Experiment no.

Standardization of NaOH and Determination of a Weak Acid Dissociation Constant

Group No: 1 Date Due: September 7, 2022

Group Member: Aguilar, Jasmin A. Date Performed: August 17 & 31, 2022
Alih, Ahmed Qad’r A.
Name: Bassar, Sharmaine G.
 Abstract

This experiment involves two separate acid-base standardization procedures. In the first
standardization, the molarity of a sodium hydroxide solution (NaOH) was determined by
titrating a sample of potassium acid phthalate (KHP; HKC8H4O4) with the NaOH. In the second
procedure, the standardized NaOH was used to determine the dissociation constant of unknown
weak acid. The indicator used in this experiment was phenolphthalein which causes the solution
to reveal a faint pink color upon gradual titration. The tabulated data determine the exact
concentration of standard NaOH solution and the titration curve, half-equivalence point, first
and second derivative for the dissociation constant of the unknown weak acid through a titration
method. The three trials yield precise values for the standardization of NaOH. For NaOH,
0.08640 M, 0.08161 M, and 0.09802 M were calculated from the respective trials, with an
average of 0.08628 M. For the unknown weak acid, salicylic acid, the identity of the acid was
determined using the the estimated equivalence point at 34.00 mL and a half-equivalence point
of 17.10 mL with a pKa of 2.37. Also, a spiked curve was produced with its peak at the
equivalence point. The percent error was calculated to be 20.47% where the pKa true value of
salicylic acid was 2.98 and the obtained experimental pKa value was 2.37. Thus, several factors
may have contributed with regards to the percent error obtained.

Keywords: salicylic acid, sodium hydroxide, dissociation constant, standardization of NaOH,

 Chapter I
Introduction

Volumetric analysis, also known as titrimetric analysis, is a common quantitative analytical

approach. As the name implies, this method involves determining the concentration of the analyte
by measuring the volume of a known concentration solution (Yoder et al., n.d.). Titration is a type
of analytical procedure that is frequently used in standardization and involves reacting an exact
volume of one substance with a known amount of another substance (Kim, 2018). Titration with
an acid-base solution is used to standardize sodium hydroxide. In a titration, the endpoint is the
point at which the reaction is complete. The chemical substance phenolphthalein is used as an
indicator in the standardization of NaOH, allowing the endpoint to be observed. Organic
compound phenolphthalein is colorless in acidic solution and pink in basic solution (Yoder et al.,
n.d.). As a result, the equivalence point is determined by the reaction's stoichiometry, whereas the
endpoint is simply the color change from the indicator.

Moreover, a standard solution is used, the concentration of which is known with high
accuracy or which reacts stoichiometrically with the analyte. Standard solutions are described
using terms such as primary standards and secondary standards. Primary standards are produced
by weighing and dissolving the reagent that will react with the analyte into a specific volume.
Given its stability, high purity, non-hygroscopicity, high solubility, non-toxicity, high molecular
weight, and high availability, potassium hydrogen phthalate (KHP) is an excellent primary
standard (Kim, 2018). Hence, the sodium hydroxide solution is standardized using KHP. The
balanced chemical equation for the reaction is shown below:

KHC8H4O4(aq) + NaOH(aq) → H2O(l) + NaKC8H4O4(aq)

As antipyretic drugs and their derivatives are used as constituents in some aspirin products,
salicylic acid is one of the most popular skin care products. Numerous methods for analyzing
salicylic acid and its combinations in pharmaceuticals or biological fluids have been reported.
Salicylic acid has been measured in pharmaceutical preparations using titrimetric, UV-
spectrophotometer, and quantitative thin-layer chromatography (GC) (Sanghavi et al., 2013).

