CN111855645A - Method for jointly measuring phosphorus in soil by high-pressure digestion-inductively coupled plasma spectrometer - Google Patents
Method for jointly measuring phosphorus in soil by high-pressure digestion-inductively coupled plasma spectrometer Download PDFInfo
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Abstract
The invention provides a method for jointly measuring phosphorus in soil by using a high-pressure digestion-inductively coupled plasma spectrometer, and relates to the technical field of environmental monitoring. The method adopts the high-pressure digestion and the inductively coupled plasma spectrometer to jointly measure the content of the phosphorus in the soil, 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 difficult phosphorus loss under a closed condition, and the accuracy of a measurement result is improved while the operation is simple and convenient; and because the digestion process is carried out in the closed container, toxic and harmful substances can not be released due to the reaction of the soil and the aqua regia, and the harm to the analysts and the environment can be effectively avoided. The calibration curve used by the invention is a working curve, and compared with a standard curve, the calibration curve can effectively avoid the interference of a matrix on an analysis result, so that a measured value is closer to a true value.
Description
Technical Field
The invention relates to the technical field of environmental monitoring, in particular to a method for jointly measuring phosphorus in soil by using a high-pressure digestion-inductively coupled plasma spectrometer.
Background
The content of phosphorus in the soil is measured, the soil fertility can be effectively reflected, quantitative data is provided for adsorption, fixation and conversion of phosphorus in the soil, and the method has great research value in the aspects of agriculture and environmental protection. How to rapidly, simply and accurately measure the content of phosphorus in soil is still a research hotspot at present. The most used method for determining the content of phosphorus in soil at present is an alkali fusion-spectrophotometry method and a tetraacid digestion-inductively coupled plasma spectrometer method. The pretreatment operation of the alkali fusion-spectrophotometry is complicated, a platinum crucible is required in the fusion process, the method is not suitable for conventional analysis, and phosphorus loss is easy to occur, and the sensitivity is relatively low by adopting the spectrophotometry for detection; the pretreatment process of the tetra-acid digestion-inductively coupled plasma spectrometer measurement method needs personnel on duty, the types of used acids are more, the steps are complicated, the acids need to be added repeatedly, and the digestion temperature and the digestion liquid residual quantity are not easy to control.
Therefore, it is a difficult problem to be solved in the art to find a method for measuring phosphorus content with simple operation and high accuracy.
Disclosure of Invention
The invention aims to provide a method for jointly measuring phosphorus in soil by using a high-pressure digestion-inductively coupled plasma spectrometer.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for jointly measuring phosphorus in soil by using a high-pressure digestion-inductively coupled plasma spectrometer, which comprises the following steps of:
placing standard soil into a first digestion tank, placing soil to be detected into a second digestion tank, and respectively adding aqua regia into the first digestion tank and the second digestion tank;
placing the first digestion tank and the second digestion tank in the same pressure cooker for digestion to obtain a standard soil digestion solution and a soil digestion solution to be detected;
preparing a phosphorus standard strain solution by taking the standard soil digestion solution as a mother solution, and carrying out inductively coupled plasma spectrum detection on the phosphorus standard strain solution to obtain a phosphorus concentration-spectral line intensity working curve;
and carrying out inductively coupled plasma spectrum detection on the soil digestion solution to be detected to obtain spectral line intensity, and obtaining the content of phosphorus in the soil to be detected according to the phosphorus concentration-spectral line intensity working curve.
Preferably, the first digestion tank and the second digestion tank are made of polytetrafluoroethylene.
Preferably, the ratio of the dosage of the standard soil to the dosage of the aqua regia to be detected to the dosage of the soil to be detected to the dosage of the aqua regia is 0.1 g: 8-15 mL.
Preferably, the digestion temperature is 120-130 ℃, and the digestion time is 80-100 min; the digestion pressure is 97-169 kPa.
Preferably, the inductively coupled plasma spectrum detection condition includes:
and (3) analyzing spectral lines: 214.9nm or 213.6 nm;
the number of repetitions: 2-3 times;
the viewing direction is horizontal.
Preferably, the volume of the solution used in preparing the phosphorus standard series solution is 1 wt.% nitric acid solution.
Preferably, the particle size of the soil to be detected is 100 meshes.
