Introduction:

Ka is the ionization constant for the ionization of an acid, representing the acids affinity to dissociate.
This experiment will determine an unknown acids identity by experimentally determining the Ka value
quantitatively by the process of titrating 45 mL of 0.10002 M NaOH into 25 mL of the unknown acidic
solution in discrete increments. The experimentally determined Ka value (by averaging the Ka values at
0%, 20%, 40%, 60%, 80% and 100% titration points) will then be compared to the known Ka values for
acetic acid and its three chloro-substitued structures. This experiment also consists of a qualitative
analysis, which is done using various indicators to determining the pH range of the unknown acidic
solution through comparison with the known acids reacting with the indicators, Thymol Blue, Malachite
Green and Crystal Violet. Thus, through comparison of the results obtained from the qualitative as well
as the quantitative processes, the acid can be identified successfully.
Purpose:
The purpose of this experiment is to determine the identity of an unknown acid by experimentally
determining the Ka value.
Experimental:
Quantitative Identification
Initially, due to the pH meter not reading the absolute values for the pH it was necessary that it be
calibrated with buffer solutions of known pHs, being 4, 7, and 10 with the assistance of a guide. After
conducting the calibration process, 25 mL of unknown acid was transferred into a 100 mL beaker using a
pipette. This solution was placed on an electronic heater, at low heat. In addition, a magnetic stirring bar
was added into the beaker, to make sure the solution was thoroughly being mixed. As the electrode of the
pH meter was placed within the beaker (not touching the stirring bar), the titration process was initiated,
NaOH being the titrant. Initially, small increments of titrant were added, leading to 1 mL increments.
Once the pH meter began to rise noticeably, smaller quantities of titrant was added to prevent the
equilibrium point from passing. Once a total of 45 mL of titrant was added, the titration process was
completed. Furthermore, prior to the titration being completed, observations including the volume as well
as the pH were recorded after each addition of titrant. Materials were cleaned, disposed of as told and
work station was cleaned.

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Qualitative Identification
Initially, the demonstration bench had three racks of test tubes set up. Each rack contained 4 test tubes,
each containing 5 mL of 1 of the acids, acetic acid and its three chloro-substitued structures, numbered 1
4. Since indicators were already present in these acids, all that was done was recording observations of
each numbered acid qualitatively that contained thymol blue, malachite green, or crystal violet. According
to the colors of each tube, the 4 acids were identified by comparing the observed colors with the pH
range for color change table on page 115 in Lab Manual. Furthermore, the unknown acid was poured (5
mL) into 3 test tubes, and 1 of the 3 indicators was placed in each of the three test tubes. The test tubes
were then shaken, mixing the indicators with the unknown acid thoroughly, and observations were
recorded. Materials were cleaned, disposed of as told and work station was cleaned.
Results:
Quantitative Identification:
Unknown No. 67
[NaOH] = 0.10002 M
Temperature = 23.6 C
Qualitative Identification
Table 1: Observations made when performing a series of qualitative tests
Acid

Colors with
Thymol Blue

Malachite Green

Crystal Violet

More red/pink in color

Clear light blue tint in

Light blue in color

Peach/orange pink in

color
Paler, & lighter blue

Aqua green / blue in

color
Yellow /orange in color

than #1(lime green)

Dark blue in color

color
Royal purple in color

Similar to #2, but a bit

Clear in color

Similar to #1, but a little

Unknown #:67

darker pink
Dark blue in color (no

Clear in color (perfect

bit lighter in color

Aqua in color (match

match with Acids)

match with Acid #4)

with Acid #4)

Calculations:
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(Attached)
Figure 1: Titration of NaOH Graph: Amount of NaOH Added VS pH Level

pH Curve of Unknown Acid

pH

Volume of NaOH Added (mL)

Figure 2: Graph of Derivative Plot Method: Average Volume (mL) VS

pH / Volume

Derivative Plot of pH / Voume VS Volume (mL)

pH / Volume (mL)

Average Volume (mL)

Table 2: Summary table of pH and Ka values at different Vb percentages

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Percentage of Vb (NaOH in mL)

0%
20%
40%
60%
80%
100%
Average

Corresponding pH
1.65
1.53
1.57
1.70
2.02
8.32

Ka Value
6.068 x 10 -3
3.466 x 10 -2
8.424 x 10 -2
1.906 x 10 -1
2.844 x 10 -1
3.109 x 10 -5
9.981 x 10 -2

