Analysis
Lead is not present in any nutrient solutions. Due to possible environmental contamination, Pb²⁺ ions must be tested for. Ideally, lead should not be present in any trace. This makes it all the more important to test both the air and the water used (contaminated, for example, by old lead pipes, deposits on leaves due to dust and air pollution).
There are various methods for determining lead:
- Atomic absorption spectroscopy (AAS): Very precise method for the quantitative determination of lead.
- Complexometric titration with EDTA: A reliable method for the determination of lead with indicator color change.
- Dithizone spectrophotometry: A colorimetric method for determining lead concentrations.
Detailed complexometric titration of lead with EDTA
1. Principle of the method
Lead ions (Pb²⁺) react with ethylenediaminetetraacetic acid (EDTA, C₁₀H₁₆N₂O₈) to form a stable complex:
The endpoint of the titration is detected using the xylenol orange (XO) indicator . The color changes from red to yellow .
2. Chemicals
- 0.01 mol/L EDTA solution (C₁₀H₁₆N₂O₈)
- Acetic acid/acetate buffer solution (pH 5-6)
- Xylenol orange (indicator)
3. Experimental setup
Required equipment:
- Burette (25 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 10 mL of acetate buffer solution (pH 5-6).
- Add 2-3 drops of xylenol orange indicator.
- Titrate with 0.01 mol/L EDTA until the color changes from red to yellow.
5. Calculation of lead concentration
The concentration of Pb is calculated using the formula:
6. Example calculation:
- EDTA concentration: 0.01 mol/L
- Consumed volume: 9.2 mL (0.0092 L)
- Sample volume: 50 mL (0.050 L)
Conclusion
Complexometric titration with EDTA using xylenol orange as indicator is a precise method for the quantitative determination of lead.
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Lithium occurs in nutrient solutions primarily as the lithium ion (Li+) . Li+ can increase the chlorophyll content of some plants (e.g., potato and pepper plants). A non-essential micronutrient.
There are different methods for determining lithium:
- Atomic absorption spectroscopy (AAS): High-precision method for determining lithium.
- Flame photometry: A simple and sensitive method for measuring lithium.
- Complexometric titration with EDTA: A less common method, but possible with selected indicators.
Detailed precipitation titration of lithium with ammonium tetraphenylborate
1. Principle of the method
Lithium ions (Li⁺) react with ammonium tetraphenylborate (NH₄BPh₄) and form a poorly soluble precipitate:
The end point of the titration is determined by turbidity or gravimetrically.
2. Chemicals
- 0.01 mol/L ammonium tetraphenylborate solution (NH₄BPh₄)
- Ethanol-water mixture as solvent
- Phenolphthalein as a turbidity indicator
3. Experimental setup
Required equipment:
- Burette (25 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 20 mL of ethanol-water mixture.
- Titrate with 0.01 mol/L ammonium tetraphenylborate solution until a permanent turbidity is visible .
5. Calculation of the lithium concentration
The concentration of lithium is calculated using the formula
:
6. Beispielrechnung:
- Ammoniumtetraphenylborat-Konzentration: 0,01 mol/L
- Verbrauchtes Volumen: 7,5 mL (0,0075 L)
- Probenvolumen: 50 mL (0,050 L)
Fazit
Die Fällungstitration mit Ammoniumtetraphenylborat ist eine zuverlässige Methode zur quantitativen Bestimmung von Lithium in Nährstofflösungen.
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There are different methods for determining manganese:
- Atomic absorption spectroscopy (AAS): High-precision determination of Mn²⁺.
- Oxidimetric titration with KMnO₄: direct determination by redox reaction.
- Complexometric titration with EDTA: Precise determination by chelation.
- Spectrophotometry: Color complex formation with suitable reagents.
Detailed titration of manganese with potassium Permanganate (KMnO₄)
1. Principle of the method
Manganese ions (Mn²⁺) are oxidized by potassium Permanganate (KMnO₄). In acidic solution, Mn²⁺ reacts with KMnO₄ according to the equation:
The end point of the titration is identified by the faint pink color of the unreacted Permanganate.
2. Chemicals
- 0.01 mol/L potassium Permanganate solution (KMnO₄)
- Sulfuric acid (H₂SO₄), 1 mol/L
- Distilled water
3. Experimental setup
Required equipment:
- Burette (25 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 10 mL of 1 mol/L sulfuric acid.
- Titrate with 0.01 mol/L KMnO₄ until a faint pink color persists.
5. Calculation of manganese concentration
The concentration of Mn²⁺ is calculated using the formula:
6. Example calculation:
- Potassium permanganate concentration: 0.01 mol/L
- Consumed volume: 7.2 mL (0.0072 L)
- Sample volume: 50 mL (0.050 L)
Conclusion
Redox titration with KMnO₄ is a precise method for the quantitative determination of manganese in nutrient solutions.
ID: 634
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Mercury (Hg) is a highly toxic heavy metal that is normally not found in drinking water. However, it can get into the environment through industrial emissions, mining activities or fossil fuels. Due to its toxicity and enrichment in organisms, the detection of mercury in drinking water is of great importance.
