Method for detecting content of indium element in zinc and copper concentrate

Abstract

The invention relates to a method for detecting the content of an indium element in zinc and copper concentrates. The content detection method comprises the following steps: adding an indium-containing zinc and copper concentrate sample and sodium peroxide into a corundum crucible, heating and melting, adding deionized water and hydrochloric acid to completely separate out the zinc and copper concentrate sample, and centrifuging after volume metering to obtain a to-be-detected solution; and setting working parameters of the inductively coupled plasma emission spectrometer, drawing an indium standard working curve, detecting the intensity of the solution to be detected, and calculating the content value of the indium element on the indium standard working curve according to the intensity value.

Description

Technical Field

[0001] The present application relates to the technical field of nonferrous metal smelting, and in particular to a method for detecting the content of indium in zinc and copper concentrates. Background Art

[0002] In the analysis and detection of non-ferrous metal ore components, indium is one of the precious metals. The determination methods of indium in non-ferrous metal ores include atomic absorption method, etc. The atomic absorption method requires the addition of hydrobromic acid, hydrochloric acid, nitric acid, etc. to dissolve the sample, and the volatilization of the acid causes certain pollution to the environment. It has certain harm to the human body. The sensitivity of indium to atomic absorption is low when determining indium, and the indium lamp is unstable after a period of use during the determination, and the replacement frequency is high.

[0003] A company in Yunnan needs to analyze the indium content in mining, ore dressing, geological exploration, experimental samples, etc. Indium content ≥450g / t needs to be priced. The atomic absorption analysis method is used to determine the indium content in zinc and copper concentrates. The operation is cumbersome and time-consuming. When hydrochloric acid and nitric acid dissolve the samples, they evaporate into the air, causing environmental pollution. Hydrobromic acid will produce certain harm to the human body.

[0004] Therefore, it is necessary to provide a method for detecting the indium content with simple operation and high sensitivity. Summary of the invention

[0005] In order to solve or partially solve the problems existing in the related art, the present application provides a method for detecting the content of indium in zinc and copper concentrates. The detection method can sensitively detect the content of indium in zinc and copper concentrates.

[0006] The present application provides a method for detecting the content of indium in zinc and copper concentrates, comprising the following steps:

[0007] S1: Spread sodium peroxide on the bottom of the reaction container, place the zinc and copper concentrate samples containing indium on the sodium peroxide, and then cover them with sodium peroxide;

[0008] S2: continuously heating the reaction container of step S1 at the initial temperature to a preset temperature, and then cooling the reaction container to room temperature;

[0009] S3: placing the reaction container of step S2 into a container filled with deionized water for leaching, continuously adding hydrochloric acid, and continuously stirring until all the zinc and copper concentrate samples in the reaction container are removed; fixing the obtained solution to volume and then centrifuging to obtain a test solution;

[0010] S4: Prepare standard solutions of different concentrations according to the indium content in the zinc and copper concentrates, put each standard solution into an inductively coupled plasma emission spectrometer, measure the intensity of each standard solution, and draw an indium standard working curve with the standard solution concentration as the horizontal axis and the corresponding intensity as the vertical axis;

[0011] The analytical line wavelength of indium is 410.176nm;

[0012] The operating parameters of the inductively coupled plasma emission spectrometer were: RF power 1250 W, cooling gas 13 L / min, argon (purity 99.99%) flow rate, carrier gas 0.60 L / min; reading time 5 s;

[0013] S6: placing the solution to be tested in step S3 into an inductively coupled plasma emission spectrometer to obtain the intensity of the solution to be tested, and calculating the indium content value on an indium standard working curve according to the intensity value.

[0014] Optionally, in step S1, the mass ratio of sodium peroxide to indium zinc and copper concentrate samples is 1.5:0.15.

[0015] Optionally, in step S2, the initial temperature is 650°C; the preset temperature is 700°C, and the melting time after heating to the preset temperature is 5 minutes.

[0016] Optionally, in step S3, the mass fraction of hydrochloric acid is 36.5%.

[0017] Optionally, in step S3, the temperature of the deionized water is 50-60°C.

[0018] Optionally, in step S5 and step S6, the testing method is axial observation.

[0019] Optionally, the reaction vessel is a corundum crucible.

[0020] The detection mechanism of this technical solution is: the sample is melted at high temperature with sodium peroxide to oxidize all heavy metals to the highest valence state, and then the melt is leached with deionized water and acidified. The metal elements exist in the solution in the form of ions, and the solution is introduced into ICP-OES to determine the content of indium in zinc and copper concentrates.

