CHE-142L Titration lab

A weak acid titrated against a strong base

Titration: Titration is a very common lab technique in which the amount of a sample is
determined by measuring how much reactant it takes to use up all of the sample. The sample
with unknown amount is called the analyte, and the reactant is called the titrant. Titrations
with acids and bases are probably the most common type of titration. Today your analyte is
the weak acid potassium hydrogen phthalate (abbreviated KHP) and your titrant is the strong
base sodium hydroxide.

Notice in the reaction shown, as the weak acid (potassium hydrogen phthalate) donates an H +
to the OH- provided by sodium hydroxide, it turns into its conjugate base form.

Titrations usually are set up so that a solution of analyte is placed in a flask, then a buret is used
to slowly add the titrant until the reaction is complete:
Indicator: Titrations depends on knowing when the reaction is complete, with the exact molar
ratio of titrant added to react with the analyte (in this case, 1 mol of OH - is needed for each 1
mol of KHP). An indicator can be used to show when the correct volume of titrant has been
added, today’s indicator is phenolphthalein. Phenolphthalein is colorless when the pH of the
solution is acidic (less than pH 7.00), such as the KHP solutions at the beginning of the titration.
The phenolphthalein will turn bright pink right after all of the acid has reacted with base, and
any extra base added causes the pH of the solution rises above pH 7.00. Therefore, for this
titration, you have reached the endpoint when the color of the solution is just starting to turn
pink. The volume that it takes to reach the perfect reaction stoichiometry is called the
equivalence point, or Veq. (NOTE: indicators don’t always give you the perfect V eq)

In this lab, you will also record the pH of your solution as the titration proceeds, and create a
figure that shows a titration curve of pH vs volume titrant added.

Titration calculations: The volume of titrant added at the endpoint is then used in a
stoichiometry calculation to determine
-mols of titrant needed

-mols of analyte reacted

-molar mass of the analyte can be calculated from your data as = (mols analyte)/(mass analyte)

Materials:

0.100M NaOH (approx. 100mL) KHP, solid (approx. 1.5g)

phenolphthalein solution in dropper bottle dH20 (approx. 50mL)

buret and stand funnel

flask to hold at least 100mL waste beaker

balance weight boat/paper

pH paper or pH meter

Procedure:

1. Don your lab coat, gloves, and eye protection. The sodium hydroxide used is a strong base.
It can burn your skin or eyes, and will make white spots on your clothes that eventually fall
apart.
2. Empty the water already in your buret by opening the stopcock, and draining the water into
the waste beaker. Dump the waste beaker down the drain. CLOSE THE STOPCOCK!
Practice titration:
3. Fill your buret: you must do this part as directed, to prevent spilling the NaOH solution on
yourself!. Lower the buret, place the funnel in the top, and stand up on the stepstool if you are
less than 6’6” tall. Carefully pour the 0.10M NaOH into the buret until the meniscus is just
under the 0.00mL mark.
4. Record the intial volume (Vi) on your buret to two decimal places. Remember, the
measurements on a buret start at 0.00mL at the top, and increase as you go down!
5. Prepare your KHP: measure approximately 0.6 g onto a weigh boat. Record the exact mass
to as many decimal places as the balance give.

6. Put the KHP into your flask, add about 20mL of dH2O (doesn’t have to be exact), and swirl to
dissolve.
7. Add 3 drops of phenolphthalein indicator and swirl.

8. Place flask under the buret. Slowly add titrant, have it run down the side of the flask instead
of dropping in and splashing. Stop after about every 1mL added and swirl the flask.

9. WATCH FOR FLASHES OF PINK. That means you are getting close to the endpoint, so SLOW
DOWN, add a drop or so at a time, swirl, and wait to see if the pink color stays. STOP AT LIGHT
PINK not DARK PINK (that is too far) record your final volume from the buret (Vf). Now you
know about how much titrant it will take, and will not overshoot the endpoint on your real
titration.

The real titration:

10. Dump the contents of the flask down the drain, and rinse the flask thoroughly.

11. Put the funnel back in the buret, climb back up on the stool, and refill the buret. Record V i.
11. Measure another approx. 0.6 grams of KHP and record its exact mass, then dissolve in
water as before. Add 3 drops of the indicator.

