CN107589140B - Method for detecting contents of chlorine, phosphorus and potassium in compound fertilizer product by energy dispersion X-ray fluorescence spectrum - Google Patents
Method for detecting contents of chlorine, phosphorus and potassium in compound fertilizer product by energy dispersion X-ray fluorescence spectrum Download PDFInfo
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Abstract
The invention discloses a method for detecting the contents of chlorine, phosphorus and potassium in a compound fertilizer product by energy dispersion X-ray fluorescence spectrum, which comprises the following steps: 1) selecting compound fertilizer products composed of different types and contents as calibration samples, and accurately measuring the contents of chlorine, phosphorus and potassium; 2) measuring a compound fertilizer calibration sample with known chlorine, phosphorus and potassium contents by using an energy dispersion type X-ray fluorescence spectrometer, and determining the test conditions of chlorine, phosphorus and potassium elements; 3) testing the compound fertilizer sample to be tested by adopting an energy dispersion type X-ray fluorescence spectrometer, and obtaining the contents of chlorine, phosphorus and potassium in the compound fertilizer sample to be tested according to the relation between the X-ray fluorescence spectrum intensity and the contents of chlorine, phosphorus and potassium elements in the calibration working curve constructed in the step 2). The invention can rapidly measure the contents of chlorine, phosphorus and potassium in the products such as compound fertilizers, bulk blended fertilizers and the like, reduces the usage amount of chemical reagents, and has convenient and rapid detection process, accurate detection result and good consistency.
Description
Technical Field
The invention belongs to the technical field of compound fertilizer detection, and particularly relates to a method for rapidly determining the contents of chlorine, phosphorus and potassium in compound fertilizer products of different types, in particular to a method for detecting the contents of chlorine, phosphorus and potassium in the compound fertilizer products by using a handheld energy dispersive X-ray fluorescence spectrometer.
Background
The chemical fertilizer is used as a main production material of modern agriculture and is a national economy basic industry. In the new century, the chemical fertilizer industry in China is stepped into the rapid development period, and important contribution is made to continuous eight-year grain yield increase in China. Chemical fertilizers are generally divided into nitrogenous fertilizers, phosphate fertilizers, potash fertilizers and compound fertilizers, and the most important product category is the compound fertilizers at present. The compound fertilizer is prepared by chemical method and/or mixing method, wherein at least two of the three nutrients of nitrogen, phosphorus and potassium have the indicated amount. The compound fertilizer can meet the comprehensive requirements of crops on various nutrients under different production conditions, has the advantages of improving the fertilizer efficiency, simplifying the fertilization technology and the like, is more and more emphasized by people in production and use, and is developed rapidly in recent years. The nutrients of nitrogen, phosphorus and potassium in the compound fertilizer are main indexes of product quality, and the using range of the product is directly influenced by the content of chlorine, so that the crops are adversely affected once the compound fertilizer is improperly used, and the yield of the crops is reduced, even the crops are not harvested. Therefore, the method is particularly important for measuring the content of the nutrients and the chlorine elements in the compound fertilizer, and the related detection requirements are in a significant rising trend no matter government supervision or product quality control of enterprises. The nitrogen, phosphorus, potassium nutrient and chlorine element content of the current compound fertilizer product mainly adopt a chemical analysis method, the method is complex in operation process and long in period, a large amount of chemical reagents are required to be used, obvious environmental pollution is caused, and time is consumed in detection, so that a novel green detection technology needs to be developed urgently, the detection efficiency is improved, and the development of modern agriculture is served better. In recent years, the energy dispersion X-ray fluorescence technology is rapidly developed, and the energy dispersion X-ray fluorescence technology has the advantages of small size, portability, capability of realizing rapid on-site measurement, low equipment cost and the like, and is widely applied to quality control and quality certification detection of products.
