Project Experiment 4: Analysis

of the % Cobalt in a Cobalt

Amine Halide Complex 
Coordination complexes

 Coordination complexes are the chemical compounds in which metal ions/atoms with
certain ligands. Here ligands are the organic molecules with extra electrons in the form of
lone pair or negative charge whereas metal atoms/ions must have empty orbitals to accept
these extra electrons to form the coordination bond.  
 Spectroscopy

 Is the study of the interaction

of light & matter
 Spectrophotometer –
instrument that uses
electromagnetic radiation
from UV, visible or IR to
analyze the absorption or
transmission of a sample
 We will use visible in our lab
Instruments of Measurement

 What do visible spectrophotometers measure?

 Amount of light absorbed by the dissolved substance

 Qualitative – color gives info about the solution composition

 Quantitative – provides numerical data for the concentration
Colors & Wavelengths
COLOR WAVELENGTH (λ in nm)
Ultraviolet < 380
Visible Light Violet 380 – 435

Blue 436 – 480

Greenish-blue 481 – 490

Bluish-green 491 – 500

Green 501 – 560

Yellowish-green 561 – 580

Yellow 581 – 595

Orange 596 – 650

Red 651 – 780

Near Infrared > 780

Purpose

This experiment demonstrates the linear relationship between the absorbance and the
concentration of a colored solution.
Beer’s Law will be used to determine the concentration of a sample (Co) for which the
concentration is unknown.
Spectrophotometry

Transmitted
Incident Light Light
Light Wavelength I0 I
Sample Detector
Source Selector

l = 1 cm
Qualitative Distinction

 Chemical solutions owe their color to light-absorbing species in the solution, whether
these are ions or complex molecules. For example:
 Your metal complex is either orange or purple. This is because your complex will absorb energy
in the visible part of the electromagnetic spectrum. We can take advantage of this by using
spectroscopy to determine the percent cobalt in your unknown complex. 
The coordination complexes can be
analyzed with the help of a spectrometer.  

In spectrometer analysis, absorbance (A) is measured with the help of a spectrometer for a certain solution
with concentration 'c' and path length 'l'. The molar absorptivity constant can be shown as 'ε’.

A= ε x c x l 
Parameters: 
 l – sample pathlength (usually 1cm) 
 c – concentration (M) 
 ε – molar absorption coefficient (because metals will absorb differently than organic molecules, there is a constant to take it into
account) in units of M-1cm-1. 
 A – light intensity (absorbance) 

We use Beers-Lambert Law to calculate concentration based on absorbance. Absorbance is directly proportional to
concentration. 
Calculations
 Percent Cobalt

 Weigh out 0.1500g of the synthesis product on the analytical balance to 4 decimal places and add it to a
volumetric flask.
 Then, under the hood, you will add a few drops of acid (synthesis 1, 2, and 6 HCl; synthesis 3, 4, and 5
HBr). To add these drops, you can put acid into a beaker then use a dropper.
 Properly dispose of the excess acid in the beaker by adding the acid to water then putting in the acid
waste.
 Then you will fill the flask to a volume of 100mL. You should know how a volumetric flask works, look at
the line that is 100mL.
 After the water is added, then you can place a stir bar into the flask (not before, so the volume is correct).
 Once the product is in solution, you will fill 2 cuvettes (with a dropper) with the solution.
 Percent Cobalt

 If confused Ask me or your TAs to set up all the specs to the proper setting for analysis.
 You are taking the reading between 400 and 800nm, so the screen will show a curve with a peak. You should move
the arrow buttons to the peak where the wavelength for the maximum absorbance. Have a TA show you this in a
demo before they start.
 The peak absorbance wavelength is the lambda max and there will be an absorbance on the screen as well.
 You should write down the wavelength with the maximum absorbance (lambda max) and the absorbance (A).
 Use the lambda max to get the extinction coefficient e using the chart on page 41.
 The formula A =ecl is used, absorbance is the number they collected from the spec, e is from the lambda max, c is
what you are solving for a l = 1cm.
 When you get the concentration, it is in M (mol/L) so you need to multiply by 0.1L and the molecular weight of
cobalt to get grams of cobalt in solution.