CHEMICAL ANALYSIS OF SOIL

1. DETERMINATION OF NITROGEN CONTENT

1.1. MATERIALS
1.1.1. Analytical balance
1.1.2. Beaker
1.1.3. Distilling flask
1.1.4. Hot plate
1.1.5. Pipette
1.1.6. Buret
1.1.7. Funnel
1.1.8. Erlenmeyer flask

1.2. REAGENTS
1.2.1. CuSO4
1.2.2. K2SO4
1.2.3. H2SO4
1.2.4. NaOH

1.3. PROCEDURE
1.3.1. Weigh 1.0 g of air-dried sample and place in 500 ml flask.
1.3.2. Add 0.7 g of CuSO4, 1.5 g of K2SO4, and 30 ml of H2SO4.
1.3.3. Mix the contents of the flask until complete solution results
1.3.4. Heat gently the solution using hot plate until frothing ceases. Bring to boil until
the solution is clear then continue the digestion for 30 minutes.
1.3.5. Cool the solution and dilute 50 ml of distilled water
1.3.6. Swirl and transfer in distilling flask.
1.3.7. Place 25 ml standard acid (0.1M H2SO4) in the receiving conical flask and add 3
drops of Methyl red indicator. Add enough distilled water to cover the end of the
condenser outlet tubes. Run water through the condenser.
1.3.8. Add 30 ml of 35% NaOH in distilling flask. Do not mix the solution.
1.3.9. Heat the solution for 35 minutes to distill the ammonia content. Remove the
receiving flask and wash the outlet tube into the receiving flask with distilled
water.
1.3.10. Titrate the excess acid with 0.1 M NaOH solution until the pink color changes to
yellow.
1.3.11. Determine the blank on reagents using the same quantity of standard acid in a
receiving conical flask.
 Calculation:

1.401⦋ ( V 1 M 1−V 2 M 2 )−( V 3 M 1−V 4 M 2 ) ⦌

%N= X 100(df )
W
Where:
V1- ml of standard acid put in receiving flask for sample;
V2- ml of standard NaOH used in titration;
V3- ml standard acid put in receiving flask for blank;
V4- ml standard NaOH used in titrating blank;
M1- molarity of standard unit;
M2- molarity of standard NaOH;
W- weight of sample taken(g);
df- dilution factor (100)

Note: 1000 ml of 1.0 M HCl corresponds to 1.401 n of N.

2. DETERMINATION OF POTASSIUM CONTENT

2.1. MATERIALS
2.1.1. Polyethylene bottle
2.1.2. Shaker
2.1.3. Spectrometer
2.1.4. Bottle with stopper
2.1.5. Pipette
2.1.6. Beaker

2.2. REAGENTS
2.2.1. Ammonium acetate
2.2.2. Potassium standards

2.3. PROCEDURE
2.3.1. Weigh 10 g of air-dried soil sample and place 100 ml polyethylene bottle. Then
add 50 ml of ammonium acetate solution.
2.3.2. Seal the bottle with stopper and shake for 30 minutes.
2.3.3. Allow to stand for 5 minutes and decant the supernatant liquid using Whatman
no.2 filter paper.
2.3.4. The prepared potassium standard solutions should cover the range 0 to 100ppm
potassium. Set the photometer at 100 using the 100 ppm potassium solution.
2.3.5. Aspirate the 20, 40, 60, and 80 ppm potassium standard solutions and prepare a
calibration graph.
2.3.6. The potassium content of the soil sample will be determine by aspirating the
solutions. If necessary, dilute the solution in ammonium acetate solution.
 2.3.7. Calculate the concentration by reference to the calibration graph into dilution
factors.

3. DETERMINATION OF PHOSPHORUS CONTENT

3.1. MATERIALS
3.1.1. Analytical balance
3.1.2. Conical flask
3.1.3. Pipette
3.1.4. Volumetric flask
3.1.5. Filter paper
3.1.6. Spectrometer
3.1.7. Shaker

3.2. REAGENTS
3.2.1. Bray’s extractant
3.2.2. SnCl2
3.2.3. Molybdate reagent
3.2.4. Soil extract

3.3. PROCEDURE
3.3.1. Weigh 5 g of air-dried soil sample. Place in conical flask then add 50 ml of the
Bray’s Extractant solution.
3.3.2. Shake for 5 minutes and filter using Whatman no.2
3.3.3. Pipette 5 ml of the filtered solution and place in a 25 ml volumetric flask.
3.3.4. In a separate measuring flask, dilute the 5 ml molybdate reagent in 20 ml distilled
water. Shake well and add 1 ml of SnCl2 solution using e-pipette.
3.3.5. Fill the 25 ml mark of the flask (with soil extract solution) with the second
solution and shake thoroughly.
3.3.6. After 10 minutes, read the blue color in the spectrometer.

REFERENCES
1. Blakemore, L. C., Searle, P. L. and B. K. Daly. 1987. Methods for chemical analysis of
soils. NZ Soil Bureau Scientific Reprt 80. Dept. of Scientific and Industrial Research.
Lower Hutt, New Zealand.
2. International Rice Research Institute Crop and Environmental Sciences Division
Analytical Service Laboratory. Title: Available Phosphorus (Olsen Phosphorus)
3. ISO 11464 Soil quality – Pretreatment of samples for physico-chemical analysis
4. EN 13342 Characterization of sludges - Determination of Kjeldahl nitrogen
5. Rural Development Service Technical Advice Note 31; Defra, November 2005.