Method for simultaneously and rapidly determining contents of multiple elements in ferrovanadium

Abstract

The invention discloses a method for simultaneously and rapidly determining the contents of multiple elements in ferrovanadium, which comprises the following steps: firstly, selecting 3-5 ferrovanadium standard substances with known contents of silicon, manganese, phosphorus and vanadium to form a concentration gradient, and crushing a sample to be detected and the selected standard substances into particles of less than 60 meshes; dissolving a to-be-detected sample and the selected standard substance in the solution; carrying out data acquisition on the emission spectrum light intensity of the standard substance silicon, manganese, phosphorus and vanadium elements, drawing a standard working curve of each element according to the corresponding relationship between the element content and the emission spectrum light intensity, and substituting the emission spectrum light intensity of the silicon, manganese, phosphorus and vanadium elements of the sample to be detected, which is acquired by the instrument, into the standard working curve; and calculating the contents of silicon, manganese, phosphorus and vanadium elements in the sample to be detected. The method solves the problem of sample solution preparation when ferrovanadium is measured by the ICP spectrometer, the sample solution preparation process is simple, and the measurement process is not interfered.

Description

Technical Field

[0001] The invention relates to a method for simultaneously and quickly determining the contents of multiple elements in ferrovanadium, and belongs to the field of quality detection. Background Art

[0002] Ferrovanadium is an iron alloy composed of vanadium and iron. It is mainly used as an alloy additive in steelmaking. Vanadium can improve the strength, toughness, ductility and heat resistance of steel. The traditional analysis method is chemical method, in which silicon is analyzed by photometry; manganese is analyzed by titration; phosphorus is analyzed by photometry, and vanadium is analyzed by titration. The disadvantages are cumbersome operation, lengthy analysis process, high analysis cost and low accuracy.

[0003] Inductively coupled plasma (ICP-AES) emission spectrometry is the most commonly used analytical method for elemental analysis of metal materials. It has the advantages of low detection limit, high sensitivity, good stability, small matrix effect, wide linear range of concentration determination, and simultaneous determination of multiple elements, and has been widely used.

[0004] However, the traditional chemical sample pretreatment method requires the use of a variety of chemical reagents. The addition of a large amount of chemical reagents to the test solution will interfere with the instrument test and affect the accuracy and repeatability of the measurement. Summary of the invention

[0005] The purpose of the present invention is to provide a method for determining the contents of silicon, manganese, phosphorus and vanadium in ferrovanadium by ICP-AES method which is fast, accurate and pollution-free to the instrument, so as to overcome the shortcomings of the prior art.

[0006] The objective of the present invention is achieved through the following technical solutions:

[0007] The method for simultaneously and rapidly determining the content of multiple elements in ferrovanadium of the present invention comprises the following specific steps:

[0008] 1) Selection of ferrovanadium standard substances: Select 3-5 ferrovanadium standard substances with known silicon 0.1%-1.5%, manganese 0.1%-2.0%, phosphorus 0.01%-0.15%, and vanadium 40.0%-60.0% element contents to form a concentration gradient;

[0009] 2) Preparation method of solid sample: crush the sample to be tested and the selected ferrovanadium standard material into particles smaller than 60 mesh;

[0010] 3) Preparation of standard substance solution: weigh 0.1000-0.2000g of ferrovanadium standard substance, place them in 100-300ml conical flasks, add 8-15ml of 30%-50% sulfuric acid-nitric acid mixed acid aqueous solution by volume, heat at 200-230℃ until the reaction is complete, add 5-15ml of 5%-10% ammonium persulfate aqueous solution by mass, boil until the ammonium persulfate is completely decomposed, cool and transfer to an appropriate volumetric flask, dilute quantitatively with deionized water, and mix well;

[0011] The volume ratio of sulfuric acid to nitric acid in the sulfuric acid-nitric acid mixed acid aqueous solution is 1:1;

[0012] 4) Preparation of the sample solution: weigh 0.1000-0.2000g of the sample to be tested, place them in 100-300ml conical flasks, add 8-15ml of a 30%-50% sulfuric acid-nitric acid mixed acid aqueous solution by volume, heat at 200-230°C until the reaction is complete, add 5-15ml of a 5%-10% ammonium persulfate aqueous solution by mass, boil until the ammonium persulfate is completely decomposed, cool and transfer to an appropriate volumetric flask, dilute quantitatively with deionized water, and mix well;

[0013] 5) Determination of the sample to be tested: Data collection is performed on the emission spectrum intensity of silicon, manganese, phosphorus and vanadium elements of the ferrovanadium standard substance, and the standard working curve of each element is drawn based on the corresponding relationship between the element content and the emission spectrum intensity. The emission spectrum intensity of silicon, manganese, phosphorus and vanadium elements of the sample to be tested collected by the instrument is brought into the standard working curve to calculate the silicon, manganese, phosphorus and vanadium content of the sample to be tested;

[0014] 6) Select certified reference materials to verify the accuracy of the test results of silicon, manganese, phosphorus and vanadium content.

