Lab 7 Updated Titration w21

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CHEM 162: EXPERIMENT 7

Titration of a Weak Acid


OVERVIEW

This lab will be conducted at home using lab kits. Students are expected to complete all parts of the lab by
following all instructions and then creating a typed formal lab report. Once completed the lab report word
document can be saved as a pdf and uploaded to the canvas assignment page.

Students will titrate a weak acid, household vinegar (CH3CO2H), with a strong base, milk of magnesia (Mg(OH)2)
and generate an acid-base titration curve.

TECHNIQUES TO LEARN:
 Titration of a weak acid
 Using a pH meter to measure hydronium ion concentration
 Determine the pKa of an acid and its concentration.

MATERIALS

 20 mL of Mg(OH)2, milk of magnesia


 30 mL of 5% (v/v) CH3CO2H
 Red cabbage indicator
 3 x plastic pipette
 Digital pH meter & calibration
solutions
 100 or 150 mL beaker

CRITERIA FOR SUCCESS

Students that attempt the lab report in


good faith will receive a complete, C, grade.
Students that meet the expectations
outlined in the rubric below will receive a
mastery, M, grade.
Weak Acid Titration

This lab will be conducted at home using a lab kit and will require data analysis and then presenting student
work in a typed formal lab report.
1) Read the introduction and procedure of the lab to familiarize yourself with the objective and calculation
methods you will be expected to use.
2) Follow the lab procedure and conduct a titration of acetic acid and record pH data.
3) Perform a series of calculations to analyze your data & create a titration curve.
4) Write a formal lab report to communicate the experimental results.

INTRODUCTION
In this experiment you will generate an acid-base titration curve. A titration curve typically shows how the pH of
a solution changes as acid or base is added. In your titration, you will add strong base to a weak acid and
monitor the change in pH. While performing this titration, you will record the volume of titrant added and the
pH of the solution. You will then generate a titration curve using an analysis program such as Excel.

A plot of the pH vs. the volume of titrant added can reveal much of the underlying chemistry of the system,
including the relative strengths of the acid and base involved, the K a values of any weak acids or weak bases, and
the equivalence point of the titration. You will analyze your curves in the following ways:

1) Compare and contrast three regions of the titration curve

2) Estimate the pKa for a weak acid from its titration curve

3) Determine the exact concentration of a weak acid from its equivalence point

Acid – Base Reactions

In a typical strong acid, the acid ionizes 100% in solution:

(1) HA(aq)  H+(aq) + A-(aq)

Because the initial ionization is 100%, the H+ in solution is exactly equal to the initial concentration of the strong
acid itself.

If the acid is a weak acid, however, it will only partially ionize, according to the following equilibrium ionization:

(2) HA(aq) ⇌ H+(aq) + A-(aq)

In this case, the H+ in solution is determined by the Ka for the equilibrium above:

+ −
𝐻 𝐴
(3) Ka = 𝐻𝐴

The Ka value, in turn, can be calculated by using the pH of the solution when the titration is exactly half-finished.
This point is called the “half-equivalence” point on the titration curve.
The meaning of equivalence and half-equivalence points

At the equivalence point for an acid-base neutralization reaction, the amount of base added is equal to the
amount of acid initially present. On a titration curve, this point can be determined graphically (even without an
indicator) by identifying the volume where the pH rises the most dramatically (see Figure 1 below).

Note that the equivalence point should (but does not always) perfectly coincide with the endpoint of the
titration, which is the point where the indicator changes color. To make the endpoint line up with the
equivalence point, chemists use an indicator that changes color as close to the equivalence point as possible.

The half-equivalence point, as its name suggests, is the volume half-way to the equivalence point during the
titration of a weak acid by a strong base. At this point, one-half of the weak acid, HA, has been converted to its
conjugate base, A-. Thus, at this half-equivalence point, the concentration of the remaining acid is equal to the
concentration of the conjugate base formed. In other words, [HA] = [A -]. The expression for the Ka of the acid
simplifies to:

+ −
𝐻 𝐴
(4) Ka = 𝐻𝐴
= [H+]

By taking the negative log of both sides, (4) above simplifies to:

(5) pKa = pH

Therefore, the pH at half-equivalence can be used to identify the unknown weak acid.

