A10

Experiment 10
Determination of molybdenum using solvent extraction
Aim: To determine the concentration of molybdenum in a solution by the thiocyanate

method, using solvent extraction and ultraviolet spectrophotometry.
Introduction
Solvent extraction is a rapid technique for isolating a substance of interest, often as

a chelate complex, with the ability to concentrate the (trace) material by using a small
volume of extractant for a large volume of analyte solution.
Molybdenum(VI) in acid solution when treated with stannous chloride (in the
presence of a little Fe2+) is converted largely into Mo(V). This forms a complex with
thiocyanate anion, probably largely Mo(SCN)5, which is red and may be extracted by
oxygenated solvents (herein: isoamyl alcohol). The colour depends upon the acid
concentration (optimum 1M), and the concentration of thiocyanate anion (not less than 1%,
with the colour intensity being constant in the range 2-10%). The colour is not changed by
excess of stannous chloride. The molybdenum complex has maximum absorption at 465
nm.
Under the experimental conditions the following elements interfere in the stated
amounts, giving an error >3%, when the amount of Mo is 10 µ g:
V 0.4 mg - gives a yellow colour. The interference may be prevented by washing the
extract with stannous chloride solution.
Cr(VI) 2 mg - gives a purple colour.
W(VI) 0.15 mg - gives a yellow colour.
Co 12 mg - gives a slight green colour.
Cu 5 mg; Pb 10 mg; Ti(III) 30 mg.
32
Method
Caution: Concentrated acids must be used and kept in the fumehood, with the glass
pulled down, and handled by gloves. Mop up any spillage immediately by excess water.
You are provided with a 0.001 w/w% Mo stock solution (i.e. containing 10 µ g Mo
per cm3). Make up calibration solutions by pipetting 1.0, 2.0, 3.0, 4.0 and 5.0 cm3 of this
solution into 50 cm3 separatory funnels and diluting each with an equal volume of water.
Note: these solutions contain 10, 20...50 µ g of Mo.
Add to each funnel 2.0 cm3 (from a 10 cm3 measuring cylinder) conc. HCl, 1.0 cm3
ferrous ammonium sulphate (FAS) solution (containing 10 g FAS in 100 cm 3 of very dilute
acid), and 3.0 cm3 of 10% aqueous potassium thiocyanate solution. Shake gently, then add
3.0 cm3 of stannous chloride solution (containing 10 g SnCl2.2H2O in 100 cm3 1 M HCl).
Add water to bring the total volume in each separatory funnel to 25 cm3, then mix. Pipette
10 cm3 of redistilled isoamyl alcohol into each funnel and shake for 30 seconds. Remember
that vigorous shaking is not required: use the movement of air bubbles on inversion to mix
the contents. Release the pressure that may build up. Then allow the phases to separate,
and carefully run out the lower aqueous layer. Remove the glass stopper and pour the
alcoholic extract through a small plug of purified glass wool in a small funnel and collect
the organic extract in a test tube. Stopper the tube.
Determine the wavelength of maximum absorbance by plotting absorption vs
wavelength between 460-470 nm at 1 nm intervals for the solution of middle concentration
of Mo. Remember to reset the zero and 100%T at each wavelength before taking
measurements. Choosing the optimum wavelength, plot the calibration curve for
absorbance vs mass of Mo in the original solution, for the range 10-50 µ g Mo.
Determine the concentration of Mo in the unknown sample provided, containing

less than 50 µ g Mo in 10 cm3. Use the calibration curve after subjecting the unknown to
the same treatment as the standard solutions above.
33
Marking scheme:
Hand in the write-up on the following week after the experiment.

Write-up, presentation and conciseness. [3]
Calibration curve [2]
Concentration of Mo in unknown [2]
Questions:
1. Write the electronic structure, and common oxidation states of Mo. [1]
2. State 4 factors which govern the choice of a solvent for extraction. [1]
3. Suggest how the procedure might be modified for the determination of Mo in a steel
sample. [1]
Source: A.I. Vogel, Quantitative Inorganic Analysis, 3rd Ed. Longmans.
34

A10

Uploaded by

Copyright:

Available Formats

A10

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

A10

Uploaded by

Copyright:

Available Formats

Experiment 10

Determination of molybdenum using solvent extraction

Aim: To determine the concentration of molybdenum in a solution by the thiocyanate

Solvent extraction is a rapid technique for isolating a substance of interest, often as

Note: these solutions contain 10, 20...50 µ g of Mo.

Determine the concentration of Mo in the unknown sample provided, containing

Hand in the write-up on the following week after the experiment.

Source: A.I. Vogel, Quantitative Inorganic Analysis, 3rd Ed. Longmans.

You might also like