FINAL LABORATORY REPORT

EXPERIMENT 1: DETERMINATION OF TOTAL ACIDITY OF VINEGAR

Don King O. Evangelista1, Geneizzel B. Gotuato1, Jackielyn B. Ocbina1, Jann Andre H. Padua1
1
Group 2, III-Bachelor of Science in Chemistry for Teachers, Philippine Normal University
Performed June 21, 2012
Professor Allen A. Espinosa, CHEM5 Professor

ABSTRACT
The experiment aims to determine the accurateness of the data presented
by vinegar-manufacturing factories in the Philippines as their acetic acid
content in their labels using the direct titration method, specifically the
analyte Datu Puti. Three samples of 25.0 mL aliquot volumes were titrated
using the KHP-standardized NaOH sample which is found to be of 0.05962
M using the indicator phenolphthalein with observance to its equivalence
point. Data shows that the percent acetic acid of Datu Puti whether by
weight or by volume is less than the alleged 8% acetic acid content
according to its label, but with consideration to the computed relative error
of 35.73%. The experimenters commend the titration process but
recommend to lessen errors such as systematic and instrument errors.

I. Introduction

Acid-base titrations are used routinely in virtually all fields of chemistry and in related areas,
such as biology, pharmacy, medicine and geology. In addition to inorganic compounds, thousands of
organic compounds exhibit sufficient acidity and basicity that they can be determined by titration.
Excellent understanding of acid-base properties, together with the relative ease, speed and low-cost of
performing titrations, are major factors contributing to the popularity of the acid-base titration. 1 In this
experiment, an organic compound, household vinegar which is mainly used in cooking and bleaching, is
subjected to the titration process, specifically direct titration, for analyses of its concentration and percent
acetic acid as compared to its reported percent acetic acid written on its labels. Direct titration is a kind of
titration where the reactants involved are primarily the titrant and the analyte aA + tT  pP. 2
This experiment aims to (1) Test the reliability of the reported vinegar content of acetic acid in
the label by titration process, (2) Experience how analysts go over the processes of quantitative analysis
through the experiment and (3) Manifest appreciation of Chemistry by maintaining accuracy and
precision in the experiment without sacrificing time and resources.
Generally, titrations are performed to determine the amount of analyte present in a sample. To do
this, the volume of titrant needed to reach the equivalence point must be measured. An “equivalence
point” by definition means “occurs when all the moles of H+ ions present in the original volume of
acid solution have reacted with an equivalent number of moles of OH- ions added from the buret. 4”

1 Determination of Total Acidity of Vinegar | GROUP 2 – III-BSCT

These equivalence points were determined most often by chemical indicators, in this case
phenolphthalein, primarily because of the inherent simplicity of this technique, but also because of
availability of many excellent indicators. These acid-base indicators are weak organic acids or bases
whose conjugate forms different colors. The indicator acts as a second acid or base in the solution being
titrated and must be weaker than the analyte acid or base so that it reacts last with the titrant. The amount
of indicator added must be kept small compared to that of the analyte present so that it does not consume
an appreciable amount of titrant in the process of “indicating” or changing from one conjugate form to the
other. For this reason, indicators must be very intensely colored so that only a few drops of a dilute
solution, for this experiment, phenolphthalein with a color of pink, are needed to produce a color that is
observed by the eye. 1
Before titration, the standardization of the molarity of NaOH must be made using potassium
hydrogen phthalate, often abbreviated KHP with a molecular formula of KHC 8H4O4. This compound has
a high equivalent weight and is not hygroscopic. This compound, being a weak acid, the pH at the
equivalence point of its titration with a strong base is in the alkaline region makes it as a good primary
standard on standardizing bases.
Acetic acid, the acid found in vinegar, is in definition a weak acid. Therefore, the titration to be
made is a weak acid titration to a strong base, which is NaOH. The reaction of this titration is:
CH3COOH + OH-  CH3CO2- + H2O1
In this reaction, we can divide it into four. Before the addition of the titrant, the main constituent
is only the acetic acid, which the experimenters will treat as a weak acid. Before the equivalence point,
acetic acid is also present plus the presence of CH 3COONa that is now a buffer. At the equivalence point,
CH3COONa is only present which a weak base is now. After the equivalence point, CH 3COONa is
present plus NaOH, which is now a strong base. 1
Another concept is that vinegar has a high acid concentration, thus it is good to dilute the sample
by incorporating aliquots to it. By diluting it, the quantity of the acetic acid in the bottle of vinegar can be
determined by introducing a “dilution factor.” This factor will relate the amount of acetic acid in the
diluted vinegar solution per volume of portions of the aliquot. 3
With these concepts in hand, the percent by weight and percent by volume of acetic acid in the
sample can now be easily determined and calculated.

