Method for determining content of selenium in soil by adopting microwave digestion-atomic fluorescence technology

A technique of atomic fluorescence and microwave digestion, applied in fluorescence/phosphorescence, preparation of test samples, material excitation analysis, etc., can solve problems such as soil matrix interference, and achieve the effect of solving soil matrix interference

Active Publication Date: 2015-03-18
SHANGHAI BAOSTEEL IND TECHNOLOGICAL SERVICE
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Problems solved by technology

[0006] The technical problem to be solved by this invention is to provide a method for measuring selenium content in soil by microwave digestion-atomic fluorescence method. ...

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  • Method for determining content of selenium in soil by adopting microwave digestion-atomic fluorescence technology
  • Method for determining content of selenium in soil by adopting microwave digestion-atomic fluorescence technology
  • Method for determining content of selenium in soil by adopting microwave digestion-atomic fluorescence technology

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Embodiment Construction

[0027] The method that the present invention adopts microwave digestion-atomic fluorescence method to measure selenium content in soil comprises the steps:

[0028] Step 1. Sample pretreatment. Accurately weigh 0.2000 (±0.010) g of the soil sample into a microwave digestion tank, add 9ml of nitric acid and 1ml of hydrofluoric acid in sequence, shake well, and put the sample into the microwave digestion apparatus after standing for half an hour. Inside, open the microwave digestion program for digestion;

[0029] Step 2. Put the digested sample into the acid catching rotor, open the acid catching program, and carry out acid catching;

[0030] Step 3. Transfer the sample after acid removal to a 50ml volumetric flask, add 0.5ml concentrated HNO 3 , set the volume to 50ml and let it stand for more than five hours;

[0031] Step 4, the drafting of standard curve, accurately prepare the selenium standard use liquid of 20 μ g / L, the selenium standard use liquid contains the HCl tha...

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Abstract

The invention discloses a method for determining the content of selenium in soil by adopting a microwave digestion-atomic fluorescence technology. The method comprises the following steps: weighing a soil sample, putting the soil sample in a microwave digestion pot, sequentially adding a proper amount of nitric acid and hydrofluoric acid, shaking up, allowing the obtained solution to stand for 0.5h, and carrying out microwave digestion; carrying out acid removal treatment after the digestion; transferring the sample to a volumetric flask, adding a proper amount of concentrated HNO3, adding a solvent to a constant volume, and allowing the obtained solution to stand for above 5h; taking the obtained sample to a sample tube, sequentially adding 1ml of 100g/L K3Fe(CN)6 and 4ml of concentrated HCl, heating in a 90DEG C water bath for 0.5h, cooling, and testing by adopting an atomic fluorescence spectrophotometer; and making a serial standard curve, and corresponding the tested data to the serial standard curve in order to obtain the content of selenium in soil. The method adopting effective pretreatment of soil, reasonable reagent proportioning and apparatus parameter setting overcomes the defects of traditional selenium content determination methods, solves the soil matrix interference problem in determination, and can be used to accurately determine the content of selenium in soil.

Description

technical field [0001] The invention relates to a method for measuring selenium content in soil by microwave digestion-atomic fluorescence method. Background technique [0002] Selenium is one of the important trace elements in the soil. Plant growth and human development require adequate intake of selenium, but excessive selenium can cause organism poisoning, and the required amount is relatively close to the toxic amount. Therefore, accurately grasping the content of selenium in soil has guiding significance for the rational planning and use of land and the protection of human health. [0003] At present, the determination method of selenium content in soil is mainly electric heating plate digestion-ICP method, but the electric heating plate digestion reagent consumes a large amount, takes a long time, and the detection limit of selenium in ICP is high. The graphite furnace method is also used for detection, but the precision and stability are poor, and it cannot be opera...

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Application Information

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IPC IPC(8): G01N21/64G01N1/44
Inventor 高巨鹏杨四川刘亭伶龚俊杰
Owner SHANGHAI BAOSTEEL IND TECHNOLOGICAL SERVICE
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