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Calcareous sediment organophosphorus extraction and constitutes analysis method

A composition analysis and sediment technology, applied in thermal excitation analysis, material excitation analysis, analysis by nuclear magnetic resonance, etc., can solve the problem of low extraction rate of organic phosphorus, and achieve the effect of improving the analysis effect and increasing the extraction amount.

Inactive Publication Date: 2009-01-07
NANJING INST OF GEOGRAPHY & LIMNOLOGY
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Problems solved by technology

[0005] The object of the present invention is to provide a method for extracting organic phosphorus from calcareous deposits and analyzing its composition. This method aims at the problem of low extraction rate of organic phosphorus from calcareous deposits. The organic phosphorus in the sediment is extracted by using NaOH+EDTA in combination with the traditional method. 31 P NMR ( 31 P-NMR) technology to further analyze the composition of organic phosphorus in the extract

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  • Calcareous sediment organophosphorus extraction and constitutes analysis method
  • Calcareous sediment organophosphorus extraction and constitutes analysis method
  • Calcareous sediment organophosphorus extraction and constitutes analysis method

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Embodiment Construction

[0021] Required reagents

[0022] 1.50 mM ethylenediaminetetraacetic acid (EDTA): Weigh 18.6 g of EDTA (Na salt) and dissolve it in 1.0 liter of deionized water.

[0023] 2. 0.25M NaOH+50mM EDTA mixed solution: Weigh 10g NaOH and 18.6g EDTA (Na salt) and dissolve in 1.0 liter of deionized water.

[0024] 3. Heavy water (H 2 o 2 )

[0025] required equipment

[0026] 1. Reciprocating oscillator

[0027] 2. Centrifuge

[0028] 3. Rotary evaporator

[0029] 4. Water bath vacuum pump

[0030] 5. Inductively coupled plasma emission spectrometer (ICP-AES)

[0031] 6. Bruker AV400 nuclear magnetic resonance instrument

[0032] Steps

[0033] 1. Sediment sample preparation: collect fresh sediment, freeze in -80°C ultra-low temperature refrigerator for 4 hours, and then put it on a freeze dryer for vacuum drying. The dried sediment samples were ground, sieved (100 mesh), and sealed at room temperature.

[0034] 2. Washing: Weigh 2.0g (dry weight) of sediment into a 100ml ce...

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Abstract

The invention relates to an extracting and composition analyzing method of organic phosphorus of calcareous sediment. The method is characterized in that acidic EDTA solution is used for flushing and centrifuging the sediment; a traditional extraction method that the mixed solution of NaOH and EDTA (NaOH plus EDTA) is used for oscillating, extracting and centrifuging the sediment; a part of the extracted solution of NaOH plus EDTA is tested by a spectrometer to determine the total phosphorus; the rest extracted solution is concentrated; ultimately, the <31>P nuclear magnetic resonance technique (<31>P-NMR) is used for analyzing the composition of organic phosphorus in the extracted solution.

Description

technical field [0001] The invention relates to the evaluation and analysis of phosphorus in calcareous sediments of lakes, in particular to a method for extracting and analyzing the composition of organic phosphorus in calcareous sediments, and is also suitable for ocean and river sediments with high calcium content. Background technique [0002] Phosphorus is the limiting factor for lake eutrophication. Most of the phosphorus in lakes is accumulated in sediments. Sediment phosphorus can be released into water bodies in large quantities under appropriate conditions, causing water quality deterioration and eutrophication. The release potential of phosphorus in sediments is mainly related to the occurrence forms of phosphorus in sediments. At present, the analysis and evaluation methods for the form and activity of inorganic phosphorus in sediments are relatively mature, but the research methods for organic phosphorus are still very lacking. Only the total amount of organi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N24/08G01N1/34
Inventor 丁士明白秀玲刘韬范成新
Owner NANJING INST OF GEOGRAPHY & LIMNOLOGY
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