The Number of Water Molecules in a Salt Hydrate

The Determination of the Empirical Formula of Hydrous

Copper(II) Sulfate
practical performed: 27/9/21
report written: 27/9/2021

Table of contents
1.
DESIGN...............................................................................................................................................
........3
1.1. RESEARCH QUESTION
................................................................................................................3
1.2. BACKGROUND THEORY
..............................................................................................................3
1.3. EQUIPMENT AND CHEMICALS
....................................................................................................4
1.4. METHOD
.....................................................................................................................................4
1.5. SAFETY AND ENVIRONMENTAL CONSIDERATIONS
....................................................................4
2. DATA COLLECTION AND
PROCESSING.................................................................................................5
2.1. DATA COLLECTION........................................................................................................ 5
2.2. DATA PROCESSING....................................................................................................... 5
2.3. ERROR CALCULATIONS ................................................................................................. 7
3. CONCLUSION AND
EVALUATION............................................................................................................8
3.1. CONCLUSION .............................................................................................................. 8
3.2. EVALUATION ............................................................................................................... 8
3.2.1. RANDOM ERRORS
.............................................................................................................................8
3.2.2. SYSTEMATIC ERRORS
.....................................................................................................................10
3.3. IMPROVEMENT SUGGESTIONS .................................................................................... 10
4.
BIBLIOGRAPHY.................................................................................................................................
.......11
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1. Design

1.1. Research question

The purpose of this experiment is to determine the number of water molecules,
hence the value x, in the empirical formula of hydrous copper sulfate CuSO4 x
H2O.
1.2. Background theory
When certain ionic solids crystallize from aqueous solutions, they combine with water, which
then
becomes a part of the crystalline solid. Salts that contain water as part of their crystal structure
are
called hydrates (or hydrated salts) and the water in the crystal structure is called the water of
hydration. When the water of hydration is removed from the hydrate, the salt that remains is
anhydrous. (Brady & Senese 2004, 43-44.)
Anhydrous copper(II) sulfate is the chemical compound with the formula CuSO4. This salt exists
also in a hydrous form. This is because when copper sulfate is dissolved in water, it exists as the
free ions Cu²⁺ and SO₄²ˉ. In solution, the partial charges of water molecules, called dipoles, are
attracted to the charged ions, thus forming ion-dipole bonds. As the water is let to evaporate,
some
of the water molecules remain bonded to the, leading to crystallized water in the now hydrous
solid
copper(II) sulfate. The crystallized water can be easily removed by heating the compound:

CuSO4.xH2O → CuSO4 + xH2O

(Brady & Senese 2004, 43-44.)
The molar ratio between the salt and the crystallized water can be calculated using the formula

(2)
where n equals amount of substance expressed in moles (mol), m the mass (g) and M the molar
mass (g/mol). (Brady & Senese 2004, 118-120).
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Gravimetric analysis describes a set of methods in analytical chemistry for the quantitative
determination of a sample based on the mass of a solid. A simple example is the measurement of
a
solid before and after heating/vaporization: the sample is weighed before and after it is dried;
the
difference between the two masses gives the mass of substance, in this investigation water, lost.
(http://en.wikipedia.org/wiki/Gravimetric_analysis, 29.5.2012.)

1.3. Equipment and chemicals

pasteur pipette
scale (±0,0001 g)
clay triangle
tripod
Bunsen burner
spatula
hydrous copper(II) sulfate
CuSO4 x H2O

1.4. Method
A dry and empty Pasteur pipette was weighed on an analytical scale. Using a spatula,
approximately
0,3 g of hydrous CuSO4 was then placed in the pipette, which was carefully re-weighed.
The pipette was then placed on a tripod above a Bunsen burner, as seen in Figure 1. The pipette
was
heated, first gently, then more vigorously, for approximately 5 minutes. During the heating the
blue
color of the copper(II) sulfate faded and water vapor was seen to leave the compound.
After all of the copper(II) sulfate had turned into
a grey powder and no water droplets could be
seen in the pipette, the pipette was let to cool. The
cooled pipette was then weighed once more.
The procedure described above was repeated
twice (until constant measurements for the mass
of the cooled pipette + anhydrous copper(II)
sulfate were obtained).