Potentiometry has been used to identify the endpoint in most titration setups for centuries
(Skoog et al., 2004). Potentiometric titrations measure the potential of an appropriate indicator
electrode as a function of titrant volume. The hydronium ion, H3O+, is detected by this indicator
electrode. The dissociation constant can be calculated by determining the pH at half-equivalence
(Peaper et al., 2013). Ka is calculated at half-equivalence using the formula below, according to
Reijenga et al. (2013):
[A−] = [HA], V= V(equiv.) /2

The purpose of this experiment involves two separate acid-base titration procedures. For
the standardization, the molarity of a sodium hydroxide solution (NaOH) was determined by
titrating a sample of potassium acid phthalate (KHP) with the NaOH. The standardized NaOH was
then used in the second procedure to determine the dissociation constant of the unknown weak
acid, salicylic acid (SA).
 Chapter II
Methodology

Experimental Locale
This experiment was conducted by the 2nd year BS Chemistry students at Chemistry
Department, CSM 101 laboratory at Western Mindanao State University located at Normal Road,
Baliwasan, Zamboanga City.

Gathering of Materials
A 100 mL Beaker, three 250 mL Erlenmeyer flask, 500 mL Erlenmeyer flask, 50 mL
burette, burette clamp, iron stand, Denver model top loading balance and analytical balance were
borrowed from the laboratory stock room. Also, 0.1 M NaOH pellets, KHP, and phenopthalein
indicator were also acquired. In the experiment for the potentiometric titration, a 250 mL Beaker,
100 mL graduated cylinder, 250 mL Erlenmeyer flask, 50 mL burette, hot plate, stirring rod,
spatula, iron stand, buret clamp, and pH meter were also borrowed. For the other materials such as
detergent liquid, wash bottle, distilled water, and so on were provided by the experimenters.

Preparation and Standardization of 0.1 M NaOH

In this process, a 1.88 g (Analytical grade reagent) was weighed through a top loading scale
(Denver model) and prepared on a 100mL beaker to be dissolved using a stirring rod and just
enough distilled water. Afterwards, it was transferred to a volumetric flask, then rinsing the beaker
two times to completely collect reagent into the flask. The flask was filled until the mark and then
was mixed by inverting it 3 times while holding its lid covering it tightly. Then, the flask was set
aside.
The burette was rinsed 3x with small amounts of NaOH solution draining it to the sink.
Afterwards it was filled with the solution and the initial volume was recorded. After putting it into
the clamp, KHP solution was titrated through dropwise addition of NaOH and succeedingly
dispensed 13.60 mL, 27.40 mL, and 39.80 mL to the flask until a color indication of faint pink
remained more than 30 seconds for each trial while swirling it. Lastly, the final volumes were
recorded, henceforth, coming upon the average amount that resulted in the reaction.

Preparation of Standard KHP

After the preparation of 0.1 M NaOH, three trials were prepared for the KHP weighing
0.24 g, 0.23 g and 0.23 g in a 250 mL Erlenmeyer flask. 75 mL distilled water and 4 drops of
phenolphthalein indicator was added to each of the flasks, afterwards was set aside.

Determination of Weak Acid Dissociation Constant

On a 250 mL beaker, two trials were prepared for an unknown acid sample with a mass of
0.35 g Salicylic acid (Analytical grade reagent) for trial 1 and 0.38 g for trial 2 weighed using
Analytical balance (Denver model) to be dissolved with a 100 mL distilled water each using a hot
plate then was set aside covered with watch glass after it was dissolved. Thereon, setting the
tabulated data for the computations in the excel spreadsheet was done. Before the experimenter’s
turn to use the electrode, a clean and dry 50 mL burette was prepared and filled with 0.08628 M
NaOH solution (Analytical grade reagent) and drain it to its tip. Thereafter, when the electrode
was already vacant to use, the experiment was then proceeded. Since the magnetic stirrer was still
in use, the experiment was equally performed by the three group members, one was responsible
for holding the electrode and stirring the sample manually and the other one for dispensing the
NaOH solution and reading the pH every 10 seconds then the other was responsible for recording
data and calculating. For the first half, 2 mL of NaOH solution was dispensed and recorded until
10 mL was reached, thereon decreased to 1 mL until the 34 mL mark. Lastly,it was raised again to
2 mL until 50 mL mark. Trial 2 was not performed due to shortage of time. After gathering data,
the graph was then plotted and data was calculated.

