Samples for total and dissolved phosphorus and nitrogen analysis (as well as dissolved silicon, calcium, magnesium, sodium, potassium, iron, and manganese) are collected together with a peristaltic pump and tubing and in-line filtered, when necessary, (through a 40 micron polycarbonate filter) into 120 ml LDPE bottles and acidified to a 1% HCl matrix by adding 1 mL of ultra pure concentrated HCl to 100 mls of sample. For every sample acidification event, three acid blanks are created by adding the same acid used on the samples to 100 mls of ultra pure water supplied from the lab. Once acidified, the samples are stable at room temperature until analysis, which should occur within one year. Until acidification, the samples should be refrigerated at 4 degrees Celsius.
The samples must first be prepared for analysis by adding an NaOH–Persulfate digestion reagent and heated for an hour at 120 degrees C and 18-20 psi in an autoclave.
The samples are analyzed for total nitrogen and total phosphorus simultaneously by automated colorimetric spectrophotometry, using a segmented flow autoanalyzer. Total phosphorus is determined by forming a phosphoantimonylmolybdenum complex and the absorption is monitored at 880 nm.
The detection limit for total phosphorus is approximately 3 ppb and the analytical range for the method extends to 800 ppb.
Method Log: Prior to January 2006 samples, total phosphorus was determined on a Technicon segmented flow autoanalyzer. From 2006 to present, total phosphorus is determined by an Astoria-Pacific Astoria II segmented flow autoanalyzer.
field & laboratory