A rapid and sensitive analysis of inorganic and organic phosphorus (P) is needed to analyze water and soil extracts at submicromolar concentrations. The proposed method, based on the complexation of malachite green with phosphomolybdate under acidic conditions, was adapted to a 96-well microtiter plate format, and was tested for matrix interferences using 15 soils and some common extractants, including water, KCI, CaCl2, NaOH, and HCl. The accuracy of P determination was affected when CaCl2 and HCl concentrations were greater than 0.1 M and when NaOH concentration exceeded 0.4 M. Potassium chloride concentration up to 1 M did not interfere with P determination. The molar absorptivity was 46 841 M(-1) cm(-1) and the reagent blank absorbance was 0.071+/-0.003 (n = 10). At the 99% confidence limit, the method detection limit was calculated to be 0.006 mg P L(-1). Recovery of added inorganic P in different types of soils and extracts ranged between 95 and 112% with an average of 102%. The proposed microplate method allows P to be determined rapidly in a wide range of soil types and extracts and requires limited volume (20-200 microL). The procedure uses limited quantities (40 microL) of two stable reagents (>1 yr), and generates low amounts of hazardous waste.

Under Fe(3+)-reducing conditions, soil Fe(2+) oxidation has been shown to be coupled with nitrate (NO3(-)) reduction. One possible secondary reaction is the involvement of NO3(-) and nitrite (NO2(-)) with magnetite, a mixed valence Fe(2+)/Fe(3+) mineral found in many natural environments. Currently, little information exists on NO3(-) and NO2(-) reactivity with magnetite. This study investigates NO3(-) and NO2(-) reactivity with magnetite under anoxic conditions using batch kinetic experiments across a range of pH values (5.5-7.5) and in the presence of added dissolved Fe(2+). Solid phase products were characterized using X-ray diffraction (XRD), Mössbauer spectroscopy, and scanning electron microscopy (SEM). Nitrate removal by magnetite was much slower when compared with NO2(-). There was a pH-dependence in the reduction of NO2(-) by magnetite; the initial rate of NO2(-) removal was two times faster at pH 5.5 than at pH 7.5. The influence of pH was explained by the binding of NO2(-) to positively charged sites on magnetite (≡ S-OH2(+)) and to neutral sites (≡ S-OH(0)). As NO2(-) was removed from solution, nitric oxide (NO) and nitrous oxide (N2O) were identified as products confirming that nitrite was reduced. Structural Fe(2+) in magnetite was determined to be the reductant of NO2(-) based on the lack of measurable dissolved Fe(2+) release to solution coupled with Mössbauer spectra and XRD analysis of solid phase products. Addition of dissolved Fe(2+) to magnetite slurries resulted in adsorption and an acceleration in the rate of nitrite reduction at a given pH value. In summary, findings reported in this study demonstrate that if magnetite is present in Fe(3+)-reducing soil and NO2(-) is available, it can remove NO2(-) from solution and reduce a portion of it abiotically to NO and subsequently to N2O by a heterogeneous electron transfer process.

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