Proper Storage of Apparatus and Proper Waste Disposal

After the experiment, cleaning of the workplace and apparatus used was done to ensure the
place was clean for the other experimenters to utilized the workplace and to return the apparatus
properly to the stock roon in its normal condition. Also, the wastes were properly disposed.

Data Gathering Procedure

The volume and molarity of the standardized NaOH solution and weight of KHP was
recorded and calculated. In the determination of weak acid dissociation constant, the pH and
volume of NaOH solution was obtained to determine the equivalence point, half-equivalence point,
first and second derivative. Hence, the obtained data were graphed using Microsoft Excel.
 Chapter III
Results and Discussion

RESULTS

Table 1. NaOH Pellet Analysis

Weight of NaOH pellets (g) 1.88 g
Total volume of diluted sample (mL) 500 mL

Table 1 shows the weight of NaOH pellets of 1.88 g with the total volume of diluted sample
of 500 mL.

Table 2. Titration Data

Trial 1 Trial 2 Trial 3
Weight of KHP (g) 0.24 g 0.23 g 0.23 g
Initial volume of NaOH solution (mL) 0.00 mL 13.60 mL 27.40 mL
Final volume of NaOH solution (mL) 13.60 mL 27.40 mL 39.80 mL
Volume of NaOH solution used (mL) 13.60 mL 13.80 mL 12.40
Average volume of NaOH (mL) 13.26 mL
Average molarity of NaOH (M) 0.08628 M

Table 2 shows the weight of KHP for the three trials yielding a result of 0.24 g, 0.23 g, and
0.23 g, respectively. The initial volume of the NaOH solution (0.1 M) yielded a result of 0.00 mL,
13.60 mL, and 27.40 mL for each trials. Whereas, the final volume of the NaOH solution (0.1 M)
garnered a result of 13.60 mL, 27.40 mL, and 39.80 mL with the volume of NaOH solution used
of 13.60 mL, 13.80 mL, and 12.40 mL, respectively. Hence, the average volume of NaOH yielded
an average of 13.26 mL while the average molarity of NaOH calculated was 0.08628 M.

Table 3. Weight of the Unknown Weak Acid

Trial Mass of SA (g)
1 0.35 g
2 0.38 g

Table 3 indicates the weight of the unknown weak acid for the two trials with a garnered
mass of 0.35 g and 0.38 g.

Table 4. Sample Titration Data of the Unknown Weak Acid

TRIAL 1
Volume of NaOH pH Volume of NaOH pH
0.00 mL 1.66 24.00 mL 2.78
2.00 mL 1.76 25.10 mL 2.85
4.00 mL 1.79 26.00 mL 2.93
6.10 mL 1.81 27.00 mL 3.02
8.00 mL 1.90 28.10 mL 3.12
 10.10 mL 2.01 29.00 mL 3.23
11.00 mL 2.07 30.00 mL 3.36
12.10 mL 2.12 31.00 mL 3.54
13.20 mL 2.17 32.00 mL 3.81
14.10 mL 2.22 33.10 mL 4.38
15.00 mL 2.26 34.00 mL 9.87
16.00 mL 2.31 36.00 mL 11.15
17.10 mL 2.37 38.00 mL 11.48
18.00 mL 2.41 40.10 mL 11.67
19.00 mL 2.47 42.10 mL 11.80
20.00 mL 2.52 44.00 mL 11.89
21.00 mL 2.58 46.00 mL 11.97
22.00 mL 2.64 48.00 mL 12.04
23.10 mL 2.71 50.20 mL 12.09

Table 4 presents the volume of NaOH solution dispensed in the titration process by
increments and the pH of the unknown weak acid solution was recorded after each addition of
solution.

Table 5. Half-equivalence Point Data

Trial 1
Volume of NaOH (mL) pH
14.10 2.22
15.00 2.26
16.00 2.31
17.10 2.37
18.00 2.41
19.00 2.47
20.00 2.52

Table 5 indicates the obtained half-equivalence of 17.10 mL with a pKa of 2.37 from the
estimated equivalence point of 34.00 mL.

