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TRAYA, CLYDE CHLOE D.

BSE BioSci II

ANALYTICAL CHEMISTRY

EXPERIMENT 6
Standardization of NaOH against KHP
I.OBJECTIVES
At the end of the experiment, the students will be able to:
1. Perform standardization of NaOH with the use of KHP
2. Apply techniques in titration
II. MATERIALS
Equipments:
Polyethylene bottle
Burette
Burette stand and clamp
Conical flask
Crucible with cover
Spatula
Graduated cylinder
Wash bottle
Dropper
Reagents:
Distilled water
50% NaOH
Potassium hydrogen phthalate
Phenolphthalein indicator
III. PROCEDURE
1. As usual, before starting any experiment, the students prepared themselves - they wore laboratory
gowns, tying back of long hairs and the materials needed were prepared as well the glassware
were washed thoroughly and rinsed with distilled water.
2. Carbonate-free Sodium hydroxide solution was prepared.
a. 50% NaOH solution was first prepared by adding 12.5g NaOH to 25mL water in a conical flask.
Extra care was applied to keep NaOH from coming contact with skin.
b. Then, 1L of distilled water was poured into a polyethylene bottle and was added with 6-7mL of
50% NaOH. The prepared solution was given attention so that it wont get any unnecessary
contact with the atmosphere to prevent carbon contamination present in air, it was covered.
3. NaOH was then standardized.
a. A quantity of primary-standard KHP was dried for 2 hours at 100 OC in an oven and then was
cooled in the desiccators.
b. 0.7-0.8g of the dried primary-standard KHP sample was weighed into a 250mL Erlenmeyer
flask and dissolved with 50-70mL distilled water by swirling the flask. 2 drops of
phenolphthalein was then added.
c. The solution in the Erlenmeyer flask was then titrated with the 50% NaOH by letting the 50%
NaOH drain drop by drop into the flask until the faint pink color was achieved.
4. The concentration of the NaOH solution used up during titration was then calculated using the formula:

M=

mass of KHP x 1000


volume of NaOH used x 204.3

IV. DATA/TABLE
Table 1. Preparation of the Carbonate-free NaOH
Mass of NaOH
12.5g
Volume of Distilled Water in the Conical Flask
25mL
Volume of water for stirring
10mL
Table 2. Standardization of NaOH
Mass of KHP
Number of phenolphthalein drops
Volume of water used for dissolving in beaker

TRIAL NO.
1
2
3

0.7g
2 drops
50mL

Table 3. Buret Reading


Initial Reading (mL)
Final Reading (mL)
0.00mL
47.2
2(0.00mL)
63.3
2(0.00mL)
59.3

V. RESULTS
Table 1 shows the data about the reagents used in preparing the Carbonate-free Sodium
hydroxide.12.5g of NaOH was placed inside a beaker and was added with 10mL of water to swirl and
dissolve the solid NaOH 15mL distilled was then added to complete the 25mL distilled water needed to
make the 50% Carbonate-free Sodium hydroxide.
Table 2 illustrates the amount of reagents used for the standardization of NaOH. For the three
trials, the group used 0.7g KHP, 2 drops of phenolphthalein, and 50mL distilled water constantly.
Table 3 showcases the recorded buret readings. For trial 1, 47.2mL of NaOH was used up. For trial
2, the buret the filled with 50mL NaOH twice and the total amount used up was 63.3mL. for the last trial,
trial 3, the buret was filled with 50mL NaOH twice too and the total amount used up was 59.3mL.
NaOH concentration calculation for every trial:
M =0.054 1
mass of KHP x 1000
M=
TRIAL 2:
volume of NaOH used x 204.3
mass of KHP x 1000
M=
volume of NaOH used x 204.3TRIAL 3:
0.7 g x 1000
mass of KHP x 1000
M=
M=
47.2 mL x 204.3
volume of NaOH used x 204.3
0.7 g x 1000
M=
63.3 mL x 204.3
700
0.7 g x 1000
M=
M=
964.96
59.3 mL x 204.3
700
M=
12932.19
M =0.072 6

