Analysis of a Copper Coordination Compound

A Laboratory Report for CHEM 2140

Performed by: Melanie Cucunato
Date Performed: March 24, 2016
Date Due: April 28, 2016

Abstract
Starting with copper sulfate pentahydrate, a copper coordination complex is synthesized
using ammonia and ethanol. Using different methods like gravimetric, volumetric, and
spectrophotometric analyses each ion within the compound is isolated and investigated to
calculate a mass percentage. The mass percentages were then used to calculate an empirical
formula to identify the mole ratio of the unknown complex. The mass percentages for sulfate,
ammonia, copper, and water were 40.7%, 26.63%, 26.0%, and 6.67%. From this, the formula
was found to be Cu(NH3)4SO4 H2O, a mole ratio of 1:4:1:1. The name identification of this
complex is tetraamminecopper (II) sulfate monohydrate.

Introduction
A copper coordination complex was synthesized using the starting material copper sulfate
pentahydrate, or CuSO4 5H2O. The preparation of the complex was completed by adding
ammonia and ethanol to the compound. The complex that is being studied has a formula of
Cux(NH3)y(SO4)z aH2O [1]. It is apparent that there are many variables in this formula, which is
what this experiment set out to do: to use a variety of methods to isolate the different components
of the complex in order to then calculate the empirical formula of the product of interest. The
variable x was determined through spectrophotometry. The variable y was determined
through volumetric analysis. The variable z was determined through gravimetric analysis.
After using these methods to find the mass percentage of each component of the complex, the
difference of the percentages was used to determine the variable a. The mole ratio is then used
to discover an identity for the complex synthesized.
For the gravimetric analysis of sulfate, the compound is added to nitric acid. This causes
a dissolution to occur, leaving free sulfate ions in the solution. Adding barium nitrate (Ba(NO3)2)
caused a precipitate reaction to occur: Ba2+(aq) + SO42-(aq) BaSO4(s) [2]. This is where the mass
percentage of sulfate is found from the complex.
For the volumetric analysis of ammonia, a titration with hydrochloric acid was
completed, the complex was dissolved in water. The reaction that occurs is NH3(aq) + H+(aq)
NH4+(aq) [3]. When the endpoint is reached, the number of moles for hydrochloric acid matches
the number of moles of ammonium. This is then used to determine the mass percentage of
ammonia in the complex.
For the spectrophotometry analysis of copper, the complex was dissolved in nitric acid
and then a spectrophotometer was used to find the absorbance of the solutions. By using a
standard curve from a stock solution of copper solution, the concentration of copper in the

solutions dissolved with the complex is found. Using these concentrations, the mass percentage
of copper in the complex is found.
Mass percentages can be investigated to find the empirical formula. It is important for
chemists to use empirical formulas, which is to find the smallest possible ratio of atoms of each
of the elements found in a compound [4], in order to identify compounds. The ratio of atoms is
the equivalent to the mole ratio of a compound. The significance of mass percentages is that it
relates different samples to a same sample size [5], which in this case is 100 grams.
Experimental
First, the preparation of the copper complex was completed. Copper sulfate pentahydrate
was dissolved in water, then concentrated ammonia was added under a fume hood. At this point,
a pale blue precipitate formed. Ammonia was added until the precipitate dissolved completely,
leaving a dark blue-violet color. Once this was achieved, ethanol was added to form a new
precipitate which was the copper coordination of interest. The resulting solution, after being
cooled, was put through vacuum filtration to separate the precipitate from the solution.
Next, the analysis for the sulfate ion was completed. The compound synthesized was
dissolved in 6M nitric acid. As it was dissolved, the dark blue complex changed the color of the
nitric acid to a light blue color. Saturated barium nitrate was added to the nitric acid solution to
form a precipitate. Suction filtration was completed to separate the precipitate from the solution.
It was imperative to check that the filtrate remained clear as cloudy filtrate meant that the
product that was of interest was going through the filter paper and was being lost. Acetone was
used to aide in the drying process of the product.
After that, volumetric analysis for ammonia was completed. This was accomplished
through an acid-base titration. The compound was dissolved in water. Methyl orange was used as

an indicator for the titration. Hydrochloric acid was the titrant, meaning acid was added to the
basic solution containing the compound. The indicator had an array of colors, but at the endpoint
the solution changed to a red-orange color.
Finally, spectrophotometry was used to determine the presence of the copper ion. After
calibrating the spectrophotometer with a stock solution of copper ion, the compound, using
different masses for three different trials was dissolved in 1 M nitric acid. The solution was then
placed into the spectrophotometer and the absorbency was recorded at 820 nm.
Results and Discussions
Using the different methods of analysis, the mass percentages were found for the ions that
are in the composition of the copper complex; copper, sulfate, ammonia, and water.
Figures are presented for the spectrophotometric analysis that was completed for the
copper ion in the complex because it shows numerical evidence of the calculation to find the
mass percentage of copper. Figure 1 shows that the standard curve that was used to calculate the
molarities of the copper concentrations used, which in turn was then used to find the moles of
copper in the solution, the mass of copper, and finally the mass percent of copper in the complex.
Figure 2 shows the absorbency curves for the three trials completed with the complex as well as
a standard that was used using the stock solution of copper ion. The standard can be used for a
comparison for the other absorbencies.
The gravimetric and volumetric analyses of sulfate and ammonia do not have figures as
they do not have the same numerical way to show evidence of finding the mass percentage. The
gravimetric analysis of sulfate does not have a way to show evidence other than weighing the
product and the volumetric analysis of ammonia could have a titration curve, but a probe was not
used during the experiment.

f(x) = 13.31x + 0.03

R = 0.99

Figure 1.
Standard Curve for Stock Solution of Copper
Figure 1 shows the standard curve that was found for the stock solution of copper ion using
spectrophotometry. This curve can be used to find the absorbance of any copper solution
regardless of the molarity. The molarity of the copper ion that was used was 0.0901.
The curve can be used to find any absorbance with any concentration of copper. The
equation shown in the figure can be used because it shows: absorbance = 13.3(concentration of
copper[M]) + 0.0291. This equation was used to calculate the concentrations of copper in the
complex, which then was used to find the mass percentage of copper ions in the complex.