In recent years, the research on the content and composition of chemical elements of products such as minerals and steel products is carried out by using an X-ray fluorescence spectrometry, the chemical composition of the products is mainly measured by using a solid mode, the main problems of the method include serious matrix interference, obvious granularity effect and poor universality of the method, and related research works for solving the problems and developing technical improvement and the like are carried out, for example, the steel products are generally classified according to the chemical composition, calibration working curves are independently constructed for different types of products, the matrix interference with large difference of the content of the chemical elements is reduced, and the accuracy and precision of detection are improved; the problem faced in mineral detection is further complicated by the fact that researchers have constructed calibration work curves by selecting different types of minerals to reduce matrix interference, but the particle effect of the current sample is still quite significant in the outcome, and therefore this method is often used as a semi-quantitative measure of the chemical composition of minerals. The most important is that the needed standard sample system is very complex, the universality of the standard sample is poor, and the popularization and the application of the method are seriously influenced.
No literature reports a method for detecting the contents of chlorine, phosphorus and potassium in the compound fertilizer product by adopting an energy dispersion X-ray fluorescence technology.
Disclosure of Invention
The chemical composition of a compound fertilizer product is tested by adopting a traditional solid mode, so that the problems need to be solved, firstly, the complexity of a sample matrix is far higher than that of the prior art, and the compound fertilizer sample is prepared from minerals with different sources and compositions by a physical or chemical method, so that the selection of a calibration sample is very difficult, the interference difference of the matrix of the sample is large, the content difference of chemical compositions of different elements in the sample is large, and the requirement on the change of instrument test conditions is more strict; meanwhile, after the sample is tabletted and prepared, water is very easy to absorb, so that the effect on the result is large, and the pretreatment of the uniformity of the sample is very difficult. In the process of testing the compound fertilizer product by adopting the traditional solid mode in the initial stage of research and development, the inventor tries to adjust various testing parameters, the linear correlation coefficient of a calibration curve is difficult to reach 0.99, and the method has poor precision, so that the reproducibility of the final detection result is very poor, and therefore the traditional solid testing method cannot meet the requirements of detecting the content of chlorine, phosphorus and potassium in the compound fertilizer product. In order to solve the problems in the prior art, the invention aims to provide a method for detecting the contents of chlorine, phosphorus and potassium in a compound fertilizer by using an energy dispersive X-ray fluorescence spectrum, which has the advantages of rapidness and convenience in detection and accurate detection result.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a method for detecting the contents of chlorine, phosphorus and potassium in a compound fertilizer product by energy dispersion X-ray fluorescence spectroscopy comprises the following steps:
firstly, selecting compound fertilizer products composed of different types and contents as calibration samples, and accurately measuring the contents of chlorine, phosphorus and potassium by adopting the existing national standard method; wherein the national standard method for measuring chlorine is GB 15063-2009, the national standard method for measuring phosphorus is GB/T8573-2010, and the national standard method for measuring potassium is GB/T8574-2010; extracting chlorine, phosphorus and potassium elements in compound fertilizer samples with different types and contents and preparing a calibration solution;
step two, measuring a compound fertilizer sample with known chlorine, phosphorus and potassium contents by using a handheld energy dispersive X-ray fluorescence spectrometer, constructing a calibration working curve of the relation between the X-ray fluorescence spectrum intensity and the contents of chlorine, phosphorus and potassium elements, and determining the test conditions of the chlorine, phosphorus and potassium elements;
thirdly, according to the testing conditions of the chlorine, phosphorus and potassium elements determined in the first step and the second step, a hand-held energy dispersion type X-ray fluorescence spectrometer is adopted to measure the compound fertilizer sample to be tested, according to the relation between the X-ray fluorescence spectrum intensity and the contents of the chlorine, phosphorus and potassium elements in the calibration working curve constructed in the second step, the contents of the chlorine, phosphorus and potassium in the compound fertilizer sample to be tested are calculated by using a formula, and the content calculation formula of the target object is:
in formula (1):
Wipercent: represents the mass percentage of the target object i;
v: the unit of the constant volume of the extraction solution of the sample to be detected is mL;
m: the weighing amount of the compound fertilizer in the prepared extraction solution of the sample to be tested is expressed in g;
Ci: the concentration of the solution read by the instrument test is expressed in g/mL.
