Potentiometry

Experiment 7 Potentiometric Titration
Valdosta State University
Purpose
To accurately determine the molar mass and pKa of an unknown weak acid.
Background
In this experiment, the pH of a solution will be measured directly as the sodium hydroxide is added. The pH will be measured using a glass combination electrode. This device measures pH (or [H3O+]) as voltage.
Background
pH Combination Electrode combination refers to the ion sensing cell and the reference cell.
Background
pH Combination Electrode combination refers to the ion sensing cell and the reference cell.
Background
Consider the following graph:
13
12
11
10
pH
3 0 5 10 15 20 25 30 35
Volum e NaOH (m L)
Background
13 12 11
10
pH
3 0 5 10 15 20 25 30 35
Volum e NaOH (m L)
In this region H+ dominates, the small change in pH is the result of relatively small changes in H+ concentration.
Background
13 12 11
10
pH
3 0 5 10 15 20 25 30 35
Volum e NaOH (m L)
In this region, relatively small changes in H+ concentration cause large changes in pH, The midpoint of the vertical region is the equivalence point.
Background
13 12 11
10
pH
3 0 5 10 15 20 25 30 35
Volum e NaOH (m L)
In this region OH- dominates, the small change in pH is the result of relatively small changes in OH- concentration.
Background
HA(aq) + NaOH(aq) NaA(aq) + H2O(l)
This experiment will use monoprotic acids. Therefore, at the equivalence point, moles HA = moles NaOH Using the definition of moles, the molar mass can be determined:
Background
This experiment will use monoprotic acids. Therefore, at the equivalence point, moles HA = moles NaOH Using the definition of moles, the molar mass can be determined:
sample weight moles ! molar mass

Background
pKa can be determined by using the Henderson-Hasselbach equation.
Background
?conjugate base A pH ! pK a log ?weak acid A
Background
HA(aq) + NaOH(aq) NaA(aq) + H2O(l) pKa can be determined by using the Henderson-Hasselbach equation.
If the pH is measured at the point where [conjugate base] = [weak acid]
?conjugate base A pH ! pK a log ?weak acid A
Background
?conjugate baseA pH ! pK a log ?weak acid A If the pH is measured at the point where [conjugate base] = [weak acid]
pH ! pK a log 1 pH ! pK a
Background
This assumption is valid at the half-titration point. If the equivalence point is 20.00mL, the half-titration point is at 10.00mL. The pH is then obtained directly from the graph.
Background
13 12
11
10
pH
3 0 5 10 15 20 25 30 35
Volum e NaOH (m L)
Background
13 12
11
10
pH
3 0 5 10 15 20 25 30 35
Volum e NaOH (m L)
Background
13 12
11
10
pH
3 0 5 10 15 20 25 30 35
Volum e NaOH (m L)
Procedure Experiment 7
- For this experiment, work in pairs.
Technique - Titration
Clean The Buret 1. Rinse a buret twice with distilled water. 2. Rinse the buret twice with 10-mL portions of your standardized NaOH solution. 3. Run some of the NaOH solution through the tip of the buret. 4. Drain the buret, then fill it with the standardized NaOH solution. 5. Let some NaOH solution run through the tip of the buret so that all air bubbles are removed.
Clean The Buret
Prepare the Unknown 1. Weigh 0.300 0.400g of solid unknown or 0.120 0.180g of liquid unknown to the nearest 0.001 g into a 250mL beaker. 2. Add approximately 50 mL of distilled water to the beaker and stir until all the unknown is dissolved.
Set-up the pH electrode GLX Computer
Set-up the pH meter - Calibration
Get a 400 mL beaker of distilled water to rinse the electrode between readings. Rinse the electrode with distilled water.
Performing The Experiment
1. Put the electrode tip in the unknown acid solution. Start button on 2. Fill the buret to 0.00mL and record this initial pH and buret reading. 3. Slowly add NaOH with stirring until either the pH increases by 0.20 units or 2.0 mL of NaOH have been added, whichever occurs first. Stop and record both the pH and the buret reading. 4. Repeat step 3 until the pH reaches 12, or until the titration has gone 15 mL past the equivalence point.
Data
Mass of unknown: 0.449g mL NaOH 0.00 2.30 3.00 4.80 6.10 8.48 10.61 12.80 15.08 16.90 17.82 pH 4.02 4.36 4.47 4.67 4.81 5.03 5.21 5.42 5.72 6.09 6.47 mL NaOH 18.80 19.00 19.40 19.92 21.25 23.95 25.10 27.28 28.12 29.80 pH 10.08 10.60 10.98 11.24 11.46 11.69 11.84 11.94 11.94 12.00
Data
13.00 12.00
Experiment 7, trial 1
11.00
10.00
9.00
8.00 pH 7.00 6.00 5.00 4.00 3.00 2.00 0.00
5.00
10.00
15.00
20.00
25.00
30.00
35.00
Volum e NaOH (m L)
Data
13.00 12.00
11.00
10.00
9.00
8.00 pH 7.00 6.00 5.00 4.00 3.00 2.00 0.00
5.00
10.00
15.00
20.00
25.00
30.00
35.00
Volum e NaOH (m L)
Calculation Molar Mass

