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Department of Chemical Engineering

College of Engineering
Bicol University
Legazpi City

Experiment 3 in Chemistry for Engineers

“Introduction to Titration”

A Laboratory Report

John Kimuel M. Bello


Aura Marie Dawn Sabucor
B.S. ChE-1A
Group 5

Engr. Jun-jun A. Pajara


Instructor
Experiment 3 in Chemistry for Engineers
Introduction to Titration
I. Objectives

A. To be introduced to the titration process.


B. To determine the concentration of Acetic Acid in a Vinegar solution.

II. Materials.
Materials / Apparatus Quantity
Burette setup 1
5mL Volumetric Pipet 2
250mL Erlenmeyer Flask 4
1L Volumetric Flask 1
25mL Volumetric Flask 1
50mL Beaker 2
Analytical Balance 1
50mL Graduated Cylinder 1
Funnel 1
Dropper 1
Chemical Reagents Amount MSDS
4% Concentrated Can cause eyes, skin and
20mL gastrointestinal irritation
Vinegar (D.S. brand)
Can cause eye and skin
burns. Causes digestive
Sodium hydroxide 4g and respiratory tract
burns. Hygroscopic.
Not classified for physical
Distilled water 500mL or health hazard.
Can cause serious eye
irritation. May cause
genetic defects. May
cause cancer. May
damage fertility or the
unborn child. May cause
Phenolphthalein respiratory irritation. May
0.5g cause drowsiness or
Powder
dizziness. Causes
damage to organs
through prolonged or
repeated exposure.
Highly flammable liquid
and vapor.
Can cause severe eye
irritation. Flammable
liquid and vapor. Causes
respiratory tract irritation.
This substance has
95% Ethanol caused adverse
25mL reproductive and fetal
Solution effects in humans. May
cause central nervous
system depression. May
cause liver, kidney and
heart damage. Causes
moderate skin irritation.

III. Procedure

A. Preparation of reagents.
1. 1L of 0.1M Sodium hydroxide
a. The amount of Sodium hydroxide in grams was calculated as shown in the equation
below.
0.1𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 39.997𝑔 𝑁𝑎𝑂𝐻
( ) (1𝐿) ≈ 4𝑔 𝑁𝑎𝑂𝐻
1𝐿 1𝑚𝑜𝑙 𝑁𝑎𝑂𝐻
b. 4g of Sodium hydroxide was weighed using the analytical balance.
c. The weighted sodium hydroxide was transferred to a beaker and then dissolved to a
small but significant amount of distilled water.
d. Through a funnel, the solution was then transferred to a 1L volumetric flask and diluted
to a 1L solution.
e. The diluted solution was distributed to each group in beakers.
2. Phenolphthalein indicator
a. 0.125g of phenolphthalein powder was weighed out.
b. 12.5mL of 95% ethanol was measured.
c. The prepared amount of phenolphthalein was thoroughly dissolved to the 12.5mL
ethanol in a beaker.
d. The solution was then transferred to a 25mL volumetric flask and was diluted with
distilled water to a 25mL solution.
e. The prepared indicator was distributed to each group.

B. Setting-up for titration


1. Rinsing the apparatuses
a. We rinsed the inside of the burette with distilled water and made sure the tip was also
rinsed by draining out the water through it.
b. Then, we also rinsed its entire inner surface with a small amount of the diluted Sodium
hydroxide solution by continually twirling the burette diagonally.
c. We filled the burette with a significant amount of Sodium hydroxide solution by
slowly pouring it from the beaker over a funnel and then flushed it over the sink right
after.
d. We also rinsed our pipets with distilled water and then with the vinegar sample for
the second and final rinse.
These steps were done to prevent or at least heavily minimize contamination that may
arise due to the previous usage of both the burette and the pipets.
2. Preparing the titrant
a. We made sure that the burette’s dropper was locked by turning its knob horizontally.
b. We held the burette over the sink and below eye level.
c. The burette was filled with 50mL of the titrant which was the Sodium hydroxide
solution from the beaker and through the funnel.
However, the burette that we received was faulty and was leaking despite the knob being
turned horizontally, so we resorted to manually blocking the gradual leakage by holding a
plastic cap against its tip until our preparations were complete.
3. Preparing the analyte
a. The volumetric pipet was used to transfer 5mL of the vinegar sample to each of the
four clean Erlenmeyer flasks.
b. The solutions in the Erlenmeyer flasks were diluted with 20mL distilled water to make
a 25mL solution.
c. 5 drops of the prepared phenolphthalein indicator were then dropped to each flask.
d. We also labelled each flask with numbers one to four.
At this juncture, we were misinformed by our classmates that the phenolphthalein
indicator was already prepared so we then dropped the presumed indicator to our analyte
setups. However, we were later told that what we had dropped in our setups was pure
ethanol and the phenolphthalein powder was yet to be mixed, therefore we had to rinse
the flasks and redo the setups of the analyte. Fortunately, our second attempt at preparing
the analyte setups had gone smoothly and well with the proper phenolphthalein indicator
utilized.

