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Department of Chemical Engineering

ELA 301

University of Benin

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TITLE PAGE
Title of Experiment: ACID VALUE OF OIL
Aim of the Experiment: TO DETERMINE THE ACID VALUE OF THE GIVEN
SAMPLE OF OIL

Date of the Experiment: 13/04/2023


Experiment Number: 02
Name of Student: MORDI FAVOUR GOD’SPOWER
Matriculation Number: ENG1905016
Serial Number: 50
Group: A6
Level: 300
Course Code: ELA 301
Name of Instructor: MR MOSES OGHENEVO

TABLE OF CONTENTS
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TITLE PAGE.................................................................................................................II
TABLE OF CONTENTS................................................................................................III
List of Figures and Tables.........................................................................................IV
List of figures........................................................................................................IV
List of Tables.........................................................................................................IV
ABSTRACT..................................................................................................................V
INTRODUCTION.........................................................................................................1
THEORY......................................................................................................................3
DESCRIPTION OF APPARATUS...................................................................................6
PROCEDURE...............................................................................................................9
RESULTS AND CALCULATIONS.................................................................................10
DISCUSSION.............................................................................................................11
SAFETY PRECAUTIONS TAKEN.................................................................................11
CONCLUSION...........................................................................................................12
RECOMMENDATIONS..............................................................................................13
REFERENCES............................................................................................................14
APPENDIX................................................................................................................15

List of Figures and Tables


List of figures

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Figure 1: Structures of some common lipids. At the top are cholesterol and oleic
acid. The middle structure is a triglyceride composed of oleoyl, stearoyl, and
palmitoyl chains attached to a glycerol backbone. At the bottom is the common
phospholipid phosphatidylcholine............................................................................3
Figure 2: Chemical reaction between glycerol and fatty acids when forming
Triglyceride................................................................................................................3
Figure 3: Measuring Cylinder....................................................................................6
Figure 4: Retort Stand...............................................................................................6
Figure 5: Funnels.......................................................................................................7
Figure 6: Beaker.........................................................................................................7
Figure 7: Burette........................................................................................................7
Figure 8: Weighing Balance.......................................................................................8

List of Tables
Table 1: Experimental Values..................................................................................10

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ABSTRACT
In this experiment, the quality of a sample of palm kernel oil was examined by determining the
acid value of the oil. The determination of acid value is an important process in the food
industry to analyze the quality of oils before commercial distribution. The obtained average
acid value for the oil sample was 2.805 mg KOH/g. Based on the data, the rancidification of the
used oils are apparent due to the higher level of acid value as compared to the acceptable one
at 1 mg KOH/g. This showed the occurrence of rancidification, or the production of foul odor
and taste in fats.

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INTRODUCTION
Lipids are compounds that are defined based on solubility. They have low solubility in water
and high solubility in nonpolar solvents. The nonpolar nature of lipid is due to the large portion
of hydrocarbons in the molecule. Lipids have diverse biological functions, including being highly
concentrated energy sources, membrane components (structure), and molecular signals.

Biological lipids are either hydrophobic, containing only nonpolar groups, or amphipathic,
possessing both polar and nonpolar groups. Fatty acids are amphipathic lipids because they
have polar carboxylic acid group and a long nonpolar hydrocarbon tail. They normally have
even number of carbon atoms. Presence of carbon-carbon double bonds in a fatty acid chain
makes it unsaturated. While fatty acids with only single bonds are saturated. Unsaturated fatty
acids are usually in cis configuration rather than trans.

Derivatives of fatty acids include fats and oils which serve as stored forms of energy in living
organisms. Fats and oils are triglycerides or triacylglycerols. They are lipids that are formed
through ester linkages between three hydroxyl groups (of glycerol) and fatty acids. The
apparent distinction between fat and oil is that the former is a solid at room temperature
making it saturated while the latter is liquid at room temperature making it unsaturated. Fatty
acid composition in fats and oils has been explored due to its association with health-related
risks.

The objective of the experiment is to determine the acid value of commercially available palm
kernel oil.