Figure 1 shows a typical titration curve for the titration of a weak acid by NaOH.

pH equivalence point
half- equivalence
point
pKa

volume NaOH

Figure 1. Titration curve for a WEAK monoprotic acid

SAFETY PRECAUTIONS

CAUTION: 5% CH3COOH is NOT for consumption. If swallowed, seek medical attention. Mild skin irritant.
Severe eye irritant.

CAUTION: Mg(OH)2 is NOT for consumption. If swallowed, seek medical attention. Skin and eye irritant.
EXPERIMENT 7: Procedure & Data Analysis

LAB PROCEDURE
1. You do not need to calibrate your pH meter, as this was done recently for experiment 6. Open the
containers of acetic acid and magnesium hydroxide.

2. Pour the acetic acid into your beaker and take a measurement of the pH with the pH meter.

3. Add a small amount of the cabbage powder as a pH indicator. Start with a very tiny amount (about
enough powder to fit on this O), you can always add more. The goal is to make the solution a pink color,
but not such a dark red that it will be difficult to see the color change.

4. Using the pipette, add 1.0 mL of magnesium hydroxide to the container of acetic acid.

5. Stir the solution then measure the pH using the digital pH meter. Record the total volume of titrant
added and the pH in Table 1 provided.

6. Repeat steps 4 and 5, 4 more times.

7. Note any changes in color with each addition of magnesium hydroxide.

8. Using the pipette, add 0.5 mL of magnesium hydroxide.

9. Stir the solution then measure the pH using the digital pH meter. Record the total volume of titrant
added and the pH in Table 1 provided.

10. Repeat steps 8 and 9, 5 more times.

11. Using the pipette, add 0.1 mL of magnesium hydroxide.

12. Stir the solution then measure the pH using the digital pH meter. Record the total volume of titrant
added and the pH in Table 1 provided.

13. Repeat steps 11 and 12, 9 more times.

14. Using the pipette, add a single drop of magnesium hydroxide. Assume 1 drop is 0.05 mL.

15. Stir the solution then measure the pH using the digital pH meter. Record the total volume of titrant
added and the pH in Table 1 provided.
16. Repeat steps 14 and 15, until in your measurements, there is a large spike in the pH and then upon
taking more measurements, the pH begins to level off.

17. Once the pH has leveled off, add 0.5 mL of magnesium hydroxide using the pipette.

18. Stir the solution then measure the pH using the digital pH meter. Record the total volume of titrant
added and the pH in Table 1 provided.

19. Repeat steps 17 and 18, 5 more times.

20. Using the pipette, add 1.0 mL of magnesium hydroxide.

21. Stir the solution then measure the pH using the digital pH meter. Record the total volume of titrant
added and the pH in Table 1 provided.

22. Repeat steps 20 and 21, 3 more times.

DISPOSAL Thoroughly wash all equipment and place it back into your kit to return later to SSC Department of
Chemistry. All leftover solids may be disposed of in the trash. All leftover liquids may be poured down your sink
drain with running water.

DATA ANALYSIS

1. During the titration experiment students will need to record pH data. The table below can be used to track pH
measurements either by printing and hand-writing in values, or typing into a word document, or recording in an
excel worksheet.

Table 1. pH of acetic acid solution as it is titrated with Mg(OH)2.

Volume Titrant pH Color Volume Titrant pH Color


Added (mL) Change Added (mL) Change
2. Plot the data you recorded in Table 1 using an analysis program such as Excel in the following manner. You
way also print and do this analysis by hand using a ruler if you have access to a printer.

a. Separate your data into three different sections: the acidic buffer portion, the equivalence point,
and the basic buffer portion.

b. Plot each section on the same plot, but as different data sets.

c. Use the analysis program to insert a trendline for both the acid portion and the basic portion, not
the equivalence point portion.

d. Insert a vertical line ( to x-axis) between points A and B as shown in Figure 2b. Be sure to
position this vertical line so that its midpoint crosses your curve. (To find the midpoint of the
vertical line, find the length of the line you inserted then divide by 2 to find the exact middle –
don’t eyeball it!). The equivalence point occurs right at the midpoint of the vertical line, where it
crosses the curve.

e. Refer to your graph to estimate the volume and the pH at the equivalence point for both curves.

f. At the equivalence point, place a dot and note the corresponding pH and volume on the graph. At
the half-equivalence point, place a dot and note the corresponding pH and volume on the graph.

