Acid-Base Titration Lab

I. Research Question:
How can the unknown concentration of a sodium hydroxide (NaOH) solution be
determined using 10.0 cm3 of 0.1 mol dm-3 hydrochloric acid (HCL) solution?

II. Introduction:

Background Information:

Analytical chemistry is the science of obtaining, processing, and communicating

information about the composition and structure of matter. In other words, it is the art
and science of determining what matter is and how much of it exists.

Titration is a widely used technique in the field of analytical chemistry. It allows us to

find the concentration of an unknown solution (analyte) using a solution whose
concentration we know (titrant), To determine the concentration of an alkali like
sodium hydroxide in this lab, we can use a known concentration of acid, like
hydrochloric acid. This type of titration is called an acid-base titration. The type of
reaction taking place is a neutralisation reaction, where salt and water are products of
the reaction:

Acid + Base → Salt + Water

In this experiment:

HCl + NaOH → NaCl + H2O

We can use an acid-base indicator, a chemical that changes colour depending on the
pH of a solution, to indicate the end-point of the reaction (when the reaction is
complete). The point where all of the base in the analyte has been completely used is
called the equivalence point. This is the point when the solutions have been mixed in
exactly the right stoichiometric proportions to complete the reaction. Using an
appropriate indicator ensures we can get as close as possible to the equivalence point
of the reaction. (This colour change actually happens slightly after equivalence, but
the pH change is so rapid that the volume difference usually doesn’t matter).

This lab will use phenolphthalein the pH range of which can be found in section 22 of
the data booklet. It is pink when present in basic solutions and colourless in acidic
solutions. This lab represents a strong acid-strong base titration making
phenolphthalein suitable as the pH change would take place within a fraction of a
drop of actual neutralisation, since the strength of the base is high. The higher the pH,
the stronger the pink colour. The end-point will be when the faintest pink colour
persists for at least fifteen seconds. Keep your flask with acid and indicator over a
white piece of paper to ensure you can see the colour change.

Titration reactions are not always acid-base reactions - they may be REDOX
reactions, precipitation reactions, or synthesis (combination) reactions. A colour
change is also not the only way to determine the end-point of the reaction. It can also
be determined by a change in electrical conductivity of the reaction mixture, by the
formation of a precipitate, or by a variety of other means.

III. Hypothesis:
If an unknown sodium hydroxide (NaOH) solution is titrated with 10.0 cm3 of 0.1 mol
dm-3 hydrochloric acid (HCl) solution, a pH indicator can be used to indicate the
endpoint of the titration, and the concentration of NaOH can be determined by
calculations with the titre.

IV. Variables

Independent Variable Dependent Variable

Concentration and volume of HCl Concentration of NaOH solution

solution

Controlled Variable How it will be kept controlled

Temperature The experiment is done in the same room, at room

temperature

Concentration and 10.0 cm3 of 0.1 mol dm-3 solution of HCl will be used for
volume of HCl each trial

Stirring speed The flask will be swirled by the same person continuously at
a moderate speed

Time taken stirring The endpoint of the titrations will be determined by if the
to determine colour from the pH indicator remains after stirring for 15
endpoint of titration seconds

V. Material/Apparatus:

● Burette ● The unknown NaOH solution

 ● Clamp-stand and burette clamp ● 0.1 mol dm-3 Hydrochloric acid
● White tile/paper solution (standard)
● 10 cm3 volumetric pipette or ● Phenolphthalein indicator
graduated pipette ● Wash bottle with distilled water
● Pipette filler
● 100 cm3 or 250 cm3 conical
Erlenmeyer flask
● Burette funnel
● 3 x 100 cm3 beakers (labelled waste,
for HCl and NaOH)

VI. Safety, Environment, Ethics:

● Treat all solutions as harmful and in case of skin contact rinse the affected area
immediately.
● Always wear goggles
● All solutions can be safely disposed of down the sink
● Small volumes of solutions are being used to minimise waste

VII. Methodology/Procedure:

1. ​Securely attach a burette to a clamp-stand, and place a white tile/paper on the base
to help with identifying colour changes.

2. Rinse all glassware with distilled water then:

a. Rinse one beaker with NaOH and the other with HCl solution.

b. Rinse burette with the HCl solution.

c. Rinse the pipette with NaOH solution.

d. The conical flask should not be rinsed with either solution, it can remain
wet.

3. Making sure the tap is closed, fill the burette with the unknown NaOH solution, until
slightly above the zero mark. Remove any air bubbles and adjust the volume. Be sure to
remove the hanging drop at the tip of the burette by touching the tip to the inside of the
waste beaker. Record the initial burette reading in your data table.