The acid value (or neutralization number or acid number or acidity) is the mass of potassium
hydroxide (KOH) in milligrams that is required to neutralize one gram of a chemical substance.
The acid number is a measure of the number of carboxylic acid groups in a chemical compound,
such as a fatty acid, or in a mixture of compounds. The acid value of a chemical compound
affects the compound in the following ways:

a. Higher acid value means increased health risk if consumed


b. Higher acid value compounds allow faster appearing but less stable froth creation.
c. Lower acid value compounds allow slower to appear but more stable froth formation.
d. Lower acid value means more cleansing (detergency).
e. Acid value is used only on fatty acids to provide an estimate of saponification value. The acid
value for fatty acids is very close to the saponification. Acid value usually runs about 2 points
lower than the saponification value.
f. Higher acid value allows faster corrosion of metals.

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The acid value of an oil is determined by titrating a solution of the oil with an alcoholic
solution of sodium or potassium hydroxide. It is expressed as the amount of KOH (in mg) to
neutralize 1 g of oil.

Fats undergo rancidification or production of foul odor and taste. There are three types:
oxidative rancidity, hydrolytic rancidity, and microbial rancidity. Oxidative rancidity is due to the
fats undergoing oxidation reaction and consequent elevation of peroxide values in the sample.
Hydrolytic rancidity is due to the cleavage of double bonds in unsaturated fatty acids, producing
volatile aldehydes and ketones, as well as free fatty acids. Microbial rancidity is due to the
presence of microorganisms and enzymatic activity that break down fat. This results to a lower
quality of fats. The World Health Organization Food and Agriculture Organization (WHO/FAO)
guideline sets the maximum allowable limit for edible oils quality parameters including acid
value (0.6 mg potassium hydroxide/g oil) moisture (0.2%), and peroxide value (10
millequivalents oxygen/kg oil) [19].

Often, the acid value is converted to a Free fatty acids (FFA) value. FFA are produced by
the hydrolysis of oils and fats. The level of FFA depends on time, temperature and moisture
content because the oils and fats are exposed to various environments such as storage,
processing, heating or frying. Since FFA are less stable than neutral oil, they are more prone to
oxidation and to turning rancid. Thus, FFA is a key feature linked with the quality and
commercial value of oils and fats.

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THEORY
A lipid is a macro-biomolecule that is soluble in nonpolar solvents. Non-polar solvents are
typically hydrocarbons used to dissolve other naturally occurring hydrocarbon lipid molecules
that do not (or do not easily) dissolve in water, including fatty acids, waxes, sterols, fat-soluble
vitamins (such as vitamins A, D, E, and K), monoglycerides, diglycerides, triglycerides, and
phospholipids. The functions of lipids include storing energy, signaling, and acting as structural
components of cell membranes. Lipids have applications in the cosmetic and food industries as
well as in nanotechnology.

Figure 1: Structures of some common lipids. At the top are cholesterol and oleic acid. The middle structure is a triglyceride
composed of oleoyl, stearoyl, and palmitoyl chains attached to a glycerol backbone. At the bottom is the common
phospholipid phosphatidylcholine

Oils are called triglycerides (or triacylglycerols) because they are esters composed of three fatty
acid units joined to glycerol, a trihydroxy alcohol:

Figure 2: Chemical reaction between glycerol and fatty acids when forming Triglyceride

An oil is any nonpolar chemical substance that is a viscous liquid at ambient temperatures and
is both hydrophobic (does not mix with water, literally "water fearing") and lipophilic (mixes
with other oils, literally "fat loving"). Oils have a high carbon and hydrogen content and are
usually flammable and surface active. Most oils are unsaturated lipids that are liquid at room
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temperature. The general definition of oil includes classes of chemical compounds that may be
otherwise unrelated in structure, properties, and uses. Oils may be animal, vegetable, or
petrochemical in origin, and may be volatile or non-volatile. They are used for food (e.g., olive
oil), fuel (e.g., heating oil), medical purposes (e.g., mineral oil), lubrication (e.g. motor oil), and
the manufacture of many types of paints, plastics, and other materials.