Table 6. First Derivative Data

Vol. NaOH pH pH V Vavg pH/V

31.00 3.54
32.00 3.81 0.27 1.00 31.50 0.27
33.10 4.38 0.57 1.10 32.55 0.52
34.00 9.87 5.49 0.90 33.55 6.10
36.00 11.15 1.28 2.00 35.00 0.64
38.00 11.48 0.33 2.00 37.00 0.17
40.10 11.67 0.19 2.10 39.05 0.09
 Table 6 shows the obtained result for the first derivative yielding a rate of change in pH
and volume to produce a spiked curve.
Table 7. Second Derivative Data and Plot
Vavg pH/V (V) (pH/V) Vavg (pH/V)/(V)
31.50 0.27
32.55 0.52 1.05 0.25 32.03 0.24
33.55 6.10 1.00 5.58 33.05 5.58
35.00 0.64 1.45 -5.46 34.28 -3.77
37.00 0.17 2.00 -0.48 36.00 -0.24
39.05 0.09 2.05 -0.07 38.03 -0.04

Table 7 shows the obtained result for the second derivative with the rate of change of the
first derivative with respect to the average volume.

Weak Acid Titration

14.00
12.00
10.00
8.00
pH

6.00
4.00 Estimated as 34.00 mL
2.00
0.00
0.00 5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00 45.00 50.00 55.00
Vol. NaOH

Figure 1. Titration curve of the pH against the volume of unknown weak acid

Shown in figure 1 was the plot of the first titration curve with the volume of NaOH on the
x-axis and the pH on the y-axis. The location of the equivalence point was estimated to be 34.00
mL wherein this point of the curve signifies the maximum slope in the titration.
 At half-equiv. pt. pH vs. Vol. SA
2.55
2.50
2.45
2.40
pH 2.35
2.30
2.25
2.20
14.00 15.00 16.00 17.00 18.00 19.00 20.00
Vol. NaOH

Figure 2. Estimation of pKa at the half-equivalence point

Shown in figure 2 was the point of the curve or the buffer point at which the estimate of
the dissociation constant of unknown acid was titrated. The equivalence point in this titration was
34.00 mL with the buffer point at 17.10 mL and pKa of approximately 2.37. Hence, this was a
significant factor in determining the unknown acid sample.

First Derivative Curve

7.00
6.00
5.00
pH/V

4.00
3.00
2.00
1.00
0.00
31.00 32.30 33.60 34.90 36.20 37.50 38.80
Vavg

Figure 3. First Derivative Curve

Shown in figure 3 was the plot of the rate of change with the change in volume against the
volume calculated in the first derivative plot. And so, a spiked curve was produced and its peak
was at the equivalence point.
 Second Derivative Curve
8.00

6.00

(pH/V)/(V)
4.00

2.00

0.00
31.00 32.00 33.00 34.00 35.00 36.00 37.00 38.00 39.00
-2.00

-4.00

-6.00
Vavg

Figure 4. Second Derivative Curve

Shown in figure 4 was the plot for the second derivative which presents a more precise
perspective in the determination of the titrant’s volume. Also, this passes through the x-axis at
equivalence point of approximately 34.00 mL.

DISCUSSIONS
The preparation of 0.1 M NaOH solution for 500 mL of 0.1 M NaOH was done by
determining the weight of the reagent-grade NaOH pellets, 1.88 g of NaOH pellets placed in a 100
mL beaker were obtained using a top loading balance (Denver model). As such, the distilled water
was added to the beaker containing the NaOH pellets to completely dissolve the pellets by stirring
using a stirring rod. The beaker started to feel slightly warm due to the reaction being exothermic.
The solution was transferred entirely into a 500 mL volumetric flask by washing it with distilled
water and then adding more until the marker of the flask was reached.