4. Using either a bulb-pipette, or a graduated pipette, add exactly 10.0 cm3 of your HCl
solution to a conical flask, along with 3 or 4 drops of phenolphthalein indicator.
5. Create a data table similar to that above in google docs or excel (do not forget to note
uncertainties).

6. Perform your rough titration.

e. Run the solution into the conical flask at a steady rate (about 1 cm3) every
3-4 seconds
f. Swirl the conical flask in a continuous circular motion (don’t shake it as this
causes splashes to form on the side making it less accurate)
g. Close the tap as soon as the pink colour of phenolphthalein remains for 15
seconds, and note the final volume in the table. Calculate the titre.
h. Pour your waste into the sink, and rinse the conical flask with distilled
water.

7. Perform your accurate titrations:

i. If you have significantly more base remaining in the burette than your
calculated titre it is not necessary to re-fill the burette, simply adjust the
volume to the nearest whole cm3 and record this in the table under ‘initial
volume’.

j. Run your solution into the flask rapidly until you are within 2-3 cm3 of
your rough titre and then stop.

k. Carefully open the tap, until you have about 1 drop per second. As you
approach the end-point, use the ‘tip to flask’ technique you were shown,
rinsing with the wash bottle each time.
l. The end-point will be when the solution becomes pink color
m. Pour your waste into the sink, and rinse the conical flask with distilled
water.
n. Repeat until you have two consecutive titres within an acceptable
uncertainty (WHAT IS THAT UNCERTAINTY? Add the uncertainty in
your burette and pipette, there you go).

Calculate the average titre; this should be the average of your two closest runs
(those within the calculated uncertainty). Always exclude the rough titre.

Rinse the burette with one complete rinsing with tap water, followed by another
rinsing with distilled water. Place the burette securely upside-down, with the
stopcock left open.
 VIII. Data:

Trial # volume of Initial Final Titre of Volume of Average

HCL (ml) volume of Volume of NaOH(ml) mixture Titre of
NaOH (mL) NaOH (mL) (ml) NaOH (mL)

1 10 50 47.8 2.2 12.2

2.2 + 2.3 + 2.4
2 10 50 47.7 2.3 12.3 3

3 10 50 47.6 2.4 12.4 = 2.3

IX. Analysis

Determining the experimental value of the concentration of NaOH:

HCl + NaOH → NaCl + H2O
Concentration = n/v
𝑛𝐻𝑐𝑙= 𝑛𝑁𝑎𝑂𝐻= 𝐶𝐻𝑐𝑙 × 𝑉𝐻𝑐𝑙= 0. 1 · 0. 01 = 0.001 mol
𝑛𝑁𝑎𝑂𝐻 0.001
𝐶𝑁𝑎𝑂ℎ = 𝑉𝑁𝑎𝑂𝐻
= 0.0023
= 0.43478260869 ≈ 0.435
−1 −3
𝐶𝑁𝑎𝑂ℎ ≈ 4. 35 · 10 𝑚𝑜𝑙 𝑑𝑚

Propagation of Uncertainties:
−3
Uncertainty of burette: ± 0. 1 𝑚𝑙 = ± 0. 0001 𝑑𝑚
−3
Uncertainty of pipette: ± 0. 1 𝑚𝑙 = ± 0. 0001 𝑑𝑚

𝑎
𝑖𝑓 𝑦 = 𝑏
,
△𝑦 △𝑎 △𝑏
𝑡ℎ𝑒𝑛 𝑦
= 𝑎
+ 𝑏
.
𝑛𝑁𝑎𝑂𝐻
𝑆𝑖𝑛𝑐𝑒 𝐶𝑁𝑎𝑂ℎ = 𝑉𝑁𝑎𝑂𝐻
,
△𝐶𝑁𝑎𝑂ℎ △𝑛𝑁𝑎𝑂𝐻 △𝑉𝑁𝑎𝑂𝐻 △𝑛𝑁𝑎𝑂𝐻 △𝑉𝑁𝑎𝑂𝐻
𝑡ℎ𝑒𝑛 𝐶𝑁𝑎𝑂ℎ
= 𝑛𝑁𝑎𝑂𝐻
+ 𝑉𝑁𝑎𝑂𝐻
, or △𝐶𝑁𝑎𝑂ℎ = 𝐶𝑁𝑎𝑂ℎ × ( 𝑛𝑁𝑎𝑂𝐻
+ 𝑉𝑁𝑎𝑂𝐻
).
△𝐶𝐻𝐶𝑙 △𝑉𝐻𝐶𝑙
and △𝑛𝑁𝑎𝑂𝐻 = 𝑛𝐻𝐶𝑙 × ( 𝐶𝐻𝐶𝑙
+ 𝑉𝐻𝐶𝑙
) = ± 0.000011 mol
0.000011 0.0001
So, △𝐶𝑁𝑎𝑂ℎ = 0. 435 × ( 0.001
+ 0.0023 ) ≈ ± 0.0483 mol dm-3
𝑢𝑛𝑐𝑒𝑟𝑡𝑎𝑖𝑛𝑡𝑦 0.0483
Percentage uncertainty = 𝑚𝑒𝑎𝑠𝑢𝑟𝑒𝑑 𝑣𝑎𝑙𝑢𝑒
= 0.435 × 100 ≈ 11.1 %

