Mindanao University of Science and Technology

C.M. Recto Ave., Lapasan

Cagayan de Oro City, Philippines
Inorganic Chemistry
Department of Chemistry
College of Arts and Sciences

Preparation and Analysis of a Coordination Compound:

Analysis of [Co(NH3)5Cl]Cl2
Experiment No. 10

Submitted by:
Group 1
Basa, Marla C.
Baytion, Ana Margarita L.
Tomas, Izza May L.

Date performed:
October 1, 2015
Submitted to:
Sir Glenn D. Ongayo

INTRODUCTION
Once a compound has been prepared, a chemist usually does some analysis of it. This
analysis can be used to establish the formula of the compound, or if the formula is known, it can
be used to determine the purity of the compound. One can analyze for an element within the
compound and compare the % found with the % expected from the formula. In this experiment,
we will be determining the % Co in the compound prepared and, by an indirect method we will
determine the charge on the Co(III) ion.
The Co will be analyzed by a technique called atomic absorption spectroscopy, AAS. In
this method a solution of the metal ion that is to be analyzed is aspirated into a flame. While in
the flame, the compound decomposes into gas phase metal atoms, Co(g). At the same time a
beam of radiation of the exact wavelength that Co(g) absorbs is passed through the flame. The
Co(g) atoms absorb some of this radiation and this change in intensity is measured by a detector.
This change, which is called the absorbance, is proportional to the concentration of Co in the
solution. By comparing the absorbance of the solution which you prepare with the absorbance of
a series of standards, you can determine the concentration of Co(III) complex in your solution.
This method has four very important advantages. 1) It is a very rapid method. Ten samples and
a series of standards can be run in about 15 minutes. 2) It is a very sensitive method. The
detection limit for most metal ions is about 1 mg/L. 3) The analysis does not depend on the
form of the metal ion in solution. Since the compound is completely decomposed in the flame,
all forms of Co respond the same. 4) Since we use exactly the wavelength of radiation that
Co(g) absorbs, and only that wavelength, other elements in the solution do not interfere. The
only significant restriction that applies to Co analysis by AAS is that the compound must be in
solution. The presence of solid particles would cause problems.

OBJECTIVES
The objectives of this experiment were to calculate the percent (%) yield and get the Co%
by Atomic Absorption Spectroscopy (AAS) method.
MATERIALS
The materials used in the experiment were: wash bottle, 25-mL and 50-mL graduated cylinder,
500-mL volumetric flask, 150-mL beaker, stirring rod, filter paper, funnel stand and funnel.
CHEMICALS
The chemicals used were: purified [Co(NH3)3Cl ] Cl2, and standard Co solution for AAS.

PROCEDURE
A. Prepararion of Solid Sample
We accurately weighed the purified [Co(NH3)5Cl]Cl2 that we stored for 2 days and used the
mass obtained to calculate the %yield. We weighed out accurately 0.15 - 0.20 g of pure solid,
into a clean, dry 250 mL beaker and added about 60 mL of de-ionized water to the beaker, and
swirled to dissolve the compound and quantitatively transferred it to a 100 mL volumetric flask,
and diluted it to the mark with de-ionized water.
B. Determination of %Co (AAS).
We cleaned a 5.00 mL volumetric pipet, and rinsed it with a small portion of the solution in
the 100 mL flask (from prep of solid sample above). We pipette 5.00 mL of the solution in the
100 mL volumetric flask into a clean 500 mL volumetric flask, and diluted to the mark with deionized water and inverted several times to mix the solution. The solution prepared was used for
analysis for Co by AAS. When the analysis was done we were told the concentration of our
sample solution, in parts per million (ppm) from the instrument printout and recorded the value
in our notebook. We calculated the mass percent Co in our compound and compared the expected
value by calculating % absolute error.
C. Analysis for ion charge. (This analysis was not done due to lack of materials such as, ion
exchange column.)
1.) Set up the ion-exchange column and rinse it with de-ionized water until the effluent is
colorless and has a pH of 6 (as the pH of the de-ionized water in the laboratory). Test for pH by
allowing a drop of effluent to touch a small strip of pH paper: this may take as much as a
hundred mL of water. At least half of the bottom part of the resin column should be a pale
yellow color. Allow the water to drain from the column until the water level is just above the
resin bed. Never permit the water level to drop below the top of the resin bed.
2.) Clean, rinse, and fill a 25.00 mL pipet with the sample solution in the 100 mL flask (from
prep of solid sample above), and add that 25.00 mL of sample solution to the column. Allow
the resin to settle back in the column and then open the stopcock so that the effluent flows out at
a rapid drip rate.
3.) Collect all of the effluent and the rinse effluent to follow in a clean 250 mL Erlenmeyer flask.
As the solution in the column drains just to the top of the resin bed, add 20 mL of de-ionized
water from your wash bottle to the column. After this 20 mL of wash has gone through the
column and been collected, add more de-ionized water and begin testing the effluent with pH
paper. When the effluent has a pH of 6, close the stopcock: the effluent collected should be
colorless.
4.) Fill a buret with standard NaOH solution (record its molarity in your notebook).