II. Methodology

Ample amounts of vinegar from the bottle of Datu Puti randomly picked in the supermarket were
undergone in an analysis. This was undergone into a quantitative analysis using direct titration and

2 Determination of Total Acidity of Vinegar | GROUP 2 – III-BSCT

phenolphthalein as an indicator against sodium hydroxide to determine the acetic acid content. The
following are the procedures in the direct titration process:
First, standardize the prepared assumed .1M NaOH against KHP in three trials with ranges of
weights from 0.2 to 0.3 g. These samples were distilled in 50 mL of distilled water and was titrated with
phenolphthalein indicator as endpoint. According to the data, the NaOH called for 16.07 mL, 18.22 mL
and 17.32 mL for the 0.195 g, 0.2171 g and 0.2074 g samples of KHP respectively.
Next, the density of the vinegar, denoted by d = m/v, is measured by the different groups by the
process of weighing and concept of the Archimedes principle which deducts the mass of the container
itself. From these data, the experimenters got the average mass of the 10 mL vinegar versus the volumes
and found out that the average density of vinegar is 0.98706 g/mL.
Lastly, the standardized NaOH from the first part, which is now measured with concentration of
0.05962 mol/L (M) was now utilized to direct titrate the three samples of vinegar aliquot with
phenolphthalein indicator. The vinegar aliquot is produced by diluting a 25-mL sample of pure vinegar
with 250-mL of volumetric flask. Then, the titration proceeded. Phenolphthalein endpoint is indicated by
a faint pink color, exceeding this pink color means that the titration is above its endpoint. According to
the data tables, each 25.0 mL aliquot of acetic acid needed volumes of 37.4 mL, 35.9 mL and 46.9 mL of
NaOH for the three trials respectively.
The photo that follows shows the reactions and the succession of the titration process:

Figure 1: The Titration Process (from: Chemistry, The Molecular Nature of Matter and Change 4th Edition by
Silberberg)

After gathering all the data from the three parts, these data is plotted in data tables and are subject
for statistical treatments, specifically the usage of the mean, which indicated the central measurement and
the deviation, standard deviation, variance and coefficient of variance which are measures of variability.
3 Determination of Total Acidity of Vinegar | GROUP 2 – III-BSCT
 The schematic diagram on the following page explains and summarizes all procedures done in the
experiment.

Standardization of the Prepared 0.1 M NaOH Solution

KHP Weighing with ranges Dissolving it in 50 mL distilled Titrating it using the Titrate until end point of
from 0.2 to 0.3 g water prepared NaOH phenolphthalein is reached

Measurement of Density of Vinegar Sample

Measure mass of dry 50 mL beaker, 50 Get density of vinegar using the
Get the value of the mass of vinegar
mL beaker and 10 mL vinegar poured computed mass on Step 2 and the
using these data.
via pipeting. volume of vinegar (10 mL).

Determination of Acetic Acid Content in Vinegar

Make the vinegar aliquout by diluting
Titrate until end point of
25 mL acetic acid in 250-mL volumetric
Titrate these aliquot portions. phenolphthaleinis reached. Note the
flask by adding sufficient water. Add 2-3
final volume of NaOH in the base buret.
drops phenolphthalein afterwards.

