CN113504254A - Combined measurement method for nickel, copper, iron and cobalt elements in solid material in nickel pyrometallurgical process - Google Patents
Combined measurement method for nickel, copper, iron and cobalt elements in solid material in nickel pyrometallurgical process Download PDFInfo
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Abstract
The invention discloses a method for jointly measuring nickel, copper, iron and cobalt elements in solid materials in the nickel pyrometallurgical process, which adopts concentrated hydrochloric acid and concentrated nitric acid to heat and dissolve the solid materials in the nickel pyrometallurgical process at low temperature, and then adopts a Supermini type X-ray fluorescence spectrometer to measure the nickel, copper, iron and cobalt elements, thereby improving the safety in the sample processing process, overcoming the influence of potassium ions on the X-ray fluorescence analysis technology to measure the nickel, copper, iron and cobalt in the sample, solving the influence of particle effect and matrix effect on the sample measurement result, and ensuring the precision and result accuracy of the sample analysis; the Supermini X-ray fluorescence spectrum technology is successfully applied to solid materials for the first time, and a feasible way for quickly detecting the element content at low cost is found for solid material analysis; meanwhile, the simultaneous analysis of multiple elements by one-time film pressing is realized, the labor productivity is obviously improved, and the operating environment is improved.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, relates to a method for jointly measuring nickel, copper, iron and cobalt elements in solid materials in a nickel pyrometallurgical process, and particularly relates to a method for measuring the contents of nickel, copper, iron and cobalt in solid materials in a pyrometallurgical process such as high-nickel matte on a Supermini type X-ray fluorescence spectrometer.
Background
The method for measuring the major components of nickel, copper, iron and cobalt in the solid material in the nickel pyrometallurgy process has been a chemical analysis method for many years. Such as: ni is measured by an EDTA titration method or an indicative dimethylglyoxime spectrophotometry, Cu is measured by sodium thiosulfate titration, Fe is measured by a sulfosalicylic acid spectrophotometry, and Co is measured by a nitroso-red salt spectrophotometry or an atomic absorption spectrometry, but the analysis methods have the problems of long flow, multiple varieties of consumed chemical reagents and low working efficiency. With the continuous energy expansion of a production system and the reduction of post analysis personnel, the existing method cannot meet the time limit requirement of rapid analysis, and meanwhile, volatile substances are often used in the existing analysis method, so that the field operation environment is not satisfactory, the method is unfavorable for the occupational health of workers, the process detection means and method for optimizing samples are urgently needed, the analysis working efficiency is improved, and the operation environment is further improved.
In recent years, the application range of X fluorescence spectrum analysis in various industries is continuously expanded, and the X fluorescence spectrum analysis is widely applied to various fields such as metallurgy, geology, nonferrous materials, building materials, commodity inspection, environmental protection, sanitation and the like. In the early test, when the solid material in the nickel pyrometallurgical process is analyzed by X fluorescence spectrum, the powder tabletting technology has the defects that the surface of a sample wafer is rough, powder is easy to fall off, and an XRF instrument sample chamber is easy to pollute; part of samples have small adhesive force and can not be directly molded, and various adhesives are required to be added for molding; the granularity effect and the mineral effect cause the defects of poor detection precision, poor accuracy and the like. If the glass melting X-ray fluorescence method is adopted for measurement, a large amount of sulfur is contained in a sample, so that a platinum crucible is seriously corroded, and analysis cannot be carried out.
The Supermini X-ray fluorescence spectrometer has the advantages of good spectral peak resolution capability and good stability, and can be used for liquid analysis and solid sample analysis. However, when the solid material in the nickel pyrometallurgical process is measured on a Supermini type X-ray fluorescence spectrometer by adopting the existing sample dissolving mode (hydrochloric acid + nitric acid-potassium chlorate saturated solution), the problems that the working curves of nickel, copper, iron and cobalt in a sample cannot be drawn, the precision is poor, and the analysis result is greatly different from that of a chemical method occur.