Standard

Trial One

Trial Two

Trial Three

Figure

2. Representative Absorption Spectrum

The peak absorbance for the copper ion was at 820.6 nm. The trials each had different masses of
the copper complex, trial one being the smallest amount (0.124 g) and trial three being the most
(1.127 g).
Absorbance works because it tells how much light a compound absorbs and how much
light it transmits. By having all three trials have a peak at 820.6 nm, as can be seen in Figure 2, it
obviously tells that each trial was a copper solution. The change in molarity did not change the
peak absorbance. The absorbencies of these three trials were plugged into the standard curve
equation explained in Figure 1 which, in turn, gave the mass percentages of copper ion in the
complex.

Table 1. Mass Percentages of the Components of the Copper Complex

Mass Percent (Class Data)
Standard Deviation
Cu2+
26.0%
3.34
2SO4
40.7%
5.69
NH3
26.63%
2.514
H2O
6.67%
--This table shows the calculated mass percentages of the class data. These percentages also have
standard deviations to account for possible error of the class. Using these percentages, the
empirical formula can be calculated as well as an identification for the copper coordination
complex that was synthesized.
The mass percentages were used to calculate the empirical formula of the complex.
Assuming that that the total amount of complex is 100 grams, the percentages can be easily
converted grams of each ion. The percentage for water was calculated by adding the percentages
of copper, ammonia, and sulfate and subtracting that number from 100, which can be seen in
Table 1.
Using this information, the copper coordination complex was found to have a formula of
Cu(NH3)4SO4 H2O. The mole ratio is 1:4:1:1. Being that there are four moles of ammonia, the
name of the complex is tetraamminecopper (II) sulfate monohydrate [6], MM=245.7460 g/mol.
The evidence that supports this claim can be seen in Table 2. The theoretical mass
percentages are found using the molar mass of tetraamminecopper (II) sulfate monohydrate.
Comparing these percentages with the percentages of the class, it can be seen that the
percentages calculated in the experiment match those of the theoretical mass percentages.

Table 2. Theoretical Mass Percentages [7]

Ion
Atomic Weight (g)

Moles found in
Theoretical Mass
complex
Percent
2Sulfate (SO4 )
96.1
1
39.1%
Copper (Cu2+)
63.5
1
25.8%
Ammonia (NH3)
17.0
4
27.7%
Water (H2O)
18.0
1
7.33%
This table attempts to act as a comparison for the experimental calculations. These mass
percentages were calculated using the molar mass of the tetraamminecopper (II) sulfate
monohydride.
These mass percentages are able to be used as a comparison because by using the molar

mass of the complex, it tells how much copper should be present in the complex in relation to
actual masses of the atoms and the complex. Between the two tables, it is proven that the copper
coordination complex that was synthesized was, in fact, tetraamminecopper (II) sulfate
monohydrate, or Cu(NH3)4SO4 H2O.
A major source of error is that this is a quantitative experiment. For the gravimetric
analysis, some product could have been lost during the vacuum process. This would cause the
mass of the product to be lower, thus a lower mass percentage would be calculated. If not all the
sulfate ions were reacted with, this would also result in a decrease in the mass percentage. For
the volumetric analysis, if the endpoint was passed this would result in the moles of ammonia
being too high which would result in a higher percent mass than what is the accurate number. If
the endpoint was not quite reached yet, the mass percentage would be lower than what it is
supposed to be. In the spectrophotometer, it was easy to pick out errors due to using LoggerPro,
it would be easy to identify if the graph looked abnormal. An issue could be not using exactly 10
mL of the solution. This could result in a false molarity, which would result in a skewed mass
percentage as well.

Conclusion
Using different methods of analyzation allowed for the identification of a copper
coordination complex. Only knowing an outline of the formula, Cux(NH3)y(SO4)z aH2O, each
individual ion was isolated to calculate the mass percentage. The mass percentages were then
used to calculate an empirical formula which allowed for the identification of the unknown
compound. The sulfate ion was found by first a dissolution reaction, then a precipitate reaction
with barium nitrate. The ammonia ion was found through an acid-base titration. The copper ion
was found using spectrophotometry. After studying the data, the copper coordination complex
was identified as tetraamminecopper (II) sulfate monohydrate, or Cu(NH3)4SO4 H2O. This mole
ratio was found to be 1:4:1:1. Using the molar mass of tetraamminecopper (II) sulfate
monohydrate, theoretical mass percentages were able to be calculated and compared to the
experimental data. This proved that the compound was identified correctly and the mass
percentages were accurate.

References
1.

Chemistry Program. CHEM 2140 Laboratory Manual: Experiment 8; Stockton

University: Galloway, NJ, 2016

2. Reference 1
3. Reference 1
4. Chemistry; The Molecular Nature of Matter 7th Edition. Jespersen, Hyslop. 2015, 2012,
2009, 2004, Chapter 3.
5. Reference 4
6. Molar Mass, Molecular Weight and Elemental Composition Calculator. Chemical Portal.
2016. http://www.webqc.org/molecular-weight-of-%5BCu(NH3)4%5DSO4*H2O.html
accessed 22-April-2016
7. Reference 6