The detection limit calculation formula of the method is as follows:
(2) in the formula:
CL: represents the detection limit of the L element;
m: represents the slope of the curve for the L element;
IB: represents the background intensity of the blank calibration sample in cps;
TB: represents the background count time, in units of s;
k: representing the confidence factor, in this method 3.
The detection limits of the components are shown in Table A.
TABLE A detection limits for the components
Preferably, in the step one, the selected fertilizer types comprise compound fertilizers, compound fertilizers and blend fertilizers which are used as calibration samples for preparing a standard solution, 2.0-10.0 g of the samples (accurate to 0.1mg) are weighed for extracting chlorine, phosphorus and potassium elements, and a calibration solution is prepared; the preparation method of the chlorine, phosphorus and potassium calibration solution comprises the steps of adding a sample into a 100mL volumetric flask, adding 60mL of 40g/L EDTA solution into the volumetric flask, keeping the temperature in a constant-temperature water bath at 80 ℃, shaking for 1.5h, taking out the volumetric flask, cooling, fixing the volume to 100mL, and filtering to obtain a clear solution serving as the calibration solution of chlorine, phosphorus and potassium. Preparing a blank calibration blank solution by performing chlorine, phosphorus and potassium according to the same steps;
in the second step, the test conditions of the chlorine element are as follows: test time was 40s, X-ray tube pressure was 7kV, X-ray tube flow was 40 μ Α, filter: al;
the test conditions of the phosphorus element are as follows: test time was 60s, X-ray tube pressure was 9kV, X-ray tube flow was 50 μ a, filter: al;
the test conditions of the potassium element are as follows: test time was 50s, X-ray tube pressure was 9kV, X-ray tube flow was 50 μ a, filter: mo;
three elements tested the selected background-subtracted range: the chlorine element is 4.75-6.75 eV, the phosphorus element is 5.05-7.05 eV, and the potassium element is 4.63-7.63 eV.
Thickness of sample liquid: 1-20 mm, the liquid interface film is: polyethylene material with thickness of 8 μm;
compared with the prior art, the method has at least the following beneficial effects:
1) the method comprises the steps that a handheld energy dispersion type X-ray fluorescence spectrometer is adopted to measure different types of compound fertilizer samples with known concentrations to construct a calibration working curve, and the calibration working curve considers the types of the compound fertilizers (such as compound fertilizers, compound fertilizers and blend fertilizers) which are mainstream in the market, so that the calibration working curve is suitable for detecting various types of compound fertilizer samples;
2) according to the invention, target elements in the sample are effectively extracted and transferred into the aqueous solution, so that the problems which cannot be solved by the traditional tabletting method, such as influence of matrix interference, granularity effect, sample uniformity and the like on the result, are solved, and the accuracy and precision are obviously improved;
3) the invention simultaneously screens the test conditions for measuring the contents of chlorine, phosphorus and potassium elements, respectively selects the best test conditions for measuring the contents of the chlorine, phosphorus and potassium elements in unknown samples, realizes the rapid detection of the contents of the chlorine, phosphorus and potassium elements in compound fertilizer products, and realizes the Cl detection-The measurement range of (2): 0.17 to 43.81%, P2O5The measurement range of (2): 0.31 to 17.23%, K2Measurement range of O: 0.21-16.27%;
4) the invention finds that the minimum sample solution thickness of the sample solution to be measured can be as thin as 1mm, and the result is consistent with that of the larger sample solution usage amount. The technology has the greatest advantages that the detection process is convenient and quick, the usage amount of chemical reagents is greatly reduced, the detection result is accurate, the consistency is good, and the technology is an environment-friendly novel detection technology.
