Determination of phosphorus in turbid freshwaters using alkaline peroxodisulphate digestion

Methods for determining phosphorus in turbid lake and river water using heating with an autoclave or a microwave and employing alkaline peroxodisulphate digestion have been investigated. Suspensions (up to 100 ugP/L) of two standard reference materials (NIES No. 3 Chlorella and NEES No. 2 Pond Sediment) were used to optimised procedures. Quantitative recoveries of phosphorus were achieved when the final solution to be digested contained 0.045 M potassium peroxodisulphate and 0.04 M sodium hydroxide and solutions were autoclaved at 120C for 60 min. or microwaved at 450 Watts for 5-10 min. Complete recoveries of phosphorus (99- 103%) from 20 ugP/U 50 ugP/L and 100 ugP/L Chlorella suspensions were obtained using autoclave and microwave heating. For the Pond Sediment suspensions complete recoveries of phosphorus (99-104%) from the 20 ugP/L and 50 ugP/L were obtained using both heating methods. Higher recoveries from the 100 u.gP/L Pond Sediment suspensions were obtained using microwave heating (961%) than autoclaving (885%). Further analysis of Pond Sediment suspensions using the autoclave heating showed that complete recovery of phosphorus (98l%) from 60 ngP/L suspensions was achieved with incomplete recoveries (92.30.7%, 91?2% and 91?1%) from 70 ugP/L, 80 ugP/L and 90 ug P/L suspensions respectively. Recoveries of phosphorus compounds (orthophosphate and phosphonates) added to distilled water and turbid lake water were near quantitative (91-117%) for both digestion methods. A range of turbid lake and river water (TP = 57-106 ugP/L; Turbidity = 16-200 NTU) were analysed for total phosphorus (TP) using the optimised alkaline peroxodisulphate digestion procedures and the APHA AWWA WPCF, sulphuric acid - nitric acid digestion procedure. No difference in total phosphorus measurements were found between the microwave digestion procedure and the APHA AWWA WPCF, nitric acid - sulphuric acid procedure. The autoclave procedure gave significantly lower recoveries of phosphorus (p