Beruflich Dokumente
Kultur Dokumente
EXPERIMENT NO. 8
Cristine D.Z.Concepcion
2018-02771
BS CHEMISTRY II
approach for assessing acidity and stability constants in chemistry and is similar to direct titration
of a redox reaction. This experiment aims to determine the equivalence point for the titration of
20mL benzoic acidwith 0.1M sodium hydroxide. Standardizatiojnof NaOH was done before
titrating to be used on the potentiometric titration. There were four trials of KHP as the analyte.
and with these. the experimental cocnentration value was determined, which is 0.090019487M.
This concentration was used in the potentiometric titration of the mentioned titrant and analyte.
Two trials were established, one for each group. The standard deviation is lower than 1.00%, or
is too small - means that the measurements of the analyte are precise. A titration curve is
established with an equivalence point result to approximately 15.70mL. After which, the data
from the titration curve was used for the first derivative plot which resulted to an equivalence
point of approximetely 15.70mL and with the second derivative plot which is 15.80mL. The
INTRODUCTION
different fields regarding in analytical chemistry aspect. Titrimetry is known for having its
superior speed, its precision in simplicity, and a little sacrifice of accuracy, giving justice as to
why it is one of the most significant methods used in analytical chemistry. The potentiometric
method, with a glass electrode, is most likely used in some analytical laboratories in
preferred approach for assessing acidity and stability constants in chemistry and biochemistry in
and locating the point of maximum slope, or the inflection point, of the titration curve. In some
cases, very sharp breaks in the titration curve are bound to be the basis, making it at ease in
locating the equivalence point. Nevertheless, when very weak acids are titrated with strong
bases, the curves are more difficult to evaluate. It is then a necessity to locate the equivalent
point by plotting the differential curves, ΔpH/ΔV or ΔE/ΔV against volume of titrant added. The
peak shown on the curves correlates to the point of maximum slope of the normal titration curve.
Such differential methods need values of potential corresponding to very small change in volume
A typical cell for measuring the pH of a certain sample comprise of a glass indicator
electrode and a saturated calomel reference electrode that are consumed in the solution whose pH
is unknown. The indicator electrode contains a thin, pH sensitive glass membrane that is sealed
into one end of a heavy-walled glass or a plastic tube. A little portion of hydrochloric acid that
saturated with silver chloride, is contained in the tube. A silver wire in this solution forms a
silver/silver chloride inner-reference electrode, which is connected to one of the terminals of the
vi. determine equivalence point of the potentiometric titration of benzoic acid with 0.1M
sodium hydroxide
Potentiometric titration is applied in measuring the change in the electrical potential when
a neutralizing agent or the titrant is added to a chemical solution. Potentiometric titration can also
surfaces. This method provides an accurate data over wide concentration ranges and, with help of
automatic measuring and data collecting systems, it has become possible to collect large amounts
METHODOLOGY
This chapter shows the system of methods done in the activity and provides an outline for
A burette was properly washed and cleaned by rinsing with several portions of
distilled water. This rinse water was poured down the drain. An amount of 4.00g of
sodium hydroxide was obtained and was used from standardizing the strong base. This
amount was dissolved with about 50mL of carbon-free distilled water. A 1000mL
volumetric flask was procured in the experiment. The dissolved sodium hydroxide was
poured into the flask, and a distilled carbon-free water was then drained into the flask
until it reached the certain line in the flask. The burette was rinsed with three portions of
the NaOH solution. The rinsed portion was drained and discarded. The burette was then
filled with NaOH slightly the zero mark and the burette was clamped up vertically. The
air bubbles from the tip of the burette were removed by draining the NaOH into a small
beaker. The NaOH level value was read and recorded within + 0.02 mL.
A clean 250mL beaker was obtained. An amount of 0.24g of a dried acidic salt
compound, potassium hydrogen phthalate or KHP, was poured into the beaker. The KHP
was then dissolved with a 20mL carbon-free distilled water by constantly stirring the
solution with a glass rod. The solution was then transferred into a clean 250mL
Erlenmeyer flask.