C. Performing titration
1. The members present had one attempt in performing the titration in our corresponding
samples. Katherine was first, followed by Kimuel, Rez, and lastly Lance. We first made
a table consisting of our names, the initial and final volumes of the titrant, the total change
in volume for each titration done, and the final coloration of each sample. The data table
prepared is shown below.

Member Initial Volume of Final Volume of Change in Volume


NaOH NaOH of NaOH Final Color
Katherine
Kimuel
Rez
Lance
2. We then swirled the flask below the burette as drops of the titrant trickled to the solution.
The knob was turned vertically to trickle and horizontally to stop.
3. Subtle pink coloration gradually appeared at the surface of the solutions as more drops
of the titrant was mixed with the analyte. However, the color immediately dispersed into
the liquid and disappears.
4. When the pink color was evident and did not disappear, we then only added the titrant
drop by drop until the color of the vinegar solution reached the standard light pink color.
5. When the titrant in the burette ran out for the last sample, we simply recorded its
remaining volume, titrated the last sample and then refilled the burette to a certain
recorded amount and continued titrating until done.
6. After performing the titration and recording the data required, we rinsed our glassware,
collected all the liquids we used in a waste bottle, wiped our countertops clean, and
returned our apparatuses in the instrumentation room.

IV. Presentation and Analysis of Data

A. Performance Results

Member Initial Volume of Final Volume of Change in Volume


NaOH NaOH of NaOH Final Color
Katherine 50mL 35mL 15mL
Kimuel 35mL 19.5mL 15.5mL
Rez 19mL 3.5mL 15.5mL
Lance 23.5mL 12.5mL 11mL
The table above shows the recorded data based on the performance of each
present group member. Between the second and third titration, the titrant lost a total
volume of 0.5mL due to unsought leakage. For the final titration, we had to refill the burette
by 20mL of the titrant because the remaining base solution would not had been enough.
Katherine’s sample was over-titrated due to her colorblindness that she wasn’t able to
discern when the titration should come to a halt. Everyone else’s results were in close
proximity to each other and to the standard expected color. However, the final coloration
in our samples deviated relative to other groups because the vinegar that we used had a
brownish yellow color. Our samples were less transparent and contained a hint of orange
derived from the vinegar’s initial coloration, which was most apparent in Lance’s sample.
The discrepancies between the results in each setup must had been due to the
unexecuted standardization for the Sodium hydroxide titrant which should had been
observed in order to allow for more precise and better results.

B. Post Lab Questions


1. What is the purpose of the indicator?
The indicator serves the purpose of making the equivalence point in titrations
apparent to the eye so that the person performing the titration may discern whether
more drops of the titrant should be added or the titration should be halted. Without an
indicator in an acid-base titration, there would not be an evident and active signal of
the acid-base neutralization.
2. The phenolphthalein was added to the acetic acid. To which solution did the indicator
react to, the base or to the acid?
Typically, the indicator should react to the titrant when gradually being mixed
with the analyte, such as in the experiment when the vinegar solution slowly progressed
into a pinkish color as it was being neutralized by the Sodium hydroxide; because
naturally, phenolphthalein is colorless in acidic solution and pink in basic solutions.
Therefore, the phenolphthalein turned pink because it reacted to Sodium hydroxide
which was the titrant and the base.

