Ammoniacal nitrogen: Take 5 g soil, add 25 mL 2 (M) KCl solution, shake for half an hour, filter using whatman 42 filter paper. Use 10-20 mL extra KCl solution to rinse out the entire soil from conical flask. Transfer the entire filtrate in micro-kjeldahl flask, add 0.5 g MgO powder, set the flask in kelplus distillation system. Distill it for 6 mins ( no hard and fast rule, you need at least 50 mL distillate) and collect the evolved NH3 in 15 mL 4% boric acid-mixed indicator, titrate the distillate against 0.02/0.05 N H2SO4.
Calculation: Exchangeable NH4-N % in soil= (Vs-VB) * S * 0.014 * 100/W= Z
Exchangeable NH4-N (ppm)= Z * 104
Where, Vs= vol. of H2SO4 required for sample titration
VB= vol. of H2SO4 required for blank titration
S= strength of H2SO4 W= wt. of oven dry soil.
N.B. keep the experimental soil in deep freeze before analysis to restrict conversion of NH4+ to NO3-. Don't air dry the sample. Take two samples before analysis, one for determination of ammonium and nitrate and another for moisture determination (as you need the oven dry weight).
Nitrate nitrogen: Now take the micro-kjeldahl flask again and add a pinch of Devarda's alloy and 10 mL 1% NaOH and distill it again and collect ammonia in 4% boric acid-mixed indicator solution. Titrate it in same way.
Ammoniacal nitrogen: Take 5 g soil, add 25 mL 2 (M) KCl solution, shake for half an hour, filter using whatman 42 filter paper. Use 10-20 mL extra KCl solution to rinse out the entire soil from conical flask. Transfer the entire filtrate in micro-kjeldahl flask, add 0.5 g MgO powder, set the flask in kelplus distillation system. Distill it for 6 mins ( no hard and fast rule, you need at least 50 mL distillate) and collect the evolved NH3 in 15 mL 4% boric acid-mixed indicator, titrate the distillate against 0.02/0.05 N H2SO4.
Calculation: Exchangeable NH4-N % in soil= (Vs-VB) * S * 0.014 * 100/W= Z
Exchangeable NH4-N (ppm)= Z * 104
Where, Vs= vol. of H2SO4 required for sample titration
VB= vol. of H2SO4 required for blank titration
S= strength of H2SO4 W= wt. of oven dry soil.
N.B. keep the experimental soil in deep freeze before analysis to restrict conversion of NH4+ to NO3-. Don't air dry the sample. Take two samples before analysis, one for determination of ammonium and nitrate and another for moisture determination (as you need the oven dry weight).
Nitrate nitrogen: Now take the micro-kjeldahl flask again and add a pinch of Devarda's alloy and 10 mL 1% NaOH and distill it again and collect ammonia in 4% boric acid-mixed indicator solution. Titrate it in same way.
Reference: Keeney, D.R., and D.W. Nelson. (1982) Nitrogen—Inorganic forms. In: A.L. Page et al., editors, Methods of soil analysis. Part 2. Chemical and microbiological properties. 2nd ed. Agron. Monogr. 9. ASA and SSSA, Madison, WI. p. 642–698.
Please find attached a link to a paper that describes extraction of inorganic N forms from soil samples with KCl and readings using an UV spectrophotometer. I also suggest you to look for papers using flow injection analysis (FIA).
The available NH4+-N in fresh soil samplescould be determined by extracting NH4+-N with 2N KCl solution. soil is equilibrated with 2N KCl for 1 hour and then filtered . NH4+-N content is determined using modified Berthelot reaction (Krom. 1980).
Available nitrate nitrogen content could be determined by the method described by Keeney and Nelson (1982). soil is equilibrated with 2N KCl for 1 hour and filtered . Then develop a yellow colour with trinitryl salicylic acid under alkaline condition. The intensity of the colour is measured.