[0015] The beneficial effects of the present invention are as follows: a method for simultaneously determining the contents of silicon, manganese, phosphorus and vanadium in ferrovanadium by ICP-AES method is provided, which is fast, accurate and pollution-free to the instrument; the present invention solves the problem of sample solution preparation when the ICP spectrometer is used to determine ferrovanadium, the sample solution preparation process is simple, and no interference is generated in the determination process; the determination method of the present invention can be applied to the sample pretreatment technology for determining the ferrovanadium content by other element analysis instruments, and has broad application prospects in the field of material analysis. DETAILED DESCRIPTION

[0016] The present invention will be further described below in conjunction with the embodiments.

[0017] Example

[0018] 1) Select a series of standard substances with silicon content of 0.15%, 0.42%, 0.93%, and 1.46%; manganese content of 0.16%, 0.62%, 1.10%, and 1.95%; phosphorus content of 0.013%, 0.052%, 0.090%, and 0.140%; and vanadium content of 40.80%, 46.55%, 53.90%, and 59.40%;

[0019] 2) After the samples to be tested and the standard substances are crushed, particles smaller than 60 mesh are selected;

[0020] 3) Weigh 0.1500±0.0002g of a series of standard substances and place them in 250ml conical flasks respectively, add 10ml of sulfuric acid-nitric acid mixed acid aqueous solution (volume ratio concentration 45%, sulfuric acid: nitric acid = 1:1), heat at 215±5℃ until the reaction is complete, add 10ml of ammonium persulfate aqueous solution (mass ratio concentration 5%), boil until the ammonium persulfate is completely decomposed, cool and transfer to an appropriate volumetric flask, dilute quantitatively with deionized water, and mix well;

[0021] 4) The preparation process of the sample solution with unknown content is the same as step 3);

[0022] 5) Using an inductively coupled plasma (ICP-AES) emission spectrometer, set the RF generator power to 1.25kw, the atomization pressure to 26.0psi, the argon flow rate to 0.5L / min, the analysis pump speed to 2.60ml / min, the sample flushing time to 60s, the integration time to 30s for short wave and 10s for long wave; element analysis line (nm): silicon 251.611, manganese 257.610, phosphorus 213.618, vanadium 309.311; collect data for a series of standard substances, draw standard working curves for each element, and determine the element content of the sample to be tested when the linear correlation coefficient of each curve is greater than 0.999;

[0023] 6) Select standard substances GSB03-2471-2008 and YSBC37655-11 to verify the accuracy of the test results of silicon, manganese, phosphorus and vanadium content of the samples to be tested. (n=10), relative standard deviation RSD (%) is shown in the following table. As can be seen from the table, the RSD determined by this method is less than 2%, and the error of the determination result compared with the standard value is within the allowable range of the national standard for chemical analysis.

[0024] Precision and accuracy (n=10)

[0025]

Claims

1. A method for simultaneously and rapidly determining the content of multiple elements in ferrovanadium, characterized in that: The specific steps are as follows: 1) Selection of ferrovanadium standard substances: Select 3-5 ferrovanadium standard substances with known silicon 0.1%-1.5%, manganese 0.1%-2.0%, phosphorus 0.01%-0.15%, and vanadium 40.0%-60.0% element contents to form a concentration gradient; 2) Preparation method of solid sample: crush the sample to be tested and the selected ferrovanadium standard material into particles smaller than 60 mesh; 3) Preparation of standard substance solution: weigh 0.1000-0.2000g of ferrovanadium standard substance, place them in 100-300ml conical flasks, add 8-15ml of 30%-50% sulfuric acid-nitric acid mixed acid aqueous solution by volume, heat at 200-230℃ until the reaction is complete, add 5-15ml of 5%-10% ammonium persulfate aqueous solution by mass, boil until the ammonium persulfate is completely decomposed, cool and transfer to an appropriate volumetric flask, dilute quantitatively with deionized water, and mix well; The volume ratio of sulfuric acid to nitric acid in the sulfuric acid-nitric acid mixed acid aqueous solution is 1:1; 4) Preparation of the sample solution: weigh 0.1000-0.2000g of the sample to be tested, place them in 100-300ml conical flasks, add 8-15ml of a 30%-50% sulfuric acid-nitric acid mixed acid aqueous solution by volume, heat at 200-230°C until the reaction is complete, add 5-15ml of a 5%-10% ammonium persulfate aqueous solution by mass, boil until the ammonium persulfate is completely decomposed, cool and transfer to an appropriate volumetric flask, dilute quantitatively with deionized water, and mix well; 5) Determination of the sample to be tested: Data collection is performed on the emission spectrum intensity of silicon, manganese, phosphorus and vanadium elements of the ferrovanadium standard substance, and the standard working curve of each element is drawn based on the corresponding relationship between the element content and the emission spectrum intensity. The emission spectrum intensity of silicon, manganese, phosphorus and vanadium elements of the sample to be tested collected by the instrument is brought into the standard working curve to calculate the silicon, manganese, phosphorus and vanadium content of the sample to be tested; 6) Select certified reference materials to verify the accuracy of the test results of silicon, manganese, phosphorus and vanadium content.

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