Statistical Treatment of Data

4 Determination of Total Acidity of Vinegar | GROUP 2 – III-BSCT

III. Data and Results with Sample Calculations
The following data tables were computed first using a scientific calculator then rechecked using
MS Excel.
Table 1: Data for the Standardization of prepared 0.1 M NaOH
Details Trial
1 2 3
Mass of KHP (g) 0.195 0.2171 0.2074
mmol of KHP (204.23 g/mol) 0.9548 1.0680 1.0155
mmol of NaOH 0.9548 1.0680 1.0155
Final volume of NaOH (mL) 16.07 18.22 17.32
Initial volume of NaOH (mL) 0.00 0.20 0.50
Delivered volume of NaOH (mL) 16.02 18.02 16.82
Molarity of NaOH (mmol/mL or M) 0.0596 0.0589 0.06037
Average Molarity (mmol/mL or M) 0.05962
Deviation 0.00002 0.00072 0.00075
Relative Deviation 3.35 x 10-4 0.01207 0.01257
Standard Deviation 0.00105
Coefficient of Variance 1.7611 %

Supporting Calculations for Table 1 (using Data in Trial 1 with reference to Table 1)

1 mole KHP 1000 mmol KHP

 mmol of KHP = ( 0.195 g KHP ) ( 204.23 g KHP )( 1mole KHP )
=0.9548 mmol KHP

 Balanced equation of NaOH and KHP

NaOH + KHC8H4O4  KNaC8H4O4 + H2O
Mole ratio: 1 mmol of NaOH = 1 mmol of KHP, thus, mmol of NaOH corresponds also to each mmol of
KHP, therefore, mmol of NaOH = mmol of KHP.

 Molarity of NaOH = ( 0.9548 mmol NaOH

16.02mL NaOH )
=0.0596 M NaOH

0.0596 M + 0.0589 M +0.06037 M

 Average Molarity of NaOH = ( )=0.05962 M NaOH
3
 Deviation (|d|) = M – Mave
 d1 = 0.0596 – 0.05962 = 0.00002
 d2 = 0.0589 – 0.05962 = 0.00072
 d3 = 0.06073 – 0.05962 = 0.00075
 Relative deviation (dr) = di/M
 dr1 = 0.00002 / 0.05962 = 3.35 x 10-4

5 Determination of Total Acidity of Vinegar | GROUP 2 – III-BSCT

  dr2 = 0.00072 / 0.05962 = 0.01207
 dr3 = 0.00075 / 0.05962 = 0.01257

Σ di 2 (0.00002+ 0.00072+ 0.00075)2

 Standard Deviation (s) =
√ √ n− 1
S
=

0.00105
3 −1
=1.05 ×10− 3∨0.00105

 Coefficient of Variance (CV) = ×100 %= ×100 %=1.7611 %

M 0.05962

Table 2: Determination of Average Density and Mass of Vinegar

Volume Added
Entry 1 2 3
Volume of Vinegar (mL) 10.00
Mass of 50-mL beaker (g) 38.0696 40.0615 29.0932
Mass of beaker + 10 mL vinegar (g) 48.0853 49.7062 39.0447
Mass of 10 mL vinegar (g) 10.0157 9.6447 9.9515
Average mass of 10 mL vinegar (g) 9.8706
Average density (g/mL) 0.98706 g/mL
Volume of Vinegar taken from bottle (mL) 25.00
Mass of vinegar (g) 24.6765 g

Supporting Calculations for Table 2

Mass of 10 mL vinegar (g) = (Mass of beaker + 10 mL vinegar) – Mass of beaker

= 48.0853 – 38.0696
= 10.0157 g
Average Mass of 10 mL vinegar = (Sum of Three masses) / 3
= (10.0157 + 9.6447 + 9.9515)/3
=9.8706 g/mL
Average Density = Average Mass / Volume
= 9.8706 g / 10.00 mL
= 0.098706 g/mL
Mass of vinegar from Vinegar Taken from Bottle:
Density of vinegar = mass of vinegar / volume of vinegar
Therefore: Mass of vinegar = (density of vinegar)(volume of vinegar)
Since: Density of vinegar does not change (Intensive property)
Mass of Vinegar = (0.098706 g/mL)(25 mL)
= 24.6765 g

