Analysis

Vanadium, quantitative analysis

Quantitative Analyse von Vanadium

Vanadium occurs in nutrient solutions primarily as the vanadate ion (VO₄³⁻) or the vanadyl ion (VO²⁺) . It is beneficial for rhizobial N2 fixation.

There are various methods for determining vanadium:

  • Atomic absorption spectroscopy (AAS): High-precision method for trace analysis.
  • Spectrophotometry with peroxovanadate complexes: color development with hydrogen peroxide.
  • Redox titration with iron(II) sulfate: A chemical method for the quantitative determination of vanadium.

Detailed redox titration of vanadium with iron(II) sulfate

1. Principle of the method

Vanadium in the oxidation state +5 (VO₂⁺) is reduced with iron(II) ions (Fe²⁺):

VO₂⁺ + 2H⁺ + Fe²⁺ → VO²⁺ + Fe³⁺ + H₂O

The reduced vanadium(IV) can then be determined by back titration with potassium permanganate (KMnO₄).

2. Chemicals

  • 0.01 mol/L iron(II) sulfate solution (FeSO₄)
  • 0.01 mol/L potassium permanganate solution (KMnO₄)
  • 1 mol/L sulfuric acid (H₂SO₄) as acid medium
  • Diphenylamine sulfonate as a redox 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 10 mL of 1 mol/L sulfuric acid (H₂SO₄).
  3. Add 10 mL of 0.01 mol/L iron(II) sulfate solution.
  4. Titrate with 0.01 mol/L potassium permanganate until the color changes from colorless to light pink .

5. Calculation of the vanadium concentration

The concentration of vanadium is calculated using the formula:

c ( V ) = V KMnO₄ ⋅ c KMnO₄ ⋅ 5 V Probe

6. Example calculation:

  • Potassium permanganate concentration: 0.01 mol/L
  • Consumed volume: 9.2 mL (0.0092 L)
  • Sample volume: 50 mL (0.050 L)
c ( V ) = 0.0092 ⋅ 0.01 ⋅ 5 0.050 = 0.0092 mol/L = 9.2 mmol/L

 

Conclusion

Redox titration with iron(II) sulfate and potassium permanganate is a reliable method for the quantitative determination of vanadium in nutrient solutions.

ID: 662
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Parent Category: Technology
Category: Analysis
Also available: German (Hochdeutsch)

Xylenol orange tetrasodium salt

Xylenol orange tetrasodium salt

Xylenol orange contains one sulfonic acid, four carboxyl groups, two amino groups, and two hydroxy groups, each of which can be protonated or deprotonated. At pH ≈ 4.5, xylenol orange exists in a lemon-yellow form. In this form, xylenol orange forms a weak red to red-violet complex with some polyvalent metal ions, which is destroyed by the addition of a stronger complexing agent such as EDTA.

Use : As an indicator in titration. Typical concentration: 1 ml / 100 ml (1% solution). Approximate price: 1 g ~ €37.00. Purchase:  https://www.carlroth.com/de/de/ph-indikatoren/xylenolorange-tetranatriumsalz/p/2727.3

Technical information on Xylenol Orange Tetrasodium Salt

To determine Bi 
Cd 
Co 
Cu 
Fe 
Hg 
In 
Pb 
Sc 
Th 
Tl(III) 
V(V) 
Zn 
Zr 
rare earth metals 
Color change yellow -> orange-red 
pH transition range 6.4 - 10.4 

ID: 654

Context: 

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Parent Category: Technology
Category: Analysis
Also available: German (Hochdeutsch)

Zinc, quantitative analysis

Zinc occurs in nutrient solutions mainly as zinc ion (Zn²⁺) .

There are different methods for determining zinc:

  • Atomic absorption spectroscopy (AAS): High-precision determination of zinc.
  • Complexometric titration with EDTA: formation of a stable Zn-EDTA complex.
  • Spectrophotometry with dithizone: color development by complex formation.

Detailed titration of zinc with EDTA

1. Principle of the method

Zinc ions (Zn²⁺) react with ethylenediaminetetraacetic acid (EDTA, C₁₀H₁₆N₂O₈) to form a stable complex:

Zn²⁺ + EDTA⁴⁻ → [Zn(EDTA)]²⁻

The endpoint of the titration is detected using the Eriochrome Black-T (ErioT) indicator . The color changes from wine red to blue .

2. Chemicals

  • 0.01 mol/L EDTA solution (C₁₀H₁₆N₂O₈)
  • Buffer solution (pH 10, NH₃/NH₄⁺ buffer)
  • Eriochrome Black-T (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 10 mL of buffer solution (pH 10).
  3. Add 2-3 drops of Eriochrome Black-T indicator.
  4. Titrate with 0.01 mol/L EDTA until the color changes from wine red to blue.

5. Calculation of zinc concentration

The concentration of Zn is calculated using the formula:

c ( Zn ) = V EDTA ⋅ c EDTA ⋅ 1 1 V Probe

6. Example calculation:

  • EDTA concentration: 0.01 mol/L
  • Consumed volume: 8.5 mL (0.0085 L)
  • Sample volume: 50 mL (0.050 L)
c ( Zn ) = 0.0085 ⋅ 0.01 ⋅ 1 1 ⋅ 0.050 = 0.0017 mol/L = 1.7 mmol/L

 

Conclusion

Complexometric titration with EDTA is a precise method for the quantitative determination of zinc in nutrient solutions.

ID: 637

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Parent Category: Technology
Category: Analysis
Also available: German (Hochdeutsch)

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