[0021] The technical solution provided by this application may have the following beneficial effects:

[0022] 1) This method is simple to operate, can quickly determine the indium content in zinc and copper concentrates, effectively improve the detection efficiency of indium results in zinc and copper concentrates, the detection process has low requirements on equipment, the test results are reliable and stable, and no expensive auxiliary reagents are required.

[0023] 2) In this application, the analytical line wavelength of indium element is set to 410.176nm, and the operating parameters of the inductively coupled plasma emission spectrometer are: RF power 1250W, cooling gas 13L / min, argon (purity 99.99%) flow rate, carrier gas 0.60L / min; reading time 5s, which can sensitively and accurately detect the content of indium element in zinc and copper concentrates.

[0024] It should be understood that the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the present application. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] The above and other objects, features and advantages of the present application will become more apparent through a more detailed description of exemplary embodiments of the present application in conjunction with the accompanying drawings, wherein the same reference numerals generally represent the same components in the exemplary embodiments of the present application.

[0026] Figure 1 It is the spectrum line diagram corresponding to the low point of indium element shown in this application;

[0027] Figure 2 It is the spectrum line diagram corresponding to the high point of indium element shown in this application;

[0028] Figure 3 It is a schematic diagram of the standard working curve of indium shown in this application. DETAILED DESCRIPTION

[0029] The embodiments of the present application will be described in more detail below with reference to the accompanying drawings. Although the embodiments of the present application are shown in the accompanying drawings, it should be understood that the present application can be implemented in various forms and should not be limited by the embodiments described herein. On the contrary, these embodiments are provided to make the present application more thorough and complete, and to fully convey the scope of the present application to those skilled in the art.

[0030] Example 1

[0031] A method for detecting the content of indium in zinc and copper concentrates comprises the following steps:

[0032] S1: Weigh 0.6g of sodium peroxide and spread it on the bottom of the corundum crucible, then weigh 0.1g-0.15g of zinc and copper concentrate samples containing indium that have passed through a 200-mesh sieve and place them on the sodium peroxide and mix well. Then weigh 0.6g of sodium peroxide and cover the indium-containing ore sample;

[0033] S2: Place the corundum crucible in a 650°C box-type resistance furnace for melting. When the temperature rises to 700°C, melt for 5 minutes to melt the sample and sodium peroxide in the corundum crucible. Then take out the corundum crucible, place it in the air, and wait for it to cool to room temperature.

[0034] S3: Place the corundum crucible into a 100mL beaker filled with 30mL of deionized water (temperature 50-60°C), then add 15mL of 36.5% hydrochloric acid into the beaker and stir continuously to dissolve the zinc and copper concentrate samples in the corundum crucible;

[0035] S4: After washing the high-alumina crucible, take it out and continue to stir until the solid matter in the solution is completely dissolved and clear, then transfer the solution to a 100 mL volumetric flask and dilute it to the mark with deionized water, then transfer the solution to a centrifuge tube and centrifuge it (or dry filter) for testing;

[0036] S5: Prepare standard solutions of different concentrations according to the indium content in zinc and copper concentrates. The concentrations of the indium standard solutions are 0.00 μg / mL, 0.50 μg / mL, 1.00 μg / mL, 3.00 μg / mL, 5.00 μg / mL, and 7.00 μg / mL. Put each standard solution into an inductively coupled plasma emission spectrometer, measure the intensity of each standard solution, and draw an indium standard working curve with the standard solution concentration as the horizontal coordinate and the corresponding intensity as the vertical coordinate;

[0037] The analytical line wavelength of indium element is 410.176nm; the inductively coupled plasma emission spectrometer is Agilent Technology ICP-oes5110; an argon humidifier is added between the argon gas and the nebulizer. The use of the argon humidifier can effectively reduce the influence of sodium ions in the sample on the nebulizer and prevent the nebulizer from being blocked;

[0038] The operating parameters of the inductively coupled plasma emission spectrometer were: RF power 1250 W, cooling gas 13 L / min, argon (purity 99.99%) flow rate, carrier gas 0.60 L / min; reading time 5 s;

[0039] S6: placing the solution to be tested into an inductively coupled plasma emission spectrometer to obtain the intensity of the solution to be tested, and calculating the indium content value on an indium standard working curve according to the intensity value.

[0040] Comparative Example 1: Verification of the effect of excitation parameters of inductively coupled plasma emission spectrometer

[0041] With other conditions unchanged, only the RF power was changed to 1250W. The test results are shown in Table 1.

[0042] Table 1 Relationship between RF power change and (In) signal strength

[0043] RF power(KW) 1.0 1.1 1.15 1.20 1.25 1.30 (In)Signal Strength 5147 5482 5599 5731 5858 5899

[0044] From the data in Table 1, it can be seen that the signal intensity of indium does not change much after the RF power reaches 1.25 (kw), so 1.25 (kw) is selected as the power for measuring indium.