The invention adopts the handheld energy dispersion X-ray fluorescence spectrum technology to rapidly measure the contents of phosphorus, potassium and chlorine in the compound fertilizer product, and the method has simple operation process and is a novel green and environment-friendly detection technology. The method creatively extracts phosphorus, potassium and chlorine in the compound fertilizer and transfers the phosphorus, potassium and chlorine into the water solution, solves the problems of long-term chemical composition in substances tested by the X-ray fluorescence spectroscopy technology, such as serious matrix effect, particle size effect, sample nonuniformity and the like, and remarkably improves the accuracy and precision of the detection method. The development of the method obviously improves the detection efficiency, can realize the rapid detection of the contents of phosphorus, potassium and chlorine in the compound fertilizer product, greatly reduces the use amount of chemical reagents, and is an environment-friendly detection method. The method provides more effective interest for government market supervision, promotes long-term development of market health, and provides important technical support for chemical composition determination of agricultural production data.
Drawings
Fig. 1 is a calibration work graph of the relationship between the X-ray fluorescence spectrum intensity and the chlorine content constructed by the invention (y-1917.775X + 384.734);
fig. 2 is a calibration work graph of the relationship between the X-ray fluorescence spectrum intensity and the content of phosphorus element constructed by the present invention (y-85.539X + 22.044);
fig. 3 is a calibration work graph of the relationship between the X-ray fluorescence spectrum intensity and the content of potassium element (y-1377.435 × X +1066.532) constructed by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention.
Example 1
A method for rapidly measuring the contents of chlorine, phosphorus and potassium in a compound fertilizer product mainly comprises the following steps:
the method comprises the following steps that firstly, compound fertilizer test samples come from 17 compound fertilizer samples produced by main production enterprises of 4 provinces in Jiangsu, Anhui, Shandong and Sichuan, the samples come from different production enterprises and comprise the existing main compound fertilizer production formula, wherein 15 samples are used as samples selected for constructing a calibration working curve, and the content ranges of chlorine, phosphorus and potassium are as follows: cl-The measurement range of (2): 22.51E43.81％，P2O5The measurement range of (2): 4.73 to 17.23%, K2Measurement range of O: 4.44-16.27%, and 2 samples are used for verifying the consistency of the detection result of the method and the detection result of the current national standard method. Respectively selecting chlorine, phosphorus and potassium samples with different contents in the 15 samples, drying the samples for 2 hours at the temperature of 45 ℃, weighing 5g of the samples, accurately extracting chlorine, phosphorus and potassium elements to 0.1mg, and preparing a calibration solution for constructing a calibration working curve of the relation between the X-ray fluorescence spectrum intensity and the contents of the chlorine, phosphorus and potassium elements. Wherein the contents of chlorine, phosphorus and potassium in the 15 samples are respectively measured by the methods of GB 15063-2009, GB/T8573-2010 and GB/T8574-2010, and the results are shown in the following table 1.
TABLE 1 content of chlorine, phosphorus, potassium elements in the calibration samples of the Compound fertilizers
The compound fertilizer sample is tested by adopting a handheld energy dispersion type X-ray fluorescence spectrometer, the handheld energy dispersion type X-ray fluorescence spectrometer is an Explorer 9000 model produced by Jiangsu Tianrui instrument company, the power is 4W, the resolution ratio is less than or equal to 135eV, 5 groups of adjustable optical filters are adopted, and the detector is an SDD detector. The optimal test conditions of the chlorine element are as follows: test time was 40s, X-ray tube pressure was 7kV, X-ray tube flow was 40 μ Α, filter: al; the test conditions of the phosphorus element are as follows: test time was 60s, X-ray tube pressure was 9kV, X-ray tube flow was 50 μ a, filter: al; the test conditions of the potassium element are as follows: test time was 50s, X-ray tube pressure was 9kV, X-ray tube flow was 50 μ a, filter: and Mo. Three elements tested the selected background-subtracted range: the chlorine element is 4.75-6.75 eV, the phosphorus element is 5.05-7.05 eV, and the potassium element is 4.63-7.63 eV. Thickness of sample liquid: 1-20 mm, the liquid interface film is: polyethylene material, thickness 8 μm. The test results, as shown in table 2, show that the X-ray fluorescence spectrum intensity of different elements and the content of the target element show increasing trend.
