Phosphorus extraction procedures, selective

Methyl parathion was determined in dog and human serum using a benzene extraction procedure followed by GC/FID detection (Braeckman et al. 1980, 1983 DePotter et al. 1978). An alkali flame FID (nitrogen-phosphorus) detector increased the specificity of FID for the organophosphorus pesticides. The detection limit was in the low ppb (pg/L). In a comparison of rat blood and brain tissue samples analyzed by both GC/FPD and GC/FID, Gabica et al. (1971) found that GC/FPD provided better specificity. The minimum detectable level for both techniques was 3.0 ppb, but GC/FPD was more selective. The EPA-recommended method for analysis of low levels (<0.1 ppm) of methyl parathion in tissue, blood, and urine is GC/FPD for phosphorus (EPA 1980d). Methyl parathion is not thermally stable above 120 °C (Keith and Walters 1985). 

Phosphorus extracted from sediment by NaOH has been related to non-occluded, surface-exchangeable, bioavailable forms (22). Hydrochloric acid extraction yields occluded phosphorus incorporated in hydrous metal oxides, carbonate and phosphate minerals of sediment. Hydroxylamine reagent specifically removes hydrous manganese oxides, while amorphous hydrous oxides of iron and aluminijm are removed by the oxalate reagent. Total available sediment phosphorus analyses includes sediment organic phosphorus components in addition to the inorganic portion determined by the selective extraction procedures. 

Several chemical reactions, including calcium carbonate and hydroxyapatite precipitation, have been studied to determine their relationship to observed water column and sediment phosphorus contents in hard water regions of New York State. Three separate techniques have been used to Identify reactions important in the distribution of phosphorus between the water column and sediments 1) sediment sample analysis employing a variety of selective extraction procedures 2) chemical equilibrium calculations to determine ion activity products for mineral phases involved in phosphorus transport and 3) seeded calcium carbonate crystallization measurements in the presence and absence of phosphate ion. 

Ruban, V., Ldpez-Sanchez, J. F., Pardo, P., Rauret, G., Muntau, H., and Quevauviller, Ph. (1999). Selection and evaluation of sequential extraction procedures for the determination of phosphorus forms in lake sediment. J. Environ. Monit. 1, 51-56. 

The determination of phosphorus after precipitation and solvent extraction as molybdophos-phoric acid (MPA) and reduction to molybdenum blue is a classical procedure,30 40 while cerium can be determined directly as molybdocerophosphoric acid (MCPA emax 7300 at 318 nm). A more selective method is to strip excess of MPA by extraction with chloroform, then to decompose residual MCPA and determine the phosphate liberated therefrom as MPA after extraction into isobutyl acetate. Alternatively AAS can be used to determine the amount of molybdenum. 

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