CN110927144A - ICP-AES (inductively coupled plasma-atomic emission Spectrometry) measuring method for content of impurity phosphorus in steel - Google Patents
ICP-AES (inductively coupled plasma-atomic emission Spectrometry) measuring method for content of impurity phosphorus in steel Download PDFInfo
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Abstract
The invention discloses an ICP-AES (inductively coupled plasma-atomic emission Spectrometry) measuring method for the content of impurity phosphorus in steel, and particularly relates to the technical field of element content measurement, and the method comprises the following steps: pre-treating; step two: preparing a standard solution; step three: digesting a sample; step four: establishing an MSF model: (1) respectively collecting spectrograms of the reagent blank solution and the pure solution of each element to be detected; (2) opening a data set when a spectrogram is collected under an MSF window, defining the role of each component in analysis under each element analysis line, and then establishing an MSF model; (3) analyzing a known sample by using the established MSF model; step five: and (5) applying the model. The MSF model is established by adopting a spectral interference and multivariate spectral fitting correction mode and a standard solution adding method is adopted, so that a standard solution and a sample do not need to be matched with each other, a standard curve does not need to be made in the measuring process, the obtained data is still accurate and reliable, and the measuring time is greatly shortened.
Description
Technical Field
The invention relates to the technical field of element content determination, in particular to an ICP-AES (inductively coupled plasma-atomic emission Spectrometry) measuring method for the content of impurity phosphorus in steel.
Background
The method for measuring and analyzing the phosphorus in the steel is commonly used as follows: chemical colorimetry, direct-reading spectrometry, inductively coupled plasma emission spectrometry, and the like. The phosphorus in the steel is measured by adopting a chemical colorimetric method, and the content of the phosphorus is difficult to accurately measure due to the poor stability of phosphorus-molybdenum blue; when the direct-reading spectrometry is adopted to measure the high-content phosphorus in the steel, the high-content standard steel does not exist, so that the accurate quantification cannot be realized; the inductively coupled plasma emission spectrometry has the characteristics of high sensitivity, good resolution, high accuracy, wide linear range, low detection limit and the like, and is increasingly widely applied.
However, phosphorus is the most difficult impurity element in steel to be measured by the ICP-AES method because of interference of spectral lines of copper, iron, molybdenum and the like in the measurement process. The current newer analysis and test method is to adopt multi-component spectrogram fitting (MSF) plasma emission spectrometry to measure phosphorus in steel, but the method needs to establish a reasonable MSF file according to the chemical composition of an analyte, and in order to prevent excessive or insufficient correction, the establishment of a model needs to be corrected for many times, so that the measurement takes longer time.
Disclosure of Invention
In order to overcome the above defects in the prior art, embodiments of the present invention provide an ICP-AES measurement method for measuring the content of phosphorus as an impurity in steel, which establishes an MSF model by means of spectral interference and multivariate spectral fitting correction, and is assisted by a standard solution addition method, so that a standard solution and a sample do not need to be matched with each other, and a standard curve does not need to be made in the measurement process, and the obtained data is still accurate and reliable, so that the measurement time is greatly shortened, and the problems proposed in the background art are solved.
In order to achieve the purpose, the invention provides the following technical scheme: an ICP-AES measuring method for the content of impurity phosphorus in steel specifically comprises the following operation steps:
the method comprises the following steps: pretreatment: before sample treatment, all the utensils to be used were first measured and washed clean with detergent and then with 10% by volume of HNO3Soaking overnight, continuously washing for 3-5 times with cleaning solution, and air drying;
step two: preparing standard solution: taking 5ml of phosphorus mother liquor with the concentration of 1000mg/L, diluting by 10 times, and preparing 50ml of phosphorus standard working solution with the concentration of 100 mg/L;
step three: sample digestion: accurately weighing 0.2 g in a 100ml glass beaker, adding 1ml of cleaning solution for wetting, then adding 25ml of sample dissolving system, covering a watch glass, heating on an electric heating plate at low temperature until the solution is transparent, then removing the cover and adding 1ml of HClO4Heating to remove white smoke, cooling the residue, and adding HNO with volume concentration of 7%3Extracting with slight heat, and coolingTransferring to room temperature, fixing the volume to a 50ml volumetric flask, uniformly mixing to be detected, and preparing a reagent blank solution;
step four: establishing an MSF model: (1) respectively collecting spectrograms of the reagent blank solution and the pure solution of each element to be detected; (2) opening a data set when a spectrogram is collected under an MSF window, defining the role of each component in analysis under each element analysis line, and then establishing an MSF model; (3) analyzing a known sample by using the established MSF model, if the result is not consistent, correcting until the requirement is met, and finally performing conventional analysis by using the MSF model;
step five: application of the model: and (3) adding a proper amount of standard solution into the solution to be measured, and performing on-machine measurement on the standard solution by using the MSF model established in the step four without making a standard working curve.