3. How does the indicator help/interfere with the reaction of Acetic acid and Sodium
hydroxide?
As aforementioned in the answer to the previous question, when phenolphthalein
is imparted to a base, it becomes pink. Ergo, the neutralization of Acetic acid and
Sodium hydroxide may easily be distinguished when a light pinkish color begins
manifesting in the Acetic acid due to an increasing presence of base which is the Sodium
hydroxide.

4. From the experiment, what is the molarity of Acetic acid? Show all necessary calculations.
Shown below is the balanced chemical equation for the chemical reaction between
the Acetic acid and the Sodium Hydroxide.
HC2H3O2(aq) + NaOH(aq) → NaC2H3O2(aq) + H2O(l)
The mole ratio of both the Acetic acid and Sodium Hydroxide is one-to-one.
therefore, to find the molarity of Acetic acid, use the formula: (derived from
M1V1=M2V2)
𝑀𝐵 𝑉𝐵
𝑀𝐴 = where: MA = Molarity of Acid (Acetic acid)
𝑉𝐴 MB = Molarity of Base (Sodium hydroxide)
MB = 0.1M
VA = Volume of Acid (Acetic acid)
VA = 25mL
VB = Volume of Base (Sodium hydroxide)

For the first set-up (Katherine’s sample); VB = 15mL:


(0.1𝑀)(15𝑚𝐿)
𝑀𝐴 = = 𝟎. 𝟎𝟔𝟎𝑴
25𝑚𝐿
For the second set-up (Kimuel’s sample); VB = 15.5mL:
(0.1𝑀)(15.5𝑚𝐿)
𝑀𝐴 = = 𝟎. 𝟎𝟔𝟐𝑴
25𝑚𝐿
For the third set-up (Rez’ sample); VB = 15.5mL:
(0.1𝑀)(15.5𝑚𝐿)
𝑀𝐴 = = 𝟎. 𝟎𝟔𝟐𝑴
25𝑚𝐿
For the fourth set-up (Lance’s sample); VB = 11mL:
(0.1𝑀)(11𝑚𝐿)
𝑀𝐴 = = 𝟎. 𝟎𝟒𝟒𝑴
25𝑚𝐿
5. What would be the molarity of Acetic acid if you use Barium hydroxide instead of Sodium
hydroxide? How about Lithium hydroxide. Show all necessary calculations.
Shown below is the balanced chemical equation for the chemical reaction between
the Acetic acid and the Barium Hydroxide.
2HC2H3O2(aq) + Ba(OH)2(aq) → Ba(C2H3O2)2(aq) + 2H2O(l)
The mole ratio of the Acetic acid to the Barium hydroxide is two-to-one, therefore
relate the moles of the reactants find the molarity of the Acetic Acid.
𝑀𝐵 𝑉𝐵 𝑚𝑜𝑙𝐴 where: molA = mole of Acid (Acetic acid) = 2mol
𝑀𝐴 = 𝑉𝐴 𝑚𝑜𝑙𝐵 molB = mole of Base (NaOH) = 1mol
For the first set-up; VB = 15mL:
(0.1𝑀)(15𝑚𝐿)(2𝑚𝑜𝑙)
𝑀𝐴 = = 𝟎. 𝟏𝟐𝟎𝑴
25𝑚𝐿(1𝑚𝑜𝑙)
For the second set-up; VB = 15.5mL:
(0.1𝑀)(15.5𝑚𝐿)(2𝑚𝑜𝑙)
𝑀𝐴 = = 𝟎. 𝟏𝟐𝟒𝑴
25𝑚𝐿(1𝑚𝑜𝑙
For the third set-up; VB = 15.5mL:
(0.1𝑀)(15.5𝑚𝐿)(2𝑚𝑜𝑙)
𝑀𝐴 = = 𝟎. 𝟏𝟐𝟒𝑴
25𝑚𝐿(1𝑚𝑜𝑙)
For the fourth set-up; VB = 11mL:
(0.1𝑀)(11𝑚𝐿)(2𝑚𝑜𝑙)
𝑀𝐴 = = 𝟎. 𝟎𝟖𝟖𝑴
25𝑚𝐿(1𝑚𝑜𝑙)
Shown below is the balanced chemical equation for the chemical reaction between
the Acetic acid and the Lithium Hydroxide.
HC2H3O2(aq) + LiOH(aq) → LiC2H3O2(aq) + H2O(l)
The mole ratio of the Acetic acid to the Barium hydroxide is two-to-one, therefore
the computations would simply be the same as with Sodium hydroxide.
For the first set-up; VB = 15mL:
(0.1𝑀)(15𝑚𝐿)
𝑀𝐴 = = 𝟎. 𝟎𝟔𝟎𝑴
25𝑚𝐿
For the second set-up; VB = 15.5mL:
(0.1𝑀)(15.5𝑚𝐿)
𝑀𝐴 = = 𝟎. 𝟎𝟔𝟐𝑴
25𝑚𝐿
For the third set-up; VB = 15.5mL:
(0.1𝑀)(15.5𝑚𝐿)
𝑀𝐴 = = 𝟎. 𝟎𝟔𝟐𝑴
25𝑚𝐿
For the fourth set-up; VB = 11mL:
(0.1𝑀)(11𝑚𝐿)
𝑀𝐴 = = 𝟎. 𝟎𝟒𝟒𝑴
25𝑚𝐿
6. Can you perform a titration to which the acid is the titrant and the base is your analyte?
(the concentration of acid is known while the concentration of base is unknown). Why or
why not? And if yes, briefly discuss how would you prepare for its titration.
Yes, since acid-base titration is basically a manifestation of neutralization used to
determine the unknown concentration of either the acid or the base as the analyte, using
another solution of polar pH level to the analyte as the titrant. In such instance of an
unknown base concentration or in other words a basic analyte and an acidic titrant, methyl
orange indicator is recommended for it is initially yellow in basic solutions and
progresses into a stronger orange color as it arrives at the equivalence point when titrating.
In order to prepare a such titration, fill the burette with the acidic solution of a known
concentration as the titrant (standardize if necessary), and then put certain amount of the
basic solution with an unknown concentration in an Erlenmeyer flask and add five drops
of the indicator. Begin the titration by gradually adding drops of the acidic titrant to the
basic analyte. If methyl orange indicator was used, the initial yellow color of the analyte
solution should turn orange as it approaches the equivalence point. Once it reaches the
standard color, the titration is complete.