Questions:
1) The actual concentration of the sodium hydroxide solution is 0.8 mol dm-3.
Calculate the percentage error in your result.
 |𝑚𝑒𝑎𝑠𝑢𝑟𝑒𝑑−𝑟𝑒𝑎𝑙|
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝐸𝑟𝑟𝑜𝑟 = 𝑟𝑒𝑎𝑙
× 100
|0.435−0.8|
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝐸𝑟𝑟𝑜𝑟 = 0.8
× 100 = 45.6%

2) Compare the percentage error with the overall percentage uncertainty.

Comment on this.

The percentage error was 45.6%, meaning that the calculated value was significantly
different from the true value. Also, the percentage uncertainty was 11.1%, indicating
that there were some sources of measurement uncertainty. From these values, it can be
concluded that the results of this experiment are not very reliable or accurate, and
since the percentage error is much larger than the percentage uncertainty, it suggests
that there were significant sources of error that need to be addressed in future
experiments.

X. Conclusion

Hypothesis: If an unknown sodium hydroxide (NaOH) solution is titrated with 10.0

cm3 of 0.1 mol dm-3 hydrochloric acid (HCl) solution, a pH indicator can be used to
indicate the endpoint of the titration, and the concentration of NaOH can be
determined by calculations with the titre.

Validity of hypothesis:
The validity of the hypothesis that an unknown sodium hydroxide (NaOH) solution
can be titrated with 0.1 mol dm-3 hydrochloric acid (HCl) solution, using a pH
indicator to determine the endpoint of the titration, and the concentration of NaOH can
be calculated from the titre, depends on several factors, including the accuracy and
precision of the experimental method used and the quality of the reagents and
equipment used.

Assuming that the experiment was conducted under standard laboratory conditions,
using calibrated glassware, accurate balances, and fresh reagents, the validity of the
hypothesis can be assessed by comparing the experimental result obtained with the
actual value of the concentration of NaOH.

In this case, the experimental result of 0.435 M is significantly lower than the actual
value of 0.8 M. This suggests that there may have been errors in the experimental
method or the measurement of the titre, which will be further discussed in the next
section.
Possible sources of error could include incorrect preparation or measurement of the
solutions, improper use of the pH indicator, errors in reading or recording the
volumes, or incomplete or uneven mixing of the solutions.

To ensure the validity of the hypothesis, it is important to repeat the experiment

multiple times, using different techniques and conditions, to confirm the accuracy and
precision of the results. Additionally, it may be necessary to use more precise
analytical methods, such as gravimetric analysis or spectrophotometry, to confirm the
concentration of NaOH.

In conclusion, while the hypothesis that an unknown NaOH solution can be titrated
with HCl solution and the concentration of NaOH can be calculated from the titre
using a pH indicator is a valid method, the accuracy and precision of the results
depend on several factors and must be carefully evaluated and confirmed by multiple
experiments and analytical techniques.

XI. Evaluation:

What do you think are the main sources of error in the titration were?

1. Incorrect measurement of the volumes of solutions used can happen if the

measuring instruments are not calibrated properly, or if the person conducting
the experiment does not read the volumes accurately.
2. If either the sodium hydroxide or hydrochloric acid solution contains
impurities, it can affect the accuracy of the titration. This can happen if the
solutions are not properly prepared or stored.
3. the reaction between the NaOH and HCl may not be complete, which can lead
to an incorrect determination of the concentration of the NaOH solution.
4. Air bubbles in the burette or pipette can lead to inaccurate volume
measurements, which can affect the accuracy of the titration.
5. The amount of phenolphthalein added was not accurately measured, which
could make it more difficult or inaccurate to measure the endpoint of the
titration

What do you think are the main sources of error in the making a standard
solution?

Inaccurate measurements can happen when equipment is not properly calibrated or

clean. For example, a balance that's not calibrated correctly could lead to incorrect
readings, or using a measuring cylinder that's not clean can result in inaccurate
volume measurements. Impurities in the solute or solvent can also affect concentration
measurements, as they can change the mass or density of the solution. Additionally,
temperature can also impact concentration measurements, as it can affect the volume
of the solvent and the solubility of the solute. Errors can occur when diluting the
standard solution, due to problems with mixing, evaporation, or inaccurate volume
measurement. Finally, incomplete reactions between the solute and solvent can lead to
inaccuracies in the concentration measurement.

Which sources of error are most significant?

For titration:
The volume measurements of the NaOH and HCl solutions may not be exact, or the
pH indicator used could be flawed. The NaOH and HCl solutions may also react
slowly or incompletely, leading to inaccurate results. If the concentrations of the
NaOH and HCl solutions are not measured accurately, this can also cause errors in the
titration results.

For making standard solutions:

Errors can occur due to issues with measuring equipment, such as inaccuracies in
mass or volume measurements. Impurities in the solute or solvent used can also affect
the concentration measurement. Incomplete solute dissolution, temperature
fluctuations, and problems with dilution can also lead to errors in the preparation of
the standard solution.

What could you do to reduce two of these sources of error? – RESEARCH

ONLINE

1. To improve errors because of inaccuracies of volume measurements, it should be

made sure that the equipment is clean and dry before using them. Additionally, larger
volumes of the solutions could be used to reduce the relative error, as the error will be
small compared to the amount. Lastly, the volume should be read carefully at eye level
at the bottom of the meniscus in the burrette.

2. To improve errors because of incomplete or slow reaction, a magnetic stirrer could

be used instead of mixing by holding the beaker, as some of the body heat could be
transferred and warm up the beaker, changing the rate of reaction, and also by using a
human to stir, the speed and consistency of stirring may be inaccurate. Also, the titrant
should be added slowly so that the endpoint of the titration is more accurate.

XII. Extension:

How would it affect your results if you used a beaker with residual water in it to
measure out your standardized hydrochloric acid solution?
Using a beaker with residual water in it to measure a hydrochloric acid solution can
lead to inaccurate results because the water can dilute the solution, making it less
concentrated than intended. This can cause the calculated concentration of the solution
being titrated with the HCl solution, the NaOH solution, to be lower than the actual
concentration. To prevent this from happening, it is crucial to use clean and dry
equipment when measuring out solutions. If a beaker with water droplets is used, it
should be rinsed with the solution being measured to make sure all the water is
removed before measuring out the solution.

In the procedure (2d) it stated that ‘The conical flask should not be rinsed with
either solution’. Why?
It is important not to rinse the conical flask with either of the solutions during the
experiment as it can affect the concentration of the solution being titrated and lead to
inaccurate results. Even if the flask is rinsed thoroughly, residue from the previous
solution may remain, altering the concentration. To avoid these errors, a clean and dry
conical flask should be used for each titration. This ensures that the concentration of
the solution being titrated is consistent and the results obtained are reliable.

Why does the residual water in the flask not change anything?

The reason why residual water in the conical flask usually does not affect the accuracy
of titration results is that water is distilled water so it does not react with the solutions
used in the experiment. Additionally, the amount of residual water is usually small
compared to the volume of solution added during titration, so it can be negligible.
However, because this experiment uses small volumes of the solutions, it is better to
minimise the residual water as it is less negligible than if larger volumes were being
used.

When performing titrations, why should the analyte be constantly stirred?

Stirring the analyte during titration experiments is important to ensure that the reaction
occurs evenly and completely. It helps to mix the analyte and titrant thoroughly,
minimising variations in concentration that could affect the accuracy of the results.
Constant stirring allows for more precise measurements and reliable outcomes.

Why should you perform an acid/base titration many times?

Performing an acid/base titration multiple times increases the accuracy of the results
by identifying variations and errors in the experiment. Repeating the experiment helps
to obtain a more reliable measurement of the concentration of the solution being
analysed.
Can I titrate a solution of unknown concentration with another solution of
unknown concentration and still get a meaningful answer? Explain your answer
in a few sentences.

When titrating two solutions of unknown concentrations, it is possible to determine

whether the solutions are acidic, basic, or neutral based on pH changes. However, it is
not possible to calculate the exact concentrations of the solutions. If both solutions are
acidic or basic, it may be possible to estimate the relative concentrations based on the
volume of titrant needed to reach the endpoint. These estimates are not very accurate,
so they should be used with caution.