7C1b (Nitrate + Nitrite)-N – steam distillation

Following removal of NH4-N as described in 7C1a, add 0.2 g of Devarda’s alloy (0.35 g if not ball-milled; see Notes 4 and 5) rapidly through a dry powder funnel that reaches into flask. It is convenient to use a distillation flask fitted with a side-arm, complete with a ground glass joint to facilitate this operation. The stem of the dry-powder funnel should extend at least 1 cm below base of the ground glass joint.

Immediately reseal flask and proceed to determine the NH4-N liberated following steam distillation as described in 7C1a.

Calculation

For a Y mL aliquot of a 10 g/100 mL air-dry soil extract and 0.01 M HCl:

NO3–N + NO2–N = [(sample titre – blank titre) × Y × 100 × 0.1401]mg N/kg

Report NO3-N + NO2-N (mg N/kg) on an oven-dry basis. Use the air-dry moisture to oven-dry moisture ratio to make the oven-dry conversion. Refer to Method 2A1 for guidance with regard to this soil moisture calculation.

Notes for 7C1 Methods

1.  Make periodic checks on recovery of the various mineral-N components by substituting relevant aliquots of the two N standard solutions, diluted as necessary with 2 M KCl extracting solution.

2.  Field extraction or use of field-moist soil is necessary for accurate estimates of NO2-N and are often preferred for precise studies of soil mineral-N content. Make due allowances for a variable soil/solution ratio and for the additional moisture added.

3.  Unfiltered soil extracts based on 2 M KCl can be stored safely up to 24 h at 25°C and for up to 48 h at 4°C. Filtered extracts can be stored for at least 45 days at 25°C and for up to 4 months at ≤4°C.

4.  It is not necessary to use accurately weighed amounts of MgO and Devarda’s alloy. Calibrated glass or stainless steel scoops are satisfactory.

5.  Best and Craswell (1985) have shown that 2 M KCl soil extracts containing in excess of 0.02 M Mg can interfere in the determination of NO3-N based on use of Devarda’s alloy and subsequent steam distillation. Recoveries can be as low as 25%. The 1:10 soil/solution ratio used in this method overcame the interference on all soils tested. For narrow soil/solution ratios, as might occur with field extraction of moist soil, 0.4 g of Devarda’s alloy for a 20 mL aliquot of the 2 M KCl soil extract was always sufficient to achieve full recoveries.