6 Determination of Total Acidity of Vinegar | GROUP 2 – III-BSCT

Table 3: Data on Determination of Datu Puti’s Acetic Acid Content
Details Trial
1 2 3
Average Molarity of NaOH (Table 1) (mmol/mL) 0.05962
Final volume of NaOH (mL) 37.4 35.9 46.9
Initial volume of NaOH (mL) 0.00 0.00 0.00
Delivered volume of NaOH, Vf – Vi (mL) 37.4 35.9 `46.9
Volume of aliquot (mL) 25.0
mmol NaOH 2.2297 2.1403 2.7961
mmol CH3COOH in aliquot 2.2297 2.1403 2.7961
Volume of Aliquot (mL) 25.0
Volume of Diluted Vinegar in Volumetric flask (mL) 250.0
Dilution Factor 10
mmol CH3COOH in volumetric flask (mL) 22.297 21.403 27.961
Mass of CH3COOH (60.06 g/mol) (g) 1.3393 1.2854 1.6793
Mass of 25.0 mL vinegar (from table 2) 24.6765 24.6765 24.6765
% CH3COOH (w/w) 5.4276 5.2090 6.8052
Average % of CH3COOH 5.8138%
Molarity of Vinegar (Acetic acid sol’n, mmol/mL) 0.053572 0.051416 0.067172
% CH3COOH (w/v) 5.3572% 5.1416% 6.7172%
Average % CH3COOH (w/v) 5.7386%
Deviation 0.3814 |-0.2156| 1.36
Relative Deviation 0.9335 0.8907 1.1705
Standard Deviation 1.3838
Coefficient of Variance 24.1138%
Accepted % acid value (from vinegar label) 8%
Absolute error (E) | -2.6428| |-2.8584| |-1.2828|
Relative error (Er ,%) 33.035% 35.73% 16.035%

Supporting Calculations for Table 3 using Trial 1

 mmol of NaOH = ( 37.4 mL NaOH ) ( 0.05962mLmmol

NaOH
NaOH
)=2.2297 mmol NaOH
 Balanced equation of NaOH and KHP
CH3COOH + NaOH  H2O + NaC2N3O3
Mole ratio: 1 mmol of NaOH = 1 mmol of acetic acid, thus, mmol of NaOH corresponds also to each
mmol of acetic acid, therefore, mmol of NaOH = mmol of acetic acid.
 mmol of acetic acid = 2.2297 mmol NaOH
 mmol of CH3COOH in aliquot =

( 2.2297 mmol acetic acid ) ( 250 mL vinegar

25 mL aliquot )
=22.297 mmol AceAcid

7 Determination of Total Acidity of Vinegar | GROUP 2 – III-BSCT

  mass of CH3COOH in volumetric flask =

( 22.297 mmol acetic acid ) ( 60.06 mmol acet . acid 1g

1 mmolacet . acid )( 1000 mg )
=1.3393 g AceAcid

 Molarity = 1.3393 g / 25 mL = 0.053572 M

 % acetic acid (w/v) = (1.3393 g/ 25 mL) x 100 % = 5.35%
 % acetic acid (w/w) = (1.3393 g/(25 mL x 0.98706 g/mL)) x 100% = 5.4272%
 Absolute error for (w/v) = 5.3572 % - 8% = |-2.6428|
 Relative error for (w/v) = (2.6428/8) x 100% = 35.73%

