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) :
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
- Pour 10 mL of the nutrient solution into a 250 mL Erlenmeyer flask.
- Add 5 mL of acetate buffer solution (pH 5-6).
- Add 2-3 drops of xylenol orange as an indicator (color: red).
- 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:
6. Example calculation:
- EDTA concentration: 0.01 mol/L
- Consumed volume: 12.4 mL (0.0124 L)
- Sample volume: 50 mL (0.050 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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