Discussion:
Qualitative Identification
Table 3: Observations based on the qualitative analysis
Acid
1
2
3
4

Order of Strength
Second
Third
Fourth
first

Identity of Acid
Dichloroacetic Acid
Monochloroacetic Acid
Acetic Acid
Trichloroacetic Acid

According to the data obtained in the qualitative portion of this experiment, it can be deduced that
the order of the acids based upon the strength can be given as shown in table 3. The values incorporated
within these tables are based on the colors of the solutions observed in the experiment when the
respective indicators were added to the acid containing test tubes. The acid labeled number 3 had the
colors that corresponded to the acid with the highest pH, representing the weakest acid, hence, determined
as being acetic acid. In addition, pH observations that were concluded from table 3 were based upon the
pH range for color change table, located on page 115 from the CHEM150 Lab Manual. Furthermore, a
similar process was preceded with acids 1, 2, and 4, concluding, acid 4 being the strongest acid, thus,
being trichloroacetic acid. With a similar process, unknown acid # 67 was tested. Initially, with the thymol
blue indicator, the solution turned a dark blue, a color that none of the known acids were, thus, was
insignificant in determining the identity of the unknown acid. With the malachite green and crystal violet
indicators, the unknown acid resembled acid 4. Hence, being labeled as dichloroacetic acid, by qualitative
analysis. The significance of these results show that a qualitative analysis can also reveal a tremendous
amount about an unknown substance. However, in this experiment, quantitative analysis was also
conducted.
Quantitative Identification
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Initially, as 25 mL of the unknown acid was poured into a 100 mL beaker, a magnetic stirring bar
was placed within the solution, thoroughly mixing the solution. As the titration was in process, the titrant
was added in small increments as the pH began to rise noticeably, thus signifying the nearing of the
equivalence point as the pH began to change the most rapidly, as seen in figure 1 in the 20 30 mL range.

Titration curves are represented with the volume of the titrant (NaOH in this case) and the pH of
the solution on the X and Y axis respectively. These graphs allow the determination of the
equivalence point through locating the volume with the highest point on the curve1. The
equivalence point is when the amount of titrant (in this case, the base) is equal and thus
neutralizes the acid in the solution2. Furthermore, by calculating dpH/dV for the average values of V
near the 20 30 mL mark (where pH was rising noticeably) as shown in sample calculations, a graph
containing a local maximum was obtained, as seen in Figure 2, signifying the equivalence point, at 26.25
mL, having a corresponding pH of 8.32. Therefore, with this data, the concentration of the acid was
obtained, as the moles of acid present equaled moles of based added, thus, leading to the concentration of
the acid being 0.1050 M. The average Ka value was calculated to being 9.981 x 10 -2 by the addition and
average of all 6 Ka values, from the 0%, 20%, 40%, 60%, 80%, and 100% titration points. After
conducting the titration process as well as the qualitative identification process, both lead to the
conclusion of the unknown acid being dichloroacetic acid. The accepted Ka value of dichloroacetic acid is
5.5 x 10-2, showing a reasonable similarity with margins of error present leading to a difference of 0.04,
being justified by errors that could have occurred during the experiment.
Possible errors that could have occurred within this experiment include human errors, lack of
skill, or simply carelessness. Initially, human errors include uncertainly in reading the apparatus and
volume levels, which could have altered volume readings as well as pH readings from the pH meter.
Secondly, through a lack of skill, the magnetic stirring bar could have touched the pH meter electrode
unnoticeably, leading to inaccurate data.

Error Analysis:
(Attached)
Conclusion:

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The main purpose of this experiment was to experimentally calculate the Ka value of the unknown acid,
which was 9.981 x 10 -2. Therefore the identity of the unknown acid is dichloroacetic acid.

References:

1. "Acids and Bases - Table of Common Ka values." Chemistry - Periodic Table, Chemistry
Projects, and Chemistry Homework Help. Web. 08 Feb. 2010.
<http://chemistry.about.com/od/chartstables/a/pkatable.htm>.
2. "How do acid/base indicators work? - Yahoo! Answers." Yahoo! Answers - Home. Web.
07 Feb. 2010. <http://answers.yahoo.com/question/index?
qid=20070528191849AAFKQVc>.
3. CHM 140Y5Y Course Manual. University of Toronto Mississauga. Print. S. S. Zumdahl
"Chemical Principles," 6th edition, Houghton Mifflin, Boston, MA (2008)

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