Disclosure of Invention
The invention aims to solve the technical problem of element detection in solid materials in the nickel pyrometallurgical process, provides a method for jointly detecting nickel, copper, iron and cobalt elements in the solid materials in the nickel pyrometallurgical process,
so as to achieve the aim of multi-element joint measurement of the sample on a Supermini type X-ray fluorescence spectrometer and improve the analysis efficiency.
The purpose of the invention is realized by the following technical scheme: heating and dissolving solid materials in the pyrometallurgical process of nickel by adopting concentrated hydrochloric acid and concentrated nitric acid at low temperature, and then measuring nickel, copper, iron and cobalt elements by adopting a Supermini type X-ray fluorescence spectrometer; the method specifically comprises the following steps:
step one, weighing 0.2-0.6 nickel solid materials in the pyrometallurgical process, adding concentrated hydrochloric acid, heating at low temperature for dissolving, and continuing heating and concentrating to 3-5 mL;
step two, adding concentrated nitric acid into the concentrated solution obtained in the step one, heating at a low temperature for dissolving, continuously heating and concentrating to 3-5mL, cooling after completely dissolving salts, transferring into a volumetric flask, diluting with water to a scale, and uniformly mixing to obtain a solution to be measured;
and step three, preparing a sample of the solution to be detected by adopting a liquid compression mold, measuring the fluorescence intensity of the sample on a Supermini type X-ray fluorescence spectrometer, and calculating corresponding concentrations according to respective working curves of nickel, copper, iron and cobalt elements to obtain the content of each element in the solution to be detected.
Further, in the first step, the adding amount of the concentrated hydrochloric acid is 10-30 mL.
Further, in the second step, the adding amount of the concentrated nitric acid is 10-30 mL.
The invention researches the interference factor when the sample is digested by hydrochloric acid + nitric acid-potassium chlorate saturated solution, innovates the sample dissolving mode of solid materials in the nickel pyrometallurgical process such as nickelous matte and the like, and has the following beneficial effects:
1. the method adopts a sample dissolving mode of concentrated hydrochloric acid and concentrated nitric acid to dissolve the sample, innovatively dissolves the sample dissolving mode of solid materials in the pyrometallurgical process of nickel such as high-nickel matte and the like, improves the safety in the sample treatment process, overcomes the influence of potassium ions on the detection of nickel, copper, iron and cobalt in the sample by an X-ray fluorescence analysis technology, solves the influence of particle effect and matrix effect on the sample determination result, and ensures the precision and result accuracy of sample analysis.
2. The invention successfully applies the Supermini type X-ray fluorescence spectrum technology to the solid materials for the first time, finds a feasible, low-cost and quick effective way for detecting the content of elements for the analysis of the solid materials, provides scientific basis for establishing an analysis method of corresponding elements in other materials, and makes a quick analysis means more perfect.
3. The invention realizes the simultaneous analysis of multiple elements by one-time film pressing, solves the problems of multiple operation links, long flow and poor field operation environment of the original method, obviously improves the labor productivity and improves the operation environment.
