Determination of phosphorus and potassium in commercial inorganic fertilizers by inductively coupled plasma-optical emission spectrometry: single-laboratory validation.

A two-part single-laboratory validation study was conducted for determination of the P and K content in commercial fertilizer materials by inductively coupled plasma-optical emission spectrometry (ICP-OES). While several methods exist for determination of P and K in fertilizer products, the main focus of this study was on ICP-OES determination, which offers several unique advantages. Fertilizer samples with consensus P and K values from the Magruder and Association of Fertilizer and Phosphate Chemists (AFPC) check sample programs were selected for this study. Validation materials ranging from 4.4 to 52.4% P205 (1.7 to 22.7% P) and 3 to 62% K20 (2.5 to 51.5% K) were utilized. Because all P and K compounds contained in fertilizer materials are not "available" for plants to use, this study was conducted in two parts. Part A focused on ammonium citrate-disodium EDTA as the extraction solvent, as it estimates the pool of fertilizer P and K that is considered available to plants. Part B focused on hydrochloric acid as the digestion solvent, as it estimates the total P and K content of the fertilizer product. Selectivity studies indicated that this method can have a high bias for fertilizer products containing sources of phosphite or organic P compared to gravimetric or colorimetric methods that measure just orthophosphate. Provided the analytical challenges outlined in this study are addressed, this method offers the potential for a quick, accurate, and safe alternative for determining the P and K content of commercial inorganic fertilizer materials.

Simultaneous determination of arsenic, cadmium, calcium, chromium, cobalt, copper, iron, lead, magnesium, manganese, molybdenum, nickel, selenium, and zinc in fertilizers by microwave acid digestion and inductively coupled plasma-optical emission spectrometry detection: single-laboratory validation of a modification and extension of AOAC 2006.03.

A single-laboratory validation study was conducted for the simultaneous determination of arsenic, cadmium, calcium, cobalt, copper, chromium, iron, lead, magnesium, manganese, molybdenum, nickel, selenium, and zinc in all major types of commercial fertilizer products by microwave digestion and inductively coupled plasma-optical emission spectroscopy analysis. This validation study proposes an extension and modification of AOAC 2006.03. The extension is the inclusion of calcium, copper, iron, magnesium, manganese, and zinc, and the modification is incorporation of hydrochloric acid in the digestion system. This dual acid digestion utilizes both hydrochloric and nitric acids in a 3 to 9 mL volume ratio/100 mL. In addition to 15 of the 30 original validation materials used in the 2006.03 collaborative study, National Institute of Standards and Technology Standard Reference Material 695 and Magruder 2009-06 were incorporated as accuracy materials. The main benefits of this proposed method are a significant increase in laboratory efficiency when compared to the use of both AOAC Methods 965.09 and 2006.03 to achieve the same objective and an enhanced recovery of several metals.

Determination of total sulfur in fertilizers by high temperature combustion: single-laboratory validation.

Asingle-laboratory validation study was conducted for the determination of total sulfur (S) in a variety of common, inorganic fertilizers by combustion. The procedure involves conversion of S species into SO2 through combustion at 1150 degrees C, absorption then desorption from a purge and trap column, followed by measurement by a thermal conductivity detector. Eleven different validation materials were selected for study, which included four commercial fertilizer products, five fertilizers from the Magruder Check Sample Program, one reagent grade product, and one certified organic reference material. S content ranged between 1.47 and 91% as sulfate, thiosulfate, and elemental and organically bound S. Determinations of check samples were performed on 3 different days with four replicates/day. Determinations for non-Magruder samples were performed on 2 different days. Recoveries ranged from 94.3 to 125.9%. ABS SL absolute SD among runs ranged from 0.038 to 0.487%. Based on the accuracy and precision demonstrated here, it is recommended that this method be collaboratively studied for the determination of total S in fertilizers.