Table 2. concentration of target in Compound Fertilizer sample extract with constant volume of 100mL
TABLE 3 concentration of chlorine, phosphorus, potassium in the Compound Fertilizer samples and X-ray fluorescence Spectroscopy intensity
According to the test results in table 3, a relevant change chart is constructed, and the results show that the X-ray fluorescence spectrum intensity of chlorine, phosphorus and potassium elements shows obvious linear correlation with the concentration change of the target object in the compound fertilizer product within the concentration range of the calibration sample, and the results are shown in fig. 1, fig. 2 and fig. 3. The results in the figure show that the linear correlation coefficient of the constructed calibration working curve of the chlorine, phosphorus and potassium elements is greater than 0.995, and the optimal test condition of each element is explored simultaneously, so that the foundation is laid for the detection of the contents of the chlorine, phosphorus and potassium in the compound fertilizer product. Content range of each target of calibration sample, Cl-The content range of (A): 22.51-43.81% of P2O5The content range of (A): 4.44-17.23%, K2The content range of O is as follows: 4.74-16.27% of the chlorine content is obviously linear correlation, and the detection limit of the method is combined, so that the method can definitely determine the measurement range of each target object, and the measurement range of the chlorine is Cl-The method comprises the following steps: 0.17 to 43.81 wt%, and the measurement range of phosphorus is P2O5The method comprises the following steps: 0.31-17.23 wt%, K being the measurement range of potassium2The O is: 0.21 to 16.27 wt%, but the measurement range of the method is not limited to this range, and measurement outside this range requires relevant experimental verification.
X-ray radiation penetrates different substances in different thicknesses, generally speaking, the greater the atomic number of a substance, the smaller the thickness it penetrates, typical examples being X-ray shielding devices such as: lead glass, lead gloves, etc. In the invention, the matrix of the sample is water, and the main compound is composed of light elements with smaller atomic numbers, so the influence of the thickness of the sample on the measurement result is researched. The effect of film material and thickness on the results was also investigated and the results are shown in tables 4 and 5. The results in table 4 show that the thickness of the sample solution to be tested is within the range of 1-20 mm, and the influence of the thickness change on the measurement result can be reflected very little through the standard deviation, so that the appropriate sample dosage can be selected according to the sampling convenience and the sample amount in the test process.
TABLE 4 influence of sample solution thickness on measurement results
The results in table 5 show that the content of the element to be measured tends to decrease with the increase of the thickness of the interface film of the sample solution, and although the change is not obvious when the thickness of the film is small, the change is enough to affect the accuracy of the test result, so that the thickness of the interface film of the sample solution used in the calibration curve is consistent with the thickness of the film used in the test sample. In order to improve the accuracy and precision of the measurement result and reduce the absorption of the X-ray fluorescence spectrum line of the target element of the film on the interface of the sample solution, the film with small thickness should be selected as much as possible to improve the measurement sensitivity.
TABLE 5 influence of the interfacial film thickness of the sample solution on the measurement results under the condition that the thickness of the test solution is 4mm
6 compound fertilizer samples are selected to carry out chlorine, phosphorus and potassium content accuracy verification experiments, and the 6 compound fertilizer samples are prepared by adopting the existing national standard method. Extracting chlorine, phosphorus and potassium elements from the sample, testing the content of the chlorine, phosphorus and potassium elements by using a handheld energy dispersion type X-ray fluorescence spectrometer, selecting 3 different points for each sample, and taking an average value, and comparing the accuracy of the test result with the national standard methods of GB 15063-. The test results are shown in table 6.
