Experiment 3 March 7, 2023

Introduction:
This experiment aims to determine the acid number for both used and fresh oil to relate it
to changes in the structure of the oil. The method being used to do so is a modified ASTM
standard method procedure. We were assigned used oil to titrate by preparing a diluted sample of
KOH, using 15 mL of 0.1 M KOH [2] diluted with isopropyl alcohol.
Oils are mainly composed of hydrogen and carbon molecules. Oils we use to cook food
are triglycerides, consisting of a molecule of glycerol with three fatty acids attached to it.
These molecules have ester linkages connecting the fatty acids; however, they are weak, and by
cooking/ frying the oil, they can break, releasing free fatty acids (FFA). These FFA are essential
to a certain degree, but oils get thicker and darker afterwards and contain a lousy taste. [1]
To keep track of the level of the oil, we measure the acid number of the oil in KOH/g:
Acid number = mgKOH/ g Oil sample [1]
This is done by calculating the amount of potassium hydroxide required to complete a reaction
with an oil sample, in our case, a used oil sample. The endpoint is determined by using thymol
blue. The KOH will then react with the FFA[1]
The suggested acid number is 2.5 mg KOH/g oil. [1]
We also need a blank titration to determine the difference between the KOH required to achieve
the endpoint colour and the amount needed for a reaction to occur.
We prepared a 0.006M KOH titrant [1] during the lab by diluting a 15 mL 0.1 M KOH
[2] solution with isopropyl alcohol. Then weighed empty 250 conical flasks and the ones with 2
mL of used canola oil to calculate the mass of the oils used in the 4 samples we had. Then added,
a pump of titration solvent [2]. Then added 3 drops of thymol blue.
We added the KOH to the oils until a teal coloured was reached and stayed for 20 seconds.
Then repeat the same titration steps without the oil for the blank titration.[3]
And after the lab, we shared answers with a group with fresh oil samples.[4]
During this lab, I learned the point of a blank titration because, during previous courses, I
had never done a blank. This is important because we were trying to reach the teal colour; it was
not immediate and took a couple of mL of titrant to achieve the colour.[3]
Procedure:
No errors were made from the steps of the procedure in the experiment 3 lab manual [1]

Data:
Table 1: FRESH oil sample raw data [4]
KOH concentration
(M)
Fresh oil sample # 1 2 3 4
Weight of flask (empty) 117.841 110.196 118.245 100.192
(g)
Weight of flask + oil 122.173 114.493 122.261 104.473
(g)
Weight of oil 4.332 4.297 4.016 4.281
(g)
Initial burette reading 24.00 40.00 16.00 26.00
(mL)
Final burette reading 36.30 48.42 24.70 32.60
(mL)
Volume of KOH 7.30 8.42 6.70 6.60
(mL0
Endpoint colour Teal Teal Teal Teal
Table 2: blank fresh oil raw data [4
Fresh oil sample # 1 2 3 4
Initial burette reading 33.00 25.00 28.91 32.85
(mL)
Final burette reading 37.30 28.91 32.85 36.40
(mL)
Volume of KOH 4.56 3.91 3.94 3.55
(mL)
Average KOH vol. (mL) 3.99
Table 3: used oil raw data [3]
KOH concentration
(M)
used oil sample # 1 2 3 4
Weight of flask (empty) 121.020 120.984 123.458 122.655
(g)
Weight of flask + oil 122.382 122.578 124.814 124.241
(g)
Weight of oil 1.362 1.594 1.356 1.586
(g)
Initial burette reading 10.30 21.26 31.50 16.85
(mL)
Final burette reading 19.85 31.50 41.50 26.55
(mL)
Volume of KOH 9.55 10.24 10.00 9.70
(mL)

Table 4: blank used oil raw data [3]

Fresh oil sample # 1 2 3 4
Initial burette reading 3.20 4.65 5.90 7.20
(mL)
Final burette reading 4.65 5.90 7.20 8.65
(mL)
Volume of KOH 1.45 1.25 1.35 1.45
(mL)
Average KOH vol. (mL) 1.38
Results:
Table 5: Fresh oil calculated data:
Fresh oil sample # 1 2 3 4
Corrected KOH value 3.31 4.43 2.71 2.61
(mL)
Weight of KOH 0.37 0.50 0.30 0.29
(mg)
Acid number 0.087 0.12 0.075 0.068
(mg KOH/g oil)
Grubbs test 0.022 1.4 0.54 0.85
Final calculated average
acid number 0.088
(mg KOH/g oil)

Table 6: used oil calculated data:

Used oil sample # 1 2 3 4
Corrected KOH value 8.17 8.86 8.62 8.32
(mL)
Weight of KOH 2.75 2.98 2.90 2.80
(mg)
Acid number 2.02 1.88 2.14 1.77
(mg KOH/g oil)
Grubbs test 0.418 0.449 1.18 1.13
Final calculated average
acid number 1.95
(mg KOH/g oil)
Sample calculation:

Average KOH vol. from table 4:

Ave = 1.45 + 1.25 + 1.35 + 1.45 /4.00
= 1.375 ml = 1.38 mL

Grubbs Test of Blank volumes:

Volume of KOH used from table 4:
1.45mL 1.25mL 1.35 mL 1.45 mL
Ave = 1.38

[5]
(".$%&".'()! *(".+%&".'()! *(".'%&".'()! *(".$%&".'()!
S=! $&"

S = 0.09574 = 0.0957
Questionable value = 1.25
G calculated = |questionable value – Ave| / S [5]
= |questionable value – Ave| / S
= | 1.25 – 1.38| / 0.0957
= 1.36
We can keep the value since table E.1 [5] states a 95% confidence is 1.463 or lower.