The invention provides a method for jointly measuring phosphorus in soil by using a high-pressure digestion-inductively coupled plasma spectrometer, which comprises the following steps of: placing standard soil into a first digestion tank, placing soil to be detected into a second digestion tank, and respectively adding aqua regia into the first digestion tank and the second digestion tank; placing the first digestion tank and the second digestion tank in the same pressure cooker for digestion to obtain a standard soil digestion solution and a soil digestion solution to be detected; preparing a phosphorus standard strain solution by taking the standard soil digestion solution as a mother solution, and carrying out inductively coupled plasma spectrum detection on the phosphorus standard strain solution to obtain a phosphorus concentration-spectral line intensity working curve; and carrying out inductively coupled plasma spectrum detection on the soil digestion solution to be detected to obtain spectral line intensity, and obtaining the content of phosphorus in the soil to be detected according to the phosphorus concentration-spectral line intensity working curve. In the invention, the digestion process is carried out in a closed digestion tank and 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, difficult phosphorus loss under a closed condition and the like, and the accuracy of a measurement result is greatly improved while the operation is simple and convenient; and because the digestion process is carried out in the closed container, toxic and harmful substances can not be released due to the reaction of the soil and the aqua regia, and the harm to the analysts and the environment can be effectively avoided. The calibration curve used by the invention is a working curve, and compared with a standard curve, the calibration curve can effectively avoid the interference of a matrix on an analysis result, so that the measured value is closer to a real value, and the content of phosphorus in soil can be more accurately measured. The invention adopts the inductively coupled plasma spectrometer for detection, has the advantages of high sensitivity, wide linear range, simple and convenient operation and high analysis speed, and can further ensure the accuracy of the measurement result. The detection method provided by the invention can be widely applied to the determination of the phosphorus content in soil and sediments.
Detailed Description
The invention provides a method for jointly measuring phosphorus in soil by using a high-pressure digestion-inductively coupled plasma spectrometer, which comprises the following steps of:
placing standard soil into a first digestion tank, placing soil to be detected into a second digestion tank, and respectively adding aqua regia into the first digestion tank and the second digestion tank;
placing the first digestion tank and the second digestion tank in the same pressure cooker for digestion to obtain a standard soil digestion solution and a soil digestion solution to be detected;
preparing a phosphorus standard strain solution by taking the standard soil digestion solution as a mother solution, and carrying out inductively coupled plasma spectrum detection on the phosphorus standard strain solution to obtain a phosphorus concentration-spectral line intensity working curve;
and carrying out inductively coupled plasma spectrum detection on the soil digestion solution to be detected to obtain spectral line intensity, and obtaining the content of phosphorus in the soil to be detected according to the phosphorus concentration-spectral line intensity working curve.
According to the method, standard soil is placed in a first digestion tank, soil to be detected is placed in a second digestion tank, and aqua regia is added into the first digestion tank and the second digestion tank respectively. In a specific embodiment of the invention, the standard soil is from the institute of geophysical and geochemical exploration, national academy of geology; the standard soil is preferably GBW07430(GSS-16), GBW07446(GSS-17) or GBW07448 (GSS-19). In the present invention, the particle size of the soil to be measured is preferably 100 mesh.
In the invention, the dosage ratio of the standard soil and the aqua regia to be tested is independent and preferably 0.1 g: 8-15 mL, more preferably 0.1 g: 10 mL. In the specific embodiment of the invention, the standard soil and the soil to be detected have the same dosage, and the volume of the added aqua regia is also the same, so that the accuracy of the detection result can be improved.
In the invention, the material of the first digestion tank and the second digestion tank is preferably polytetrafluoroethylene. In the invention, the polytetrafluoroethylene has good chemical inertness, can not react with the sample and the reagent, and avoids interfering the experimental result. In the invention, the first digestion tank and the second digestion tank are preferably sealed tank bodies with covers, so that the overflow of substances in the digestion process is avoided.
The first digestion tank and the second digestion tank are placed in the same pressure cooker for digestion to obtain standard soil digestion liquid and soil digestion liquid to be detected. The first digestion tank and the second digestion tank are arranged in the same pressure cooker, so that the consistency of digestion conditions is ensured, and the accuracy of a detection result is improved.
In the invention, the digestion temperature is preferably 120-130 ℃, and more preferably 120-125 ℃; the digestion time is preferably 80-100 min, and more preferably 80-90 min; the digestion pressure is preferably 97-169 kPa, and more preferably 110-130 kPa. In the digestion process, the strong oxidizing property of aqua regia, the complexing property of chloride ions and the catalytic action of chlorine, nitrosyl chloride and chloride ions are utilized to oxidize organic matters and convert insoluble matters (apatite, phospho-boehmite, octacalcium phosphate, phospho-zincite, phospho-potash-aluminate and the like) into soluble matters (orthophosphate).