The quality of an oil can be measured in several different ways:

• Acid Value
• Free Fatty Acid measurement
• Peroxide Value Measurement
• Oil Color Measurement Kit
• TPM Method
ACID VALUE: The acid value is the mass of potassium hydroxide (KOH) in milligrams that is
required to neutralize one gram of chemical substance. The acid value of an oil is derived from
the following equation:
X x Mm x M 1
𝐴𝑐𝑖𝑑 𝑉𝑎𝑙𝑢𝑒 = Wo
Equation 1

Where:

X is the volume of KOH required to neutralize the oil solution


Mm is the molar mass of KOH
M1 is the concentration of KOH used
Wo is the weight of the oil

Often, the acid value is converted to an FFA content by multiplying the acid value with a factor
that equals the molecular weight of the fatty acid concerned (usually oleic acid, MW = 282.4)
divided by ten times the molecular Visit www.chearchive.tk for more 9 weight of the potassium
hydroxide (56.1). This factor ten stems from the fact that the acid value is expressed as mg/g,
whereas the FFA content is expressed as a percentage. When the FFA content is expressed as
‘wt% oleic acid,’ this factor therefore equals 0.50. And the relationship can be expressed as:

Acid Value
𝐹𝐹𝐴 = Equation 2
2

Hydrolysis of oil creates Free Fatty Acids in them. Raw oils and fats in their natural form contain
a small amount of free fatty acids but they are removed while refining the oil. FFA should not be
present in edible oils as oils with high FFA content decrease oxidative stability of the product
and increase acidity which results in off-flavor formation. Chemical analysis kits and several
automated hand-held instruments are also used to determine FFA concentrations in oils. FFA

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measurement color strips react to the presence of fatty acids in the tested oil. When they are
dipped in the oil, the colors will be visible on the strip, which is then compared to the given
color reference chart to define FFA levels. Standard test strips are made for the measurement
of free fatty acid levels from 2% – 7%, with 5.5%-7% as the discard range.

Other Methods for Analyzing the Quality of Oil

a. Peroxide Value Measurement: Detection of peroxide gives the initial evidence of rancidity in
unsaturated fats and oils. Other methods are available, but peroxide value is the most widely
used. It gives a measure of the extent to which an oil sample has undergone primary oxidation,
extent of secondary oxidation may be determined from p-anisidine test.

b. Total Polar Material (TPM) Method: The mass concentration of TPM is used as an indicator of
the quality of frying fats. According to official methods, the fat or oil is separated into polar and
non-polar fractions by preparative column chromatography (PCC).

c. Oil Color Measurement kit: Color is measured by the Lovibond tintometer, usually in red and
yellow terms. Most finished edible oils are less than 10 yellow and 2.5 red, with high-grade
shortenings being less than 1.0 red

Different fat samples may contain varying amounts of fatty acids. In addition, the fats often
become rancid during storage and this rancidity is caused by chemical and enzymatic hydrolysis
of fats into free fatty acids and glycerol. The amount of free fatty acids can be determined
volumetrically by titrating the sample with potassium hydroxide. The acidity of fats and oils is
expressed as its acid value or number which is defined as the mass of KOH required to
neutralize the free fatty acid present in 1g of fat or oil. The amount of free fatty acid present or
the acid value of fat is a useful parameter which gives an indication about the age and extent of
deterioration.

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DESCRIPTION OF APPARATUS
The apparatus used during the experimental work were:

 Measuring cylinder
 Retort Stand
 Funnels
 Beakers
 Burette
 Weighing Balance

The chemicals used for the experimental work were: palm kernel oil, benzene, ethanol,
potassium hydroxide, phenolphthalein indicator.

 Measuring Cylinder: A measuring cylinder, graduated cylinder or mixing cylinder is a


common piece of laboratory equipment used to measure the volume of a liquid. It
has a narrow cylindrical shape. Each marked line on the graduated cylinder
represents the amount of liquid that has been measured.

Figure 3: Measuring Cylinder

 Retort Stand: A retort stand, sometimes called a clamp stand or a ring stand, is a
piece of scientific equipment to which clamps can be attached to hold other pieces
of equipment and glassware – for instance, burettes, test tubes and flasks.