Two to three drops of phenolphthalein indicator was drained to the KHP solution
in the Erlenmeyer flask. The flask containing the acid solution and indicator was placed
under the burette set-up. NaOH from the burette was slowly added to the flask with
swirling until the color of the solution in the flask is a faint pink. This faint pink color
should last only 45 to 60 seconds. There should be a one-drop difference between when
the solution is colorless and when it is pink. If too much base is added discard the
solution and repeat the titration. A white piece of paper placed under the flask will aid in
the color detection. The final volume of the NaOH was read and recorded. The molarity
An amount of 0.18g of benzoic acid was obtained in a clean 250mL beaker. The benzoic
acid solids were poured into a 20mL carbon-free distilled water. The solution was mixed
thoroughly. The solution was then transferred into a 250mL Erlenmeyer flask, ready for titration.
AEutech pH meter was used in the analysis. The pH meter was readily calibrated.
The iron stand with the burette that has the strong base was placed beside the pH meter.
2.3.2 Potentiometric titration
The Erlenmeyer with the analyte was properly placed under the burette. The pH
electrode was thoroughly mixed between measurements with distilled water to prevent
carryover contamination of the tested solutions. The electrode was gently blotted on a
laboratory cleaning tissue to remove the excess rinse water. The pH electrode was dipped
into the testing solution or suspension. A magnetic stirring bar was placed in the analyte.
The NaOH was dispensed slowly but surely per 0.50mL and 1.00mL. The titration
process was occurred, done with one trial each per group.
CHAPTER III
This chapter discusses the data and result gathered from doing the activity.
Average 0.090019487
The Table above shows the summary data for the standardization procedure of sodium
hydroxide. Four trials were done in the process, of which two are of the same mass of KHP.
Each trial has different volume of sodium hydroxide that has dispensed. In the first trial, the mass
of KHP used is 0.24g, with a volume dispensed by the sodium hydroxide to be 13.75mL. By the
aid of the calculations, the resulting mole of the KHP is 1.17514x10 -3, with a concentration of
0.087272727M. For the second trial, 0.25g of KHP was used. The volume dispensed is 13.60mL.
With calculations, the mole of the KHP in the second trial is 1.22413x10 -3 with a concentration
of 0.088235294M. For the third and fourth trials, the mole and concentration of the KHP are the
same as of the first and second respectively. The average of the concentrations of the four trials
is 0.090019487, which is the final concentration of the NaOH to be used in the potentiometric
3.2 Standard deviation and percent error of the concentration of the analyte
Table 3.2 Summary table for the standard deviation and percent error of the concentration of the
analyte
The data in Table 3.2 shows the experimental and theoretical concentrations of the titrant.
The calculated value for concentration of sodium hydroxide was determined by standardizing the
NaOH with KHP in four trials. After getting the concentrations from these trials, the average was
value is 0.1000M.
The standard deviation of the analyte tells how close the values are. It is a statistical
measurement of the precision of a group. The smaller the s is, the more precise the measurement
is. The computed value for the standard deviation of the analyte is 0.002255 or 0.02%. The
standard deviation is lower than 1.00%, or is too small - means that the measurements of the
analyte are precise. The repeated values are close with each other. The percent error is calculated
by subtracting the experimental value to the theoretical value, and the difference was divided by
the theoretical value, multiplied by 100. The percent error is 0.09980 or 9.98%. The accepted
value of percent error is 5%, or lower, but in this case the percent error is 9.98% - slightly
acceptable.
3.3 Quantitative Analysis by potentiometric titration of benzoic acid with 0.1M sodium
hydroxide
The potentiometric titration was done with two trials, each of different groups.
Phenolphthalein was used as the indicator. Using Excel, data were plotted for each titration. Two
groups titrated individually, each had one set list of pH corresponding to how many volume the
titrant had dispensed. The values obtained were used to calculate for the average pH from the
two trials.
12.00
10.00
8.00
pH
6.00
4.00
2.00
0.00
0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 24.00 26.00
NaOH volume
Figure 3.1 titration curve of 20mL benzoic acid with 0.1m sodium hydroxide
The figure above shows the titration curve of 20mL benzoic acid with 0.1m sodium
hydroxide. On the x-axis lies the volume of the titrant dispensed while the y-axis shows the H
reading. The highest slope in the titration curve is characterized as an inflection point and that it
is regarded to be the equivalence point. Thus an inflection point has to be present in the titration
curve in order to locate the equivalence point. From the data shown above, it is safe to assume
6.00
4.00
2.00
0.00
0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 24.00 26.00
NaOH volume
Figure 3.2 titration curve of 20mL benzoic acid with 0.1m sodium hydroxide with corresponding
points
The titration curve shows different points located on the curve. The red point on the
titration curve indicated the point where no NaOHwas added. So, the pH of the analyte is low.