According to the invention, the digestion system is preferably naturally cooled to room temperature to obtain the standard soil digestion solution and the soil digestion solution to be detected.
After the standard soil digestion solution and the soil digestion solution to be detected are obtained, the method takes the standard soil digestion solution as a mother solution to prepare a phosphorus standard series solution, and performs inductively coupled plasma spectrum detection on the phosphorus standard series solution to obtain a phosphorus concentration-spectral line intensity working curve.
In a specific embodiment of the present invention, the preparation method of the mother liquor comprises: and filtering the standard soil digestion solution and transferring the standard soil digestion solution to a 50mL volumetric flask, repeatedly washing the inner wall and the cover of the first digestion tank by using 1 wt.% of nitric acid solution, transferring the washed solution into the volumetric flask together, washing for at least 3 times, fixing the volume to a scale mark by using 1 wt.% of nitric acid solution, shaking uniformly and placing to be measured. The method can calculate the concentration of the mother liquor according to the known content, the sampling amount and the constant volume of phosphorus in the standard soil.
In an embodiment of the present invention, the preparation method of the phosphorus standard line solution comprises: accurately transferring 1.00mL, 2.00mL, 5.00mL, 10.00mL and 20.00mL of mother liquor into a series of 50mL volumetric flasks by using a pipette, fixing the volume to a scale mark by using 1 wt.% of nitric acid solution, and shaking up to obtain the phosphorus standard strain solution.
In the present invention, the inductively coupled plasma spectrum detection conditions preferably include: and (3) analyzing spectral lines: 214.9nm or 213.6 nm; the number of repetitions: 2-3 times; the viewing direction is horizontal.
After a phosphorus concentration-spectral line intensity working curve is obtained, the method carries out inductively coupled plasma spectrum detection on the soil digestion solution to be detected to obtain spectral line intensity, and obtains the content of phosphorus in the soil to be detected according to the phosphorus concentration-spectral line intensity working curve. Before the soil digestion solution to be detected is subjected to inductively coupled plasma spectrum detection, the volume of the soil digestion solution to be detected is preferably determined to obtain a constant volume solution, and the constant volume method is preferably the same as the preparation method of the mother solution, and is not repeated here. In the present invention, the detection condition of the inductively coupled plasma spectrum is the same as the detection condition when the phosphorus concentration-spectral line intensity working curve is prepared, and details are not repeated here.
According to the phosphorus concentration-spectral line intensity working curve, the concentration of phosphorus in the constant volume solution is obtained after the spectral line intensity of the soil digestion solution to be measured is substituted. According to the method, the content of phosphorus in the soil to be measured is calculated according to the sampling volume and the constant volume of the soil to be measured and the measured concentration of phosphorus in the constant volume solution.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Respectively weighing 0.1g (accurate to 0.1mg) of standard soil (GSS-16) and soil (GSS-19) to be detected in polytetrafluoroethylene digestion tanks, respectively adding 8mL of aqua regia into the two digestion tanks, screwing the covers of the digestion tanks, placing the digestion tanks in a pressure cooker for digestion, wherein the digestion temperature is 120 ℃, the digestion time is 80min, and the pressure is 97 kPa; after the reading of the pressure gauge is reduced to zero, taking out the pressure gauge for natural cooling, and after complete cooling, obtaining standard soil digestion liquid and soil digestion liquid to be measured;
filtering the standard soil digestion solution, transferring the standard soil digestion solution into a 50mL volumetric flask, repeatedly washing the inner wall and the cover of the digestion tank by using 1 wt.% nitric acid solution, transferring the washed solution into the volumetric flask together, washing for 3 times, finally fixing the volume to a scale mark by using 1 wt.% nitric acid solution, shaking uniformly, and placing to-be-measured solution to obtain mother liquor for drawing a working curve;
accurately transferring 1.00mL, 2.00mL, 5.00mL, 10.00mL and 20.00mL of mother liquor into a series of 50mL volumetric flasks by using a transfer pipette, fixing the volume to a scale mark by using 1 wt.% of nitric acid solution, and shaking up to obtain a phosphorus standard strain solution; carrying out inductively coupled plasma spectrum detection on the phosphorus standard strain solution to obtain a phosphorus concentration-spectral line intensity working curve; the inductively coupled plasma spectrum detection conditions are as follows: the analytical line is 214.9 nm; the number of repetitions was 2; the observation direction is horizontal;
filtering the soil digestion solution to be detected, transferring the soil digestion solution to a 50mL volumetric flask, repeatedly washing the inner wall and the cover of the digestion tank by using 1 wt.% nitric acid solution, transferring the washed solution to the volumetric flask together, washing for 3 times, finally fixing the volume to a scale mark by using 1 wt.% nitric acid solution, shaking up, and placing the solution to be detected to obtain a constant volume solution; performing inductively coupled plasma spectrum detection on the constant volume solution to obtain spectral line intensity, and obtaining the concentration of phosphorus in the constant volume solution according to the phosphorus concentration-spectral line intensity working curve; the detection condition of the inductively coupled plasma spectrum is the same as the detection condition when the phosphorus concentration-spectral line intensity working curve is prepared;
and calculating to obtain the content of phosphorus in the soil to be detected according to the sampling amount of the soil to be detected, the constant volume and the concentration of phosphorus in the constant volume solution. The phosphorus content in 3 groups of soils to be tested (GSS-19) were tested according to the above-mentioned measurement procedures, and the results are shown in Table 1.
