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Experiment-1 Visible Spectroscopy of Hexaaquacobalt (II) Ion

This experiment involves preparing a series of standard solutions of varying concentrations of the hexaaquacobalt(II) ion, [Co(H2O)6]2+, and measuring their absorbance values. A calibration plot of absorbance versus concentration is constructed. This plot is used to determine the concentration of cobalt in an unknown sample solution. The maximum absorbance wavelength of the [Co(H2O)6]2+ complex is 512 nm, corresponding to the blue-green region of the visible light spectrum. Analysis of the sample using the calibration plot allows the percent cobalt in the sample to be calculated.

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119 views

Experiment-1 Visible Spectroscopy of Hexaaquacobalt (II) Ion

This experiment involves preparing a series of standard solutions of varying concentrations of the hexaaquacobalt(II) ion, [Co(H2O)6]2+, and measuring their absorbance values. A calibration plot of absorbance versus concentration is constructed. This plot is used to determine the concentration of cobalt in an unknown sample solution. The maximum absorbance wavelength of the [Co(H2O)6]2+ complex is 512 nm, corresponding to the blue-green region of the visible light spectrum. Analysis of the sample using the calibration plot allows the percent cobalt in the sample to be calculated.

Uploaded by

Vidit Dixit
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© © All Rights Reserved
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Download as PDF, TXT or read online on Scribd
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EXPERIMENT-1

Visible spectroscopy of Hexaaquacobalt(II) ion

Pre-lab
Introduction to Visible Spectroscopy and Beer’s Law
Color changes have always been important identifiers of reaction for chemists.
Colorimetry- the use of light absorption of colored solutions for the quantitative analysis of
dissolved substances-quickly became an important tool in inorganic chemical analysis. Although
strictly speaking colorimetry refers to analysis by direct color comparison, today this refers to
any technique that involves absorption of visible light. In coordination chemistry class, we learn
that the wavelength or color of light absorbed is what gives a transition metal complex its
particular color. For this reason, visible spectrophotometry is often used for both qualitative and
quantitative analysis of inorganic compounds. The visible region of the electromagnetic
spectrum includes wavelengths from about 380 to 750 nm. The familiar color wheel, Figure 1,
shows that a solution that is red transmits red light and absorbs primarily green light (~ 500 nm).
The absorption of light leads to a decrease in the intensity of light passing through the solution.
The ratios of intensities going into and out of the solution are measured using a visible
spectrophotometer and are used to calculate the absorbance of the solution.
A typical instrument used in visible analysis is the diode array spectrophotometer, Figure 1. This
instrument uses a limited number of optical components in its construction and a single
deuterium lamp source provides significant radiant throughput in the 200 – 820 nm range. A
single collimated beam of light is formed after passing through the source lens, which enters the
cuvette that holds the sample. The transmitted light reaches a grating that disperses the light into
wavelengths. The light is collected and converted into measurable current using a photodiode
array detector. [Photodiode arrays are composed of silicon diode elements (typically 1024) with
reverse-biased on junctions.] The current is proportional to the amount of light reaching each
diode element. The full spectrum is acquired almost simultaneously and allows multiple scans
that can be averaged to enhance the signal to noise ratio. The resolution for a diode array
instrument is typically 2 nm (Figure 2).

Figure 1. Color Wheel


The Beer–Lambert equation predicts that the absorbance A of a solution at wavelength λ is
linearly proportional to the concentration (c, in mol l-1) of the absorbing solute and the path
length of sample that the light passes through (b, in cm). The Beer–Lambert equation, equation
is:

where ε is a proportionality constant known as the molar absorptivity (or molar extinction
coefficient) that depends on the nature of the absorbing solute; these values are typically (Figure
1 Color wheel).

small for transition metal complexes. The molar absorptivity has units of l mol-1 cm-1, and is
determined by the electronic structure of the metal complex. A plot of A vs c for a solution is
commonly known as a “Beer’s law plot.” Such a plot can be used to determine ε for a metal
complex electronic transition, provided that the path length, b, is known. A Beer’s law plot can
also be used to determine the concentration of a solute in solution when ε for the solute is known
simply by measuring the absorbance of the solution. In order to prepare a Beer’s law plot, several
solutions (at least four) of precisely known metal complex concentrations must be prepared and
the absorbance of each measured.