The chemical equation is denoted as: C6H5COOH + H2O ↔ C6H5COO- + H3O+. As the sodium
hydroxide is added in a drop-wise motion, the H3O+ is slowly starting to be consumed by the
OH- that is produced by the dissociation of the NaOH. Moreover, the analyte is still acidic due to
the predominance of the H3O+ ions. The green point in the titration curve represents the pH
recorded at a point in time just before the completion of neutralization is taking place. Lastly, the
yellow point in the curve is the point where the NaOH is in excess, the point beyond the
equivalence point.The point of maximum slope, or the inflection point, is where the equivalence
point is located. At this point, the moles of the titrant and the analyte are the same. The H 3O+
ions are now completely neutralized by the OH - ions. The solution only contains C6H5COONa
salt and H2O. This reaction is denoted as: C6H5COOH + NaOH ↔ C6H5COONa + H2O. From
this reaction, the solution contains C6H5COONa salt. This salt dissociates intoC6H5COO- and
Na+. According to the principle of weak acid/strong base titration, C6H5COO- is the conjugate
base of C6H5COOH. So C6H5COO- is the strong base that will react with H2O to produce
The equivalence point is located to be at approximately 15.75mL with the help of the first
titration curve. The estimated acid dissociation constant of the acid can now be calculated, this is
called the buffer point, or the half-equivalence point. Generally, the equilibrium for a weak acid
is denoted as: HA (aq) + H2O ↔ H3O+ + A-. The half-titration point is the conversion of half of
Half-titration curve
4.80
4.60
4.40
4.20
4.00
pH
3.80
3.60
3.40
3.20
3.00
0.00 0.80 1.60 2.40 3.20 4.00 4.80 5.60 6.40 7.20 8.00 8.80 9.60 10.40 11.20 12.00
Volume of NaOH
Figure 3.3. Half-titration curve of 20mL benzoic acid with 0.1m sodium hydroxide
The data from Figure 3.3 shows the half-titration curve of 20mL benzoic acid with 0.1m
sodium hydroxide. The equivalence point from the previous determination was determined,
occurring at 15.75mL. The half equivalence of this point is 7.88mL with a pKaof approximately
4.10.
The first derivative plot is an aid to obtain a better and more improved approximation of
the volume at the equivalence point. The plot in the first derivative graph is the change of pH
8
7.52
7
6
5
ΔpH/ΔV
4
3
2
1.5 1.34
1
0.26 0.32 0.54 0.45 0.3
0 0.2
13.00 13.40 13.80 14.20 14.60 15.00 15.40 15.80 16.20 16.60 17.00 17.40 17.80 18.20
Average Volume of NaOH
The data from Figure 3.4 shows first derivative plot, where the slope of the titration curve
changes while approaching the equivalence point. The first derivative shows a spike at the
equivalence point, approximately 15.70mL, due to slope that had reached its maximum value at
Other than having a more improved approximation of the volume at the equivalence point
with the first derivative, the second derivative can clearly depict the volume as it intersect
directly to the x-axis. Moreover, the second derivative curve gives the end point more precisely.
Second Derivative
15
10
Δ(ΔpH/ΔV)/ΔV
0
14.00 14.30 14.60 14.90 15.20 15.50 15.80 16.10 16.40 16.70 17.00 17.30 17.60
-5
-10
-15
Average Volume of NaOH
The data from the Figure 3.5 shows the second derivative plot for this titration around the
inflection point. It can be asserted that the inflection point of the original function is located
nearly 15.80mL.
CHAPTER IV
This chapter shows the summary and conclusion of the study. This aims to cover-up the
The experiment seeks to determine the equivalence point of the potentiometric titration of
20mL benzoic acid with 0.1M sodium hydroxide. The standardization of sodium hydorxide was
done first. The analyte used was the potassium hydorgen phthalate or KHP. Four trials were
conducted, of which two of the four have the sae mass of KHP. With these mass, the moles of
the KHP were determined, and as well as the four concentrations of NaOH. The average of hese
four concentrations were calculated as the experimental concenrtation of the titrant, which is
0.090019487M, that woud be used in the potentiometric titration. The data were gathered
patinetly, as the reading is recorded 0.5mL, 1mL, and 2mL difference. The NaOH was
dispensed ata certain range, thus having numerouds readings. The standard deviation is lower
than 1.00%, or is too small - means that the measurements of the analyte are precise. A titration
curve was established from the data gathered. It was found out that the highest slope on the
inflection point lies approximately 16.00mL. The data from the first curve was used to geth the
first derivative plot curve, which resulted to an equivalence point to approximetely 15.70mL, and
with the second derivative plot curve that resulted to an equivalence point to approximetely
15.80mL. From these informations, it can be concluded that the equivalence point of the
potentiometric titration of benzoic acid with 0.1m NaOH is between 15.70mL to 15.80mL, or
15.75mL.
