DETERMINING TOTAL NITROGEN CONTENT

Materials Needed:

Wastewater Samples: Collect samples of the wastewater you want to analyze.

Reagents and Chemicals:

Devarda's alloy or a similar reducing agent
Dilute sulfuric acid
Alkaline potassium per-sulfate solution
Distilled water

Apparatus:
Kjeldahl flask with a reflux condenser
Digestion apparatus or block digester
Distillation apparatus (Kjeldahl distillation unit)
Titration equipment (burette, pipettes)
pH indicator (phenolphthalein)
Standardized sulfuric acid solution (approximately 0.1 N)
Standardized sodium hydroxide solution (approximately 0.1 N)

Safety Equipment:
Lab coat
Safety glasses
Gloves
Fume hood (recommended for handling chemicals)

Procedure:

Sample Preparation:
a. Measure an appropriate volume of the wastewater sample (usually around
10-20 mL) into a Kjeldahl flask.
b. If the sample contains suspended solids, filter it to remove them.

Digestion:
a. Add a known amount of Devarda's alloy (a reducing agent) to the flask.
(0.2 to 1.0 grams of Devarda's alloy per gram of nitrogen in the sample).
b. Add a few mL of dilute sulfuric acid to the flask. (If the nitrogen content in your
sample is low, you may use a lower volume of dilute sulfuric acid, such as 5 to 10 mL per
gram of the sample; For samples with moderate to high nitrogen content, you might use a
higher volume, such as 10 to 15 mL per gram of the sample.)
c. Heat the mixture gently using a digestion apparatus or block digester until
the solution becomes clear. This step converts organic nitrogen to ammonium
sulfate.
Distillation:
a. After digestion, cool the flask and transfer the contents to the Kjeldahl
distillation unit.
b. Add alkaline potassium persulfate solution to the distillation unit to release
ammonia. (add about 5 mL to 10 mL of alkaline potassium persulfate solution to the
distillation unit for each sample.)
c. Distill the ammonia into a receiving solution containing a known amount of
sulfuric acid. (In many cases, a standard amount is used, such as 25 mL of a known
concentration of sulfuric acid (typically around 4% w/v); For samples with low nitrogen
content, you might use a lower volume, such as 20 mL of sulfuric acid; For samples with high
nitrogen content, a higher volume, such as 30 mL, might be appropriate.)

Titration:
a. Titrate
the distilled solution with standardized sodium hydroxide solution
using a burette. (In many cases, a standard amount is used, such as 50 mL of standardized
sodium hydroxide solution; For samples with low nitrogen content, you might use a lower
volume, such as 25 mL of sodium hydroxide; For samples with high nitrogen content, a higher
volume, such as 75 mL, might be appropriate.)
b. Use a pH indicator (e.g., phenolphthalein) to determine the endpoint of the
titration.

Calculations:
a. Calculate the total nitrogen content using the volume and concentration of
the sodium hydroxide solution.

Quality Control:
a. Run blank and standard samples to ensure the accuracy of the analysis.
b. Check for consistency and precision in your results.
 DETERMINING TOTAL PHOSPHORUS CONTENT

Materials Needed:

Wastewater Samples: Collect samples of the wastewater you want to analyze.

Reagents and Chemicals:

Sulfuric acid
Perchloric acid
Ammonium molybdate solution
Ascorbic acid solution
Standard phosphate solution
Distilled water

Apparatus:
Digestion apparatus (digestion tubes, digestion block)
Spectrophotometer or colorimeter
Cuvettes or test tubes for spectrophotometric analysis
Pipettes and burettes
pH meter
Fume hood (recommended for handling acids)

Safety Equipment:
Lab coat
Safety glasses
Gloves
Fume hood (if handling acids)

Procedure:

Sample Preparation:
a. Measure an appropriate volume of the wastewater sample (usually around
10-20 mL).

Digestion:
a. Transfer the sample to a digestion tube.
b. Add a mixture of sulfuric acid (add about 5 to 10 mL of concentrated sulfuric acid
per gram of the sample) and perchloric acid (a few drops to enhance the digestion
process) to the digestion tube.
c. Digest the sample using a digestion block until a clear solution is obtained.
This step converts all forms of phosphorus to orthophosphate.

Cooling and Dilution:

a. Allow the digested sample to cool.
b. Dilute the sample with distilled water.

Phosphate Reaction:
a. Add ammonium molybdate solution to the digested and diluted sample. This
forms a yellow phosphomolybdic acid complex. (a standard amount is used, such as
5 mL to 10 mL of ammonium molybdate solution; For samples with low phosphorus content,
 you might use a lower volume, such as 2 mL to 5 mL; For samples with high phosphorus
content, a higher volume, such as 10 mL to 15 mL, might be appropriate.)

Reduction:
a. Add ascorbic acid solution to reduce the yellow complex to a blue complex
(molybdenum blue). This is a crucial step for the colorimetric determination.
(a standard amount is used, such as 2 mL to 5 mL of ascorbic acid solution; For samples with
low phosphorus content, you might use a lower volume, such as 1 mL to 2 mL; For samples
with high phosphorus content, a higher volume, such as 5 mL to 10 mL, might be
appropriate.)

Calibration:
a. Prepare a series of standard solutions with known concentrations of
phosphate using a standard phosphate solution.

Colorimetric Measurement:
a. Measure the absorbance of both the sample and standards at a specific
wavelength using a spectrophotometer or colorimeter.

Calculations:
a. Use the absorbance values of the standards to create a calibration curve.
b. Determine the concentration of phosphorus in the sample based on its
sabsorbance and the calibration curve.

Quality Control:
a. Run blank and standard samples to ensure the accuracy of the analysis.
b. Check for consistency and precision in your results.