Flow injection analysis of nanomolar level orthophosphate in seawater with solid phase enrichment and colorimetric detection

摘要

Phosphomolybdenum blue (PMB) paired with cetyltrimethylammonium bromide (CTAB) can be extracted using a solid phase extraction technique on C18 sorbent. Based on this, a novel on-line solid phase extraction method coupled with flow injection (FI) analysis and colorimetric detection,has been established to determine nanomolar level orthophosphate in seawater. A stopped flow technique was employed to assure the complete formation of the PMB-CTAB compound, which was sequentially extracted on an in-line Sep-Pak C_(18) cartridge. The adsorbed PMB-CTAB can be rapidly eluted by 0.56 mol/L H_2SO_4 in ethanol, and determined with a spectrophotometer at 700 nm. Experimental parameters, including reaction temperature, sample loading flow rate, stopped time and eluting flow rate, were optimized throughout the experiments based on univariate experimental design. The results show that reaction temperature and stopped time were the major factors affecting the formation of PMB-CTAB. Silicate concentration up to 5000 times higher than that of orthophosphate would not interfere with the determination of orthophosphate. Using artificial seawater with salinity of 35 as a matrix under the optimized conditions, the standard curve shows a linear range between 3.2 and 48.5 nmol/L, and the recovery and the detection limit of the proposed method are 96.4% and 1.57 nmol/L, respectively. The relative standard deviation (RSD) (n=8), which was determined daily for 8 days, was 4.52% for the artificial seawater at a concentration of 32.4 nmol/L orthophosphate. Two typical seawater samples were analyzed using both the proposed method and the MAGnesium hydroxide-Induced Coprecipitation (MAGIC) method. The results of the two methods show no significant difference using the t test. Compared to the MAGIC method, the proposed method has the advantage of being more sensitive, faster, sample saving and easy for on-line analysis.