Drawings
FIG. 1 is a graph showing the effect of potassium nitrate chlorate dosage on element content: a is the effect on nickel; b is the effect on copper; c is the effect on iron; d is the effect on cobalt;
FIG. 2 is a graph showing the effect of potassium chlorate dosage on element content: a is the effect on nickel; b is the effect on copper; c is the effect on iron; d is the effect on cobalt;
FIG. 3 is a graph showing the results of the interference test with potassium ions: a is the effect on nickel; b is the effect on copper; c is the effect on iron; d is the effect on cobalt;
FIG. 4 is a working curve of the elements in nickel sulfide cobalt of example 1: a is the working curve of nickel; b is a working curve of copper; c is the working curve of iron; d is the working curve of cobalt;
FIG. 5 is a comparison result chart of the analysis methods of the elements in nickel sulfide cobalt of example 1: a is a comparison result of a nickel analysis method; b is the comparison result of the copper analysis method; c is the comparison result of the analysis method of iron; d is the comparison result of the analysis method of cobalt;
FIG. 6 is a working curve of each element in the secondary nickelic matte of example 2: a is the working curve of nickel; b is a working curve of copper; c is the working curve of iron; d is the working curve of cobalt;
FIG. 7 is a working curve of each element in the nickel matte of example 3: a is the working curve of nickel; b is a working curve of copper; c is the working curve of iron; d is the working curve of cobalt;
fig. 8 is a working curve of each element in the high matte board of example 4: a is the working curve of nickel; b is a working curve of copper; c is the working curve of iron; d is the working curve of cobalt;
FIG. 9 is a graph showing the comparison results of the analysis methods of the elements in the high matte plate of example 4: a is a comparison result of a nickel analysis method; b is the comparison result of the copper analysis method; c is the comparison result of the analysis method of iron; d is the comparison result of the analysis method of cobalt;
FIG. 10 is the working curves of the elements in the anode slime of example 5: a is the working curve of nickel; b is a working curve of copper; c is the working curve of iron; d is the working curve of cobalt.
Detailed Description
The method for jointly measuring nickel, copper, iron and cobalt elements in the solid material in the nickel pyrometallurgical process is explained in detail below.
The establishment of the method comprises the research of interference ions, the selection of a solvent, the selection of the dosage of hydrochloric acid, the selection of the dosage of nitric acid and the selection of sample weighing, and is suitable for the selection of a sample dissolving method for determining the contents of nickel, copper, iron and cobalt in solid materials in the pyrometallurgical process of nickel, sulfur and the like.
The instrument used in the invention is as follows: supermini type X-ray fluorescence spectrometer. The sample measurement conditions are shown in Table 1.
TABLE 1 Supermini X-ray fluorescence spectrometer measurement conditions
The reagents used were: concentrated hydrochloric acid (. rho.1.19 g/mL); concentrated nitric acid (. rho.1.42 g/mL); nitric acid-potassium chlorate saturated solution.
First, study of interfering ions
Determining interference factors when the existing concentrated hydrochloric acid + nitric acid-potassium chlorate saturated solution is adopted for sample digestion.
Influence of the amount of concentrated hydrochloric acid
Weighing 6 parts of nickel cobalt sulfide sample, respectively adding different amounts of concentrated hydrochloric acid, covering a watch glass, heating to dissolve to 3-5mL, then respectively adding 25mL of nitric acid-potassium chlorate saturated solution, dissolving to 3-5mL, taking down and cooling, purging the watch glass and the cup wall with water, heating to completely dissolve salts, cooling, transferring into a 50mL volumetric flask, diluting with water to a scale, and shaking up. The intensities of nickel, copper, iron and cobalt in the sample were measured on a Supermini X-ray fluorescence spectrometer according to the above measurement conditions. After dissolution, 1.00mL of each sample was transferred to a 500mL triangular beaker, and the chloride ion content was measured, and the measurement results are shown in Table 2.
TABLE 2 hydrochloric acid dosage selection
The data in Table 2 show that the dosage of hydrochloric acid is 4-25 mL, the sample is completely dissolved, the fluorescence intensities of the nickel, copper, iron and cobalt are determined to be consistent, and the residual chloride ions after sample dissolution are basically consistent, because the chloride ions are basically completely volatilized in the process of dissolving the sample by the hydrochloric acid, the determination of the nickel, copper, iron and cobalt in the sample is not interfered.
Influence of amount of potassium nitrate chlorate
Weighing 6 parts of nickel cobalt sulfide sample, respectively adding 20mL of concentrated hydrochloric acid, covering a watch glass, heating to dissolve to 3-5mL, then respectively adding different amounts of nitric acid-potassium chlorate saturated solution, dissolving to 3-5mL, taking down and cooling, purging the watch glass and the cup wall with water, heating to completely dissolve salts, cooling, transferring into a 50mL volumetric flask, diluting with water to a scale, shaking up, and determining on a Supermini X-ray fluorescence spectrometer according to the determination conditions, wherein the result is shown in figure 1.
