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Quantitative Analyse von Eisen

Iron is usually present in nutrient solutions as Fe²⁺ (e.g., in chelates) or Fe³⁺ (free iron). The following methods are used for determination:

  • Complexometric titration with EDTA: Frequently used method for Fe³⁺.
  • Spectrophotometry with phenanthroline: For Fe²⁺.
  • Atomic absorption spectroscopy (AAS): High-precision laboratory analysis.
  • ICP-OES: Accurate for multiple measurements, but complex.

Detailed titration of iron with EDTA

1. Principle of the method

Iron(III) ions ( Fe³⁺ ) form a stable chelate complex with EDTA (C₁₀H₁₆N₂O₈) :

Fe³⁺ + EDTA⁴⁻ Fe-EDTA

Endpoint detection is carried out using the indicator xylenol orange , which changes from red to yellow.

 

2. Chemicals

  • 0.01 mol/L EDTA solution
  • Xylenol orange (indicator)
  • Acetic acid/sodium acetate buffer solution (pH 5-6)
  • Distilled water

3. Experimental setup

Required equipment:

  • Burette (50 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 acetate buffer solution (pH 5-6).
  3. Add 2-3 drops of xylenol orange as an indicator (color: red).
  4. Titrate with 0.01 mol/L EDTA solution until the color changes from red to yellow.

5. Calculation of iron concentration

The iron concentration is calculated using the following formula:

c ( Fe³⁺ ) = V EDTA c EDTA V Probe

 

6. Example calculation:

  • EDTA concentration: 0.01 mol/L
  • Consumed volume: 12.4 mL (0.0124 L)
  • Sample volume: 50 mL (0.050 L)
c ( Fe³⁺ ) = 0.0124 0.01 0.050 = 0.00248 mol/L = 2.48 mmol/L

 

Comparison of methods

 Methode  Empfindlichkeit  Geräteaufwand  Störungen
 EDTA-Titration  Mittel (ab ca. 1 mg/L Fe)  Gering  Cu²⁺, Zn²⁺ können stören
 Phenanthrolin-Methode  Hoch (bis 0,1 mg/L)  Spektrophotometer erforderlich  pH-Wert muss exakt eingestellt sein
 AAS/ICP-OES  Sehr hoch (<0,01 mg/L)  Teure Geräte erforderlich  Sehr selektiv
 Redox-Titration  Geringer als EDTA  Keine Spezialgeräte nötig  Andere Redoxaktive Stoffe stören

 

Conclusion

  • EDTA titration is a good choice for medium to high iron concentrations (>1 mg/L).
  • Phenanthroline photometry is ideal for low concentrations (<1 mg/L).
  • AAS/ICP-OES is the most accurate but expensive.
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