Sian Zhang CHM122B

Apparatus:
Reagents:

- Potassium Iodate (solid)
- Potassium Iodide (solid)
- Sodium Thiosulphate xH20 (solid)
- Sulphuric acid 1M (H2SO4(aq))
- Starch solution (1%)
- Orange juice (Analyte)
- Deionized Water
Equipment:
- Burette; appropriate clamps and stands; Burrete clamp + Retort Stand
- Pipette; 10ml ; Pipette filler
- Volumetric flasks
- Conical Flask
- Measuring Cylinders (10ml, 25ml)
- Digital scales
- Hot Plate
- Bottles (5)
- Thermometer
- Spatula, Stirring rod
- Beakers
- Funnels
- Aluminium dishes
- Wash bottles
Method (including revisions):
A) Potassium Iodate Solution:

1. 4 grams of solid potassium iodate (KIO3) was measured using digital scales and transferred to
a volumetric flask.

2. The volumetric flask was filled up to a graduation mark at 1L. Its contents were agitated until
all the solid potassium iodate was dissolved. This created a 0.01869M solution.

B) Sodium Thiosulphate Solution:

1. 15.8 grams of solid sodium thiosulphate (Na2S2O3) was measured using digital scales and
transferred to a volumetric flask.

2. The volumetric flask was filled up to a graduation mark at 1L. Its contents were agitated until
all the solid sodium thiosulphate was dissolved. Due to the uncertainty regarding the water
content of sodium thiosulphate, standardization of the solution was necessary to ascertain the
molarity of the solution created.
Sian Zhang CHM122B


C) Triiodine Solution:

1. 10ml of potassium iodate solution from method A was transferred into a conical flask using a
pipette.

2. 0.5 grams of potassium iodide was measured out using digital scales and transferred to the
volumetric flask. Note that any amount of potassium iodide can be added, given that it is in
excess in the solution. The 8:1 stoichiometric ratio between potassium iodine and iodate,
which indicates that eight moles of potassium iodide is required to react with one mole of
potassium iodate to form three moles of triiodine.

3. 2.5ml of 1M sulphuric acid was measured in a measuring cylinder and transferred into the
volumetric flask. Upon the addition of hydrochloric acid, the contents of the volumetric flask
turned dark brown, indicating the formation of the dark-brown triiodine ion (I3
-
). The
concentration of the triiodine solution is equal to three times the molarity of the potassium
iodate solution used, as the potassium iodate solution acted as the limiting reagent in the
reaction. The molarity of the triiodine solution was 0.05607M.
Note that the triiodine solution is volatile in acidic environments, and is liable to be oxidized into iodide.
For this reason, the triiodine solution must be used immediately after it is generated.
Figure 2.1 Triiodine solution (Left pre-H2SO addition 4. Right post-addition of H2SO4)














Sian Zhang CHM122B

D) Standardization of Sodium Thiosulphate Solution:

1. A burrete filled with the sodium thiosulphate solution from method B was positioned directly
above a conical flask which contained the triiodine solution from method C.

2. Sodium thiosulphate was titrated into the flask until the solution changed from a dark-brown
colour to a pale yellow.

3. 3 drops of 1% starch solution was added to the flask, causing its contents to turn deep black-
brown. Sodium thiosulphate was added until the solution turned colourless, indicating the
endpoint of the titration.

4. The volume of sodium thiosulphate used was noted. Steps 1-3 were repeated twice to produce
three concurrent sets of data, and the average of the three values was calculated.

