 2 :
M = 4.971*10-3 mol/0.0361 L
= 0.1377 mol L-1
Flask 3 :
M = 4.910*10-3 mol/0.0290 L
= 0.1693 mol L-1

Average MolarityNaOH = (0.1364 + 0.1377 + 0.1693 )*mol L-1/ 3

= 0.1478 mol L-1
90% confidence interval = (90/100)*0.1478
= 0.13302
Calculation for weight-percentage of acetic acid
1)

M1V1 = M2V2
M1(35) = (0.13302)*(51.00)
M1 = 0.1938 M
mol, n = 0.1938 M*0.035 L

= 6.783*10-3 mol
Mass of acetic acid = (6.783*10-3 mol)*60
= 0.4070 g
%(w/w) = (0.4070 g/40 g)*100
= 1.02 %

2) M1V1 = M2V2
M1(35) = (0.13302)*(49.30)
M1 = 0.1874 M
mol, n = 0.1874 M*0.035 L
= 6.559*10-3 mol
Mass of acetic acid = (6.559*10-3 mol)*60
= 0.3935 g
%(w/w) = (0.3935 g/40 g)*100
= 0.984 %
3)

M1V1 = M2V2
M1(35) = (0.13302)*(49.00)
M1 = 0.1862 M
mol, n = 0.1862 M*0.035 L
= 6.517*10-3 mol

Mass of acetic acid = (6.517*10-3 mol)*60

= 0.3910 g
%(w/w) = (0.3910 g/40 g)*100
= 0.976 %

Average Value of %(w/w) = (1.02 + 0.984 + 0.976)/3

= 0.9933

90% confidence interval acetic acid = (90/100)*0.9933

= 0.89397

(C) Analysis of the Unknown Acetic Acid solution

Mass of empty 50 mL beaker = 52.919 g
Mass of 50 mL beaker + 10 mL vinegar = 89.007 g
Mass of vinegar = 36.158 g

Density of vinegar, = mass/volume(mL) = (36.158 g/40 mL) = 0.904 g

mL-1
mol NaOH = (Mv/1000) = (16.581*49.77)/1000
= 0.825 mol
Molarity of acetic acid
= 0.0510 L NaOH *(0.825 mol NaOH/1 L)*(1 mol HC 2H3O2/1 mol
NaOH)*(1/0.01000 L)
= 4.208 M HC2H3O2

Discussion :
In this experiment, there are several error that we have found. The
volume of NaOH used for the trial was too high and it resulting in an
incorrectly high calculated molarity of acetic acid. Another possible source
of error would be losing some volume of vinegar when transferring the
solution from the pipet to conical flask. The lower volume of acetic acid
will affect result in a lower volume of NaOH needed to titrate it in
determining phenolphthalein end point. So, we have to assuming the
volume of vinegar transferred still to be 10.00 mL. The result for
calculated molar concentration of acetic acid be incorrectly low.

Conclusion :
In this experiment, the 90% confidence interval for the Molarity is
0.13302 and the 90% confidence interval for acetic acid is 0.89397 .

References :
1) HARGIS L.G, Analytical Chemistry , principle and techniques, 1998

Questions :
1. If you want to get accurate weight for some item. First you should
weight the an empty container you want to put item, 1 st record. Then put
on item in container and weight again, 2 ndrecord. So, you can get accurate
weight for item by subtracts the 2ndrecord to 1strecord.

2. The calculation are based on the volume of acid which are put in the
flask before diluted it. So, you can get similar number of mole of acid
before and after adding the water.