Sultan Qaboos University

College of Science
Department of Chemistry
(CHEM4441)

An exercise in
volumetric analysis

Student name : Yousef Mohammed Suliman AL-Shehhi

Student ID : 123108
Bunch number : 4 .
Date of submission : 2021-10-21 .
Objective:
1. To standardize a solution of NaOH against standard solution
KH(C8H4O4).
2. Use titration to find concentration of acetic acid in the vinegar.

Introduction:

Volumetric analysis, is one of the famous analytical method which used

to determine concentration of a analyte by a standard solution that we
already know its concentration.

Titration, That will done by titrant prepared as standard solution then

known volume and concentration of titrant with adding drops of
indicator to indicate the end point then react with the analyte to find its
concentration.

Primary standard: is chemical reagent have high percent purity, stability

toward air, high molecular mass, rapidly solubility in the solvent and
low cost. The reason why it should have stability toward air is not
change its weight due to humidity. It should be inexpensive to be more
commercial so that can use it more as that possible to achieve the aim.

Examples of primary standards used in redox titrations include pure

iron, NaC2O4, As2O3 , K2Cr2O7, KBrO3 KIO3 and KH(IO3)2 .

NaOH not consider as primary standard because its hygroscopic which

means its attracts and absorbs H2O molecules from the air so its
concentration cannot be determine directly because the Wight that
shown will not represent only but also include water and carbon dioxide.

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Therefore, NaOH will standardized through reaction by standard
solution which is KH(C8H4O4) and add drops of Phenolphthalein as
indicator.

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Now the concentration of the stock sodium hydroxide solution is known

so then use these to know amount of acetic acid in the vinegar sample
then determine the concentration.

Experimental:

Equpments:

 100ml-Beaker  50mL-conical flasks

 5ml-piptte  Analytical balance
 top loading balance  Phenolphthalein indicator
 50ml-volumetric flask  10 mL micro-burette
 250ml-volumetric flask  Plastic funnel

Chemicals:
 phenolphthalein indicator.
 distilled water
 Sodium hydroxide (NaOH).
 Standard Potassium hydrogen phthalate solution KH(C8H4O4).
 Unknown concentration vinegar (number#33).
Conditions:
 Room Temperate (approximately 25-27 oC )
 Pressure = 1 atm

Procedure:
1. Prepared 250 mL of an approximately 0.1 M solution of NaOH use
about 1.0 g of it and distilled water.
2. Prepared 50mL of 0.1M solution of KH(C8H4O4) using 1.0008 g.
3. Standardized NaOH against KH(C8H4O4) and added 2-3 drops of
phenolphthalein indicator.
4. From the balanced chemical equation got the molarity of NaOH.
5. Titration was repeated 5 times.
6. Prepared 50ml by diluted 5ml of the unknown concentration vinegar
using distilled water and standardized with NaOH and 2-3 drops of
the phenolphthalein indicator.
7. Repeated titration 3 times (on step 6)

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Results:

Solution of KH(C8H4O4) (molar mass = 204.22 g\mol )

Mass used 1.0008 g
Volume 50.00 ml
Number of moles 4.9005(9) x 10-3 mol
Concentration 0.09801(1)

\ Volume of Volume of NaOH (ml)

KH(C8H4O4)
Initial reading final reading Different
ruff 5.00 ml 0.61 6.63 6.02

1 5.00 ml 0.91 6.91 6.00

2 5.00 ml 0.31 6.42 6.11

3 5.00 ml 1.02 7.29 6.27

4 5.00 ml 0.56 6.43 5.87

5 5.00 ml 0.88 6.61 5.73

VOLUME OF NaOH Titrated with KH(C8H4O4).
\ Moles of KH(C8H4O4) Moles of NaOH Molarity
1 4.9005(5) x 10-4 mol 4.9005(5) x 10-4 mol 0.08167(5) M
2 4.9005(5) x 10-4 mol 4.9005(5) x 10-4 mol 0.08020(5) M
3 4.9005(5) x 10-4 mol 4.9005(5) x 10-4 mol 0.07815(8) M
4 4.9005(5) x 10-4 mol 4.9005(5) x 10-4 mol 0.08348(4) M
5 4.9005(5) x 10-4 mol 4.9005(5) x 10-4 mol 0.08552(4) M
Average = 0.08180(7)
The molarity of NaOH by using ratio in balance equation.

\ used volume of volume of NaOH (ml)

vinegar (ml)
Initial reading final reading Different
ruff 5.00 0.71 6.76 6.05
1 5.00 0.91 6.92 6.01
2 5.00 1.41 6.89 5.48
3 5.00 1.61 7.21 6.05
Volume of NaOH titrated with unknown vinegar

Mass of NaOH = 1.05 g

Unknown number #33
Concentration of NaOH =0.08180(7)
standard deviation of molarity NaOH = 0.002851(6)
confidence interval = 0.08180 ±0.00224 (±2.73%)
Calculations:

● KH(C8H4O4) concentration:

Mass KH(C8H4O4) = 1.008 g Molar mass KH(C8H4O4)= 204.22 g/mol

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 moles of KH(C8H4O4) reacted with NaOH:

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From the equation:

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nNaOH = n KH(C8H4O4)) = ( )

Trail 1:

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Trail2:

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 Trail3:

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Trail4:

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Trail5:

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To calculate standard deviation on the molarity of NaOH:

Mean:

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So Mean = ( )
 √∑ ( )

( ( ) ( )) ( ( ) ( )) ( ( )
√

√ ( ( ) ( )) ( ( ) ( ))
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standard deviation = 0.002851(6)

- concentration of the vinegar: Unknown #33

From equation

From trail 1:
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From trail 2:
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From trail 3:
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Mean for unknown :

∑ ( ) ( ) ( )
( )

( )

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Mass percentage:

( )
DISCUSSIONS:

The experiment about titration to standardize NaOH solution through

using KH(C8H4O4) because we cannot get the concentration of NaOH
from the mass straight way due it is properties that can absorb the water
from air that is due the hygroscopic so we use concentration of
KH(C8H4O4) to get its mass for that the NaOH will standardize with
KH(C8H4O4) for determined its concentration. From results and
calculations we can see the concentrations of NaOH and acetic acid in
the vinegars and there was random errors from me because I did not do
any titrations in last 2 years.

From results, the acetic acid concentration in vinegar was =

the percentage expected was 4-6% of acetic acid in the vinegars and
what I got that show some errors in the calculations or random errors in
the experiment.

References :

 handbook
 quantitative chemical analysis book edition 9th
 https://www.britannica.com/science/volumetric-analysis