In a preferred embodiment, in the step one and the step three, the cleaning solution is triple distilled water.
In a preferred embodiment, in the third step, the solution system is HNO3Either system or dilute aqua regia system.
In a preferred embodiment, in the fourth step, when the spectra are collected, the selected lines are P213.617nm, P214.914nm, P178.221nm and P177.434 nm.
In a preferred embodiment, in step four above, the components defined in the process of establishing the MSF model include analytes, interferents and blanks.
The invention has the technical effects and advantages that:
1. the MSF model is established by adopting a spectral interference and multivariate spectral fitting correction mode and a standard solution adding method is adopted, so that a standard solution and a sample do not need to be matched with each other, a standard curve does not need to be made in the measuring process, the obtained data is still accurate and reliable, and the measuring time is greatly shortened;
2. according to the invention, different sample dissolving systems are adopted to carry out sample dissolving treatment on the standard sample, and the content of impurity phosphorus in the standard sample is extremely low (< 0.01%), so that the sample dissolving system most suitable for analyzing low content P (< 0.01%) is found out, and the detection precision can be greatly improved.
Drawings
FIG. 1 is a flow chart of the test of the present invention.
FIG. 2 shows the interference of 4 detection lines of phosphorus in the present invention and the test process in steel samples.
FIG. 3 is a standard addition operating curve for phosphorus in the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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
The invention provides an ICP-AES (inductively coupled plasma-atomic emission spectrometry) measuring method for the content of impurity phosphorus in steel, which specifically comprises the following operation steps:
the method comprises the following steps: pretreatment: before sample treatment, all the utensils to be used were first measured and washed clean with detergent and then with 10% by volume of HNO3Soaking overnight, continuously washing with triple distilled water for 3-5 times, and air drying;
step two: preparing standard solution: taking 5ml of phosphorus mother liquor with the concentration of 1000mg/L, diluting by 10 times, and preparing 50ml of phosphorus standard working solution with the concentration of 100 mg/L;
step three: sample digestion: accurately weighing 0.2 g of the extract in a 100ml glass beaker, adding 1ml of triple distilled water for wetting, and adding HNO3System (i.e. 1 volume of HNO3And 3 volumes of distilled water mixed well) was added to the sample, the cuvette was closed, the solution was heated at low temperature (38-42 ℃) on a hot plate until the solution was transparent, and then 1ml of HClO was added after removing the lid4Heating to remove white smoke, cooling the residue, and adding HNO with volume concentration of 7%3Slightly heating for extraction, cooling to room temperature, transferring to constant volume to 50ml volumetric flask, mixing well for testing, and simultaneouslyPreparing a reagent blank solution;
step four: establishing an MSF model: (1) respectively collecting spectrograms of a reagent blank solution and pure solutions of elements to be detected, wherein the selected spectral lines are P213.617nm, P214.914nm, P178.221nm and P177.434nm (namely the first four sensitive analysis spectral lines recommended by phosphorus), and as the phosphorus content in a steel sample is mostly in the order of 0.0 x%, the phosphorus concentration in the test solution is low, and phosphorus signals can not be detected at the P177.434nm and the P178.221nm almost and can not be used as analysis spectral lines; the analysis of a sample spectrogram of P213.617nm shows that the left side of the sample spectrogram is a peak of Cu 213.597nm, the right side of the sample spectrogram is a peak of Fe 213.652nm, and the interference exists on a phosphorus spectral line; analyzing the sample spectrogram of P214.914 nmn, wherein the left Cu 214.898nm spectral line interferes with the sample spectrogram, and the second line can detect the peak of phosphorus, but the interference of the spectral line is large (see the attached figure 2 of the specification), so that characteristic spectrograms of blanks, interfering elements and analyzing elements are respectively scanned by taking P213.617nm and P214.914nm as wavelengths (preferably, P214.914nm as the wavelength); (2) opening a data set when a spectrogram is collected under an MSF window, defining the role of each component in analysis under each element analysis line, and then establishing an MSF model; (3) analyzing a known sample by using the established MSF model, if the result is not consistent, correcting until the requirement is met, and finally performing conventional analysis by using the MSF model;