Thiosulphate ions react in a 2:1 ratio with the iodine present in equilibrium in the triiodine
solution. Hence the amount of thiosulphate supplied by the noted volume of solution is equal to
double the known moles of triiodine ions. From this the moles of sodium thiosulphate are
inferred, and subsequently, the molarity of the sodium thiosulphate solution is determined.
Figure 2.2 Standardization (Left pre-starch addition. Centre Starch Added. Right End-point)



Sian Zhang CHM122B

E) Preparation of Juice Samples for testing variables; Exposure duration, Temperature

Exposure Duration:

1. Five separate aliquots of 200mls of the same orange juice was prepared and stored in separate
bottles. Each bottle was left without its lid in order to expose the orange juice to atmospheric
oxygen. Samples were stored in a refrigerator set at 5-6
o
C in order to prevent the growth of
mold in the samples, which may interfere with results. Each of these aliquots represents a
sample used for each varied length of exposure-duration.

Temperature:

2. 25 ml aliquots of analyte were separated into measuring cylinders, and heated to desired
temperatures (temperature measured using thermometer) immediately prior to carrying out
experimentation, using a hot plate.

F) Titration for Ascorbic acid content in juice

1. When testing for oxygen-exposure, 25ml of orange juice from the oxygen-exposure juice
samples was measured out with a measuring cylinder and transferred into a conical flask
containing triiodine solution from method C. When testing for temperature, the contents of the
aliquot of juice prepared in E) 2. was used instead.

2. A burrete filled with the sodium thiosulphate solution from method B was positioned directly
above the conical flask.

3. Sodium thiosulphate was titrated into the flask until the solution changed from a dark-brown
colour to a pale green-yellow.

4. 3 drops of 1% starch solution was added to the flask, causing its contents to turn deep black-
brown. Sodium thiosulphate was added all traces of black and brown disappeared, with the
solution turning green. This indicated the endpoint of the titration.

5. The volume of sodium thiosulphate used was noted. Steps 1-4 were repeated twice to produce
three sets of concurrent data, the average value being calculated. This was repeated for each
different parameter of the variables (juice exposure time to oxygen; temperature) being tested.
In total, 5 parameters were tested for each variable, for each of which three sets of data was
obtained.

The known moles of sodium thiosulphate used correlates with the excess iodine in the
triiodine solution, after it has reacted with ascorbic acid in the juice. The moles of sodium
thiosulphate used are double the moles of excess iodine. The exact amount of excess iodine was
calculated and subsequently, the ascorbic acid, which reacts in a 1:1 ratio with iodine, was
determined, by finding the difference between the initial moles of iodine solution, (before it
had been reacted with ascorbic acid) and the moles of excess iodine reacted with sodium
thiosulphate.
Sian Zhang CHM122B

Figure 2.3 Titration (Left pre-starch addition. Centre Starch Added. Right End-point)










Revisions Made:
In the initially proposed method, it was suggested 20mls of potassium iodate solution was to be used
in creating the triiodine solutions used in the standardization of sodium thiosulphate solution and
ascorbic acid titration. This was changed to 10mls, in order to reduce the amount of titrant required to
reach the end-point in titrations, while maintaining accuracy.
Originally, a 0.25 M thiosulphate solution was used; however this caused each drop of solution to
contain more thiosulphate, therefore limiting the accuracy of the titrations carried out. Therefore, a
dilute solution was used instead (0.06M) to increase the accuracy of results yielded. This also reduces
the relative uncertainties in the results yielded, as a greater amount of titrant is used in each titration.
When preparing the orange juice samples for titration testing the effect of temperature, a beaker of
200ml of analyte was heated and then separated into 25ml aliquots for testing. This caused errors,
especially when the temperature being tested began to approach 100
o
C, at which point, the
evaporation of water in the juice samples occurred. This resulted in the significant reduction in juice
volume, causing the test sample to become much more concentrated for experiments testing higher
temperatures, resulting in inconsistent initial ascorbic acid values for each different (20, 40, 60, 80,
100
o
C) temperature tested. In order to remedy this, aliquots of 25mls were separated prior to heating
into separate conical flasks, and then heated. This meant that each aliquot of analyte began with
consistent ascorbic acid contents, and any subsequent variations in ascorbic acid content was due to
temperature, rather than being attributed to inconsistencies in initial content levels.