The data in figure 1 show that the addition of the saturated solution of nitric acid and potassium chlorate influences the determination of nickel, copper, iron and cobalt in the sample.
Interference test of potassium chlorate
The nitric acid-potassium chlorate saturated solution contains nitric acid and potassium chlorate, and in the previous liquid sample test, the influence of the nitric acid on the sample result is small, and the influence of the potassium chlorate on fluorescence analysis needs to be examined. 6 samples (Ni 6g/L, Cu 0.060g/L, Co 0.10.10 g/L, Fe 0.6.6 g/L) were prepared respectively, and different amounts of saturated potassium chlorate solution (74 g/L) were added into a 50mL volumetric flask, diluted to the mark with water and shaken up. The results are shown in FIG. 2.
The data in FIG. 2 show that the addition of saturated solution of potassium chlorate (74 g/L) affects the determination of nickel, copper, iron and cobalt in the sample.
Interference test of potassium ion
Because potassium chloride and oxygen are generated after the potassium chlorate solution is heated, an interference test needs to be carried out on potassium ions. 6 samples (Ni 6g/L, Cu 0.060g/L, Co 0.10.10 g/L, Fe 0.6 g/L) are prepared respectively, potassium ion solutions (50 g/L) with different amounts are added into a 50mL volumetric flask, diluted to the scale with water and shaken up. The results are shown in FIG. 3.
The data in FIG. 3 illustrates that the addition of potassium ions interferes with the determination of nickel, copper, iron, cobalt in the sample.
Second, sample dissolving mode selection
Selection of solvents
Potassium chloride and oxygen are generated after the potassium chlorate solution is heated, and potassium ions interfere the determination of nickel, copper, iron and cobalt in the sample. Therefore, the sample digestion cannot be performed with a nitric acid-potassium chlorate saturated solution. 2 samples of nickel cobalt sulfide were selected (1)# Ni 66.60%、Cu 0.71%、Co 7.53%、Fe 1.10%，2# 3 parts of each of Ni 62.84%, Cu 0.60%, Co 6.78%, and Fe 1.00%), and three different solvents were used to dissolve the samples, and the results are shown in Table 3.
TABLE 3 selection of solvents
Each part of the dissolved sample in the first scheme has floating black slag, and the dissolved samples in the second scheme and the third scheme are transparent and clear without black slag. The X-ray fluorescence spectrometry is adopted to measure nickel, copper, iron and cobalt in the samples dissolved in three different sample dissolving modes, and the data in the table 2 shows that the X-ray fluorescence spectrometry is adopted to measure the nickel, copper, iron and cobalt in the samples, and the results of the samples dissolved in the scheme I and the scheme III are lower; the results of the sample dissolved in the second protocol are consistent with the original results. Thus, the present invention identifies the use of hydrochloric acid + nitric acid as the solvent to dissolve the sample.
Selection of concentrated hydrochloric acid dosage
Weighing 5 parts of nickel cobalt sulfide samples, respectively adding different amounts of concentrated hydrochloric acid, fixing the dosage of concentrated nitric acid to be 20mL, dissolving at low temperature to be 3-5mL, taking down and cooling, blowing a watch dish and a cup wall with water, heating to completely dissolve salts, taking down and cooling, transferring into a 50mL volumetric flask, diluting with water to a scale, mixing uniformly, measuring on a Supermini X-ray fluorescence spectrometer according to the measuring conditions, and obtaining the result shown in Table 4.
TABLE 4 selection of the amount of concentrated hydrochloric acid used
The data in Table 4 show that the strength is consistent when the concentrated hydrochloric acid is used in an amount of 10-30 mL.