After all of the preparations, the solution was standardized. In NaOH, the potassium
hydrogen phthalate (KHP) was utilized and prepared by weighing 0.24 g, 0.23 g, and 0.23 g of
KHP for the three trials into a three clean 250 mL Erlenmeyer flasks and adding 75 mL of distilled
water to each of the flask to dissolve the KHP sample. 4 drops of phenopthalein indicator was
added into the solution to help the solution turn pink for at least 30 seconds during the swirling
phase, indicating its endpoint. The NaOH solution was then transferred to a burette and dispended
into the flask containing the KHP solution. After that, the solution was gradually titrated from the
burette into an Erlenmeyer flask and swirled for at least 15 to 30 seconds to see if it became pink.
Established formulas were employed to compute the volume of NaOH utilized and the molarity of
the NaOH solution. The initial reading of the burette was recorded to be 0.00 mL, 13.60 mL, and
27.40 mL with the final burette reading of 13.60 mL, 27.40 mL, and 39.80 mL, respectively. The
volume used was calculated by subtracting the final burette reading from the initial burette reading,
13.60 mL, 13.80 mL, and 12.40 mL with an average NaOH volume of 13.26 mL and average
NaOH molarity of 0.08628 M. Hence, both a good titrated solution and overtitrated solution were
obtained during the experiment.

On one hand, the weight of the unknown acid sample placed into two 250 mL beakers
obtained a 0.35 g and 0.38 g of acid sample for each two trial by using a analytical balance (Denver
model). A 100 mL of distilled water was then added to each beaker and was then covered with a
watch glass. The pH electrode was calibrated using a buffer but errors may occur due the differing
temperature of the experiment location. The electrode was thoroughly cleaned before utilization
to minimize errors in recording the pH value. The NaOH solution transferred in the burette was
dispensed by increments into the beaker containing the unknown acid solution and electrode while
manually stirring the solution. The data were then recorded and graphed. The half-equivalence
point of 17.10 mL was obtained with a pKa of 2.37 from the estimated equivalence point of 34.00
mL as shown in figures 1 and 2. With this, the identity of the unknown weak acid was determined
to be salicylic acid, a diprotic acid.

In the first derivative data, the rate of change of pH with the addition of NaOH solution
was at its maximum at the equivalence point. A spiked curved was produced as shown in figure 3
above as its peak occurs at the equivalence point. This occurred since the addition of equal
increments of NaOH solution were employed near the equivalence point. The addition of small
increments of the solution were done to lessen the calculations. The equivalence pont serves as the
maximum of figure 3, when extrapolated, occurs at 33.55 mL. Yet, this extrapolation may lead to
uncertainty although can be avoided partially in the second derivative plot shown in figure 4.

In addition, after the first derivative data and plot were obtained, the second derivative was
then plotted using the average of the two successive volumes used from the first derivative. The
second derivative was the rate of change of the first derivative with respect to the change in the
average volume. The equivalence point was taken to be 34.28 mL. Hence, extrapolation lessens
the reliability when specific numbers of more than one known points were required to infer the
unknown point as this relies on a refutable assumptions with regards to the behavior of the data
gathered.

Thus, the percent error was calculated to be 20.47%. The factors that may have contributed
to the errors were the junction potential of the electrode, lack of experimental equipments,
calibration of the electrode, the equilibration time of the electrode, and the room temperature.
 Chapter IV
Summary and Conclusions

