Chemistry 1B Experimental Procedure

Weak Acid-Strong Base Titration Curve: pH vs. Volume of Titrant

2 Changes to this lab:

1) It will be worth 10 pts instead of 20 pts [I will adjust points later].
2) you don’t have to write a pre-lab for it because I am so late in getting this up.

Discussion
Weak acids react completely with strong bases (and the reverse is also true: strong acids
react completely with weak bases). Acids and bases, in general, will react with the strongest
opposite that is available – so while the hydrolysis (reaction with water) is always an option in
aqueous solution, the acids and bases will seek out something stronger than water if available.

We will titrating 50 mLs of a 0.1 M oxalic acid solution with a 0.2 M sodium hydroxide
solution. The reactants are:

H2C2O4(aq) + NaOH (aq)
2 H2O(l) + Na2C2O4(aq)

In the case of titrating a strong acid with a strong base, the pH at the endpoint is 7, because the
salt formed as the product does not interact with water and therefore doesn’t effect the pH.

In the case of titrating a weak acid with a strong base, the salt formed as the product can interact
with water and effect the pH, so the pH in this case is not expected to be neutral at the
equivalence point. If you write the dissociation equation and hydrolysis reaction of sodium
oxalate, you will see that the sodium oxalate will change the pH toward the basic region:

Dissociation Equation: Na2C2O4(aq)
2 Na+(aq) + C2O42-(aq)

Hydrolysis reaction: C2O42-(aq) + H2O(l) <=> HC2O4-(aq) + OH- (aq)

In addition, because oxalic acid is a diprotic acid, there will actually be two equivalents points,
since the deprotonation of a polyprotic acid occurs stepwise.

H2C2O4 (aq) + H2O(l) <=> HC2O4-(aq) + H3O+ (aq) Ka1 = 5.9 x 10-2

HC2O4- (aq) + H2O(l) <=> C2O42-(aq) + H3O+ (aq) Ka2 = 6.4 x 10-5

This titration is a little different in that the objective is not to determine the concentration or mass
percent of the unknown in the Erlenmeyer flask. Instead, the objectives are 1) to construct a pH
vs. volume of titrant graph which is also called a Titration Curve graph. 2) The second objective
is to compare the data obtained with the calculated expectation of the two equivalence points.
Then, calculate a percent error for those numbers. 3) The third objective is to look at the titration
curve and determine where the solutions would behave as a buffer solution, and then
4) reproduce the solution to see if it does in fact behave like a buffer solution in that region.

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Chemistry 1B Experimental Procedure

Procedure
For this experiment there will be assigned groups of four students each, in order to accomplish
all of the objectives. Two students will physically do the titrations and collect pH data (sharing
one pH meter) and the other two students will write out the calculations and create the titration
curve as the titrations are being done. It may also be useful to have one of the non-
experimentalists calibrate the pH meters to its appropriate buffer.
The solution concentrations and indicators are:
0.2 M NaOH (check the container for the correct number of significant figures)
0.1 M H2C2O4
2H2O (check with the solution-makers for correct significant figures)
Indicators: bromphenol blue for acidic pH and phenolphthalein for neutral-basic pH.

Two Students will be assigned to the Calculations:

Using the information provided, two students should 1) independently determine each of the
equivalence points, and what volume of titrant (sodium hydroxide) will be needed (based on the
information given below) to arrive at the equivalence point, theoretically. These students will
also be responsible for 2) making sure everyone (all four students) have a copy of the
calculations and 3) creating the graph on Excel. The Excel graph should have a “connect the
dots” kind of curve on the graph, as we did for the visible spectrum of the iron-ligand complex
ion.

Two Students will be assigned to titrations:

Two students in the group should each make one solution of oxalic acid. The oxalic acid is
actually oxalic acid dihydrate, so determine the molecular weight accordingly. Using a 100 mL
volumetric flask, make a 0.1 M solution of H2C2O4
2H2O(aq) to as many significant figures as
you can using the measuring tools at hand. The volumetric flask is 100.00 mL +/- .08 mL
or +/- 0.16 mL depending on your particular flask. Once the solutions are made, check to make
sure that the concentrations are written accurately (if you used a little more or less oxalic acid
than calculated). Pipet a 25 mL aliquot (read the pipet as accurately as possible) into two
Erlenmeyer flasks. Add about 20 mLs of DI water to each flask. In each group, one Student
will use the bromphenol blue indicator, adding 12-15 drops to the flask and the other student will
use the phenolphthalein indicator, adding 2-3 drops to the flask.

The two students will titrate from ONE solution first [both work form solution A], and then both
students will titrate from the second solution. Determine which solution to use first, and label
your flasks and your solutions to avoid confusion. The first color change will be the yellow-to-
green color change of bromphenol blue indicator; this will mark the first equivalence point. The
bromphenol blue will actually change color again, to blue as the titration continues, but that
won’t be telling you anything except that the pH value has changed again. The second
equivalence point will be marked by the clear-to-pink color change of the phenolphthalein
indicator.

Instead of titrating one drop at a time to the equivalence point, add 2 mL aliquots of the titrant
(read and record accurately!), and measure the pH at each 2 mL addition. As your indicator
suggests that you are closing in on the equivalence point, slow down and check the pH value at
every 0.5 mLs until you are sure that you have passed the equivalence point – check with the
students in your group who are calculating the two equivalence points for this information. Each

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Chemistry 1B Experimental Procedure

group should have a total of six titrations, and the titrations should yield similar graphs! (Put 2-3
titration graphs on one page of Excel. Use Print Preview to ensure that you are not printing one
graph per page. If one of the titrations are off, please repeat the experiment. All four students in
each group should have all of the data in their notebooks by the end of the period.

If there are problems, ask the instructor.

Once the graphs are generated, print and show the instructor. Then the group (with the
instructor’s help) will determine where the buffer area is based on the data.

The last step is for two students (those who did the calculations) to pipet 20 mL aliquots of the
oxalic acid solution into a small clean flask or beaker for pH readings. Then, take one sample,
and add enough volume of titrant, based on the graph, to put the solution into the buffer area.
This isn’t so much a titration at this point, as it is a carefully measured addition of sodium
hydroxide. Then, using the recalibrated pH meter, take the pH of your buffer solution, and add
drops of 1.0 M HCl and find out how many drops it takes to break the buffer, by changing the pH
by 1.0 unit or more. Each student should do one trial using HCl and one trial using NaOH. Let
the instructor know immediately if the solution is not behaving like a buffer! If the answers are
not agreeing, redo the experiment. Finally, calibrate the dropper and find the average buffer
capacity of your solutions. Recall from the buffer lab previously that the buffer capacity is how
many mol hydronium ion/L of buffer it takes for the buffer to be broken; or mol hydroxide ion/L
of buffer required to break the buffer solution.

All of this information should be in all four notebooks by the end of lab. This will be 20% of
your grade.

Report Information
For this lab, there will be only one report per group, and hopefully it can be submitted at the end
of lab. Hand in, on loose leaf paper, the best version of 1) your calculations for the two
equivalence points, 2) data, 3) the printed copies of your six graphs, and 4) the calculations for
the buffer capacity.

Points: I will give everyone a “free” 10% for the pre-lab that you don’t have to do. The report
will be 70% of your grade.