Selection of concentrated nitric acid dosage
Weighing 5 parts of nickel cobalt sulfide sample, respectively adding 20mL of concentrated hydrochloric acid, dissolving different amounts of concentrated nitric acid to 3-5mL, taking down and cooling, washing a watch dish and a cup wall with water, heating to completely dissolve salts, taking down and cooling, transferring into a 50mL volumetric flask, diluting with water to a scale, mixing uniformly, and measuring on a Supermini type X-ray fluorescence spectrometer according to the measuring conditions, wherein the result is shown in Table 5.
TABLE 5 selection of concentrated nitric acid dosage
The data in Table 5 show that the dosage of the concentrated nitric acid is between 10 and 30mL, and the measured intensity is consistent.
Interference test
The test result shows that the determination of 3mgCu, 30mgFe and 5mgCo is not influenced by 400mg of Ni; 60mg of Fe did not affect 3mMeasurement of gCu, 250mgNi and 5 mgCo; the measurement of 250mgNi, 30mgFe and 5mgCo is not influenced by 100mg of Cu; 304mg of Cl-The measurement of 100mgCo is not influenced; 922mg of SO4 2-The measurement of 500mgNi and 500mgCo is not affected.
Selection of sample weighing amount
Selecting the same nickel cobalt sulfide sample (Ni 66.60%, Cu 0.71%, Fe 7.53% and Co 1.10%), weighing different samples, putting the samples into nine 500mL beakers, wetting the beakers with water, respectively adding 20mL concentrated hydrochloric acid, covering a watch glass, heating and dissolving the samples to 3-5mL at low temperature, taking down and cooling the beaker, adding 20mL concentrated nitric acid, dissolving the samples to 3-5mL at low temperature, taking down and cooling the beaker and the cup wall, flushing the watch glass and the cup wall with water, heating to completely dissolve salts, taking down and cooling the beaker, transferring the beaker into a 50mL volumetric flask, diluting the beaker with water to a scale, and uniformly mixing the beaker and the beaker. The sample was prepared using a liquid stamp, and the fluorescence intensity was measured on an X-ray fluorescence spectrometer according to the operating conditions of the instrument, the results of which are shown in Table 6.
TABLE 6 selection of the weighing amounts
The data in Table 6 show that the coexisting ions did not interfere with the measurement, and the sample weight was 0.2000g to 0.6000 g.
The present invention will be further described with reference to the following examples.
In each example, the amount of the sample was 0.5g, the amount of concentrated hydrochloric acid was 20mL, and the amount of concentrated nitric acid was 20 mL.
Example 1
Weighing a plurality of nickel cobalt sulfide samples of 0.500g (accurate to 0.0001 g), respectively placing the samples in 500mL beakers, wetting with water, adding 20mL concentrated hydrochloric acid, covering a watch glass, heating and dissolving the samples to a small volume at a low temperature, then adding 20mL concentrated nitric acid, heating and dissolving the samples to 3-5mL at a low temperature, taking down and cooling, flushing the watch glass and the cup wall with water, heating to completely dissolve salts, taking down and cooling, transferring the samples into a 50mL volumetric flask, diluting the samples to a scale with water, mixing the samples uniformly, and preparing the samples by adopting a liquid compression mold.
The calibration of the standard sample was performed. Selecting a plurality of nickel sulfide cobalt samples with different contents, and adopting a chemical method for value setting, wherein the method for value setting is shown in table 7.
TABLE 7 chemical rating method
And drawing a working curve of the sample. Selecting a plurality of nickel sulfide cobalt samples with different contents, preparing a test solution by adopting a test method, drawing a working curve, and showing the working curve in figure 4.
Precision tests were performed and the data are shown in table 8.
TABLE 8 precision test
The RSD of nickel, copper, iron and cobalt is respectively 0.47%, 4.16%, 1.01% and 1.69%, which completely meet the requirements of the analysis method.