7. What are the other indicators available for titration? Give an example to which titration
you can use each of your listed indicators.
Aside from phenolphthalein, there are two other well-known indicators for acid-
base titration such as litmus and methyl orange.
Litmus is a weak acid which is blue in an alkaline solution and red in an acidic
solution. It used to be commonly utilized in titrations with Sulfuric acid, Hydrochloric acid,
and Nitric acid as acid titrants; and Potassium carbonate and Sodium carbonate as basic
titrants
Methyl orange is a weak acid as well which is yellow in alkaline solutions and red
in acidic solutions used in strong acid-strong base and strong acid-weak base titrations.
Shown in the table below are other indicators and their color change intervals in
pH as well as their colors in acidic and basic conditions.

Color change interval


Indicator (pH) Acid Base
thymol blue 1.2 - 2.8 red yellow
methyl red 4.4 - 6.2 red yellow
chlorophenol red 5.4 - 6.8 yellow red
bromothymol blue 6.2 -7.6 yellow blue
phenol red 6.4 - 8.0 yellow red
thymol blue 8.0 - 9.6 yellow blue
alizarin yellow 10.0 -12.0 yellow green
8. For the simplicity of our experiment, we did not standardize the Sodium hydroxide
solution, but it is highly recommended. Briefly explain why it is important.
In order to compute for the unknown concentration of an analyte with
precision, it is essential to accurately determine the concentration of the titrant. Due to
the absorptive properties and tendencies of Sodium hydroxide, such as its tendency to
absorb water in the air in its solid form and, carbon dioxide gas – which is a weak acid –
in its aqueous state, the accurate measurement of quantities derived from the titration or
the visibility of the equivalence point may be subjected to errors, although quite minimally
but significant. Standardization prevents or at least minimizes errors and
discrepancies in acquiring data from the stoichiometry of the reaction.