TRIAL 1:

M=

700
12114.99

M =0.0578 VI. DISCUSSION/QUESTIONS


1. What is a primary standard reagent?
A primary standard is a reagent that is extremely pure, stable, has no waters of hydration, and has a
high molecular weight.
2. What is the purpose of standardizing NaOH solution?
Solid sodium hydroxide is hygroscopic, which means that it absorbs moisture from the atmosphere.
Once it has a little moisture it also absorbs carbon dioxide which is always present in air. The reaction
is:
2 NaOH (s) + CO2 (g) Na2CO3 (aq) + H2O (l)
Therefore solid reagent grade sodium hydroxide is not pure enough to weigh directly. Furthermore, the
carbonate ion interferes in acid-base titrations because 1) it is a base, and 2) it tends to make the color
change at the end point less sharp. This reaction also takes place in the aqueous phase, where sodium
hydroxide in solution is converted to sodium carbonate. This can change the concentration of standard
solutions if steps are not taken to minimize the carbon dioxide uptake. It is therefore necessary to prepare
sodium hydroxide solutions in such a way that they are free of carbonate impurity, NaOH must be
standardized. The most convenient method takes advantage of the fact that sodium carbonate is insoluble
in 50 % NaOH solution. Carbonate free solutions can be obtained simply by diluting 50 % NaOH.
3. Why do you protect the NaOH solution from unnecessary contact with the atmospheric air?
The NaOH solution must be protected from unnecessary contact with the atmospheric air because the
solution will absorb carbon dioxide which is always present in the atmosphere. If even a little moisture
can make the NaOH solutions absorb carbon dioxide, much more when its already in solution form.
VII. CONCLUSION
I therefore conclude NaOH must first be standardized in order to achieve accurate results in acid-base
titrations. If NaOH is not standardized, results of acid-base titration can have discrepancies caused by carbonate
impurity.
VIII. REFERENCES
http://web.pdx.edu/~atkinsdb/teach/321/NAOH.htm
http://wiki.answers.com/Q/How_do_you_prepare_a_50_percent_solution_of_sodium_hydroxide_sol
ution_from_97_percent_sodium_hydroxide_pellets
http://elchem.kaist.ac.kr/vt/chem-ed/analytic/standard.htm

TRAYA, CLYDE CHLOE D.

BSE BioSci II

ANALYTICAL CHEMISTRY

EXPERIMENT 7
Determination of Acid Content of Vinegar
I. OBJECTIVES
At the end of the experiment, the students will be able to:
1. Determine the acid content of the vinegar.
2. Enhance their skill in titration.
II. MATERIALS
Equipments:
Pipette and aspirator
Graduated cylinder
Volumetric flask
Conical flask
Dropper
Burette
Buret stand and clamp
Reagents:
Phenolphthalein indicator
Distilled water
Vinegar sample
0.1 M NaOH solution
III. PROCEDURE
1. The glassware to be used in the experiment were first washed and were rinsed with distilled water to avoid
contamination from impure water.
2. 25.0mL of Branded vinegar - the group used Silver Swan was measured using graduated cylinder and was
pipetted into a 250mL volumetric flask and was diluted with distilled water by filling the volumetric flask up to the
marking on its neck and was covered and mixed thoroughly.
3. 50mL was pipetted from the dilute solution into another Erlenmeyer flask and was added with 50mL of distilled
water. Two drops of phenolphthalein was added to the solution.
4. Titration was then performed. The buret was filled with 0.1 M NaOH and NaOH was allowed to drain drop by
drop into the solution in the volumetric flask until the permanent color of light pink was achieved.
5. The amount of 0.1 M NaOH used up to achieve the faint pink color of the solution inside the volumetric flask
was recorded. The initial and the final reading were observed and recorded. The procedure was repeated up to
3 trials.
6. The steps 2-5 was repeated but with an unbranded vinegar, a Tuba.
V. DATA/TABLE
Table 1. Data and results obtained for the Branded Vinegar
TRIAL
Initial
Volume of Vinegar
Volume
Volume of
Solution
Titrated