Figure 4: Retort Stand

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 Funnel: Funnels are apparatuses that have been made for use in the chemical
laboratory. It is used to channel liquid or fine-grained substances into containers
with a small opening.

Figure 5: Funnels

 Beaker: A beaker is a cylindrical container used to store, mix and heat liquids in
laboratories. Most are made of glass, but other non-corrosive materials, such as
metal and heat resistant plastic, are also used. Beakers usually have a flat bottoms
and a lip around the top.

Figure 6: Beaker

 Burette: A burette is a graduated glass tube with a tap at one end, for delivering
known volumes of a liquid, especially in titrations. It is a long, graduated glass tube,
with a stopcock at its lower end and a tapered capillary tube at the stopcock's
outlet.

Figure 7: Burette

 Weighing Balance: A weighing balance is a device to measure weight or mass. These


are also known as mass scales, weight scales, mass balances, weight balances. The

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traditional scale consists of two plates or bowls suspended at equal distances from a
fulcrum.

Figure 8: Weighing Balance

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PROCEDURE
a. 1.5g of palm kernel oil was weighed in a beaker
b. A mixture of 50ml benzene and 50ml ethanol was put in a separate beaker, and titrated
against potassium hydroxide using phenolphthalein indicator until the color changes to
pale pink. And the volume of KOH used was recorded.
c. Another mixture of 50ml benzene and 50ml ethanol was made and added to the 1.5g of
palm kernel oil in a beaker.
d. The new mixture was titrated against KOH using phenolphthalein indicator until the
color changed to pale pink, and the volume of KOH used was recorded.

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RESULTS AND CALCULATIONS
With Oil Without Oil
Initial Reading 0.00 0.90
Final Reading 0.90 1.70
Volume of Base Used 0.90 0.80
Table 1: Experimental Values

Volume of potassium hydroxide used for titration of benzene and ethanol mixture was 0.8ml
(Let this be given the variable Vb)

Volume of potassium hydroxide used for titration of oil, benzene and ethanol mixture was 0.9
(Let this be given the variable Vo)

Volume of potassium hydroxide required to neutralize the oil solution is

𝑋 = 𝑉𝑜 − 𝑉𝑏 𝑋 = 0.9 – 0.8; 𝑋 = 0.1𝑚𝑙

The acid value of oil can be found using equation 1:

X x Mm x M 1
𝐴𝑐𝑖𝑑 𝑣𝑎𝑙𝑢𝑒 𝑜𝑓 𝑜𝑖𝑙 =
W0

Where, The concentration of KOH used, M1 = 0.5mol/L The molecular weight of KOH, Mm =
56.1g/mol The weight of oil sample, Wo = 1.0g Volume of KOH required for neutralization, X =
0.1ml Putting all the values into equation 1.1 and solving for the acid value;

(0.90−0.80)× 56.1× 0.5


𝐴𝑐𝑖𝑑 𝑣𝑎𝑙𝑢𝑒 𝑜𝑓 𝑜𝑖𝑙 =
1.0

𝑨𝒄𝒊𝒅 𝒗𝒂𝒍𝒖𝒆 𝒐𝒇 𝒐𝒊𝒍 = 2.805𝒎𝒈 𝑲𝑶𝑯/𝒈 𝒐il

The free fatty acid value2 of oil can be found by dividing the acid value by 2.

Acid value 2.805


𝐹𝐹𝐴 = = =1.4025%
2 2

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DISCUSSION
FFA are produced by the hydrolysis of oils and fats. The level of FFA depends on time,
temperature and moisture content because the oils and fats are exposed to various
environments such as storage, processing, heating or frying.

Since FFA are less stable than neutral oil, they are more prone to oxidation and to turning
rancid. Thus, FFA is a key feature linked with the quality and commercial value of oils and fats.

The oil under analysis has a low FFA of 1.4025%; thus is fit for consumption. A major factor
which could lead to the increased FFA of the oil include the long amount of time which the oil
has been in the laboratory. Since temperature has an effect on the FFA of an oil, it is thus not
advisable to use the same oil for frying over a period of time. As the continuous heating and
reheating of the oil would lead to an increased FFA and thus become dangerous to health.