9. How do you standardize Sodium hydroxide?


To standardize Sodium hydroxide, titrate its aqueous solution with Potassium
hydrogen phthalate which is a standard acid that can easily be measured out into a
known number of moles. With a basis of 0.1M NaOH titrant, weigh 0.8g of dried KHP into
an Erlenmeyer flask, and dissolve in 50-75mL of distilled water. Then, add 4 drops of the
indicator into the flask and titrate it with NaOH. Lastly, with the formula below, calculate
the molarity of NaOH.
1𝑚𝑜𝑙 𝐾𝐻𝑃 1𝑚𝑜𝑙 𝑁𝑎𝑂𝐻
𝑚𝑎𝑠𝑠(𝑔)𝐾𝐻𝑃 ( )( )
204.23𝑔 1𝑚𝑜𝑙 𝐾𝐻𝑃
𝑀𝑁𝑎𝑂𝐻 =
𝐿 𝑁𝑎𝑂𝐻 𝑢𝑠𝑒𝑑

10. Consider a 0.586M aqueous solution of Barium hydroxide, Ba(OH)2(aq).


a. How many grams of Ba(OH)2 are dissolved in 0.191dL of 0.586M Ba(OH)2(aq)?
0.586𝑚𝑜𝑙 Ba(OH)2 171.34𝑔 Ba(OH)2 1𝐿
( ) (0.191𝑑𝐿) ( ) = 𝟏. 𝟗𝟏𝟕𝟕𝒈 𝐁𝐚(𝐎𝐇)𝟐
1𝐿 1𝑚𝑜𝑙 Ba(OH)2 10𝑑𝐿
b. How many individual hydroxide ions are found in 13.4mL of 0.586M Ba(OH)2(aq)?
0.586𝑚𝑜𝑙 Ba(OH)2 1𝐿 2𝑚𝑜𝑙 𝑂𝐻 + 6.022𝑥1023 𝑖𝑜𝑛𝑠 𝑂𝐻 +
(13.4𝑚𝐿) ( )( )( )
1𝐿 1000𝑚𝐿 1𝑚𝑜𝑙 Ba(OH)2 1𝑚𝑜𝑙 𝑂𝐻 +
= 𝟗. 𝟒𝟓𝟕𝟒𝒙𝟏𝟎𝟐𝟑 𝒊𝒐𝒏𝒔 𝑶𝑯+
c. What volume (in L) of 0.586M Ba(OH)2(aq) contains 0.466 ounces of Ba(OH)2 dissolved
in it?
1
= 𝟎. 𝟏𝟑𝟏𝟔𝑳
0.586𝑚𝑜𝑙 Ba(OH)2 171.34𝑔 Ba(OH)2 1 1𝑜𝑧
1𝐿 ( ) ( )(
0.466𝑜𝑧 28.3495𝑔 )
1𝑚𝑜𝑙 Ba(OH)2
11. Suppose you added 40mL of water to your vinegar sample instead of 20mL, would the
titration require more, less, or the same amount of NaOH(aq) for a complete reaction?
Explain.

Hypothetically, it should require less amount of the titrant due to the analyte having
significantly lesser concentration. However, in accordance with the calculations below,
only the same amount of the Sodium hydroxide titrant was necessary. Since the
vinegar was supposedly diluted, only the molarity changed but the number of moles
remained as is. Considering the fact that the number of moles of the solute do not change
in the solution despite the amount it was diluted to, the number of moles of the titrant
required to neutralize it would remain constant as well.
Volume of NaOH required as observed from the experiment:
For the first set-up
(0.060𝑀)(25𝑚𝐿)
𝑉𝐵 = = 𝟏𝟓𝒎𝑳
(0.1𝑀)
For the second set-up
(0.062𝑀)(25𝑚𝐿)
𝑉𝐵 = = 𝟏𝟓. 𝟓𝒎𝑳
(0.1𝑀)
For the third set-up
(0.062𝑀)(25𝑚𝐿)
𝑉𝐵 = = 𝟏𝟓. 𝟓𝒎𝑳
(0.1𝑀)
For the fourth set-up
(0.044𝑀)(25𝑚𝐿)
𝑉𝐵 = = 𝟏𝟏𝒎𝑳
(0.1𝑀)