NaOH
1
50mL
50mL
36.2 mL
2
50mL
25mL
18.5 mL
3
50mL
25mL
22 mL
average
50mL
33.33mL
25.6mL
Table 2. Data and results obtained for the Unbranded Vinegar - Tuba
Initial Volume Volume of Vinegar
Volume
TRIAL
of NaOH
Solution
Titrated
1
50mL
25mL
19 mL
2
50mL
25mL
19.2 mL
3
38mL
25mL
22.7 mL
average
46
25mL
20.3mL
V. RESULTS
The first vinegar being used was a branded one. 50mL of it was first tested. After achieving the faint color of
pink, the total volume used up showed to be 36.2mL for the first trial. 25mL of vinegar was used for the second trial
which used up 18.5mL to achieve faint pink color. For the third trial, 22mL of NaOH for 25mL of vinegar was used.
The second vinegar being used was an unbranded one. 25mL of it was first tested. After achieving the faint
color of pink, the total volume used up showed to be 19mL for the first trial. 25mL of vinegar was used for the
second trial which used up 19.2mL to achieve faint pink color. For the third trial, 22.7mL of NaOH for 25mL of
vinegar was used.
Branded Vinegar
moles of acid initially present =molarity of base x volume of base adde d

moles of acetic acid initially present=

0.1 m
1L
NaOH x 25.6 mL NaO H x
L
1000 mL

moles of acetic acid initially present=0.00256 mol


The molecular formula of acetic acid is CH 3CO2H with a molar mass of:
g
60.0
mol

The grams of acetic acid in 33.33 mL of vinegar is:


60.0

g
x 0.00256 mol acetic acid initially present=0. 1536 g
mol

0. 1536 g
g
x 100=0. 4608
33.33 mL
mL
Unbranded Vinegar

- Acidity of the branded vinegar as percent (w/v)

moles of acid initially present=molarity of base x volume of base adde d

moles of acetic acid initially present=

0.1 m
1L
NaOH x 20.3 mL NaO H x
L
1000 mL

moles of acetic acid initially present =0.00203 mol

The molecular formula of acetic acid is CH 3CO2H with a molar mass of:
g
60.0
mol

The grams of acetic acid in 25.00 mL of vinegar is:


60.0

g
x 0.00203 mol acetic acid initially present=0. 1218 g
mol

0.1218 g
g
x 100=0. 4872
25 mL
mL

- Acidity of theunbranded vinegar as percent (w/v)

VI. DISCUSSION
Acetic acid reacts with sodium hydroxide, a base, according to the reaction:
CH3CO2H
acetic
acid
(an acid)

+ NaOH
sodium
hydroxide
(a base)

H2O +

CH3CO2Na

water

sodium acetate

water

(a salt)

(1)

This is an example of an acid-base neutralization reaction in which an acid and a base react to produce water plus a
salt.
In the titration method, base is added to the acetic acid solution until just enough base has been added to completely
react with all of the acid. The point where just enough base has been added to neutralize the acid is called
the equivalence point. According to reaction (1), one mole of base reacts with one mole of acid. Therefore, at the
equivalence point we have the relation:
moles of base added = moles of acid initially present
moles of base added = molarity of base x volume of base added
and therefore:
moles of acid initially present=molarity of base x volume of base adde d

VII. CONCLUSION
I therefore conclude, the amount of NaOH used up to neutralize the CH 3CO2H present in the vinegar
solution is equal to the amount of the CH3CO2H present in the vinegar solution.
VII.REFERENCES
http://wwwchem.csustan.edu/consumer/vinegar/analysis.htm

TRAYA, CLYDE CHLOE D.