1 L NaOH 0.116 mol NaOH 18.50 mL NaOH v v ! 0.00215 mol NaOH 1000 mL NaOH 1 L NaOH

1 mol unknown 0.00215 mol NaOH v 1 mol NaOH ! 0.00215 mol unknown

1 mol unknown 0.00215 mol NaOH v 1 mol NaOH ! 0.00215 mol unknown
0.449 g unknown 0.00215 mol unknown ! 209 g / mol unknown
Calculation - pKa
13.00 12.00 11.00
10.00
9.00
8.00 pH 7.00 6.00 5.00 4.00 3.00 2.00 0.00
5.00
10.00
15.00
20.00
25.00
30.00
35.00
Volum e NaOH (m L)
Calculation - pKa
13.00 12.00 11.00
10.00
9.00
8.00 pH 7.00 6.00 5.00 4.00 3.00 2.00 0.00
5.00
10.00
15.00
20.00
25.00
30.00
35.00
Volum e NaOH (m L)
IMPORTANT REMINDER
Save the unused solution in a location identified by your laboratory instructor.
Safety
The NaOH solutions are corrosive. If you get some on your skin, wash with water for at least five minutes. If any NaOH solution gets in the eyes IMMEDIATELY wash with water for at least fifteen minutes. Call for medical assistance!
Waste Disposal
All wastes from this experiment can be flushed down the drain with plenty of running water.

Potentiometry

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Experiment 7 Potentiometric Titration

Valdosta State University

Valdosta State University

Valdosta State University

Valdosta State University

Valdosta State University

Valdosta State University

Valdosta State University

sample weight moles ! molar mass

pKa can be determined by using the Henderson-Hasselbach equation.

Valdosta State University

pKa can be determined by using the Henderson-Hasselbach equation.

?conjugate base A pH ! pK a  log ?weak acid A

Valdosta State University

If the pH is measured at the point where [conjugate base] = [weak acid]

?conjugate base A pH ! pK a  log ?weak acid A

Valdosta State University

pKa can be determined by using the Henderson-Hasselbach equation.

Valdosta State University

Valdosta State University

Valdosta State University

Valdosta State University

8.00 pH 7.00 6.00 5.00 4.00 3.00 2.00 0.00

8.00 pH 7.00 6.00 5.00 4.00 3.00 2.00 0.00

Calculation Molar Mass

Calculation Molar Mass

Calculation Molar Mass

0.449 g unknown 0.00215 mol unknown ! 209 g / mol unknown

8.00 pH 7.00 6.00 5.00 4.00 3.00 2.00 0.00

8.00 pH 7.00 6.00 5.00 4.00 3.00 2.00 0.00

Valdosta State University

Valdosta State University

Valdosta State University

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?conjugate base A pH ! pK a log ?weak acid A

?conjugate base A pH ! pK a log ?weak acid A