PMCH110 (2024)

Experiment 2: Preparation of a Standard Solution for Titration Analysis

Introduction
Quantitative analysis determines the exact amount of a particular substance in a sample. This can be
done using a titration of a give sample with a solution of another substance whose concentration is
known. An indicator is sometimes used to signal the exact completion of the reaction. The indicator
chosen will have one colour before the reaction is complete and another colour when completion
occurs. After the indicator is added to the sample solution, the solution of known concentration is
delivered carefully from a burette until the indicator changes colour.

The choice of indicator is very important. You will have to search for a point in the titration at which
one (1) drop of the solution being added causes the solution being titrated to change colour. This
point is called the endpoint. The equivalence point occurs when the amounts of the two reactants are
exactly sufficient for the reaction to be complete. Obviously, one should choose an indicator that will
have its end point as close as possible to the equivalence point of the reaction. This way a solution of
given concentration is used to determine the concentration of a second solution, without questioning
the reliability of the molarity (molar concentration) of the first solution.

Experiment Objective
You will prepare a standard solution of borax (Na2B4O7.10H2O), a solid that can be obtained in a high
degree of purity. Borax is a base and can be used as a primary standard for standardizing many
different acids. You will use your standard solution of borax to titrate the HCl solution provided, and
then calculate the concentration of the HCl solution. The titration you will perform today is based on
the reaction between borax and hydrochloric acid:

Na2B4O7.10H2O (aq) + HCl (aq) → H3BO3 (aq) + NaCl (aq) + H2O

The indicator you will use for the titration is methyl red, which changes colour from yellow (in basic
solution) to red (in acidic solution).

Safety:

No Eating/ Drinking Safety Glasses Lab Coat Closed Shoes HCl and Borax are
irritants.
Avoid prolonged skin
contact.
Pre-practical Questions (Do this with your group mates from Expt. 1, before you come to the lab)
1. Balance the chemical equation for the titration (given under experiment objectives)
2. Calculate the molar mass of borax from the formula Na2B4O7.10H2O.
3. What mass of borax is needed to prepare a 0.050M borax solution with a volume of:
(a) 200.00 cm3
(b) 250.00 cm3?
Note: The volume of a standard flask is accurate to 2 decimal places. Report your answer
to the correct number of significant figures.
4. What is the purpose of a trial titration?
5. Explain why the walls of the flask are washed with de-ionized water during the titration. How
does this affect the outcome of the titration?

General Instructions
1. Collect HCl solution from the demonstrator’s bench in a clean and labelled 250 cm3 beaker.
2. Collect a test tube containing 4 to 5 g of borax from the demonstrator’s bench.
3. Check that the capacity of your standard volumetric flask is 200 cm3 that the stopper is the
correct size for it.

Experiment Procedure
Part 1: Preparation of the standard borax solution
1. Accurately weigh (to 4 decimal places) a clean, dry 100 cm3 beaker.
2. Remove the beaker from the balance and tip in some borax.
3. Reweigh the beaker and record the mass. The mass of borax is the difference between this
mass and that of the empty beaker. Ensure that you have weighed out between 3 and 3.5 g of
borax. Record this mass to 4 decimal places in your notebook.
4. Pour approximately 50 cm3 of de-ionized water into the beaker, place it on wire gauze on a
tripod, and warm it gently over a Bunsen burner. Do not allow the solution to boil.
Note: It is essential to transfer all the borax from the beaker to the volumetric flask so read
through the instructions that follow before you proceed.
5. Stir the solution with a glass rod (do not remove the rod from the solution), and when all of
the solid has dissolved, allow it to cool.
6. Rinse the glass rod with a stream of de-ionized water from your wash bottle, letting the wash
water run-off into the beaker with dissolved borax.
7. Use a funnel and a glass rod to transfer the solution quantitatively to the volumetric flask. To
do this, put a glass funnel into the neck of the volumetric flask and pour the solution in the

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 beaker through the funnel into the volumetric flask as shown in the sketch below. Use your
wash bottle to rinse the beaker thoroughly and pour the washings into the funnel. Finally rinse
the inside of the funnel to make sure that any solution sticking to the inside of the funnel also
goes into the volumetric flask.

Drawing by Karen Wallace

8. Finally, add de-ionized water to make the solution exactly up to the calibration mark (make
sure that your eye is level with the mark to prevent parallax error), using your graduated
pipette to add the last few cm3 of water dropwise.
9. If you accidentally add too much water so that the water level (the meniscus) is above the
calibration mark, you have to clean all your glassware and start from the beginning.
10. Stopper the flask and invert it at least five times to ensure thorough mixing of the solution.
Calculate the molarity of your standard solution of borax to 4 significant figures.

Part 2: Titration of HCl against standard solution of Borax

Performing the Trial titration (to obtain a rough titration figure of the titre).
1. Rinse your burette with a small quantity of the HCl solution, before filling it with the HCl.
Ensure that there are no air bubbles.
2. Pipette 20.00 cm3 of your borax solution into a clean conical flask. Draw the borax solution
into the pipette directly from the standard flask, taking care that the tip of the pipette is well
below the surface of the solution.
3. Add 2 – 3 drops of the methyl red indicator (colour-blind students are reminded to use
bromocresol green).
4. Record the initial burette reading to 2 decimal places. Do not adjust the level to the 0.00 mark.
5. Place the conical flask under the burette so that the burette tip is just inside the rim of the
flask. Slip a sheet of white paper under the flask.
6. Add the HCl solution to the flask in 1 cm3 increments, swirling the flask all the while.

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 Note the colour of the solution after each addition.
7. This trial titration is complete the moment the colour of the titration mixture changes from
yellow to orange (in the case of bromocresol green: blue to yellow).
8. Record the final burette reading. Subtract the initial reading from final reading to obtain the
titration figure (the titre) for this first, rough titration.

Performing Accurate Titrations

1. Refill the burette with HCl solution. Repeat steps 1 to 5 of the procedure for the trial titration.
2. Add the HCl solution to the flask in 2 cm3 increments, swirling the flask all the while. Stop
when you have added 2 cm3 less than your rough titre obtained with the trial titration.
3. Rinse the walls of the flask with de-ionized water from the wash bottle.
4. Continue the titration in a drop-wise fashion. Swirl the flask rapidly after each addition. The
end point is recognized as the first appearance of a permanent orange (with bromocresol
green: yellow) colour in the titration mixture. If your solution turns red, you have added too
much acid. If you are unsure about the end point, record the burette reading before you add
the next drop.
5. Once the end point is reached, record the burette reading and calculate the titre.
6. Repeat this procedure with fresh samples of borax solution until you have three different titers
that agree to within 0.10 cm3.
7. Calculate and record the molarity of the HCl solution from the average titre of the three
titrations. Report your answer to the correct number of significant figures.
8. Calculate the volume of HCl solution that is equivalent to exactly 1.00 g of borax.

Your Laboratory Report Should Include the Following (Under Results & Analysis):
1. Preparation of Standard Solution
(a) Mass of beaker (g):
(b) Mass of beaker and borax (g):
(c) Mass of borax (g):
(d) Volume of volumetric flask used (cm3):
(e) Molar concentration (mol/L) of borax solution prepared (Show your calculations.):

2. Titrations: Reproduce this table and use it for your data collection.

Burette reading (cm3) Titre Volume

Portion
Initial Final (cm3)
Trial
1
2
3
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 (a) Average titre (cm3) ________
(b) Balanced chemical equation for the reaction.
(c) Molar concentration (mol/L) of HCl (Show all your calculations)

3. In-lab Questions
(a) When you calculate the mass of borax needed to make up the standard solution, do you
include the “10 H2O” in the formula for borax? Why/why not?
(b) Suppose you failed to mix the borax solution properly. How would this error be reflected
in the average titre?
(c) How does the equivalence point of a titration differ from its end point?
(d) Name two other possible sources of error in this experiment (apart from not mixing the
borax solution properly as mentioned in question (b).

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