BSE BioSci II

ANALYTICAL CHEMISTRY

EXPERIMENT 8
Determination of Percent Citric Acid in Fruit Juices
I. OBJECTIVES
At the end of the activity, the students will be able to:
1. Know how to determine the percentage of citric acid in fruit juices
2. enhance the skills they acquired in titration
II. MATERIALS
Equipments:
Buret
Buret stand and clamp
Erlenmeyer flask
Beaker
Wash bottle
Graduated cylinder
Reagents:
Distilled water
1.1 M NaOH solution
Phenolphthalein indicator
Fresh fruit juice
III.PROCEDURE
1. Before everything else, the students first got themselves ready wearing the laboratory gowns, and tying back of
long hairs. The glassware were washed too.
2. 100mL Fresh fruit juice was extracted from Pomelo by peeling the fruit first and rupturing the pulps in order for
the juice from the pulps to go out. The juice was then filtered into a beaker with filter paper.
3. 10.00mL of the filtered juice was then pipetted into a Erlenmeyer flask and was diluted with 80mL distilled
water. 0.3mL of phenolphthalein was then added using a pipette.

4. The diluted fruit juice with phenolphthalein was then titrated. 0.1 M NaOH filling the burette was allowed to flow
down into the solution in the Erlenmeyer flask until a light color of pink was achieved. Steps 3-4 were then
repeated 4 times for concordant results.
IV. DATA/TABLE
TRIAL NO.
1
2
3
4
average

Table 1. Buret Reading for amount of NaOH used up


Initial Reading (mL)
Final Reading (mL)
Volume titrated (mL)
50
48.4
1.6
48.4
46.9
1.5
46.9
45.2
1.7
45.2
43.6
1.6
1.6

V.RESULTS
Table 1 shows the data recorded during titration. For the first trial, 1.6mL was use up until faint pink color
was achieved. The second trial consumed 1.5mL, the third trial used up 1.7mL, and 1.6mL for the fourth trial.
% Citric Acid Determination Calculation
moles of acid initially present=molarity of base x volume of base adde d

moles of citric acid initially present=

0.1 m
1L
NaOH x 1.6 mL NaO H x
L
1000mL

moles of citric acid initially present=0.00 016 mol

The molecular formula of Citric Acid is H3C6H5O7 with a molar mass of:
g
192.0
mol

The grams of citric acid in 10.00 mL of fruit juice is:


192.0

g
x 0.00 016 moles of citric acid initially present=0. 03072 g
mol

0.03072 g
g
x 100=0.3072
10 mL
mL

- Acidity of the vinegar as percent (w/v)

VI.DISCUSION
In the case of the citric acid titration, a known amount of orange juice is measured into an Erlenmeyer flask
with an indicator solution containing phenolphthalein (the indicator). Sodium hydroxide, at a known concentration, is
then carefully added into the sample until all of the acid has reacted. When all of the acid has completely been
neutralized, the addition of 1 additional drop of the sodium hydroxide solution, the titrant, causes the solution to
become basic. The basic solution will be marked by the appearance of a pinkish color in the solution of orange juice.
The device used to add the titrant (NaOH) to the juice sample is called a buret. It allows one to measure the
exact amount of solution added during the titration. Knowledge of this, the concentration of NaOH solution in

moles/liter, and the known Stoichiometry of the reaction allows one to calculate the citric acid concentration in the
juice sample.
moles of acid initially present=molarity of base x volume of base adde d
VII. CONCLUSION
I therefore conclude that in order to determine the percent citric acid in a particular fruit juice, acid-base
titration can be performed. Neutralization reaction that occurs enables one to determine the concentration of the
acid present in the solution since the amount of the known base needed to neutralize the acidity of the solution is
equal to the amount of the unknown acid present in a particular solution.
VII.REFERENCES
http://en.wikipedia.org/wiki/Acid%E2%80%93base_titration
http://chemlab.truman.edu/CHEM100Labs/THE%20DETERMINATION%20OF%20CITRIC
%20ACID.pdf