According to the world health organization standards, all edible oils should have acid values of
not more than 1 mg KOH/g oil. The oil analyzed in this experiment, however, has an acid value
of 2.805. This shows that this oil is suitable for consumption, as it would not be poisonous to
humans and it has a low potential for rancidification.

SAFETY PRECAUTIONS TAKEN


a. Care was taken to avoid spilling any of the chemical compounds on the skin.

b. The observed color change on titration was allowed to remain for some time before readings
were taken.

c. The weight of the beaker was reset to zero before weighing the oil to avoid zero error.

d. A small beaker was used to weigh the oil to ensure the total weight was within the capacity
of the weighing balance.

e. Care was taken to avoid parallax error when taking burette readings

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CONCLUSION
The acid value of the oil was found to be 2.805mg KOH/g oil; whereas the FFA value was found
to be 1.4025%. Thus, the oil analyzed is fit for commercial distribution and consumption.

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RECOMMENDATIONS
These are my recommendations for future experiments having the same aim to achieve
accuracy and save time;

a. Results showed that the oil sample used in the experiment has a higher acid value to
that of the acceptable level. This is due to the type of oil used. Rancidification also
occurs over time, and repeated use of the fats can easily promote processes for either
of the three types of rancidity to occur. It is recommended to use fresh sample of oil to
test for the acid values for consumption. This will ensure the quality of the commercially
available edible oils.
b. Other values to test the quality of fats may also be tested, such as peroxide value,
anisidine value and TBA value.
c. Future experiments should involve the analysis of fuel oils for the determination of
their acid values. This would broaden the understanding of the student to how acid
value affects the corrosion of metals.

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REFERENCES
a. Allen, J.C., Hamilton, R.J. (1994). Rancidity in foods. Springer-Verlag, GmbH.

b. Campbell, M., Farrel, S. (2013). Biochemistry (8th edition). USA: Cengage Learning.

c. Freeman, I. P. (2000). Ullmann’s encyclopedia of industrial chemistry, margarines and


shortenings.

d. p-Anisidine value: (2012). Analysis system for fats and oils. FoodLab Quality Control Systems
for Food and Beverage. Retrieved (May 19, 2016):
http://www.cdrfoodlab.com/food-analysis/anisidine-valuefats.html

e. Garret, R., and Grisham, C., (2010). Biochemistry (5th ed.)

f. Grossi, M., Di Lecce, G., Arru, M., Gallina, Toschi, T., Rocco, B. (2015). Journal of food
engineering, an opto-electronic system for in-situ determination of peroxide value and total
phenol content in olive oil.

g. Luck, E., Lipinski, G-W., (2002). Ullmann’s encyclopedia of industrial chemistry, foods, food
additives. Wiley-VCH, Weinheim. Nelson, D., Cox, M. (2012). Leningher principles of
biochemistry (6th edition). USA: W.H. Freeman and Company.

h. Thomas, A. (2005). Ullmann’s encyclopedia of industrial chemistry

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APPENDIX
ACID VALUE: The acid value is the mass of potassium hydroxide (KOH) in milligrams that is
required to neutralize one gram of chemical substance. The acid value of an oil is derived from
the following equation:

X x Mm x M 1
𝐴𝑐𝑖𝑑 𝑉𝑎𝑙𝑢𝑒 =
Wo

Where:

X is the volume of KOH required to neutralize the oil solution

Mm is the molar mass of KOH

M1 is the concentration of KOH used

Wo is the weight of the oil

Acid Value
𝐹𝐹𝐴 =
2

A fatty acid is a carboxylic acid with a long aliphatic chain, which is either saturated or
unsaturated. Most naturally occurring fatty acids have an unbranched chain of an even number
of carbon atoms, from 4 to 28. Fatty acids are usually not found in organisms in their
standalone form, but instead exist as three main classes of esters: triglycerides, phospholipids,
and cholesteryl esters. In any of these forms, fatty acids are both important dietary sources of
fuel for animals and they are important structural components for cells

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