IV. Discussions and Guide Questions

According to the data tables shown in the third part of the report, these three points are noted.
(1) The expected molarity of the standard base NaOH falls short than expected.
According to Table 1 which shows the standardization of prepared 0.1 M NaOH against KHP, the
average molarity of the solution is roughly 0.05962 M, almost half than expected. Some factors that can
be accounted for is the reaction of solid sodium hydroxide with atmospheric carbon dioxide. This is the
most troublesome aspect of NaOH, as it reacts with atmospheric carbon dioxide in a reaction CO 2 + 2OH-
 CO32- + H2O. Both the solid reagent and its solutions can react this way; consequently, an already
standardized sodium hydroxide solution must be protected from atmospheric CO 2, thus before
preparation, distilled water is boiled because often distilled water is saturated with carbon dioxide and
after preparation it is immediately capped. Although the concentration of NaOH is reduced when it comes
to contact with carbon dioxide, its reactive capacity towards acids may not change. Unfortunately, the
most common application of sodium hydroxide titrants are for the titration of weak acids, which require
an indicator with a basic transition range, for this experiment, is phenolphthalein. In this case, each
carbonate ion will be titrated to bicarbonate, reacting with only one hydronium ion for the analyte in the
reaction: CO32- + H3O+  HCO3- + H2O. As a result, the effective concentration of the base solution is
decreased and a determinate error will be incurred as we can see in the results.
(2) The concentration of acetic acid in the vinegar is considerably low as compared to its reported
concentration.
Seen on Table 3, we can infer that more or less, the amount of acetic acid in the vinegar itself is
71% lower than expected. The experimenters got an average of 5.7386 than of the accepted value of 8%.
A factor that can be considered is that they may have other acids that can interfere with the results of the
experiment, for example, the carbonic acid formed with carbon dioxide.
(3) The data is not accurate but precise.

8 Determination of Total Acidity of Vinegar | GROUP 2 – III-BSCT

 According to the statistical treatment done to the data tables, the data is precise because the
deviations between the data is small and is supported by the coefficient of variance, however, it is not
accurate because there is a large error in the data as manifested by the results of the absolute and relative
errors computed.
The following are other points and the answers to the guide questions for discussion in reference
to the guide questions drawn from the laboratory manual.
[1] There is a need to boil distilled water since that distilled water is saturated with carbon dioxide. The
reaction is discussed above on the first point.
[2] The reaction of phenolphthalein with NaOH is as follows:
HC2H3OH (aq) + NaOH (aq)  H2O (l) + NaC2H3 (aq) (TITRATION RXN)
HIndic + H2O  H3O- + Indic- (INDICATOR RXN)

Figure 2: Shift of electrons in phenolphthalein that indicates its color. (Retrieved from: Fundamentals of Analytical
Chemistry 5th Edition)

[3] The faint pink color of phenolphthalein indicates that it reached its endpoint, therefore, the number of
moles of H+ is equal to the number of OH – ions in the solution. This color must be taken because excess
of this will lead to an error (darker pink color), as the equilibrium is disturbed. The factors that affect the
endpoint sharpness in this titration is the pH range of the selected indicator and the distinction of the
person of the color itself.