Molarity of Acetic acid with modified analyte volume:


For the first set-up
(0.1𝑀)(15𝑚𝐿)
𝑀𝐴 = = 𝟎. 𝟎𝟑𝟑𝑴
45𝑚𝐿
For the second set-up
(0.1𝑀)(15.5𝑚𝐿)
𝑀𝐴 = = 𝟎. 𝟎𝟑𝟒𝑴
45𝑚𝐿
For the third set-up
(0.1𝑀)(15.5𝑚𝐿)
𝑀𝐴 = = 𝟎. 𝟎𝟑𝟒𝑴
45𝑚𝐿
For the fourth set-up
(0.1𝑀)(11𝑚𝐿)
𝑀𝐴 = = 𝟎. 𝟎𝟐𝟒𝑴
45𝑚𝐿
Volume of NaOH required with modified analyte volume:
For the first set-up
(0.033𝑀)(45𝑚𝐿)
𝑉𝐵 = = 𝟏𝟓𝒎𝑳
(0.1𝑀)
For the second set-up
(0.034𝑀)(45𝑚𝐿)
𝑉𝐵 = = 𝟏𝟓. 𝟓𝒎𝑳
(0.1𝑀)
For the third set-up
(0.034𝑀)(45𝑚𝐿)
𝑉𝐵 = = 𝟏𝟓. 𝟓𝒎𝑳
(0.1𝑀)
For the fourth set-up
(0.024𝑀)(45𝑚𝐿)
𝑉𝐵 = = 𝟏𝟏𝒎𝑳
(0.1𝑀)
V. Conclusion

A. Titration is the process of determining an unknown amount of a substance in a sample


by gradually adding a standard solution with another substance of definite amount to
which the substance of unknown amount is expected to react to in a known and definite
proportion. The substance with a known amount is called the titrant which is placed in
the burette while the desired constituent is called the analyte which put in the Erlenmeyer
flask. In acid-base titrations, the addition of the titrant to the analyte is eventually halted
when the equivalence point of the acid and the base is reached which is signaled by an
appropriate indicator that morphs in color when subjected to acidic and alkaline conditions.
Standardization of the titrant is essential before titrating with the analyte so that
discrepancies can be eluded. Moreover, the concentration of the analyte does not affect the
quantity of titrant required in reaching the equivalence point so long as the moles of solute
remain constant in the analyte solution.
B. In order to determine the amount of Acetic acid in a vinegar solution, one has to perform an
Acid-base titration which involves the use of Sodium hydroxide or other strong bases as
the titrant to neutralize the solution so that the unknown concentration may be computed
using the quantity of the base required for the neutralization. A phenolphthalein indicator
is recommended due to its nature of being colorless in an acidic environment and pinkish in
alkaline conditions which makes the equivalence point in the titration apparent. To compute
for the acetic acid concentration, multiply the molarity of the titrant to the its volume required
to reach the equivalence point and then divide by the initial volume of the vinegar solution.
References

Belford, R. (2019, June 5). 17.3: Acid-Base Titrations. Retrieved October 27, 2019, from
https://chem.libretexts.org/Courses/University_of_Arkansas_Little_Rock/Chem_1403:_General
_Chemistry_2/Text/17:_Aqueous_Equilibria/17-3:_Acid-Base_Titrations.
Clark, J. (2013, November). Acid-base Indicators. Retrieved October 27, 2019, from
https://www.chemguide.co.uk/physical/acidbaseeqia/indicators.html.
Emon, S. H. (2017, December 15). Why do we standardize NaOH? Retrieved October 27, 2019, from
https://www.quora.com/Why-do-we-standardize-NaOH.
The Editors of Encyclopaedia Britannica. (2017, October 6). Titration. Retrieved October 27, 2019, from
https://www.britannica.com/science/titration#ref55408.
Titrant Standardization. (n.d.). Retrieved October 27, 2019, from
https://www.chromacademy.com/lms/sco735/03-Titrant-
Standardization.html?fChannel=22&fCourse=97&fSco=735&fPath=sco735/03-Titrant-
Standardization.html.

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