An accuracy verification test is carried out, a chemical method and a fluorescence method are adopted for comparison, and the comparison result is shown in a line chart 5.
The comparison of the method of fig. 5 with the line graph shows that the measurement result of the X-ray fluorescence spectrum is consistent with the original result and meets the analysis requirements.
Example 2
Weighing 0.500g (accurate to 0.0001 g) of secondary nickelic matte samples with different element contents, respectively placing the samples in 500mL beakers, wetting with water, adding 20mL of concentrated hydrochloric acid, covering the watch glass, heating at low temperature to dissolve the samples to 3-5mL, then adding 20mL of concentrated nitric acid, heating at low temperature to dissolve the samples to 3-5mL, taking down and cooling, flushing the watch glass and the cup wall with water, heating to completely dissolve the salts, taking down and cooling, transferring the samples into a 50mL volumetric flask, diluting the samples to scale with water, mixing the samples uniformly, and preparing the samples by adopting a liquid compression mold.
And (5) drawing a working curve of the sample. Selecting 15 secondary high-nickel matte with different contents, carrying out value setting by adopting a chemical method, and drawing a fluorescence method working curve. The operating curve is shown in figure 6.
The precision tests are carried out, the RSD of nickel, copper, iron and cobalt is respectively 0.72%, 0.56%, 1.45% and 2.07%, and the requirement of the analysis method is completely met.
Accuracy verification tests were performed and the data are shown in table 9.
TABLE 9 control test for secondary nickeliferous matte chemical method and fluorometric method
Table 9 shows that the results of the X-ray fluorescence spectroscopy are consistent with the original results and meet the analysis requirements.
Example 3
Weighing 0.500g (accurate to 0.0001 g) of nickelic matte samples with different element contents, respectively placing the samples in 500mL beakers, wetting with water, adding 20mL of concentrated hydrochloric acid, covering the watch glass, heating at low temperature to dissolve the samples to a small volume, then adding 20mL of concentrated nitric acid, heating at low temperature to dissolve the samples to a small volume, taking down and cooling, purging the watch glass and the cup wall with water, heating to completely dissolve salts, taking down and cooling, transferring the samples into a 50mL volumetric flask, diluting with water to a scale, mixing uniformly, and preparing the samples by liquid compression molding.
And (5) drawing a working curve of the sample. Selecting a plurality of high-nickel matte with different contents, carrying out value setting by adopting a chemical method, and drawing a working curve of a fluorescence method. The operating curve is shown in figure 7.
The precision tests are carried out, the RSD of nickel, copper, iron and cobalt is respectively 0.53%, 0.46%, 2.87% and 1.72%, and the requirement of the analysis method is completely met.
Accuracy verification tests were performed and the data are shown in table 10.
TABLE 10 control test for measurement of nickel-matte by chemical method and fluorometric method
Table 10 shows that the results of the X-ray fluorescence spectroscopy are consistent with the original results and satisfy the analysis requirements.
Example 4
Weighing 0.500g (accurate to 0.0001 g) of high sulfonium plate samples with different element contents, respectively placing the high sulfonium plate samples in 500mL beakers, wetting with water, adding 20mL of concentrated hydrochloric acid, covering the watch cups, heating at low temperature to dissolve the high sulfonium plate samples into small volumes, then adding 20mL of concentrated nitric acid, heating at low temperature to dissolve the high sulfonium plate samples into small volumes, taking down and cooling, purging the watch cups and the cup walls with water, heating to completely dissolve salts, taking down and cooling, transferring the high sulfonium plate samples into 50mL volumetric flasks, diluting with water to scale, uniformly mixing, and pressing the high sulfonium plate samples into samples by liquid molds.
And (5) drawing a working curve of the sample. Selecting a plurality of high matte boards with different contents, fixing values by a chemical method, and drawing a working curve. The operating curve is shown in figure 8.