Visible Spectroscopy of the Hexaaquacobalt(II) Ion

Upon dissolving the CoCl2(s) in acidic water, the hexaaquacobalt(II) ion, [Co(H2O)6]2+ is
formed. The visible spectroscopy of the [Co(H2O)6]2+ is well studied; the molar absorptivity
coefficient, ε, for [Co(H2O)6]2+ has been determined to be 4.84 M-1 cm-1 at 512 nm.

In this experiment, you will prepare a series of [Co(H2O)6]2+ complexes of varying


concentrations from a standardized stock solution of known concentration. By constructing a plot
of absorbance vs concentration, you will be able to determine the concentration of cobalt in your
sample.
Pre-lab Questions

Q1. 3.50 ml of a 0.0850 M solution of Co2+(aq) is diluted to 10.00 ml. Calculate the
Concentration of the resulting solution.

Q2. How many significant figures are in the following values?


a. 3.50 ml
b. 0.0850 M
c. 10.00 ml

Q3. Calculate the % Co in CoCl2 • 6H2O

Q4. What does a “quantitative” transfer mean?

Q5. What will happen to Beer’s law if your solution concentration goes very high?

Pre-lab Preparation
1. A stock solution of aqueous cobalt(II), Co2+(aq), of known concentration (~0.085 M) prepared
from CoCl2 •6H2O–cobalt(II) sulfate hexahydrate will be provided by the instructor.

Procedure a: Preparation of Co2+(aq) Standard Solutions

1. Record the exact concentration of the Co2+(aq) stock solution.


2. Prepare five standard solutions (10 ml each) from the Co2+(aq) stock solution in clean, dry test
tubes. The most concentrated will be the stock solution. The other four will be dilutions of the
stock solution having concentrations between ~0.040 and 0.085 M. Record your concentrations
in the Results Summary section. You can easily prepare these standard solutions using only 10
and 5 ml graduated pipettes. Keep in mind a useful equation for preparing solutions: C1V1 =
C2V2, where C1 is the concentration of your stock solution, V1 is the volume of stock solution
that you use, C2 is the concentration of your final solution and V2 is the volume of your final
solution (10 ml, which is V1 plus the volume of water added to dilute it).
Keep in mind the importance of accuracy and precision in your use of the volumetric
measurements you are making. The concentration of each standard solution should be known to
three significant figures. The graduated pipettes should be read to +0.02 ml.
3. Securely seal each tube with parafilm to prevent any evaporation of the solvent.

Procedure b: Measurement of the Visible Spectrum of the


Aquated Co(II) Ion: [Co(H2O)6]2+

This may be done as a group exercise.


1. Run a “blank” spectrum of your cuvette and solvent. Obtain the absorption spectrum of the
cobalt ion stock solution.
2. Determine the wavelength of maximum absorbance. Record in the Results Summary.
Procedure 2.3.d: Preparation of Beer’s Law Calibration Plot and
Sample Analysis
1. Select the wavelength of maximum absorbance (λmax) in the spectrophotometer software.
2. Measure the absorbance at λmax of the five standard solutions prepared in Procedure a.
3. Using a plotting program, plot absorbance vs [Co(II)]. This is your Beer’s law calibration plot.
Obtain a linear least-squares fit to the data points.
4. Use your calibration plot to determine the concentration of Co(II) in the sample solution, and
then calculate the percent cobalt in the sample.
5. Complete the Results summary sheet.

Results Summary for Spectrophotometric Determination of Cobalt

Post-lab Questions
Q1. What was the wavelength of light at which the Co(II) stock solution had the maximum
absorbance? What color of light does this correspond to? What color was the Co(II) stock
solution?

Q3. Draw the crystal field diagram for the [Co(H2O)6]2+ complex.

Q4. Use your diagram in question 3 to discuss the absorption of visible light.

Q5. What would happen to your Beer’s law calibration plot if you had forgotten to seal your test
tubes containing your metal complex solution?

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