Equivalence point
pH

volume NaOH (mL) volume NaOH (mL)


Figure 2a Figure 2b

3. Calculate the following and embed your work in the formal lab report.

a. Use the half equivalence point to determine the experimental pKa of the acetic acid.

b. Calculate the % error of your experimental pKa if acetic acid has a reported pKa of 4.76.

c. Calculate the concentration of acetic acid analyzed in this lab.


EXPERIMENT 7: Formal Lab Report

In this experiment you will prepare a formal, typed report. It must consist of the following sections Exact order is
important, and each section must be clearly labeled (except the title).

1. Title: Top of page: Provide the experiment title in YOUR own words (do not use the manual’s title), the date
the experiment was performed, and your name.

2. Purpose: Using YOUR own words, interest the reader in the investigation and explain what is being
determined, generally how the investigation is conducted, and why this determination is important in the
greater sense. If a chemical reaction is being studied in this experiment, or is critical to its outcome, it should
be listed here (and perhaps also again in the discussion).

Please note: All chemicals should be properly sub- and super-scripted for points in this report. For
instance, you should write CH3CO2-, not CH3CO2-.

3. Data & Results: Begin your results section with 1-2 sentences that report the main results with calculated
uncertainty. Your main results should include (1) the concentration of your acetic acid solution and (2) your
experimental pKa and % error.

Table 1: Embed or create a table with volume of Mg(OH)2 and pH data. Be sure to give the table a
descriptive title.

Figure 1: Embed your titration graph as a figure. Give the figure a descriptive title and be sure to label the
following in the graph:
 Label the x and y axes
 Give the table a title
 Show trendlines used to find the equivalence point
 Label the equivalence point and note the Volume of Mg(OH)2 added and pH
 Label the half equivalence point and note the Volume of Mg(OH) 2 added and pH

Table 2: Embed or create a table that summarizes your results. Be sure to give the table a descriptive title
and include the following results:
 pH at the equivalence point
 Volume of Mg(OH)2 added to reach the equivalence point
 Calculated concentration of acetic acid
 Experimental pKa of acetic acid
 % error for the experimental pKa

4. Calculations: These can be done by hand or by computer – your choice. Doing them by hand will save you
significant time and effort.

In this section, please show how you calculated:


a. The concentration of acetic acid
b. The experimental pKa
c. The % error for your experimental pKa
5. Discussion: Briefly restate and evaluate your main results, taking care to interpret them for your reader. In
order to shape your overall discussion, please discuss the evolving buffer system that is created and then
neutralized by your titration. To do so, you should consider answering the following questions as part of
your discussion (not as a numbered list – but rather as elements of your overall essay):

a. For a weak acid (HA) titration, what are the net ionic reactions for the following processes?
i. The hydrolysis (reaction with water) of pure weak acid (HA) in distilled water.
ii. The neutralization reaction between HA and sodium hydroxide.
iii. The hydrolysis equilibrium of the conjugate base, A , with water.
-

b. Besides water, what is the dominant (most concentrated) chemical species for the situations in ai,
aii, and aiii?

c. In your discussion please include a figure showing generic titration curve and label the regions that
correspond to the situations in ai, aii, and aiii.

After you have discussed the course of the titration, answer the question: Do your results make sense
chemically? For example, are the pKa values you calculated appropriate in size for a weak acid? Is your
calculated concentration similar to the 5% (v/v) concentration that is commonly reported for household
vinegar (which is the source of the sample of acetic acid)? Does the shape of your pH curve match what you
would expect from a weak acid titration curve? Finally, discuss the appearance of the cabbage powder
endpoint (color changes) … did it appear before, after, or exactly at the equivalence point of the titration? Is
red cabbage powder a useful indicator if performing this titration without a pH meter?

Your discussion should also discuss portions of the technique or your lab experience that affect your
precision and accuracy; observations made during the lab are crucial here. Suggest one or two
improvements to the lab or your technique.

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