The experiment was conducted for the purpose of standardizing NaOH and determining
the weak acid dissociation constant. Standardization determines the exact concentration of a
solution. Standardization uses titration as in titration exact volume of one substance react to find a
concentration of the unknown substance. It is an important process in chemistry as it gives
transparent and reliable results.
In the preparation of 500 mL 0.1 M NaOH, the experimenters obtained 1.88 g NaOH
pellets. The weight needed to prepare a 0.1 M concentration was 1.99≈2.0g NaOH. Meanwhile, in
the preparation of standard KHP, 0.24 g, 0.23 g, and 0.23 g were obtained for trials 1, 2, and 3
respectively. Moreover, in the standardization of NaOH the initial volume for trial 1 was 0.0 mL,
the final volume was 13.6 mL which means that the volume of NaOH that reacted with KHP is
13.6 mL. For trial 2, the initial volume was 13.6 mL and the final volume was 27.4 mL meaning
the volume of NaOH that reacted with KHP was 13.8 mL. Lastly, for trial 3, the initial volume
recorded was 27.4 mL and the final volume was 39.8 mL which signifies that the volume of NaOH
that reacted with KHP was 12.4 mL. The average volume of NaOH during titration was 13.26 mL.
The concentration of standard NaOH were 0.08640 M, 0.08161 M, and 0.09082 M for each three
trials giving an average of 0.08628 M NaOH.
Potentiometric titration belongs to chemical method of analysis in which the endpoint of
the titration was monitored with an indicator electrode that records the change of the potential as
a function of the amount (usually the volume) of the added titrant of exactly known concentration.
The weight of Salicylic acid obtained during the experiment 0.35 g. In the plot against
volume of Salicylic acid, the point at which the acid dissociation constant of the acid being titrated
was estimated as 34.00 mL. Thus, the equivalence point occurs at 34.00mL, the half-equivalence
point at 17.10 mL, and the pKa was approximately 2.37 whereas the true value of pKa was 2.98.
The first derivative plot or the maximum slope of the titration curve occurs at 33.55 mL. This
extrapolation leads to an uncertainty that can be partially avoided by a second derivative plot. In
this case, the second derivative plot occurred at approximately 34.00 mL with a percent error of
20.47%.
Hence, the electrode's junction potential, a lack of experimental equipment, electrode
calibration, electrode equilibration time, and room temperature were all factors that could have
contributed to the errors.
 Appendix

Calculations

Standardization of NaOH solution using KHP

A. Weight of NaOH needed to prepare a 0.1 M concentration

molesNaOH = MNaOH x VNaOH

MassNaOH = molesNaOH x MWNaOH

molesNaOH = (o.1 M) (0.5 L) = 0.05 mol NaOH

39.997 g
MassNaOH = (0.05 mol) ( 1 mol ) = 1.99 ≈ 2.0 g NaOH

B. Volume of NaOH required to react with KHP

VNaOH = Final Volume – Initial Volume

Trial 1: VNaOH = 13.60 mL – 0.00 mL = 13.60 mL NaOH

Trial 2: VNaOH = 27.40 mL – 13.60 mL = 13.80 mL NaOH
Trial 3: VNaOH = 39.80 mL – 27.40 mL = 12.40 mL NaOH

C. Average volume of NaOH during titration

𝒙𝟏 + 𝒙𝟐 + 𝒙𝟑 …+ 𝒙𝒏
Average volume of NaOH =
𝒏

13.60 mL + 13.80 mL + 12.40 mL

Average volume of NaOH = = 13.26 mL NaOH
3

D. Concentration of standard NaOH and its average

𝐰𝐞𝐢𝐠𝐡𝐭 𝐨𝐟 𝐊𝐇𝐏
𝐌𝐖 𝐊𝐇𝐏
Molarity (M) =
𝐕𝐨𝐥.𝐍𝐚𝐎𝐇 𝐮𝐬𝐞𝐝
0.24 g KHP
204.23 g/mol 0.001175 mol
M1 =
0.0136 L
= 0.0136 L
= 0.08640 M

0.23 g KHP
204.23 g/mol 0.001126 mol
M2 =
0.0136 L
= 0.0138 L
= 0.08161 M

0.23 g KHP
204.23 g/mol 0.001126 mol
M3 =
0.0136 L
= 0.0124 L
= 0.09082 M
 0.08640 M + 0.08161 M + 0.09082 M
Average Molarity of NaOH = = 0.08628 M NaOH
3

Potentiometric Titration of a Salicylic Acid (SA)

pKa True value of SA = 2.98

pKa Experimental value of SA = 2.37

|𝐄𝐱𝐩𝐞𝐫𝐢𝐦𝐞𝐧𝐭𝐚𝐥 𝐯𝐚𝐥𝐮𝐞−𝐓𝐫𝐮𝐞 𝐯𝐚𝐥𝐮𝐞|

% Error = x 100%
𝐓𝐫𝐮𝐞 𝐯𝐚𝐥𝐮𝐞

|2.37−2.98| 0.61
% Error = x 100% = x 100% = 20.47%
2.98 2.98

Documentations

Standardization of NaOH

Potentiometric Titration of SA
 References

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