REFERENCES
[1] Checchetti A., Lanzo J. (2015) Qualitative Measurement of pH and Mathematical Methods
for the Determination of the Equivalence Point in Volumetric Analysis. World Journal of
Chemical Education, Vol. 3, No. 3, pp. 64-69.
[2] Martín J., Ruiz, D.B., Asuero, A. (2018) . Determination of the End Point in Potentiometric
Titrations: Gran and Schwartz Methods. Journal of Laboratory Chemical Education, 6(4),
pp. 77-90. doi:10.5923/j.jlce.20180604.02
[3] Perveen S. &Mohiuddin S. (2016) Multiproticity of Weak Acids: Inflection Point vs.
Equivalence Point. World Journal of Chemical Education, Vol. 4, No. 1, pp. 21-24
. DOI:10.12691/wjce-4-1-4
[6] Steenbock H. (1912) quantitative determination of benzoic, hippuric, and phenaceturic acids
in urine. Laboratory of the Department of Agricultural Chemistry of the University of
Wisconsin.
[7] Sjöberg S., &Lövgren Lars., (1993) The application of potentiometric techniques to study
complexation reactions at the mineral/water interface. Aquatic sciences, Vol. 55, No.4,
pp 324–335
APPENDIX
Raw data
Volume of NaOH pH
4.00 3.70
5.00 3.82
6.00 3.94
7.00 4.07
8.00 4.17
9.00 4.28
10.00 4.39
11.00 4.54
Moles of KHP:
1mol
Moles KHP 1 = (0.24g) ( ) = 1.17514x10−3
204.2g
1mol
Moles KHP 2 = (0.25g) ( ) = 1.22413x10−3
204.2g
Volume of NaOH:
1L
Volume of NaOH 1 = (13.75mL) ( ) = 0.01375L
1000mL
1L
Volume of NaOH 1 = (13.60mL) ( ) = 0.01360L
1000mL
NaOH concentration:
1.17514x10−3
NaOH concentration 1 = ( ) = 0.087272727M
0.01375L
∆𝑝𝐻 = 𝑝𝐻 2 − 𝑝𝐻 1
∆𝑝𝐻 = 5.06 − 4.93
∆𝑝𝐻 = 0.13
∆𝑝𝐻 = 𝑝𝐻 3 − 𝑝𝐻 2
∆𝑝𝐻 = 5.22 − 5.06
∆𝑝𝐻 = 0.16
ΔV
∆𝑉 = 𝑉 2 − 𝑉 1
∆𝑉 = 14.00 − 13.50
∆𝑉 = 0.50
∆𝑉 = 𝑉 3 − 𝑉 2
∆𝑉 = 14.50 − 14.00
∆𝑉 = 0.50
Average V
𝑉2 + 𝑉1
𝐴𝑣𝑒. 𝑉 =
2
14.00 + 13.50
𝐴𝑣𝑒. 𝑉 =
2
𝐴𝑣𝑒. 𝑉 = 13.75
𝑉3 + 𝑉2
𝐴𝑣𝑒. 𝑉 =
2
14.50 + 14.00
𝐴𝑣𝑒. 𝑉 =
2
𝐴𝑣𝑒. 𝑉 = 14.25
ΔpH/ΔV
0.13
∆𝑝𝐻/𝑉 =
0.50
∆𝑝𝐻/𝑉 = 0.26
0.16
∆𝑝𝐻/𝑉 =
0.50
∆𝑝𝐻/𝑉 = 0.32
Δ (ΔpH/ΔV)
` Average V
𝑉2 + 𝑉1
𝐴𝑣𝑒. 𝑉 =
2
14.25 + 13.75
𝐴𝑣𝑒. 𝑉 =
2
𝐴𝑣𝑒. 𝑉 = 14.00