Titration of Vinegar

Purpose:
To determine the concentration of a vinegar (acetic acid) solution by titration.

Please Read:
The section titled “Volumetric Glassware” on your lab page. You may also wish to review the section
titled “Accuracy and Precision”.

Introduction:
Titration is the process, operation, or method of determining the concentration of a substance in solu-
tion (the analyte) by adding to it a standard reagent of known concentration (the titrant) in carefully
measured amounts until a reaction of definite and known proportion is completed, as shown by a color
change or electrical measurement, and then calculating the unknown concentration.
In this experiment, you will prepare a solution of sodium hydroxide that has a concentration of approx-
imately 0.1 mol/L. You will determine its concentration exactly by reacting it with hydrochloric acid of
known concentration; the process is sometimes called standardizing the solution. The reaction equa-
tion is:
NaOH (aq) + HCl (aq) → H2O (l) + NaCl (aq)

With your standardized NaOH solution, you will titrate vinegar. Vinegar is a solution of acetic acid
(HC2H3O2) in water, and you will determine the concentration of acetic acid. The reaction equation for
acetic acid and NaOH is:
HC2H3O2 (aq) + NaOH (aq) → H2O (l) + NaC2H3O2 (aq)

The titrations are done in the presence of phenolphthalein, an indicator that is colorless in acid solution
but turns pink in basic solution. For the titration to give an accurate result, one must stop adding titrant
exactly at the equivalence point, when the indicator changes color. At the equivalence point, all of the
analyte has reacted, and only a tiny excess of titrant has been added, just enough to change the color
of the indicator.

Safety and Waste Disposal:

NaOH solid is caustic, corrosive, and hygroscopic (it absorbs water from the air). Do not touch solid
NaOH with your hands, or transfer it over the balance. If you spill the solid, notify your instructor at
once. The solution you will make is fairly dilute, and not dangerous. It is a mild irritant, however. If you
spill it on yourself, rinse well until the slippery feeling of a basic solution is gone. Spills on benches,
etc., should be cleaned up with paper towels.
Strong NaOH solutions etch glass. Your flask should contain water before the NaOH solid is added,
and it should be swirled constantly until the solid has all dissolved.
All waste can be flushed down the sink with plenty of water.

