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

Abstract

The invention discloses a method for simultaneously and rapidly determining the contents of multiple elements in ferrotitanium, which comprises the following steps: firstly, selecting 3-5 ferrotitanium standard substances with known contents of silicon, manganese, phosphorus, aluminum and titanium elements to form a concentration gradient, and crushing a sample to be detected and the selected standard substances into particles of less than 40 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, aluminum and titanium 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, aluminum and titanium 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, aluminum and titanium elements in the to-be-detected sample. The method solves the problem of preparation of the sample solution when the ferrotitanium is measured by the ICP spectrograph, the preparation process of the sample solution 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 ferrotitanium, and belongs to the field of quality detection. Background Art

[0002] Ferrotitanium is a widely used special alloy. It is added to steel as an alloying element during the steelmaking process to refine the grain size, fix interstitial elements, and improve the strength of steel. The traditional analysis method is chemical, in which silicon is analyzed by photometry, manganese is analyzed by titration, phosphorus is analyzed by photometry, aluminum is analyzed by titration, and titanium is analyzed by photometry. The disadvantages are that the operation is cumbersome, the analysis process is lengthy, the analysis cost is high, and the accuracy is low.

[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, aluminum and titanium in ferrotitanium 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] A method for simultaneously and rapidly determining the contents of multiple elements in ferrotitanium of the present invention comprises the following steps:

[0008] 1) Selection of titanium-iron standard substances: Select 3-5 series of standard substances with known silicon 1.0%-6.0%, manganese 0.5%-3.0%, phosphorus 0.01%-0.10%, aluminum 1.0%-10.0%, and titanium 20.0%-50.0% element contents to form a concentration gradient;

[0009] 2) Preparation method of solid samples: crush the sample to be tested and the selected titanium iron standard material into particles smaller than 40 mesh for determination;

[0010] 3) Preparation of standard substance solution: weigh 0.1000-0.2000g of titanium iron standard substance, place them in 100-300ml conical flasks, add 5-10ml of 40%-60% sulfuric acid aqueous solution by volume, heat at 180-210°C until the reaction is complete, drop 2-5ml of 30% analytically pure hydrogen peroxide, add 5-10ml of 30%-60% hydrochloric acid-nitric acid mixed acid aqueous solution by volume, heat at 200-230°C until the reaction is complete, cool and transfer to an appropriate volumetric flask, dilute quantitatively with deionized water, and mix well;

[0011] The volume ratio of hydrochloric acid to nitric acid in the hydrochloric acid-nitric acid mixed acid aqueous solution is 1:2;

[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 5-10ml of 40%-60% sulfuric acid aqueous solution by volume, heat at 180-210°C until the reaction is complete, drop 2-5ml of 30% analytically pure hydrogen peroxide, add 5-10ml of 30%-60% hydrochloric acid-nitric acid mixed acid aqueous solution by volume, heat at 200-230°C until the reaction is complete, 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, aluminum, and titanium elements of the titanium-iron 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, aluminum, and titanium elements of the sample to be tested collected by the instrument is brought into the standard working curve to calculate the silicon, manganese, phosphorus, aluminum, and titanium 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, aluminum and titanium content.

[0015] The beneficial effects of the present invention are as follows: a method for simultaneously determining the contents of silicon, manganese, phosphorus, aluminum and titanium in ferrotitanium 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 ferrosilicon is determined by ICP spectrometer, the sample solution preparation process is simple and will not interfere with the determination process; the determination method of the present invention can be applied to sample pretreatment technology for determining the element content of ferrotitanium 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 1.5%, 2.8%, 4.3%, and 5.6%; manganese content of 0.60%, 1.32%, 2.10%, and 2.91%; phosphorus content of 0.015%, 0.035%, 0.077%, and 0.098%; aluminum content of 1.20%, 3.55%, 6.93%, and 9.74%; titanium content of 22.10%, 31.55%, 40.90%, and 49.40%;

[0019] 2) After the samples to be tested and the standard substances are crushed, particles smaller than 40 mesh are selected;

[0020] 3) Weigh 0.1600±0.0002g of a series of standard substances, place them in 300ml conical flasks, add 7ml sulfuric acid aqueous solution (volume ratio concentration 50%), heat at 190±5℃ until the reaction is complete, drop 3ml hydrogen peroxide (concentration 30%, analytical grade), add 8ml salt-nitric acid mixed acid aqueous solution (volume ratio concentration 40%, hydrochloric acid: nitric acid = 1:2), heat at 220±5℃ until the reaction is complete, cool and transfer to a 100ml 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 1.20 kW, the atomization pressure to 27.0 psi, the argon flow rate to 0.5 L / min, the analysis pump speed to 2.50 ml / min, the sample flushing time to 60 s, the integration time to 30 s for short wave and 10 s for long wave; element analysis line (nm): silicon 251.611, manganese 257.610, phosphorus 213.618, aluminum 396.152, titanium 336.121; 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 GSB03-1690-2004 and YSBC19605-05 to verify the accuracy of the test results of silicon, manganese, phosphorus, aluminum and titanium 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 ferrotitanium, characterized in that: The following steps are involved: 1) Selection of titanium-iron standard substances: Select 3-5 series of standard substances with known silicon 1.0%-6.0%, manganese 0.5%-3.0%, phosphorus 0.01%-0.10%, aluminum 1.0%-10.0%, and titanium 20.0%-50.0% element contents to form a concentration gradient; 2) Preparation method of solid samples: crush the sample to be tested and the selected titanium iron standard material into particles smaller than 40 mesh for determination; 3) Preparation of standard substance solution: weigh 0.1000-0.2000g of titanium iron standard substance, place them in 100-300ml conical flasks, add 5-10ml of 40%-60% sulfuric acid aqueous solution by volume, heat at 180-210°C until the reaction is complete, drop 2-5ml of 30% analytically pure hydrogen peroxide, add 5-10ml of 30%-60% hydrochloric acid-nitric acid mixed acid aqueous solution by volume, heat at 200-230°C until the reaction is complete, cool and transfer to an appropriate volumetric flask, dilute quantitatively with deionized water, and mix well; The volume ratio of hydrochloric acid to nitric acid in the hydrochloric acid-nitric acid mixed acid aqueous solution is 1:2; 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 5-10ml of 40%-60% sulfuric acid aqueous solution by volume, heat at 180-210°C until the reaction is complete, drop 2-5ml of 30% analytically pure hydrogen peroxide, add 5-10ml of 30%-60% hydrochloric acid-nitric acid mixed acid aqueous solution by volume, heat at 200-230°C until the reaction is complete, 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, aluminum, and titanium elements of the titanium-iron 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, aluminum, and titanium elements of the sample to be tested collected by the instrument is brought into the standard working curve to calculate the silicon, manganese, phosphorus, aluminum, and titanium content of the sample to be tested; 6) Select certified reference materials to verify the accuracy of the test results of silicon, manganese, phosphorus, aluminum and titanium content.

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