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Chemical luminescence detection method for ultra-trace reactive phosphate in sea water

A chemiluminescence detection and chemiluminescence technology, applied in chemiluminescence/bioluminescence, analysis by chemical reaction of materials, testing of food, etc., can solve the problems of large sample size, time-consuming and laborious, etc. Seawater base disturbance, easy to automate effects

Inactive Publication Date: 2009-07-08
XIAMEN UNIV
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Problems solved by technology

However, this method consumes a large sample volume, and is time-consuming and labor-intensive. When quantitatively determining samples with a phosphorus content below 30nmol / L, generally more than 500mL of water samples are required, and it takes 7h
Luminol chemiluminescence has been applied to the analysis of trace active phosphate in freshwater samples, but due to the interference of the substrate, the application of this method in seawater has not been successful; therefore, the key to the application of this technique in seawater is to eliminate the substrate interference

Method used

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  • Chemical luminescence detection method for ultra-trace reactive phosphate in sea water
  • Chemical luminescence detection method for ultra-trace reactive phosphate in sea water

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Embodiment 1

[0012] Standard curve drawing: take 200mL series standard solutions containing phosphorus respectively 0, 5, 16, 24, 48, 97, 194nmol / L, and mix them with 5.0mL ammonium molybdate mixed solution (the preparation method is the same as the marine monitoring specification) and 5.0mL The CTAB solution with a concentration of 0.5g / L was mixed and reacted in a water bath at 35°C for 0.5min. The reacted solution was passed through a Sep-Pak C18 column at a speed of 23.0mL / min by a peristaltic pump for extraction and enrichment. The enrichment volume 115mL; wash the C18 column with 6mL of water and 2mL of absolute ethanol in order to eliminate the interference of the seawater base, and then elute the extract with a concentration of 0.3mol / L sulfuric acid ethanol solution at a speed of 4.8mL / min; the eluent is in circulation The pool is mixed with 2mol / L luminol solution, and a chemiluminescent reaction occurs. The luminescence signal is detected and recorded by a chemiluminescence inst...

Embodiment 2

[0017] Taking the surface seawater of the South China Sea as the base, the spiked concentrations were 0, 24, 48, 97, and 194nmol / L, and the measured base spiked curve was TI=5.67×10 5 Cp(μmol / L)+4.02×10 5 , the correlation coefficient R=0.9989, the ratio of its slope to the slope of the phosphorus standard curve prepared by the phosphate-free artificial seawater as the substrate, i.e. the standard addition recovery rate of the substrate, is:

[0018]

[0019] The high recovery rate shows that the method is used to determine ultra-trace active phosphorus in actual seawater without substrate interference.

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Abstract

The invention provides a chemiluminescent detection method for an ultra trace amount of active phosphate in seawater. Under acid conditions, phosphate and a molybdate solution generate MoP; an MoP-CTAB ion-pair compound generated by a reaction between the MoP and CTAB can be enriched by a C18 column, and is eluted by an ethanol sulfate solution with certain concentration; an eluent and a luminol solution perform a chemical reaction under alkaline conditions; and a chemiluminescent instrument is utilized for detection. The ultra trace amount of the active phosphate in the seawater is determined through a MoP-CTAB ion pair-solid phase extraction-luminol chemoluminescence method. The method has the advantages that the method consumes few reagent and water sample, has short determination time, is sensitive, has low detectability, improves the sensitivity by 150 times compared with a phosphomolybdate-blue spectrophotometry, has simple and convenient steps, ensures that the whole process is easy to realize the automation, is easy to develop a ship loading type field analytical instrument, and has no interference of a seawater substrate relative to other chemoluminescence methods.

Description

technical field [0001] The invention relates to a chemiluminescent detection method for ultra-trace active phosphate in seawater. Background technique [0002] Phosphorus is an essential nutrient element for the growth of marine organisms. Due to the massive consumption of phytoplankton in the ocean surface, the concentration of phosphorus is very low, and even becomes a limiting element for the primary productivity of the ocean. With the in-depth research on the biogeochemical cycle of phosphorus, the analysis and determination method of phosphate, which is the main component of phosphorus in seawater, has become the key to the scientific research of marine environment. Phosphorus molybdenum blue (PMB) spectrophotometry is the most commonly used classic determination method of phosphate in current marine monitoring regulations, which stipulates that the part of phosphorus that can be measured by phosphorus molybdenum blue spectrophotometry is active phosphorus, including mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/76G01N33/08
Inventor 梁英袁东星李权龙马剑林庆梅
Owner XIAMEN UNIV
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