TABLE 1 EXAMPLE 1 phosphorus content in soil to be tested (GSS-19)
Example 2
Respectively weighing 0.1g (accurate to 0.1mg) of standard soil (GSS-16) and soil (GSS-19) to be detected in polytetrafluoroethylene digestion tanks, respectively adding 10mL of aqua regia into the two digestion tanks, screwing the covers of the digestion tanks, placing the digestion tanks in a pressure cooker for digestion, wherein the digestion temperature is 125 ℃, the digestion time is 90min, and the pressure is 131 kPa; after the reading of the pressure gauge is reduced to zero, taking out the pressure gauge for natural cooling, and after complete cooling, obtaining standard soil digestion liquid and soil digestion liquid to be measured;
filtering the standard soil digestion solution, transferring the standard soil digestion solution into a 50mL volumetric flask, repeatedly washing the inner wall and the cover of the digestion tank by using 1 wt.% nitric acid solution, transferring the washed solution into the volumetric flask together, washing for 3 times, finally fixing the volume to a scale mark by using 1 wt.% nitric acid solution, shaking uniformly, and placing to-be-measured solution to obtain mother liquor for drawing a working curve;
accurately transferring 1.00mL, 2.00mL, 5.00mL, 10.00mL and 20.00mL of mother liquor into a series of 50mL volumetric flasks by using a transfer pipette, fixing the volume to a scale mark by using 1 wt.% of nitric acid solution, and shaking up to obtain a phosphorus standard strain solution; carrying out inductively coupled plasma spectrum detection on the phosphorus standard strain solution to obtain a phosphorus concentration-spectral line intensity working curve; the inductively coupled plasma spectrum detection conditions are as follows: the analytical line is 214.9 nm; the number of repetitions was 2; the observation direction is horizontal;
filtering the soil digestion solution to be detected, transferring the soil digestion solution to a 50mL volumetric flask, repeatedly washing the inner wall and the cover of the digestion tank by using 1 wt.% nitric acid solution, transferring the washed solution to the volumetric flask together, washing for 3 times, finally fixing the volume to a scale mark by using 1 wt.% nitric acid solution, shaking up, and placing the solution to be detected to obtain a constant volume solution; performing inductively coupled plasma spectrum detection on the constant volume solution to obtain spectral line intensity, and obtaining the concentration of phosphorus in the constant volume solution according to the phosphorus concentration-spectral line intensity working curve; the detection condition of the inductively coupled plasma spectrum is the same as the detection condition when the phosphorus concentration-spectral line intensity working curve is prepared;
and calculating to obtain the content of phosphorus in the soil to be detected according to the sampling amount of the soil to be detected, the constant volume and the concentration of phosphorus in the constant volume solution. The phosphorus content in 3 groups of soils to be tested (GSS-19) were tested according to the above-mentioned measurement procedures, and the results are shown in Table 2.