Sian Zhang CHM122B

Results:
Figure 2.4 Ascorbic acid content vs oxygen-exposure time

Duration of Exposure (nearest hour) Ascorbic Acid (mg) Uncertainties Mg
0 15.830 2.665
43 16.095 2.661
142 11.762 3.432
167 12.381 2.715
211 11.496 2.905

Experimentation testing the duration of exposure, shown in figure 2.4, shows that the ascorbic acid
content of the analyte decreased as the duration of the juices exposure to atmospheric oxygen
increased. Hence the independent variable, duration of exposure, and the dependent variable,
ascorbic acid content, share an inversely proportional relationship, as predicted in the hypothesis. The
chosen trend-line fitted to the data points is one of exponential decay, which indicates that the rate of
ascorbic acid deterioration is proportional to its the amount of ascorbic acid in the solution. Hence,
when there is more ascorbic acid content in a solution exposed to oxygen, it will degrade relatively
faster than a similar solution with less ascorbic acid content. There are a number of points that
deviate from this trend line, however, the degree of deviation of these points lie is smaller than the
uncertainties propagated, and hence, it is concluded that these discrepancies are due to experimental
errors.


y = 16.302e
-0.002x

R = 0.8934
0
2
4
6
8
10
12
14
16
18
0 50 100 150 200 250
A
s
c
o
r
b
i
c

A
c
i
d

C
o
n
t
e
n
t

(
m
g
)

Exposure Duration (nearest hour)
Ascorbic Acid content (mg) vs Time (hours)
Expon. (Mg Ascorbic Acid)
Sian Zhang CHM122B

Figure 2.5 - Ascorbic Acid content vs Temperature

Temperature Ascorbic Acid (mg) Uncertainties Mg
20 20.693 2.593
40 19.455 2.611
60 20.340 2.598
80 16.979 2.648
100 10.258 2.923

Experimentation testing the temperature variable, shown in figure 2.5, shows that increasing the
temperature of the analyte causes a corresponding decrease in the ascorbic acid content of the sample.
Hence, the independent variable, temperature, and the dependent variable, ascorbic acid content,
share an inversely proportional relationship, as predicted in the hypothesis. The chosen trend-line for
the data points is a negative linear relation. This indicates that the rate of ascorbic acid decay, given by
the gradient of the trend-line, is constant at all temperatures. There are a number of points that
deviate from this trend line, however, the degree of deviation of these points lie is smaller than the
uncertainties propagated, and hence, it is concluded that these discrepancies are due to experimental
errors.
In figures 2.4 and 2.5, exponential and linear trend-lines were chosen for their respective data points.
Both trend-lines have the best R^2 value (excluding polynomial trends) for each of their sets of data.
Although polynomial trends have greatest R^2 value (see appendix), extension of these graphs
suggest that the ascorbic acid content of samples increases parallel to increase in the independent
variables after a certain point, which should not happen, as shown by background research.
y = -0.1167x + 24.549
R = 0.7288
0
5
10
15
20
25
0 20 40 60 80 100 120
A
s
c
o
r
b
i
c

A
c
i
d

C
o
n
t
e
n
t

(
m
g
)

Temperature (
o
C)
Ascorbic Acid content (mg) vs Temperature (
o
C)
Linear (Mg Ascorbic Acid)
Sian Zhang CHM122B

Sample Calculations:
Triiodine Solution:
Firstly, the concentration of the potassium iodate solution used in producing triiodine is found using
the equation c=m/v, where m is the moles of KIO3 and v is the volume of distilled water used. This
concentration remains constant for all calculations.
[]

There is an uncertainty of + 0.02g associated with the digital scales in measuring the mass of KIO3. A +
0.3ml uncertainty is associated with the volumetric flask used to measure 1L of distilled water. In
order to find the total uncertainty in the concentration of the KIO3 solution, these absolute
uncertainties must be converted into relative uncertainties. (Calculations involving multiplication or
division require relative uncertainties)

The total uncertainty in the potassium iodate solution is the sum of these two values

However, each time KIO3 solution was utilized; it was used in 10ml portions. Therefore the moles of
iodate used in each titration are as follows:

The pipette used to measure these moles has an associated error of 0.04ml.