TABLE 6 determination of the contents of chlorine, phosphorus and potassium in 6 samples of the compound fertilizers by the method of the present invention
The measurement results in table 6 show that the energy dispersion type X-ray fluorescence spectrum calibration working curve constructed by the invention can be used for measuring the contents of chlorine, phosphorus and potassium in compound fertilizer products, and the measurement results are quite consistent with the measurement values of the national standard method, which indicates that the method can be used as a novel detection method for rapidly and accurately measuring the contents of chlorine, phosphorus and potassium in compound fertilizer products.
And step two, testing the contents of chlorine, phosphorus and potassium in 2 compound fertilizer samples by adopting a handheld energy dispersion type X-ray fluorescence spectrometer according to the testing conditions of chlorine, phosphorus and potassium elements in the step one, repeatedly testing each sample at 7 different points, and evaluating the stability of the detection result through standard deviation. And simultaneously sampling the 2 compound fertilizer samples, testing the contents of chlorine, phosphorus and potassium by adopting the existing national standard method, and comparing the standard deviation of the test results of the two methods, wherein the test results are shown in table 7.
TABLE 7 determination of contents and standard deviations of Cl, P and K in mixed fertilizer by the method and national standard method
The determination results in table 7 fully show that the energy dispersion type X-ray fluorescence spectrum calibration working curve constructed by the invention can be completely used for determining the contents of chlorine, phosphorus and potassium elements in the compound fertilizer sample, and the standard deviation of the 7-time repeated measurement results is obviously smaller than the standard deviation of the measurement values of the national standard method, which indicates that the stability of the detection results is good, and the method can be used for rapidly and accurately determining the contents of chlorine, phosphorus and potassium elements in the compound fertilizer sample. The X-ray fluorescence spectrum technology is generally used for measuring the composition of substances by adopting a tabletting method to prepare samples and construct a calibration working curve, the accuracy and stability of the measurement result are obviously influenced by matrix interference, the compound fertilizers are various in variety, the chemical compositions of different types of compound fertilizers are very different, the mineral types are very different, and an approximate sample is difficult to find out to be used as the calibration curve for measuring the chemical compositions of the same type of sample. This is different from the chemical composition measurement of other minerals, and the interference of the matrix can be eliminated to a great extent only by using minerals with similar chemical compositions to make a calibration working curve. However, the compound fertilizer is a product obtained by artificially synthesizing different minerals by a physical or chemical method, and the product type is more complicated. Therefore, the invention can eliminate the matrix effect and mineral effect of the sample by extracting the target element to be measured and transferring the target element to be measured into the same system water solution, and simultaneously the uniformity of the sample is very good. The advantages and disadvantages of a detection method are generally obtained by evaluating the precision and accuracy of the detection method, wherein the standard deviation of a plurality of experimental measurement results can best reflect the precision of the detection method, and the results in table 7 show that the method has very small standard deviation, which indicates that the method has very good precision and can completely meet the determination of the contents of chlorine, phosphorus and potassium in compound fertilizer products.
And step three, testing the contents of chlorine, phosphorus and potassium in 3 compound fertilizer samples (numbered FHF-SY1, FHF-SY2 and FHF-SY3) which are inspected by enterprises by adopting a handheld energy dispersion type X-ray fluorescence spectrometer according to the testing conditions of the elements of chlorine, phosphorus and potassium in the step one. And simultaneously sampling the 3 compound fertilizer samples, testing the contents of chlorine, phosphorus and potassium by adopting the existing national standard method, and comparing the consistency of the test results of the two methods, wherein the test results are shown in table 8. The result shows that the detection result of the method has very high consistency with the detection result of the existing national standard detection method, and can be used as a brand new method for quickly and accurately determining the contents of the chlorine, phosphorus and potassium elements in the compound fertilizer sample.
TABLE 8 determination of the contents of Cl, P and K in unknown mixed fertilizer by the method of the present invention and the existing national standard method
The handheld energy dispersion type X-ray fluorescence spectrometer is the prior art, and the structure and the working principle of the handheld energy dispersion type X-ray fluorescence spectrometer are not described in detail.