12. Titrate as before, at the beginning before starting, and then after each 2mL: record the
volume on the buret (V), record the pH of the solution using the pH paper, and record the
solution color each time. Your life will be much easier if you make a table and record the
volumes (V) and pH into Excel.

13. Proceed until you have definitely passed the Veq.

Volume
NaOH Vdelivered pH Color
0.2 0.2 3 Clear
2.31 2.11 3 Clear
4.19 3.99 3 Clear
6.05 5.85 4 Clear
8.11 7.91 4 Clear
10.15 9.95 4 Clear
12.01 11.81 4 Clear
14.09 13.89 4.5 Clear
Flash of
16.1 15.9 4.5 pink
Flash of
18.05 17.85 4.5 pink
Flash of
20.1 19.9 5 pink
Flash of
22 21.8 5.5 pink
Flash of
23.22 23.02 5.5 pink
Flash of
24.09 23.89 5.5 pink
Flash of
25.05 24.85 6 pink
Flash of
26.29 26.09 6 pink
Flash of
27.15 26.95 6 pink
Flash of
28.3 28.1 6 pink
Flash of
29 28.8 6 pink
Flash of
29.79 29.59 6.5 pink
Flash of
31 30.8 6.5 pink
 Flash of
31.91 31.71 7 pink
32.31 32.11 7.5 Dark Pink
32.61 32.41 8 Dark Pink
33.05 32.85 8 Dark Pink
33.52 33.32 8.5 Dark Pink
34 33.8 8.5 Dark Pink
34.51 34.31 9 Dark Pink
35.12 34.92 9 Dark Pink
35.71 35.51 9.5 Dark Pink
36.11 35.91 10 Dark Pink
36.69 36.49 11 Dark Pink
37.15 36.95 11 Dark Pink
37.65 37.45 11.5 Dark Pink
38.11 37.91 11.5 Dark Pink
38.75 38.55 11.5 Dark Pink
39.1 38.9 11.5 Dark Pink

Titration Curve
14

12

10

8
pH

0
0 5 10 15 20 25 30 35 40 45
Vdelivered

Calculations:
1. Use the data from your second “real” titration.

2. For each volume recorded, you need to find the actual volume delivered (Vdelivered), which is
the volume recorded V-Vi = Vdelivered. Easy to do this in Excel. The Vdelivered at the exact moment
when the color changed, we are calling the color-change endpoint (Veq using V color change).
3. In Excel, plot a titration curve: X-axis should be Vdelivered and Y-axis should be pH. Give this
plot a title, label the axes and include units. Also show where the color changes occurred on
this plot.

Using the indictor change as the endpoint for your calculations:

4. Calculate the moles of KHP and molar mass of KHP from the color change endpoint:
a) from the known [OH-] and Vcolor change, calculate the moles of OH- used

b) from the moles of OH- used and the reaction stoichiometry, calculate the moles of
KHP present
c) from the moles of KHP present, and the mass of KHP you had weighed, calculate the
molar mass of KHP (hint: units are in grams/mol)

Doing the same calculations again, this time using the titration curve to find your endpoint:
5. A better way of finding the titration endpoint (Veq) is from the graph. Veq is at the steepest
part of the curve, at the inflection point (where the curve changes direction). Look on the
graph, and do your best to find the volume at the inflection point (Vinflection). Mark this on the
graph, too.

6. Calculate the moles of KHP and molar mass of KHP from the inflection endpoint:
a) from the known [OH-] and Vinflection, calculate the moles of OH- used

b) from the moles of OH- used and the reaction stoichiometry, calculate the moles of
KHP present

c) from the moles of KHP present, and the mass of KHP you had weighed, calculate the
molar mass of KHP (hint: units are in grams/mol)

Congratulations, nice job! Everything you just did should be in your notebook (original copy)
AND handed in on the worksheet (starting next page)

Titration lab worksheet to hand in:

-Staple a copy of the fully labelled titration curve plot you did in question 3 above, also the
labelled data table from Excel

-The formula for potassium hydrogen phthalate is KC 8H5O4. Calculate its molar mass from the
atomic weights on the periodic table:
-show all your calculations and final answer from question 4 above:

-show all your calculations and final answer from question 5 above:

-discuss the difference (if any) from your answers to questions 4 and 5 and the actual molar
mass of KHP. Include which method seems more reliable and why.

NOTES: