1. A method for measuring the sodium content in a slagging agent is characterized in that,

a. decomposing a slagging agent sample by aqua regia under the microwave condition of 200-220 ℃, dissolving the slagging agent sample in water, filtering to remove insoluble substances to obtain a target solution, and adding a potassium ion solution with the content of 0.01mg/mL into the target solution;

b. selecting five parts of 2mL coloring liquid, sequentially adding 2-10 mL of target solution into the coloring liquid, and adding water to dilute the target solution to 200mL to obtain a solution to be detected;

c. selecting the spectral line wavelength of the analytical element sodium as 589.5 as an analytical line;

d. measuring the absorbance of the solution to be measured by adopting an inductively coupled plasma atomic emission spectrometry, and making a curve;

e. sodium concentration was obtained from curve analysis.

2. The method for determining the sodium content in the slagging agent according to claim 1, wherein: in the step a, aqua regia is hydrochloric acid and nitric acid according to the volume ratio: 3: 1.

3. The method for determining the sodium content in the slagging agent according to claim 1, wherein: the coloring liquid in the step b is a single nickel salt coloring liquid which has electrolysis property.

4. The method for determining the sodium content in the slagging agent according to claim 1, wherein: and d, in the step d, the flow of plasma gas in the inductively coupled plasma atomic emission spectrometry is 15L/min.

5. The method for determining the sodium content in the slagging agent according to claim 1, wherein: the experimental water in step b is deionized water.

Background

With the development of the steel-making industry in China and the increasing shortage of international iron ore resources, the usage amount of waste steel in the steel-making process is increased continuously, steel plants generally add different heating agents and a part of slag melting agents into a furnace according to smelting requirements at the initial stage of smelting, the heating agents are high-grade ferrosilicon, silicon-carbon synthetic balls and the like, and the conventional slag melting agents comprise magnesium oxide-containing slag-making materials such as light-burned magnesium balls and light-burned dolomite. The heat generating agent generally contains a certain amount of ferrosilicon, the production cost of the ferrosilicon is high, and the ferrosilicon can bring serious environmental load, and the slagging agent is a material with high slagging and slagging speed. Various reagents are adopted to dissolve reagents such as nitric acid, perchloric acid, hydrofluoric acid, strontium chloride and the like, the dissolving steps are complicated, the analysis period is long, and the labor intensity is high.

At present, elements in the slagging agent are basically detected by ICP-AES.

However, the detection method has the disadvantages of troublesome detection steps, slow reaction speed and low precision.

Disclosure of Invention

In order to solve the problems, the technical scheme of the invention is as follows: the slag former powder sample is simply and rapidly dissolved by adopting two reagents, and the measurement is carried out by utilizing an inductively coupled plasma emission spectrometer.

A method for measuring the sodium content in a slagging agent comprises the following steps:

a. decomposing a slagging agent sample by aqua regia under the microwave condition of 200-220 ℃, dissolving the slagging agent sample in water, filtering to remove insoluble substances to obtain a target solution, and adding a potassium ion solution with the content of 0.01mg/mL into the target solution;

b. selecting five parts of 2mL coloring liquid, sequentially adding 2-10 mL of target solution into the coloring liquid, and adding water to dilute the target solution to 200mL to obtain a solution to be detected;

c. selecting the spectral line wavelength of the analytical element sodium as 589.5 as an analytical line;

d. measuring the absorbance of the solution to be measured by adopting an inductively coupled plasma atomic emission spectrometry, and making a curve chart;

e. and analyzing according to the graph to obtain the sodium concentration.

Preferably, aqua regia in the step a is hydrochloric acid and nitric acid according to the volume ratio: 3: 1.

Preferably, the coloring liquid in the step b is a mono-nickel salt coloring liquid, which has electrolytic properties.

Preferably, the flow rate of plasma gas in the inductively coupled plasma atomic emission spectrometry in the step d is 15L/min.

Preferably, the experimental water in step b is deionized water.

The method has the advantages of high analysis speed, wide dynamic linear range and higher precision, and can be widely applied to modern metallurgical analysis.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a flow chart of the method for determining the sodium content in the slagging agent according to the present invention.

Detailed Description

The main instruments and parameters used in the examples were as follows:

optima-8000DV inductively coupled plasma atomic emission spectrometer: an acid-etching resistant atomizer and an argon purifier;

when the device is used, a solution to be detected is sprayed into fog through the acid-corrosion-resistant atomizer, enters flame along with a carrier, and is dissociated into ground state ions in the flame, when the inductively coupled plasma atomic emission spectrometer radiates characteristic wavelength light of an element to be detected to pass through the flame, the characteristic wavelength light is absorbed by the flame, and under a certain condition, the change of the light intensity of the characteristic wavelength and the concentration of the ground state atoms of the element to be detected in the flame have a quantitative relation, so that the quantitative relation is formed between the change of the light intensity of the characteristic wavelength and the concentration of the ground state atoms of the element to be detected in a sample, and the percentage content of the element in the solution to be detected can be calculated through a standard addition method.

The first embodiment is as follows:

weighing 0.1g of a slagging agent sample in a 250mL beaker, adding 20mL of aqua regia, adding a potassium ion solution with the content of 0.01mg/mL (the high-concentration ion peak can be prevented from covering a low-concentration ion peak and being not detected), slightly shaking, putting the sample on a microwave heating device for heating, heating by adopting microwave heating compared with the traditional heating plate, wherein the microwave heating has better decomposition capacity so as to improve the uniformity degree of decomposition and ensure the completeness of the decomposition, the microwave temperature is controlled at 200 ℃, the volume is kept unchanged, taking down and cooling after boiling for about 15min, dissolving the sample in a 500mL volumetric flask, shaking uniformly, and filtering a test solution to a 100mL volumetric flask by using medium-speed filter paper for later use, wherein the solution is called as a target solution.

Selecting five parts of 2mL coloring liquid, sequentially adding 2-10 mL of target solution into the coloring liquid, and adding water to dilute the target solution to 200mL to obtain a solution to be detected;

specifically, five parts of 2mL electrolytic mono-nickel salt coloring solution are selected, specifically, the first part is not added with the target solution, and the second part to the fifth part are respectively added with 2mL, 5mL, 8mL and 10 mL;

measuring 1.00mL, 2.00mL, 4.00mL, 6.00mL and 8.00mL respectively, measuring to 5 conical flasks added with 10mL of water, adding 20mL of aqua regia respectively, taking down, cooling, and shaking to a volume of 100 mL. The concentrations are respectively 10mg/L, 20mg/L, 40mg/L, 60mg/L and 80 mg/L;

selecting the wavelength of a spectral line of an analytical element sodium as 589.5 as an analytical line, obtaining the analytical line through experiments, carrying out detection on the analytical line with the wavelength of 589.5 to obtain the highest accuracy, measuring the absorbance of a solution to be detected by adopting an inductively coupled plasma atomic emission spectrometry, and making a curve;

and (3) measuring the standard solution series according to the working conditions set by the instrument, and drawing a calibration curve by taking the mass concentration of the Na element as an abscissa and the emission intensity as an ordinate. The linear range, linear regression equation and correlation coefficient of the calibration curve are shown in table 1.

TABLE 1 calibration Curve first off parameters

Element(s)	Analysis line/nm	Linear range mg/L	Correlation coefficient
				Na	589.5	2-20mg/L	0.9991

The content of sodium in the slag melting agent is measured according to a test method, the precision is examined, the results are shown in the following table 2, and the relative deviation of the results calculated and measured in the table 2 is less than 0.5 percent

TABLE 2 precision of analytical results

Element(s)	Average value of measurement results x (mg/L)	Standard deviation s (%)	Relative standard deviation RSD (%)
				Na	15.14	0.072	0.47

Therefore, the RSD of the sample measured by the method is less than 5 percent, and the precision is higher.

In ICP-AES, there is less chemical interference due to the higher temperature of the plasma, the main ones being physical and spectral interference. The physical interference can be eliminated by adopting a matrix matching method and an internal standard method, namely, the difference of test data caused by different matrixes is eliminated by adding hydrochloric acid and nitric acid into a standard solution, and the interference caused by the fluctuation of the sampling amount and the atomization efficiency of an atomizer due to the fluctuation of argon gas and the fluctuation of conditions such as instrument environment and the like is eliminated by the internal standard method. Spectral interference can be avoided by selecting less interfering spectral lines and selecting appropriate background subtraction points.

Example two

Weighing 0.1g of a slagging agent sample in a 250mL beaker, adding 20mL of aqua regia, adding a potassium ion solution with the content of 0.01mg/mL (the high-concentration ion peak can be prevented from covering the low-concentration ion peak so that the low-concentration ion peak cannot be detected), slightly shaking, putting the sample on a microwave heating device for heating, heating by adopting microwave heating compared with the traditional heating plate, wherein the microwave heating has better decomposition capacity so as to improve the uniformity degree of decomposition and ensure the completeness of the decomposition, the microwave temperature is controlled at 220 ℃, the volume is kept unchanged, taking down the sample for cooling after boiling for about 15min, dissolving the sample in a 500mL volumetric flask, shaking up the sample, and filtering the sample solution into a 100mL volumetric flask by using filter paper for later use, wherein the sample solution is called as a target solution.

Selecting five parts of 2mL coloring liquid, sequentially adding 2-10 mL of target solution into the coloring liquid, and adding water to dilute the target solution to 200mL to obtain a solution to be detected;

specifically, five parts of 2mL electrolytic mono-nickel salt coloring solution are selected, specifically, the first part is not added with the target solution, and the second part to the fifth part are respectively added with 2mL, 5mL, 8mL and 10 mL;

measuring 1.00mL, 2.00mL, 4.00mL, 6.00mL and 8.00mL respectively, measuring to 5 conical flasks added with 10mL of water, adding 20mL of aqua regia respectively, taking down, cooling, and shaking to a volume of 100 mL. The concentrations are respectively 10mg/L, 20mg/L, 40mg/L, 60mg/L and 80 mg/L;

selecting the wavelength of a spectral line of an analytical element sodium as 589.5 as an analytical line, obtaining the analytical line through experiments, carrying out detection on the analytical line with the wavelength of 589.5 to obtain the highest accuracy, measuring the absorbance of a solution to be detected by adopting an inductively coupled plasma atomic emission spectrometry, and making a curve;

and (3) measuring the standard solution series according to the working conditions set by the instrument, and drawing a calibration curve by taking the mass concentration of the Na element as an abscissa and the emission intensity as an ordinate. The linear range, linear regression equation and correlation coefficient of the calibration curve are shown in table 3.

TABLE 3 calibration Curve first off parameters

Element(s)	Analysis line/nm	Linear range mg/L	Correlation coefficient
				Na	589.5	2-20mg/L	0.9991

The content of sodium in the slag melting agent is measured according to a test method, the precision is examined, the results are shown in the following table 2, and the relative deviation of the results calculated and measured in the table 4 is less than 0.5 percent

TABLE 4 precision of analytical results

Element(s)	Average value of measurement results x (mg/L)	Standard deviation s (%)	Relative standard deviation RSD (%)
				Na	15.12	0.0711	0.45

Therefore, the RSD of the sample measured by the method is less than 5 percent, and the precision is higher.

Example two

Weighing 0.1g of a slagging agent sample in a 250mL beaker, adding 20mL of aqua regia, adding a potassium ion solution with the content of 0.01mg/mL (the high-concentration ion peak can be prevented from covering the low-concentration ion peak so that the low-concentration ion peak cannot be detected), slightly shaking, putting the sample on a microwave heating device for heating, heating by adopting microwave heating compared with the traditional heating plate, wherein the microwave heating has better decomposition capacity so as to improve the uniformity degree of decomposition and ensure the completeness of the decomposition, the microwave temperature is controlled at 220 ℃, the volume is kept unchanged, taking down the sample for cooling after boiling for about 15min, dissolving the sample in a 500mL volumetric flask, shaking up the sample, and filtering the sample solution into a 100mL volumetric flask by using filter paper for later use, wherein the sample solution is called as a target solution.

Selecting five parts of 2mL coloring liquid, sequentially adding 2-10 mL of target solution into the coloring liquid, and adding water to dilute the target solution to 200mL to obtain a solution to be detected;

specifically, five parts of 2mL electrolytic mono-nickel salt coloring solution are selected, wherein the first part is not added with the target solution, and the second part to the fifth part are respectively added with 3mL, 4mL, 7mL and 9 mL;

respectively measuring 1.00mL, 2.00mL, 4.00mL, 6.00mL and 8.00mL to 5 conical flasks added with 10mL of water, respectively adding 20mL of aqua regia, taking down and cooling, fixing the volume to 100mL of volumetric flasks, and shaking up to obtain concentrations of 10mg/L, 20mg/L, 40mg/L, 60mg/L and 80 mg/L;

selecting the wavelength of a spectral line of an analysis element sodium as 589.5 as an analysis line, measuring the absorbance of the solution to be measured by adopting an inductively coupled plasma atomic emission spectrometry, and making a curve;

and (3) measuring the standard solution series according to the working conditions set by the instrument, and drawing a calibration curve by taking the mass concentration of the Na element as an abscissa and the emission intensity as an ordinate. The linear range, linear regression equation and correlation coefficient of the calibration curve are shown in table 5.

TABLE 5 calibration Curve first off parameters

Element(s)	Analysis line/nm	Linear range mg/L	Correlation coefficient
				Na	589.5	2-20mg/L	0.9991

The content of sodium in the slag melting agent is measured according to a test method, the precision is examined, the results are shown in the following table 2, and the relative deviation of the results calculated and measured in the table 6 is less than 0.5 percent

TABLE 6 precision of analytical results

Element(s)	Average value of measurement results x (mg/L)	Standard deviation s (%)	Relative standard deviation RSD (%)
				Na	15.12	0.0711	0.45

Therefore, the RSD of the sample measured by the method under the condition that the temperature is 220 ℃ is smaller and has higher precision.

The invention has been described in an illustrative manner, and it is to be understood that the invention is not limited to the precise form disclosed, and that various insubstantial modifications of the inventive concepts and solutions, or their direct application to other applications without such modifications, are intended to be covered by the scope of the invention.