A. Prepare 0.1 M NaOH

Fill a 500 mL Erlenmeyer flask to the 250 mL mark with distilled water. In your prelab, you calculated
the mass of NaOH required to make 250 mL of 0.1 M NaOH solution. Weigh approximately this
amount of NaOH into a weigh boat and transfer it to the flask and water. Swirl the liquid until all the
NaOH has dissolved.
B. Standardize the NaOH solution
1. Obtain 80 mL of standard HCl solution in a 150 mL beaker. Draw 2-3 mL of the solution into a
25.00 mL pipet and rinse it. Discard the rinsing. It’s convenient to use a 250 mL beaker for this.
Use the pipet to dispense 25.00 mL of HCl solution into each of three 250 mL Erlenmeyer flasks.
Add 2 drops of phenolphthalein to each flask.
2. Use 5-10 mL of your NaOH solution to rinse out your buret. Discard the rinsing. Fill the buret with
NaOH solution, then clamp the buret onto the ring stand. With your beaker under the buret, open
the stopcock to fill the buret tip. There should be no air bubbles. Make sure the liquid level is
below the 0.00 mL mark, and that the funnel is not in the buret.
3. Read the initial volume on the buret (remember, it reads from the top down) and record the
reading. Also, you must “read between the lines” to obtain a volume to the nearest 0.01 mL.
Titrate your first sample of hydrochloric acid by adding NaOH solution from the buret to the flask
containing HCl solution at a fast drop rate, while swirling the flask. You will see the pink color of
the phenolphthalein indicator where the NaOH contacts the solution in the flask. It's easier to see
this if you put a sheet of white paper under your flask. When the pink color starts to persist, slow
the rate at which you add sodium hydroxide. The idea is to stop adding sodium hydroxide exactly
at the endpoint, when a pale pink/purple color remains for at least 15 seconds. At the endpoint,
read the final volume in the buret and record the result. Calculate the volume of sodium hydrox-
ide used.
4. Repeat the titration on the other two samples of HCl. You should use nearly the same volume of
NaOH for each titration, so you can run most of the NaOH into the flask, then titrate carefully for
the last 2 mL or so. You should be able to do at least 2 titrations without refilling your buret.
Before the third titration, make sure you have enough NaOH solution in the buret to complete it. If
you don’t, add more solution.
5. Ideally, you will use within 0.10 mL of NaOH solution for all three titrations. If the range between
your highest and lowest volume of NaOH is greater than 0.50 mL, repeat the titration until three
runs are within this range. There are extra lines on your data sheet for these runs, if needed.
Calculate the molarity of your NaOH solution, using the volume and molarity of the standard HCl
and the average volume of NaOH required for the titrations. Show your work.
6. Empty the 250 mL flasks into the sink and rinse them well. Use a few mL of distilled water for the
final rinse. Do not discard the NaOH in the 500 mL flask.
C. Determine Concentration of Acetic Acid in Vinegar
1. Obtain about 5 mL of vinegar in a 10 mL graduated cylinder. Use a few drops of this to rinse your
2.00 mL pipet, and discard the rinse. Use the pipet to dispense 2.00 mL of vinegar into each of
two 250 mL Erlenmeyer flasks. Add 2 drops of phenolphthalein and about 15 mL of distilled water
to each flask.
2. Titrate the vinegar as you did the HCl solution. If the difference between the volumes of NaOH
used for the titrations is greater than 0.50 mL, repeat the titration until two runs are within this
range. Calculate the molarity of the acetic acid, using the molarity of your NaOH solution and the
average volume of NaOH required for the titrations. Show your work.
3. Answer the questions on the reverse side of your data sheet.
4. When you have finished your lab work, you may discard all remaining solutions in the sink. Rinse
all glassware well, using distilled water for a final rinse. Return apparatus to the lab drawer or to
the supply area.
Calculations
The calculations for titrations are essentially theoretical yield calculations, worked with volumes and
concentrations of solutions, rather than masses and molar masses of compounds. As in all theoretical
yield calculations, one must have the balanced equation for the reaction. Both reactions in this titration
lab are quite simple:
Part B: NaOH (aq) + HCl (aq) → H2O (l) + NaCl (aq)
Part C: NaOH (aq) + HC2H3O2(aq) → H2O (l) + NaC2H3O2 (aq)
The first step in any theoretical yield calculation is to determine the number of moles of one of the reac-
tants, the one for which you know both the volume and concentration. In Part B, this is the HCl solu-
tion. You used 25.00 mL of the solution; its concentration was about 0.1 mol/L, known to four signif-
icant figures. In this example, let’s say that the concentration of HCl was exactly 0.1000 mol/L. Volume
(in liters) multiplied by molarity gives moles of compound in solution:
0.1000 mol HCl x 25.00 mL HCl x 0.001 L HCl = 0.002500 mol HCl
L HCl mL HCl
The next step is to use the reaction equation to determine how many moles of NaOH are required to
react with the HCl. The coefficients in the reaction equation give the molar ratio of NaOH to HCl.
0.002500 mol HCl x 1 mol NaOH = 0.002500 mol NaOH
1 mol HCl
In this lab, purpose of the titration is to determine concentrations. Since these have units of mol/L, one
simply takes the number of moles of NaOH and divides it by the volume of NaOH used. Let’s say that
the titration required 24.50 mL of NaOH. The resulting concentration can be expressed in varying
amounts of detail, as shown.
0.002500 mol NaOH x 1 mL NaOH = 1.020 mol NaOH = 1.020 mol = 1.020 M
24.50 mL NaOH 0.001 L NaOH L NaOH L
It is possible to string the operations into one calculation; for simplicity, convert volumes from mL to L
before setting up the equation.
0.1000 mol HCl x 0.02500 L HCl x 1 mol NaOH x 1 = 0.1020 mol NaOH
L HCl 1 mol HCl 0.02450 L NaOH L NaOH

Once you have determined the molarity of NaOH, that value and the volume of NaOH solution required
to titrate acetic acid (HC2H3O2) can be used to determine the molarity of acetic acid.