step five: application of the model: adding a proper amount of standard solution into the solution to be analyzed, utilizing the MSF model established in the fourth step to carry out on-machine measurement on the solution with the standard, and not needing to make a standard working curve, wherein the object to be analyzed can be divided into a plurality of groups, adding the standard solution with non-gradient concentration (including a control group without the standard solution) according to gradient, recording the absolute intensity of the characteristic spectrum of the analysis element, after blank deducting, taking the concentration value of the object to be analyzed and the standard solution as the abscissa, taking the emission spectrum intensity of the object to be analyzed as the ordinate of a plotting, when the peak value is 0, taking the absolute value of the intersection point of the working curve and the concentration coordinate of the object to be analyzed as the concentration value of the object to be analyzed, if the analysis curve is linear, the analysis result is reliable, otherwise, the.
Example 2
The invention provides an ICP-AES (inductively coupled plasma-atomic emission spectrometry) measuring method for the content of impurity phosphorus in steel, which specifically comprises the following operation steps:
the method comprises the following steps: pretreatment: before sample treatment, all the utensils to be used were first measured and washed clean with detergent and then with 10% by volume of HNO3Soaking overnight, continuously washing with triple distilled water for 3-5 times, and air drying;
step two: preparing standard solution: taking 5ml of phosphorus mother liquor with the concentration of 1000mg/L, diluting by 10 times, and preparing 50ml of phosphorus standard working solution with the concentration of 100 mg/L;
step three: sample digestion: accurately weighing 0.2 g into a 100ml glass beaker, adding 1ml of triple distilled water for wetting, adding 25ml of a sample dissolving system of a dilute aqua regia system (namely a solution obtained by fully and uniformly mixing 1 volume of dilute aqua regia and 3 volumes of distilled water), covering a surface dish, heating on an electric hot plate at low temperature (38-42 ℃) until the solution is transparent, removing the cover, and adding 1ml of HClO4Heating to remove white smoke, cooling the residue, and adding HNO with volume concentration of 7%3Slightly heating for extraction, cooling to room temperature, transferring to a volumetric flask with a constant volume of 50ml, uniformly mixing to be detected, and simultaneously preparing a reagent blank solution;
step four: step four: establishing an MSF model: (1) respectively collecting spectrograms of a reagent blank solution and pure solutions of elements to be detected, wherein the selected spectral lines are P213.617nm, P214.914nm, P178.221nm and P177.434nm (namely the first four sensitive analysis spectral lines recommended by phosphorus), and as the phosphorus content in a steel sample is mostly in the order of 0.0 x%, the phosphorus concentration in the test solution is low, and phosphorus signals can not be detected at the P177.434nm and the P178.221nm almost and can not be used as analysis spectral lines; the analysis of a sample spectrogram of P213.617nm shows that the left side of the sample spectrogram is a Cu 213.597nm peak, and the right side of the sample spectrogram is an Fe 213.652nm peak, so that interference exists on a phosphorus spectral line; analyzing the sample spectrogram of P214.914 nmn, wherein the left Cu 214.898nm spectral line interferes with the sample spectrogram, and the second line can detect the peak of phosphorus, but the interference of the spectral line is large (see the attached figure 2 of the specification), so that characteristic spectrograms of blanks, interfering elements and analyzing elements are respectively scanned by taking P213.617nm and P214.914nm as wavelengths (preferably, taking P214.914nm as the wavelength); (2) opening a data set when a spectrogram is collected under an MSF window, defining the role of each component in analysis under each element analysis line, and then establishing an MSF model; (3) analyzing a known sample by using the established MSF model, if the result is not consistent, correcting until the requirement is met, and finally performing conventional analysis by using the MSF model;
step five: application of the model: adding a proper amount of standard solution into the solution to be analyzed, utilizing the MSF model established in the fourth step to carry out on-machine measurement on the solution with the standard, and not needing to make a standard working curve, wherein the object to be analyzed can be divided into a plurality of groups, adding the standard solution with non-gradient concentration (including a control group without the standard solution) according to gradient, recording the absolute intensity of the characteristic spectrum of the analysis element, after blank deducting, taking the concentration value of the object to be analyzed and the standard solution as the abscissa, taking the emission spectrum intensity of the object to be analyzed as the ordinate of a plotting, when the peak value is 0, taking the absolute value of the intersection point of the working curve and the concentration coordinate of the object to be analyzed as the concentration value of the object to be analyzed, if the analysis curve is linear, the analysis result is reliable, otherwise, the.