Although the embodiments of the present invention have been described in detail, it should be understood that various changes, substitutions, and alterations can be made hereto without departing from the spirit and scope of the invention.
Claims (3)
1. A method for detecting the contents of chlorine, phosphorus and potassium in a compound fertilizer product by energy dispersion X-ray fluorescence spectroscopy comprises the following steps:
firstly, selecting compound fertilizer products composed of different types and contents as calibration samples, and accurately measuring the contents of chlorine, phosphorus and potassium by adopting the existing national standard method; wherein the national standard method for measuring chlorine is GB 15063-2009, the national standard method for measuring phosphorus is GB/T8573-2010, and the national standard method for measuring potassium is GB/T8574-2010; extracting chlorine, phosphorus and potassium elements in compound fertilizer samples with different types and contents and preparing a calibration solution;
step two, measuring a compound fertilizer sample with known chlorine, phosphorus and potassium contents by using a handheld energy dispersive X-ray fluorescence spectrometer, constructing a calibration working curve of the relation between the X-ray fluorescence spectrum intensity and the contents of chlorine, phosphorus and potassium elements, and determining the test conditions of the chlorine, phosphorus and potassium elements;
thirdly, according to the testing conditions of the chlorine, phosphorus and potassium elements determined in the first step and the second step, a hand-held energy dispersion type X-ray fluorescence spectrometer is adopted to measure the compound fertilizer sample to be tested, according to the relation between the X-ray fluorescence spectrum intensity and the contents of the chlorine, phosphorus and potassium elements in the calibration working curve constructed in the second step, the contents of the chlorine, phosphorus and potassium in the compound fertilizer sample to be tested are calculated by using a formula, and the content calculation formula of the target object is:
in formula (1):
Wipercent: represents the mass percentage of the target object i;
v: the unit of the constant volume of the extraction solution of the sample to be detected is mL;
m: the weighing amount of the compound fertilizer in the prepared extraction solution of the sample to be tested is expressed in g;
Ci: the concentration of the solution read by the instrument test is expressed in g/mL;
step one the concrete steps of preparing the calibration solution are as follows: adding 2.0-10.0 g of sample into a 100mL volumetric flask, adding 60mL of 40g/L EDTA solution into the volumetric flask, maintaining the temperature in a constant-temperature water bath at 80 ℃, shaking for 1.5h, taking out the volumetric flask, cooling, fixing the volume to 100mL, and filtering to obtain a clear solution serving as a calibration solution of chlorine, phosphorus and potassium; preparing a blank calibration blank solution by performing chlorine, phosphorus and potassium according to the same steps;
and step two, the test conditions of the chlorine, phosphorus and potassium elements are as follows:
the test conditions of the chlorine element are as follows: test time was 40s, X-ray tube pressure was 7kV, X-ray tube flow was 40 μ Α, filter: al;
the test conditions of the phosphorus element are as follows: test time was 60s, X-ray tube pressure was 9kV, X-ray tube flow was 50 μ a, filter: al;
the test conditions of the potassium element are as follows: test time was 50s, X-ray tube pressure was 9kV, X-ray tube flow was 50 μ a, filter: mo;
three elements tested the selected background-subtracted range: chlorine element is 4.75-6.75 eV, phosphorus element is 5.05-7.05 eV, and potassium element is 4.63-7.63 eV;
thickness of sample liquid in measurement: 1-20 mm, the liquid interface film is: polyethylene material with a thickness of 8 μm.
2. The method of claim 1, wherein: step one, the compound fertilizer products composed of different types and contents are compound fertilizers, compound fertilizers or bulk blend fertilizers.
3. The method of claim 1, wherein: the measurement ranges of the three elements of chlorine, phosphorus and potassium are as follows: chlorine measurement range as Cl-The method comprises the following steps: 0.17 to 43.81 wt%, and the measurement range of phosphorus is P2O5The method comprises the following steps: 0.31-17.23 wt%, K being the measurement range of potassium2The O is: 0.21 to 16.27 wt%.
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