The precision tests are carried out, the RSD of nickel, copper, iron and cobalt is respectively 0.46%, 1.41%, 2.41% and 1.43%, and the requirement of the analysis method is completely met.
An accuracy verification test is carried out, a chemical method and a fluorescence method are adopted for comparison, and the comparison result is shown in a line graph 9.
The comparison of the method of fig. 9 with the line graph shows that the X-ray fluorescence spectrum measurement result is consistent with the original result and meets the analysis requirements.
Example 5
Weighing a plurality of anode mud samples of 0.500g (accurate to 0.0001 g) with different element contents, respectively placing the anode mud samples in 500mL beakers, wetting with water, adding 20mL concentrated hydrochloric acid, covering the watch glass, heating at low temperature to dissolve the anode mud samples to a small volume, then adding 20mL concentrated nitric acid, heating at low temperature to dissolve the anode mud samples to a small volume, taking down and cooling, purging the watch glass and the cup wall with water, heating to completely dissolve salts, taking down and cooling, transferring the anode mud samples into a 50mL volumetric flask, diluting with water to a scale, mixing uniformly, and preparing the anode mud samples by adopting a liquid compression mold.
And (5) drawing a working curve of the sample. Selecting a plurality of anode slimes with different contents, fixing values by a chemical method, and drawing a working curve. The results are shown in FIG. 10.
The precision tests are carried out, the RSD of nickel, copper, iron and cobalt is respectively 0.44%, 1.77%, 1.55% and 3.02%, and the requirement of the analysis method is completely met.
Accuracy verification tests were performed and the data are shown in table 11.
TABLE 11 comparative test for chemical and fluorometric determination of anode sludge
The data in table 11 show that the X-ray fluorescence spectroscopy measurement result matches the original result and meets the analysis requirements.
Claims (5)
1. A method for jointly measuring nickel, copper, iron and cobalt elements in solid materials in a nickel pyrometallurgical process is characterized in that the solid materials in the nickel pyrometallurgical process are dissolved by heating concentrated hydrochloric acid and concentrated nitric acid at low temperature, and then a Supermini type X-ray fluorescence spectrometer is used for measuring the nickel, copper, iron and cobalt elements.
2. The method for jointly measuring nickel, copper, iron and cobalt elements in the solid material in the nickel pyrometallurgical process according to claim 1, wherein the method for jointly measuring nickel, copper, iron and cobalt elements comprises the following steps:
step one, weighing 0.2-0.6g of solid material in the nickel pyrometallurgical process, adding concentrated hydrochloric acid, heating at low temperature for dissolving, and continuing heating and concentrating to 3-5 mL;
step two, adding concentrated nitric acid into the concentrated solution obtained in the step one, heating at a low temperature for dissolving, continuously heating and concentrating to 3-5mL, cooling after completely dissolving salts, transferring into a volumetric flask, diluting with water to a scale, and uniformly mixing to obtain a solution to be measured;
and step three, preparing a sample of the solution to be detected by adopting a liquid compression mold, measuring the fluorescence intensity of the sample on a Supermini type X-ray fluorescence spectrometer, and calculating corresponding concentrations according to respective working curves of nickel, copper, iron and cobalt elements to obtain the content of each element in the solution to be detected.
3. The method for jointly measuring nickel, copper, iron and cobalt elements in the solid material in the nickel pyrometallurgical process according to claim 2, wherein in the first step, the addition amount of the concentrated hydrochloric acid is 10-30 mL.
4. The method for jointly measuring nickel, copper, iron and cobalt elements in the solid material in the nickel pyrometallurgical process according to claim 3, wherein in the second step, the addition amount of the concentrated nitric acid is 10-30 mL.
5. The method for jointly measuring nickel, copper, iron and cobalt elements in the solid material in the nickel pyrometallurgical process according to any one of claims 1 to 4, wherein in the third step, the measurement conditions of the Supermini type X-ray fluorescence spectrometer are as follows:
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