The content of phosphorus in the substance to be tested is determined by the above measurement method, and the test result is shown in fig. 3 (a characteristic spectrum with P214.914nm as a wavelength) in the specification, and the analysis of the test result can show that: the test solution is corrected by an MSF model, and a standard solution adding method is adopted to measure the P214.914nm as the spectral line of light waves, so that the linear relation is formed, and the data change is minimum, so that the test result is correct.
The data of different standard samples after sample dissolution treatment are respectively measured by using the sample dissolution systems in the example 1 and the example 2 under the same condition, and the test results are shown in the following table:
according to the test results in the table, the detection results of the two sample dissolving systems are basically consistent, but HNO3The analysis effect of the sample dissolving system of the system is good when the content of P is low (less than 0.01 percent).
Finally, it should be noted that: although the present invention has been described in detail with reference to the general description and the specific embodiments, on the basis of the present invention, the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. An ICP-AES measuring method for the content of impurity phosphorus in steel is characterized in that: the method specifically comprises the following operation steps:
the method comprises the following steps: pretreatment: before sample treatment, all the utensils to be used were first measured and washed clean with detergent and then with 10% by volume of HNO3Soaking overnight, continuously washing for 3-5 times with cleaning solution, and air drying;
step two: preparing standard solution: taking 5ml of phosphorus mother liquor with the concentration of 1000mg/L, diluting by 10 times, and preparing 50ml of phosphorus standard working solution with the concentration of 100 mg/L;
step three: sample digestion: accurately weighing 0.2 g in a 100ml glass beaker, adding 1ml of cleaning solution for wetting, then adding 25ml of sample dissolving system, covering a watch glass, heating on an electric heating plate at low temperature until the solution is transparent, then removing the cover and adding 1ml of HClO4Heating to remove white smoke, cooling the residue, and adding HNO with volume concentration of 7%3Slightly heating for extraction, cooling to room temperature, transferring to a volumetric flask with a constant volume of 50ml, uniformly mixing to be detected, and simultaneously preparing a reagent blank solution;
step four: establishing an MSF model: (1) respectively collecting spectrograms of the reagent blank solution and the pure solution of each element to be detected; (2) opening a data set when a spectrogram is collected under an MSF window, defining the role of each component in analysis under each element analysis line, and then establishing an MSF model; (3) analyzing a known sample by using the established MSF model, if the result is not consistent, correcting until the requirement is met, and finally performing conventional analysis by using the MSF model;
step five: application of the model: and (3) adding a proper amount of standard solution into the solution to be measured, and performing on-machine measurement on the standard solution by using the MSF model established in the step four without making a standard working curve.
2. An ICP-AES method for measuring the content of impurity phosphorus in steel as claimed in claim 1, wherein the method comprises the following steps: in the step one and the step three, the used cleaning solution is triple distilled water.
3. An ICP-AES method for measuring the content of impurity phosphorus in steel as claimed in claim 1, wherein the method comprises the following steps: in the third step, the sample dissolving system is HNO3Either system or dilute aqua regia system.
4. An ICP-AES method for measuring the content of impurity phosphorus in steel as claimed in claim 1, wherein the method comprises the following steps: in the fourth step, when the spectrogram is collected, the selected spectral lines are P213.617nm, P214.914nm, P178.221nm and P177.434nm.
5. An ICP-AES method for measuring the content of impurity phosphorus in steel as claimed in claim 1, wherein the method comprises the following steps: in the fourth step, the components defined in the MSF model building process include analytes, interferents and blanks.
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