Corrected KOH value:

Average KOH value from table 4: 1.38 mL.
Volume of KOH from run #1, table 3: 9.55
Corrected KOH value = Ave KOH – Volume of KOH
= 8.17 mL
Weight of KOH:

‘true’ stock conc of used oil sample : 0.006 M

Volume (table 6 sample #1) : 8.17 mL / 1000 = 0.00817 L
Molar mass of KOH = 56.1g/mol [2]
,.,,- /01 203
Moles of KOH = 4
× 0.00817𝐿 𝐾𝑂𝐻
= 4.90 x 10^-5 moles of KOH
Mg of KOH = 4.90 x 10^-5 mol of KOH x 56.1g/mol
= 0.00275 g * 1000 = 2.75 mg of KOH

Acid number:
Acid number = mgKOH/ g Oil sample [1]
Oil weight sample 1 from table 3: 1.362
= 2.75 mg KOH/1.362 g Oil
=2.02 mgKOH/ g oil sample

Grubbs Test for acid #:

S = 0.1615
Ave = 1.95
Questionable value = 2.14
G calculated = |questionable value – Ave| / S [5]
= |questionable value – Ave| / S
= | 2.14 – 1.95| / 0.1615
= 1.18
We can keep the value since table E.1 [5] states a 95% confidence is 1.463 or lower.
Percent error:
Percent error = |observed value – true value| / true value x 100%
Observed value from table 6 : 1.95 mgKOH/ g oil
Literature value: 3.10mg KOH/ g oil [1]
=|1.95-3.10|/3.10 x 100 % = 37%

New oil = 41%

Standard Deviation:

[5]
Used sample:
(+.,+&".5%)! *(".((&".5%)! *(+."$&".5%)! *(".66&".5%)!
S=! $&"

S= 0.163

New: 0.023

Discussion:
We determined that the acid number of fresh oil is 0.088 mg KOH/ g oil and used oil is
1.95mg KOH/ g oil by titrating oil samples using a diluted solution of KOH, 0.002M, 0.006M
for fresh and used oil, respectively. We found the mg of KOH used to achieve a teal colour by
using the volume used to find the moles. Then, we found mg using moles and molar weight [2].
Then we used mg and g of oil to find the acid number.

Our result was not accurate, but it was not too far off from the literature value of 0.15
mgKOH/ g oil and 3.10 mg KOH/ g oil [1]. For our used sample, we got a percent error of 37%;
for new, we got 41%. We ideally want to have a low percent error between 5-10%. Ours was
higher but not wholly different than what was expected. Our precision was better, and our results
were quite precise. No outliers were present in data from the Grubbs test, and the standard
deviation was low, being 0.163 for used oil and 0.023 for new.

Our data is significant because it tells us how often the oil we use every day needs to be
replaced before it darkens, has an off taste, and possibly leads to certain diseases. The limit is 2.5
mg KOH/g oil [1] for frying oil to stay fresh. Our lab data was 1.95 mg KOH/g oil [3], which is
below the suggested limit and does not need to be changed. But according to our literature value
of 3.10 mg KOH/g, the ester linkages in our oils have separated and released FFAs into the food
[1], surpassing the required limit to cook food and causing the oil to become darker.

In our experiment, we relied on the human eye to decide the solution's endpoint being a
teal colour. This is a source of error because we estimated what colour to stop at every run we
had. It is possible we stopped too early and chose the endpoint, which would cause the acid
numbers to be lower than expected because we used a smaller volume of KOH.
Another source of error would be reading the volume amount from the burette; we are again
relying on the human eye to read the volume. This could cause an error in the KOH volume,
affecting the acid number.
One final error would be the calibration of glassware used, the pipette measuring the KOH has a
level of error, and the burette and graduated cylinder as well have an error in measuring and are
not 100% accurate. This affects our values because we are using tiny amounts for our
experiment, like 2 mL of oil, and a small error in measuring can significantly impact the acid
number.

Conclusion:
The objective of this lab was to find the acid number for both used and fresh oil to relate it to
changes in the structure of the oil. We got slightly smaller values for it, 0.088 mg KOH/ g oil and
used oil is 1.95mg KOH/ g oil. The expected values are 0.15 mgKOH/ g oil and 3.10 mg KOH/ g
oil [1].
References:

1. University of Calgary, Department of Chemistry, Chemistry 209, General

Chemistry for Engineers, Lab Manual, Winter 2023, Experiment 3, pp. 1-8
2. Personal communication, Thiago Monteiro, University of Calgary, Calgary,
Alberta, Canada, Chemistry 209, Winter 2023, Lab section B26
3. Personal communication, Cody Shorhen, University of Calgary, Calgary,
Alberta, Canada, Chemistry 209, Winter 2023, lab partner
4. Personal communication, Chris Speers, Arsal Zia, University of Calgary,
Calgary, Alberta, Canada, Chemistry 209, Winter 2023, Fresh oil data used.
5. University of Calgary, Department of Chemistry, Chemistry 209, General
Chemistry for Engineers, Lab Manual, Winter 2023, pp. 7-20