1.5. Safety and environmental considerations

Copper sulfate is toxic to the environment and should be disposed of as a heavy metal in a
separate
container. Very minute amounts may, however, be disposed in the drain.
(http://en.wikipedia.org/wiki/Copper_sulfate, 29.5.2012.)
2. Data collection and processing

2.1. Data collection

Table 1 displays the measurements taken in different stages of the
experiment. The combined mass
of the pipette and CuSO4 decreased during the heating as the crystallized
water was released and
eventually evaporated. Simultaneously the bright blue color of the hydrous
copper(II) sulfate faded into the light gray shade of the anhydrous salt.
Traces of yellow and light brown color were also detected in the salt after
heating. This could be evidence of some sources of error, which are
discussed in chapter 3.2.

Table 1.
Empty Crucible = 24.46 g
Crucible + CuSO4 = 26.46
CuSO4 = 2 g
Mass of water driven off = 0.7 g
Anhydrous CuSO4 = 1.3 g

2.2. Data processing

The values in Table 1 may now be used to calculate the molar ratio between
water and CuSO4 in the hydrous form of the salt. First the mass the sample
of hydrous copper(II) sulfate is calculated via subtraction:
Empty Crucible = 24.46 g
Crucible + CuSO4 = 26.46
24.46 - 26.46 = 2 g

The mass of anhydrous copper(II) sulfate is calculated in a similar manner

= 1.3 g

The value obtained in the last two measurements (values 4 and 5, Table 1) is
used as the combined mass of the crucible and anhydrous copper(II)
sulfate, as they are identical. It can therefore be assumed that all of the
crystallized water has by then been removed.
The mass of the crystallized water in the original hydrous sample is the
difference of the masses
calculated on the previous page:
()

For the molar ratio the amounts of substances of water and copper(II)
sulfate must be expressed in
moles instead of grams, using formula (2) on p. 3:
Moles of anhydrous Copper (II) sulfate formed = n = 1.3/160 = 0.008
moles

Moles of water driven off : n = 0.7/18 = 0.038 moles

The ratio between water and copper(II) sulfate in the hydrous sample of the
copper salt is therefore:
n (anhydrous CuSO4) : n (H2O) = 0.008 : 0.038 = 1: 4.75 ~ 5
The final result, 1 : 5, is due to rounding up to whole integers as empirical
formulas never contain
decimals.

2.3 Error calculations

As the calculated ratio 1 : 4.75 had to be rounded up to 1 : 5, the total
uncertainty margin derived from individual measurements must be taken
into consideration. As the experiment consisted of
three separate measurements, the uncertainty percentages for all three are
calculated separately.
1st weighing (empty crucible): 24.46 g
0.01/24.46 * 100 = 0.04%

2nd weighing (crucible + hydr. CuSO4) : 26.46 g

3rd weighing : (crucible + anhydr. CuSO4) = 1.3 +24.46 = 25.76 g

The total uncertainty percentage is the sum of the individual percentages

calculated above:
4.75 / 5 * 100 = 5 % error, 95 % success

It is reasonable to round up the uncertainty percentage as there is always

the factor of human error
to be considered. This value can now be used to calculate the absolute error
of the result of the
experiment:
As the absolute error calculated above is so minute in comparison to the
result obtained (4,973) it
can be safely stated that the difference between the result and the rounded
up value used in the
empirical formula CuSO4 5 H2O is not solely due to the uncertainty of the
equipment used. This
will be discussed in chapter 3.2.
3. Conclusion and evaluation
3.1. Conclusion
The molar ratio between water and copper(II) sulfate in its hydrous form
was found to be 1 : 4,973
(chapter 2.2). This could then be rounded up to 1 : 5, giving the empirical
formula of the hydrous
salt in question CuSO4 5 H2O. This empirical formula is the accepted
formula of hydrous
copper(II) sulfate, as it is widely used in chemical literature, thus enforcing
the reliability of the
experimentally deduced result. The salt is therefore called copper(II) sulfate
pentahydrate,
according to the IUPAC system of nomenclature of chemical substances
(Brady & Senese 2004, 63-
67).
The percentage difference between the experimentally deduced value and
the literary value is:

This difference is 50 times greater than the uncertainty percentage (0,01 %)

due to the uncertainty
of the equipment used, calculated in chapter 2.3. It can therefore be stated
that the minor
discrepancy between the experimental and literary values is due to other
errors in both the method
itself and its execution. These errors are discussed in the upcoming chapter
3.2.
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3.2. Evaluation
Both systematic and random errors occurred during the experiment. How
significant and to what
extent they were to the final result is evaluated individually for each source
of error.
3.2.1. Random errors
The empty pipette was not heated thoroughly before weighing it for the first
time. This could mean
that there were some impurities on the pipette, which were then oxidized
during the first heating.
This would indicate that both the mass of the empty pipette and the
combined mass of the pipette
and hydrous copper(II) sulfate were actually slightly smaller than
measured. This does not affect the
calculated value of the mass of hydrous copper(II) sulfate, but it does affect
the reliability of the
mass of the anhydrous copper salt and the calculated mass of water:
a) If the impurities led to gaseous oxides during the heating, these oxides
left the pipette with
the water vapor. The mass of the water released would therefore be smaller
than the
gravimetrically obtained value. This would lead to the calculated amount of
substance (in
moles) of water to be too high. Yet as the experimental result 4,975 is in fact
already lower
than the literary value 5, it does not seem plausible that this error source
assumption is
correct.
b) But if the impurities led to solid oxides during the heating, increasing the
mass of the heated
product (CuSO4 + oxides), the actual mass of anhydrous copper(II) sulfate
would in fact
have been smaller (hence the mass of the escaped water greater) than the
value obtain via
weighing. This would lead to a correction of the molar ratio towards the
literary value. For
instance: by using a value for the masses of anhydrous copper sulfate and
water that are
merely 0,0001 g lower respectively higher than the values used in the
calculations leads to
the value of 5,193 in the molar ratio. It can therefore be assumed that this is
one plausible
source of error.
Another source of random error is the numerous transferring of the pipette
filled with copper(II)
sulfate between the scale and the tripod. Some minute amounts of the
copper(II) sulfate were
perhaps lost during these stages of the experiment, decreasing the
measurements’ values. This
would lead to the mass of water released to seem greater and the mass of
anhydrous copper(II)
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sulfate to seem smaller than their actual values. This in turn would lead to a
ratio that would exceed
1 : 5. Therefore, this error source cannot be the reason for the difference
between the experimentally
deduced and accepted empirical formula of copper(II) sulfate pentahydrate.
The final random error could be the failure to remove all crystallized water
during the heating. That
would signify that the last two values of the combined masses of the pipette
and anhydrous copper
sulfate still contained some moisture not detectable to the naked eye. If this
were true, the value for
the anhydrous copper salt would be too high and the value for the water
released too low. These
erroneous values would lead to a ratio that differs from the literary ratio in
the same manner as the
experimental ratio does. It can therefore be safely assumed that this error
indeed happened during
the experiment.
3.2.2. Systematic errors
One significant systematic error would come from the purity of the hydrous
copper sulfate used in
the experiment. If the salt itself contained impurities such as other metals,
these metals could,
during heating, form solid oxides, thus increasing the mass of the
anhydrous copper(II) sulfate as
explained in 3.2.1. part (b). As yellow and brown discoloring was detectable
in the gray anhydrous
sample after the heating, it seems realistic that the discoloring is due to
solid metal oxides present,
confirming this source of error.
3.3. Improvement suggestions
In order to both avoid the errors mentioned above and to generally enhance
the reliability of the
experiment, the following improvements could be made to the design:
1) The empty pipette should first be heated with a bunsen burner or an oven
before weighed.
This would ensure the purity of the pipette.
2) The copper(II) sulfate should be heated more strongly and for a longer
period of time,
making sure that no moisture is present in the pipette.
3) The heated pipette (both empty and with the copper(II)sulfate) should
be cooled down in a
desiccating jar. This would avoid moisture from the air to condense on the
pipette.
4) Perhaps glassware with only one open end could be used instead of a
pipette. For instance a
test tube could prevent the loss of solid substance in-between
measurements and heatings.
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5) If possible, the copper(II) sulfate used in the experiment could be of
higher analytical grade
and thus more free from significant impurities.
6) More trials could be conducted in order to diminish the effect of the
random errors
mentioned.
7) A greater mass than 0,3 g of the copper(II)sulfate could be used. This
would decrease the
effect the random errors and the uncertainty margins of the equipment
have on the results.