5.) Add 2-4 drops of phenolphthalein indicator to the flask with the effluent and titrate with a
standardized NaOH solution, to a faint pink color.
6.) Repeat the ion exchange process and analysis twice to obtain triplicate determinations.
7.) Calculate the charge on the Co(III) complex ion. Calculate the average of the three
determinations, the standard deviation, and the %absolute error.
RESULTS AND DISCUSSION
STANDARDS
Standard 1
Standard 2
Standard 3
Standard 4
Blank

VALUES (mg/L)
0.1 ppm
0.5 ppm
2 ppm
5 ppm

ABSORBANCE
0.004
0.020
0.079
0.1814
0.014

Corr. Coefficient: 0.999812

Model of the Atomic Absorption Spectrophotometer : Perkin Elmer AA200

Sample

Trial 1
Trial 2
(Absorbance)
(Absorbance)
Group 1
0.056
0.061
Initial sample volume: 500-mL
Sample Preparation Volume: 100-mL

Trial 3
(Absorbance)
0.057

Average
(Absorbance)
0.058

OBSERVATIONS:

After preparing the sample to be analyzed, we filtered it twice. According to the lab
technician, the presence of solid particles will create a big problem.
The color of the flame was purple, not yellow or red.
The machine needed also a compressor for C2H2 and O2.
The absorbance values fitted the absorbance values of the standards, which is a good
sign.
According to Sir Glenn, the initial sample volume should be 5-mL and sample
preparation volume should be 100-mL.

REVIEW OF RELATED LITERATURE

Chemical Interferences in atomic absorption spectrometry have been studied by
numerous workers. These studies have included the effects of ligands of a complex which are
added to the solution of the metal ions to be analyzed.

o Absorption of light
When an atom absorbs a single photon of light, it causes the electron to "jump" to a

higher energy level. The difference between energy levels ( E) equals the energy of the
photon absorbed.

o Crystal Field Theory

Crystal field theory states that electrostatic interactions between the electron pairs of the
ligands and the d-sublevel electrons of the transition metal ion (recall that electrons repel each
other) lead to a splitting of the d-sublevel orbitals into groups with different energies. Electrons
from a ligand will approach the d orbitals of the transition metal when bonding. The closer these
ligands approach a particular orbital, the higher the energy of the electrons placed in that orbital.
When comparing complexes containing different ligands, the presence of different ligands will
cause the spacing between the energy levels of the transition metals d orbitals to increase or
decrease. This will change the wavelength of light needed to cause the electron to jump (and
therefore the color of that light).
There are analytical methods that are available for detecting, measuring, and/or
monitoring cobalt, its metabolites, and other biomarkers of exposure and effect to cobalt. The
intent is not to provide an exhaustive list of analytical methods. Rather, the intention is to
identify well-established methods that are used as the standard methods of analysis. Many of the
analytical methods used for environmental samples are the methods approved by federal
agencies and organizations such as EPA and the National Institute for Occupational Safety and
Health (NIOSH). Other methods presented in this chapter are those that are approved by groups
such as the Association of Official Analytical Chemists (AOAC) and the American Public Health
Association (APHA). Additionally, analytical methods are included that modify previously used
methods to obtain lower detection limits and/or to improve accuracy and precision.

CONCLUSION
We conclude that the average absorbance of our sample was 0.058; since we did not
perform the analysis of chlorides to match up the Co analysis (the purpose of this method is to
check if the molecular formula of the coordination compound is correct). There are possible
sources of error in this experiment: human error (e.g. analyzing the initial sample volume and
sample preparation volume), and impurities. Complete apparatus and further trials on the
experiment are recommended.
REFERENCES
Retrieved from:
1.) http://www.chemistrylabmanual.com/uploads/2/5/6/1/25614215/synthesiscoordinationco
mpounds.pdf
2.) http://www.atsdr.cdc.gov/toxprofiles/tp33-c7.pdf

3.) Kitao Fujiwara, et al; Study of Cobalt (III) complexes by Atomic Absorption Spectrometry:
Effects of Ligands and Distribution of Atomic Cobalt in the Flame