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Quantitative Analyse von Silizium

Silicon occurs in nutrient solutions primarily as silicic acid (H₄SiO₄) and silicate ions (SiO₄⁴⁻) . It is present in most plants and abundant in cereals, grasses, and tree bark. SiO 2− 3 is thought   to enhance plant disease resistance.

There are various methods for determining silicon:

  • Molybdenum blue spectrophotometry: formation of a molybdenum silicate complex with color change.
  • Gravimetric determination: precipitation of silicon dioxide (SiO₂) and weighing.
  • Complexometric titration with fluoride: formation of a SiF₆²⁻ complex, back titration with lanthanum.

Detailed titration of silicon with fluoride

1. Principle of the method

Silicon reacts with fluoride ions (F⁻) to form a stable hexafluorosilicate complex:

SiO2 + 6F SiF6²⁻

The excess fluoride ions are back-titrated with lanthanum(III) chloride (LaCl₃) . The endpoint is determined using alizarin complexone as an indicator. Color change: pink to violet .

2. Chemicals

  • 0.01 mol/L sodium fluoride (NaF) solution
  • 0.01 mol/L lanthanum (III) chloride (LaCl₃) solution
  • Buffer solution (pH 3, acetic acid/sodium acetate buffer)
  • Alizarin complexone (indicator)

3. Experimental setup

Required equipment:

  • Burette (25 mL, division 0.1 mL)
  • Erlenmeyer flask (250 mL)
  • Pipette (10 mL)
  • Magnetic stirrer

4. Implementation

  1. Pour 10 mL of the nutrient solution into a 250 mL Erlenmeyer flask.
  2. Add 5 mL of 0.01 mol/L NaF solution and let it react for 5 minutes.
  3. Add 5 mL of buffer solution (pH 3).
  4. Add 2-3 drops of alizarin complexone indicator.
  5. Titrate with 0.01 mol/L LaCl₃ until the color changes from pink to violet .

5. Calculation of the silicon concentration

The concentration of Si is calculated using the formula:

c ( Si ) = V LaCl c LaCl 1 1 V Probe

6. Example calculation:

  • Lanthanum(III) chloride concentration: 0.01 mol/L
  • Consumed volume: 9.2 mL (0.0092 L)
  • Sample volume: 50 mL (0.050 L)
c ( Si ) = 0.0092 0.01 1 1 0.050 = 0.00184 mol/L = 1.84 mmol/L

 

Conclusion

Back titration with lanthanum is a precise method for the quantitative determination of silicon in nutrient solutions.

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