[0045] With other conditions unchanged, only the carrier gas velocity was changed. The test results are shown in Table 2.

[0046] Table 2 Relationship between carrier gas velocity change and (In) signal intensity

[0047] Carrier gas flow rate (L / min) 0.5 0.55 0.60 0.65 0.7 (In)Signal Strength 5899 6673 6209 5831 5508

[0048] From the signal value of In determination in Table 2, the signal intensity is strongest at a carrier gas flow rate of 0.55 L / min. Taking comprehensive consideration, the carrier gas flow rate selected for this method is 0.60 L / min.

[0049] The main function of the cooling gas is to reduce the temperature of the argon gas during ionization to protect the matrix tube and also participate in the ionization of the plasma.

[0050] Reading time: 5s for three readings of sample data to ensure the stability of the injection system and the accuracy of the results.

[0051] Comparative Example 2: Determination of Indium Content by Atomic Absorption

[0052] Weigh 0.2000-0.5000g of the sample into a 250mL beaker, moisten with water, add ammonium fluoride, hydrochloric acid, and nitric acid to dissolve and remove sulfur at low temperature, cool the solution until it is almost dry, add nitric acid and rinse the surface and the wall of the cup with water, and slightly heat the sample on the electric hot plate to dissolve it. Remove and cool to room temperature, transfer to a 50mL volumetric flask to make up the volume, and shake well. Then transfer the solution to a centrifuge tube and centrifuge it (or dry filter) for testing. According to the determination method of the working curve, analyze the sample on the atomic absorption, and the analysis results are shown in the table.

[0053]

[0054] As can be seen from the above table, the error between the test results obtained by the method of this technical solution and the atomic absorption test results is small, so it is feasible to use this technical solution to determine the content of indium in zinc and copper concentrates. This method is simple to operate, can quickly obtain the indium content in zinc and copper concentrates, effectively improve the detection efficiency of indium in zinc and copper concentrates, the detection process has low requirements for equipment, the test results are reliable and stable, no expensive auxiliary reagents are required, and the detection cost is effectively reduced.

[0055] The embodiments of the present application have been described above, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The selection of terms used herein is intended to best explain the principles of the embodiments, practical applications, or improvements to the technology in the market, or to enable other persons of ordinary skill in the art to understand the embodiments disclosed herein.

Claims

1. A method for detecting the content of indium in zinc and copper concentrates, characterized in that: The following steps are involved: S1: Spread sodium peroxide on the bottom of the reaction container, place the zinc and copper concentrate samples containing indium on the sodium peroxide, and then cover them with sodium peroxide; S2: continuously heating the reaction container of step S1 at the initial temperature to a preset temperature, and then cooling the reaction container to room temperature; S3: placing the reaction container of step S2 into a container filled with deionized water, continuously adding hydrochloric acid, and continuously stirring until the zinc and copper concentrate samples in the reaction container are dissolved; fixing the obtained solution to volume and then centrifuging to obtain a test solution; S4: Prepare standard solutions of different concentrations according to the indium content in the zinc and copper concentrates, put each standard solution into an inductively coupled plasma emission spectrometer, measure the intensity of each standard solution, and draw an indium standard working curve with the standard solution concentration as the horizontal axis and the corresponding intensity as the vertical axis; The analytical line wavelength of indium is 410.176nm; The operating parameters of the inductively coupled plasma emission spectrometer were: RF power 1250 W, cooling gas 13 L / min, argon (purity 99.99%) flow rate, carrier gas 0.60 L / min; reading time 5 s; S6: placing the solution to be tested in step S3 into an inductively coupled plasma emission spectrometer to obtain the intensity of the solution to be tested, and calculating the indium content value on an indium standard working curve according to the intensity value.

2. The content detection method according to claim 1, characterized in that: In the step S1, the mass ratio of sodium peroxide to indium zinc and copper concentrate samples is 1.5:0.

15.

3. The content detection method according to claim 1, characterized in that: In the step S2, the initial temperature is 650°C; the preset temperature is 700°C, and the melting time after heating to the preset temperature is 5 minutes.

4. The content detection method according to claim 1, characterized in that: In step S3, the mass fraction of hydrochloric acid is 36.5%.

5. The content detection method according to claim 1, characterized in that: In step S3, the temperature of the deionized water is 50-60°C.

6. The content detection method according to claim 1, characterized in that: In step S5 and step S6, the testing method is axial observation.

7. The content detection method according to claim 1, characterized in that: The reaction container is a corundum crucible.

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