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Method for jointly measuring phosphorus in soil by high-pressure digestion and inductively coupled plasma spectrometer

A technology of plasma spectroscopy and inductive coupling is applied in the field of combined determination of phosphorus in soil by ion spectrometer, which can solve the problems of cumbersome steps, tediousness, and easy occurrence of phosphorus loss.

Inactive Publication Date: 2020-10-30
黄麟杰
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The pretreatment of alkali fusion-spectrophotometry is cumbersome. The melting process requires the use of platinum crucibles, which is not suitable for routine analysis and is prone to loss of phosphorus. Spectrophotometry is used for detection, and its sensitivity is relatively low; four-acid digestion-inductively coupled plasma The pretreatment process of volume spectrometer determination requires personnel to be on duty. There are many types of acids used, the steps are cumbersome, and acid needs to be added repeatedly, and the digestion temperature and residual volume of digestion solution are extremely difficult to control.

Method used

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  • Method for jointly measuring phosphorus in soil by high-pressure digestion and inductively coupled plasma spectrometer
  • Method for jointly measuring phosphorus in soil by high-pressure digestion and inductively coupled plasma spectrometer
  • Method for jointly measuring phosphorus in soil by high-pressure digestion and inductively coupled plasma spectrometer

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Weigh 0.1g (accurate to 0.1mg) of the standard soil (GSS-16) and the soil to be tested (GSS-19) in a polytetrafluoroethylene digestion tank, add 8mL of aqua regia to the above two digestion tanks, Tighten the lid of the digestion tank and place it in a pressure cooker for digestion. The digestion temperature is 120°C, the digestion time is 80 minutes, and the pressure is 97kPa. After the pressure gauge reading drops to zero, take it out and let it cool naturally. After it is completely cooled, the standard soil is obtained. Digestion solution and soil digestion solution to be tested;

[0041] Filter and transfer the standard soil digestion solution to a 50mL volumetric flask, rinse the inner wall and cover of the digestion tank repeatedly with 1wt.% nitric acid solution, transfer the rinsed solution into the volumetric flask, rinse 3 times, and finally rinse with 1wt.% nitric acid solution .% nitric acid solution to the scale line, shake well and place it for testing to...

Embodiment 2

[0048] Weigh 0.1g (accurate to 0.1mg) of the standard soil (GSS-16) and the soil to be tested (GSS-19) in a polytetrafluoroethylene digestion tank, add 10mL of aqua regia to the above two digestion tanks, Tighten the lid of the digestion tank, put it in a pressure cooker for digestion, the digestion temperature is 125°C, the digestion time is 90min, and the pressure is 131kPa; after the pressure gauge reading drops to zero, take it out and let it cool naturally, and after it is completely cooled, the standard soil is obtained Digestion solution and soil digestion solution to be tested;

[0049] Filter and transfer the standard soil digestion solution to a 50mL volumetric flask, rinse the inner wall and cover of the digestion tank repeatedly with 1wt.% nitric acid solution, transfer the rinsed solution into the volumetric flask, rinse 3 times, and finally rinse with 1wt.% nitric acid solution .% nitric acid solution to the scale line, shake well and place it for testing to obta...

Embodiment 3

[0056] Weigh 0.1g (accurate to 0.1mg) of the standard soil (GSS-16) and the soil to be tested (GSS-19) in a polytetrafluoroethylene digestion tank, add 15mL of aqua regia to the above two digestion tanks, Tighten the lid of the digestion tank, put it in a pressure cooker for digestion, the digestion temperature is 120°C, the digestion time is 100min, and the pressure is 97kPa; after the pressure gauge reading drops to zero, take it out and let it cool naturally, and after it is completely cooled, the standard soil is obtained Digestion solution and soil digestion solution to be tested;

[0057] Filter and transfer the standard soil digestion solution to a 50mL volumetric flask, rinse the inner wall and cover of the digestion tank repeatedly with 1wt.% nitric acid solution, transfer the rinsed solution into the volumetric flask, rinse 3 times, and finally rinse with 1wt.% nitric acid solution .% nitric acid solution to the scale line, shake well and place it for testing to obta...

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Abstract

The invention provides a method for jointly measuring phosphorus in soil through high-voltage digestion and an inductively coupled plasma spectrometer, and relates to the technical field of environmental monitoring. According to the method, the high-pressure digestion and the inductively coupled plasma spectrometer are combined to determine the content of phosphorus in the soil. According to the invention, the digestion process is carried out in a pressure cooker, the high-pressure digestion has the advantages of high digestion speed, controllable reaction temperature and reaction time, no need of personnel on duty, low operation difficulty and difficulty in phosphorus loss under closed conditions, and the accuracy of a measurement result is improved while the operation is simple and convenient; the digestion process is carried out in a closed container, so that toxic and harmful substances cannot be released due to the reaction between the soil and aqua regia, and the harm to analystsand the environment can be effectively avoided. The calibration curve used in the method is a working curve, and compared with a standard curve, the interference of a matrix on an analysis result canbe effectively avoided, so that a measured value is closer to a true value.

Description

technical field [0001] The invention relates to the technical field of environmental monitoring, in particular to a method for jointly determining phosphorus in soil by high-pressure digestion and inductively coupled plasma spectrometer. Background technique [0002] Determination of phosphorus content in soil can effectively reflect soil fertility, provide quantitative data for the adsorption, fixation and transformation of phosphorus in soil, and has great research value in agriculture and environmental protection. How to quickly, easily and accurately determine the content of phosphorus in soil is still a research hotspot today. At present, alkali fusion-spectrophotometry and four-acid digestion-inductively coupled plasma spectrometry are the most widely used methods for determining the content of phosphorus in soil. The pretreatment of alkali fusion-spectrophotometry is cumbersome. The melting process requires the use of platinum crucibles, which is not suitable for rou...

Claims

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Application Information

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IPC IPC(8): G01N21/73G01N1/44
CPCG01N1/44G01N21/73
Inventor 黄麟杰曾锐陈洁侯茜杨曦霞魏林廖海瑛
Owner 黄麟杰
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