9 Determination of Total Acidity of Vinegar | GROUP 2 – III-BSCT

[4] The standard reagent is a strong base rather than a weak base because a weak base will result in partial
dissociation of the ions rather than if the base is strong, even if the acid is weak, the dissociation becomes
complete and a 1:1 stoichiometric ratio is achieved.
[5] As said in the preceding page, the data is not accurate but precise.
[6] The errors that are committed in this experiment are the following:
6.1 Determinate Errors
6.1.a Method Error. As said in the first point of the discussion part, the molarity of the
standardized NaOH is lower than to the expected. Therefore, the titration period became longer, and can
trigger contamination within the NaOH with its longer contact time with atmospheric conditions. The
experimenters accept the fact that the distilled water is not totally boiled and that NaOH was not secured
immediately, that most probably be the cause of the error. Another point is that three days is the gap
between the preparation of the NaOH stock and the standardization with KHP.
6.1.b Instrument Error. Instrument errors are inevitable since they are only machines
that do their functions. The analytical balance, due to its age, is hard to tare and has the tendencies to have
errors. It is greatly manifested by the fact that vinegar is expected to have a density greater than 1.00
g/mL which is the density of water since vinegar has more components than of water. Deriving the
relationship of mass (components) with density, it is expected as there is higher mass, the density also
increases.
6.1.c Personal Judgment Error. Measuring using pipet and burette is hard, since there
is called a parallax error or viewing error. This can be eliminated as well.
6.2 Indeterminate Error
6.2a Constant Error. As said in the discussion part, there is a speculation of other acids
present in the vinegar, for example, carbonic acid, lactic acid and such acids that can be formed during the
fermentation process of the vinegar. Lactic acid is produced during fermentation in line with carbon
dioxide. Therefore, this error is constant error and unavoidable.

V. Conclusions and Recommendations

In conclusion, the experiment “Determination of Total Acidity of Vinegar” assessed the
concentration of acetic acid in a famous brand of vinegar “Datu Puti” by comparing the reported value of
acetic acid versus experimental value. Direct titration process is employed with NaOH as standard base
and phenolphthalein as indicator. Results showed that the concentration of acetic acid in Datu Puti falls
considerably short rather to the reported value, however, this result has an error with a range of 35% that
is accumulated through many errors, most of them manipulative and can be avoided.

10 Determination of Total Acidity of Vinegar | GROUP 2 – III-BSCT

 The experimenters recommend the following points to be considered if the same experiment
would be repeated. First, take note that distilled water must be boiled to remove the saturated carbon
dioxide from the water that interferes with the data. Second, NaOH must be on its considerable
concentration, therefore, must be prepared in advance and standardize in advance to reduce time
consumption. Lastly, it would be best if titration must be done in different varieties of vinegar to find out
if which of the vinegar brands had the closest value to their reported concentration in their labels and
which of them is the most “acidic.”

VI. References
A. Directly Cited Books
(The superscripts here also refer to the superscripts that were used in the introduction, thus the parts
where superscripts are found are cited and the references were found here.)
1
Harris, Larry G. (1988). Analytical Chemistry (1st Edition). New Jersey. Prentice-Hill Inc. pp. 94-109.
2
DLSU Chemistry Faculty. (unpublished). Analytical Chemistry 1 Instructional Materials.
3
Silberberg, Martin S. (2006). Chemistry: The Molecular Nature of Matter and Change. New York: Mc-
Graw Hill. pp.118-119.
4
Roque, Adolfo P. (unpublished). Analytical Chemistry Laboratory Manual.
B. Photo Credits
Harvey, David. (2000). Modern Analytical Chemistry. New York: McGraw Hill. pp. 284-287
(Electronic Format)
Skoog, Douglas A., et al (2004). Fundamentals of Analytical Chemistry (8th Edition). Canada:
Brooks/Cole. pp. 368-375 (Electronic Format)
Silberberg, Martin S. (2006). Chemistry: The Molecular Nature of Matter and Change.(4 th
Edition) New York: Mc-Graw Hill. pp.118-119. (Electronic Format)

If you are wise and understand God’s ways, prove it by living an honorable life, doing good works with the humility that comes
from wisdom. But if you are bitterly jealous and there is selfish ambition in your heart, don’t cover up the truth with boasting and
lying. For jealousy and selfishness are not God’s kinds of wisdom. Such things are earthly, unspiritual and demonic. For
wherever there is jealousy and selfish ambition, there you will find disorder and evil of every kind.
But the wisdom from above is first of all pure. It is also peace loving, gentle at all times and willing to yield to others. It is full
of mercy and good deeds. It shows no favoritism and is always sincere. And those who are peacemakers will plant seeds of
peace and reap a harvest of righteousness.
James 3:13-18 (NLT)

To God be the glory!

/dke

11 Determination of Total Acidity of Vinegar | GROUP 2 – III-BSCT