Hence, the uncertainty of the moles of KIO3 in a 10ml sample is actually the sum of the KIO3 solution
uncertainty and this uncertainty.

Here an excess of KI is added to the KIO3 solution calculated previously, as well as an excess of H2SO4.
Hence, given that the values of the moles associated with these two substances do not dictate the
molarity of the triiodine solution formed, the uncertainties associated with these two substances are
irrelevant.
Sian Zhang CHM122B

Upon inspection, it is found that KIO3 and KI to form 3 moles of triiodine. Hence the triiodine solution
(for the actual equation, refer to stage 1) has three time the number of KIO3 moles, and shares the
same relative uncertainty.
Moles of 3I3 formed:

Standardization Sample Calculation:
The sodium thiosulphate is known to react with iodine (equivalent to triiodine) in a 2:1 ratio. Hence,
the amount of thiosulphate moles required to react with the triiodine solution is:

The relative uncertainty of the moles of thiosulphate is the same as the uncertainty of the triiodine as
these moles are supplied via titration, 0.93%. There is however, another uncertainty associated with
the how these moles were supplied the error of the burrete used for titration of the solution.
Trial Start (ml)

End Delta
1 4 22.6 18.6
2 22.6 41.2 18.6
3 0 18.6 18.6
AVG 18.6

The total apparatus uncertainty (or individual uncertainty) is. All titrations yielded the same
amount of thiosulphate solution used; consequently as there is no deviation from a mean, the error
associated with the volume can be concluded to be

From this, it can be concluded that 18.6mls of the sodium thiosulphate used contains

of thiosulphate. Hence the molarity of the thiosulphate solution is as follows:

[ ]

Total uncertainty for the sodium thiosulphate concentration:

Note: all values calculated for thiosulfate and triiodine remain consistent for all ascorbic acid
calculations



Sian Zhang CHM122B

Ascorbic Acid Calculation:
The triiodine and thiosulphate solution used in determining the ascorbic acid concentration are as the
previous calculations specify.
The moles of triiodine used are

. This has an associated uncertainty of 0.68%.

The concentration of sodium thiosulphate used is , with a 1.4676% associated
uncertainty.
It was observed that after these moles of triiodine had reacted, the following volumes of thiosulphate
were required to react with the remaining moles of triiodine.
Trial Start End delta
1 31.6 47.2 15.6
2 19.7 35.3 15.6
3 19.65 35.3 15.65
AVG 15.61666667
Here, the greatest deviation from the mean was given by 15.61666667-15.65 = 0.03333... This value is
within the individual uncertainty of + 0.1 ml, hence the uncertainty of the average volume is
concluded to be + 0.1ml.
The moles of sodium thiosulphate used are given by:

The relative uncertainty of the moles of sodium thiosulphate used is the sum of the uncertainties of
the concentration and volume of the sodium thiosulphate. The concentration uncertainty is stated
above.

The moles of iodine with which the sodium thiosulphate is half the moles of the sodium thiosulphate
used (due to 2:1 ratio), and its associated errors is the same as the relative uncertainty of the moles of
sodium thiosulphate.

Sian Zhang CHM122B

From this, the amount of iodine reacted with ascorbic acid can be determined, and consequently, the
moles of ascorbic acid in the sample can be calculated.

As ascorbic acid reacts with iodine in a 1:1 ratio, the moles of ascorbic acid in the sample is:

The uncertainty of this value is equal to the sum of the absolute uncertainty of the total moles of
iodine and the absolute uncertainty of the sodium thiosulphate (addition and subtraction
calculation, therefore absolute uncertainties are used.)
( )