TABLE 2 example 2 phosphorus content in soil to be tested (GSS-19)
Example 3
Respectively weighing 0.1g (accurate to 0.1mg) of standard soil (GSS-16) and soil (GSS-19) to be detected in polytetrafluoroethylene digestion tanks, respectively adding 15mL of aqua regia into the two digestion tanks, screwing the covers of the digestion tanks, placing the digestion tanks in a pressure cooker for digestion, wherein the digestion temperature is 120 ℃, the digestion time is 100min, and the pressure is 97 kPa; after the reading of the pressure gauge is reduced to zero, taking out the pressure gauge for natural cooling, and after complete cooling, obtaining standard soil digestion liquid and soil digestion liquid to be measured;
filtering the standard soil digestion solution, transferring the standard soil digestion solution into a 50mL volumetric flask, repeatedly washing the inner wall and the cover of the digestion tank by using 1 wt.% nitric acid solution, transferring the washed solution into the volumetric flask together, washing for 3 times, finally fixing the volume to a scale mark by using 1 wt.% nitric acid solution, shaking uniformly, and placing to-be-measured solution to obtain mother liquor for drawing a working curve;
accurately transferring 1.00mL, 2.00mL, 5.00mL, 10.00mL and 20.00mL of mother liquor into a series of 50mL volumetric flasks by using a transfer pipette, fixing the volume to a scale mark by using 1 wt.% of nitric acid solution, and shaking up to obtain a phosphorus standard strain solution; carrying out inductively coupled plasma spectrum detection on the phosphorus standard strain solution to obtain a phosphorus concentration-spectral line intensity working curve; the inductively coupled plasma spectrum detection conditions are as follows: the analytical line is 214.9 nm; the number of repetitions was 2; the observation direction is horizontal;
filtering the soil digestion solution to be detected, transferring the soil digestion solution to a 50mL volumetric flask, repeatedly washing the inner wall and the cover of the digestion tank by using 1 wt.% nitric acid solution, transferring the washed solution to the volumetric flask together, washing for 3 times, finally fixing the volume to a scale mark by using 1 wt.% nitric acid solution, shaking up, and placing the solution to be detected to obtain a constant volume solution; performing inductively coupled plasma spectrum detection on the constant volume solution to obtain spectral line intensity, and obtaining the concentration of phosphorus in the constant volume solution according to the phosphorus concentration-spectral line intensity working curve; the detection condition of the inductively coupled plasma spectrum is the same as the detection condition when the phosphorus concentration-spectral line intensity working curve is prepared;
and calculating to obtain the content of phosphorus in the soil to be detected according to the sampling amount of the soil to be detected, the constant volume and the concentration of phosphorus in the constant volume solution. The phosphorus content in 3 groups of soils to be tested (GSS-19) were tested according to the above-mentioned measurement procedures, and the results are shown in Table 3.
TABLE 3 example 3 phosphorus content in soil to be tested (GSS-19)
As can be seen from tables 1-3, the detection method provided by the invention has the advantages of high accuracy, no need of complex pretreatment on the sample in the detection process, and rapidness and accuracy.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A method for jointly measuring phosphorus in soil by using a high-pressure digestion-inductively coupled plasma spectrometer comprises the following steps:
placing standard soil into a first digestion tank, placing soil to be detected into a second digestion tank, and respectively adding aqua regia into the first digestion tank and the second digestion tank;
placing the first digestion tank and the second digestion tank in the same pressure cooker for digestion to obtain a standard soil digestion solution and a soil digestion solution to be detected;
preparing a phosphorus standard strain solution by taking the standard soil digestion solution as a mother solution, and carrying out inductively coupled plasma spectrum detection on the phosphorus standard strain solution to obtain a phosphorus concentration-spectral line intensity working curve;
and carrying out inductively coupled plasma spectrum detection on the soil digestion solution to be detected to obtain spectral line intensity, and obtaining the content of phosphorus in the soil to be detected according to the phosphorus concentration-spectral line intensity working curve.
2. The method according to claim 1, characterized in that the material of the first digestion tank and the second digestion tank is polytetrafluoroethylene.
3. The method according to claim 1, wherein the ratio of the amount of the standard soil to the amount of the aqua regia to be tested is 0.1 g: 8-15 mL.
4. The method according to claim 1, wherein the digestion temperature is 120-130 ℃, and the digestion time is 80-100 min; the digestion pressure is 97-169 kPa.
5. The method of claim 1, wherein the inductively coupled plasma spectroscopy detection conditions comprise:
and (3) analyzing spectral lines: 214.9nm or 213.6 nm;
the number of repetitions: 2-3 times;
the viewing direction is horizontal.
6. The method of claim 1, wherein the volume of the solution used to prepare the phosphorus standard series solution is 1 wt.% nitric acid solution.
7. The method according to claim 1, wherein the soil to be tested has a particle size of 100 mesh.
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| CN110793836A (en) * | 2019-11-01 | 2020-02-14 | 山东省物化探勘查院 | Method for simultaneously measuring cadmium, molybdenum, germanium and boron elements in soil |
| CN110793836B (en) * | 2019-11-01 | 2022-01-11 | 山东省物化探勘查院 | Method for simultaneously measuring cadmium, molybdenum, germanium and boron elements in soil |
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