Comparison of three persulfate digestion methods for total phosphorus analysis and estimation of suspended sediments

Abstract

As a result of impairments to fresh surface water quality due to phosphorus enrichment, substantial research effort has been put forth to quantify agricultural runoff phosphorus as related to on-field practices. While the analysis of runoff dissolved phosphorus is well prescribed and leaves little room for variability in methodology, there are several methods and variations of sample preparation reagents as well as analysis procedures for determining runoff total phosphorus. Due to the variation in methodology for determination of total phosphorus and an additional laboratory procedure required to measure suspended solids, the objectives of the current study are to i. compare the performance of three persulfate digestion methods (Acid Persulfate, USGS, and Alkaline Persulfate) for total phosphorus percent recovery across a wide range of suspended sediments (SS), and ii. evaluate the ability of using Al and/or Fe in digestion solution to predict SS as a surrogate to the traditional gravimetric method. Percent recovery of total phosphorus was determined using suspensions prepared from soils collected from 21 agricultural fields in Ohio. The Acid Persulfate method was most effective, with an average total phosphorus percent recovery of 96.6%. The second most effective method was the USGS with an average total phosphorus recovery of 76.1%. However, the Alkaline Persulfate method performed poorly with an average 24.5% total phosphorus recovery. As a result application of Alkaline Persulfate digestion to edge of field monitoring may drastically underestimated runoff total phosphorus. In addition to excellent recovery of total phosphorus, the Acid Persulfate method combined with analysis of Al and Fe by inductively coupled plasma atomic emission spectrometry provides a robust estimate of total SS. Due to the large quantity of samples that can result from water quality monitoring, an indirect measure of total SS could be very valuable when time and budget constraints limit the number of procedures that can be run on a single water sample.