Limit values for mercury in drinking water
- EU limit: approx. 1 µg / L (0.001 mg / L) for inorganic mercury
- WHO guideline: approx. 6 µg / L (0.006 mg / L) (depending on the shape of the mercury)
Alternative analytical methods for mercury
- Cold vapor atomic absorption spectrometry (CVAAS): Very sensitive, suitable for trace analysis.
- Inductively coupled plasma mass spectrometry (ICP-MS): Extremely sensitive, detection in the ng / L range.
- Anodic Stripping Voltammetrie (ASV): Electrochemical method with high sensitivity.
- Spectrophotometry with dithizone: Color reaction that enables qualitative proof.
Qualitative detection reaction using dithizone
The method can be used with Dithizone for a qualitative analysis of mercury in drinking water. Dithizon reacts with Hg ²⁺ to form an intense red colored chelate complex.
1. Principle of method
In the reaction, Dithizone is converted to a stable Hg-Dithizone complex with Hg ²⁺:
Hg²⁺+Dithizon→[Hg (Dithizon)]
The resulting complex shows an intense red-violet color that is visible even at very low concentrations.
2. Chemicals
- 0,01 mol/L Dithizon-Lösung (C₁₃H₁₂N₄S)
- Diluted sulfuric acid (H ₂ SO ₄) – to adjust a suitable acidic environment
- Chloroform (CHCl ₃) – optional, for extracting the colored complex to improve visibility
- Pufferlösung (from. B. Essigsäure / Natriumacetate, pH 4 – 5)
3. Experimental setup
Required devices:
- Bürette (25 mL, division 0.1 mL)
- Erlenmeyer flask (250 mL)
- Pipettes (10 mL and 50 mL)
- Magnetic stirrer
- Separating funnel (for chloroform extraction, if used)
4. Implementation
- Transfer 10 mL of the drinking water sample into a 250 mL Erlenmeyer flask.
- Add 5 mL of the buffer solution (pH 4 – 5) to adjust the pH.
- Add 5 mL to the 0.01 mol / L Dithizone solution and mix the sample thoroughly.
- Optional: perform a chloroform extraction in a separating funnel to isolate the colored complex.
- Watch the color change. An intense red-violet hue indicates the presence of Hg ²⁺ ions.
Conclusion
The Dithizone test is a qualitative method that, due to its high sensitivity, is suitable for the detection of mercury in drinking water. It can already make Hg ²⁺ concentrations in the µg / L range visible, which is sufficient compared to the legal limit values (approx. 1 – 6 µg / L). However, instrumental methods such as CVAAS, ICP-MS or ASV should be used for a precise quantitative determination.
ID: 680
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Mercury (Hg) does not occur naturally in plant nutrient solutions. It is a heavy metal that is highly toxic to plants, animals, and humans.
Nevertheless, mercury can enter plants from contaminated soil, water sources, or the air. It is usually absorbed in the form of Hg²⁺ ions or organic mercury compounds such as methylmercury (CH₃Hg⁺).
There are various methods for determining mercury:
- Atomic absorption spectroscopy (AAS): Highly sensitive method for determining traces of mercury.
- Cold vapor atomic absorption spectroscopy (CVAAS): A special form of AAS that is particularly suitable for mercury.
- Inductively coupled plasma mass spectrometry (ICP-MS): High-precision method for determining extremely low mercury concentrations.
- Voltammetry: Electrochemical method for the determination of Hg²⁺ in solutions.
- Spectrophotometry with dithizone: Color reaction of Hg²⁺ with dithizone results in a quantifiable color change.
- Potentiometric titration with dithizone: A rare method for Hg²⁺ detection.
Detailed titration of mercury with dithizone
1. Principle of the method
Mercury ions (Hg²⁺) react with dithizone (C₁₃H₁₂N₄S) in a complexometric titration, forming a stable, colored Hg dithizonate:
The end point of the titration is identified by a clear color change from red to violet .
2. Chemicals
- 0.01 mol/L dithizone solution (C₁₃H₁₂N₄S)
- Sulfuric acid (H₂SO₄, diluted)
- Chloroform (CHCl₃, for extraction)
- Buffer solution (pH 4-5)
3. Experimental setup
Required equipment:
- Burette (25 mL, division 0.1 mL)
- Erlenmeyer flask (250 mL)
- Pipette (10 mL)
- Magnetic stirrer
- Separatory funnel for chloroform extraction
4. Implementation
- Pour 10 mL of the nutrient solution into a 250 mL Erlenmeyer flask.
- Add 5 mL of buffer solution (pH 4-5).
- Add 5 mL of dithizone solution and shake vigorously.
- Titrate with 0.01 mol/L Hg²⁺ standard until the color changes from red to violet .
- For better sensitivity, chloroform extraction can be performed.
5. Calculation of the mercury concentration
The concentration of Hg is calculated using the formula:
6. Example calculation:
- Dithizone concentration: 0.01 mol/L
- Consumed volume: 7.2 mL (0.0072 L)
- Sample volume: 50 mL (0.050 L)
Conclusion
Titration with dithizone is a possible method for determining mercury in solutions, but is rarely used because more sensitive techniques such as CVAAS or ICP-MS are more accurate.
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