Method for detecting high-content zinc element in ore

Abstract

The invention relates to a method for detecting high-content zinc element in ore. The detection method comprises the following steps: adding a zinc-containing ore sample into a mixture of ammonium fluoride, hydrobromic acid, hydrochloric acid, nitric acid and perchloric acid, dissolving, taking melt with hydrochloric acid to obtain a solution to be detected, drawing a zinc standard working curve, detecting the strength of the solution to be detected, and calculating the content value of the zinc element on the zinc standard working curve according to the strength value. According to the scheme provided by the invention, the operation is simple and convenient and the detection result is accurate when the high-content zinc element in the ore is detected.

Description

Technical Field

[0001] The present application relates to the technical field of nonferrous metal beneficiation, and in particular to a method for detecting high-content zinc in ores. Background Art

[0002] In the analysis and detection of non-ferrous metal ore components, the zinc content is one of the elements that must be detected. The methods for determining zinc in non-ferrous metal ores include precipitation separation Na2EDTA titration and extraction separation Na2EDTA titration. The operation process of precipitation separation Na2EDTA titration is long, and the sample washing is not clean, which affects the accuracy and stability of the test results. The operation process of extraction separation Na2EDTA titration is long, the process is cumbersome, more chemical reagents are used, and the results are unstable, and the test results have large deviations. A company in Yunnan needs to analyze the zinc content in mining, mineral processing, geological exploration, and experimental samples. The sample volume increases by 15% year by year. The traditional detection method is used to analyze the zinc content. The operation is cumbersome, time-consuming, and the labor cost and reagent cost are high; due to the high zinc content and more impurities in the ore, the detection method in the relevant technology cannot accurately detect the high content of zinc in the ore.

[0003] Therefore, it is necessary to provide a method for detecting high-content zinc element which is simple to operate and has accurate detection results. Summary of the invention

[0004] In order to solve or partially solve the problems existing in the related art, the present application provides a method for detecting high-content zinc in ore, which can accurately detect high-content zinc in ore.

[0005] The present application discloses a method for detecting high-content zinc in ore, comprising the following steps:

[0006] S1: Add a mixture of ammonium fluoride, hydrobromic acid, hydrochloric acid, nitric acid and perchloric acid to the zinc-containing ore sample, dissolve it at low temperature until it becomes clear, and then continue to heat;

[0007] S2: adding hydrochloric acid to the heated solution and cooling;

[0008] S3: Slightly heat the cooled solution, cool it down, and shake it to make it uniform to obtain the solution to be tested;

[0009] S4: Prepare standard solutions of different concentrations according to the zinc content in the ore sample, put each standard solution into an inductively coupled plasma emission spectrometer, measure the fluorescence intensity of the standard solution, and draw a zinc standard working curve with the standard solution concentration as the abscissa and the corresponding fluorescence intensity as the ordinate;

[0010] The analytical line wavelength of zinc is 472.215nm;

[0011] The operating parameters of the inductively coupled plasma emission spectrometer were as follows: RF power was 1200 W, auxiliary gas (Ar) flow rate was 10 L / min, nebulizer flow rate was 0.65 L / min, sample lifting time was 15 s, stabilization time was 10 s, integration time was 5 s, and sample pump speed was 80 r / min;

[0012] S5: placing the solution to be tested in step S3 into an inductively coupled plasma emission spectrometer to obtain the fluorescence intensity of the solution to be tested, and calculating the zinc content value on the zinc standard working curve according to the fluorescence intensity value.

[0013] Optionally, in step S1, the mass fraction of ammonium fluoride is 18.5%, the mass fraction of hydrobromic acid is 28.85%, the mass fraction of hydrochloric acid is 36.5%, the mass fraction of nitric acid is 63.0%, and the mass fraction of perchloric acid is 71.2%.

[0014] Optionally, in step S1, the volume ratio of ammonium fluoride, hydrobromic acid, hydrochloric acid, nitric acid and perchloric acid is 2:10:10:10:1.

[0015] Optionally, in step S1, the temperature during low-temperature dissolution is 200-250°C.

[0016] Optionally, in step S1, the continuous heating temperature is 180-380°C, and the heating time is 5 minutes.

[0017] Optionally, in step S3, the temperature during slight heating is 200-250°C.

[0018] The detection mechanism of this application scheme is: the sample is melted with acid to oxidize all heavy metals to the highest valence state, and then the melt is extracted with hydrochloric acid. The metal elements exist in the solution in the form of ions. The solution is introduced into ICP-OES to determine the content of zinc in the ore. Ammonium fluoride plays a key role in the mixed acid system. Silicon exists in the form of silicon dioxide or silicate. The fluoride ions in ammonium fluoride can form volatile silicon tetrafluoride (SiF) with silicon. The reaction formula is: SiO2+4HF→SiF↑+H2O. Silicon tetrafluoride is a gaseous substance that can evaporate from the system under heating and other conditions, thereby effectively removing the interference of silicon impurities; nitric acid has strong oxidizing properties and can oxidize low-valent sulfur into high-valent sulfate. For some sulfur-containing compounds, nitric acid can oxidize them into a form that is easily soluble in water and easier to remove in subsequent treatments. For example, sulfides are oxidized to sulfates; perchloric acid is an extremely strong oxidant under heating conditions, which can further promote the oxidation process of sulfur impurities and ensure that sulfur impurities are converted into a stable and easy-to-handle form; the strong oxidizing properties of nitric acid and perchloric acid can cause carbon impurities to be oxidized to carbon dioxide. Under high temperature conditions, carbon reacts with strong oxidants, C+4HNO→CO↑+4NO↑+H2O. Carbon dioxide is a gaseous substance that can escape from the system, thereby removing the interference of carbon impurities; the various acids in the mixed acid work together to destroy the structure of carbon-containing substances, making them easier to oxidize and remove. For example, for organic carbon-containing compounds, acids can cause them to decompose and oxidize, converting them into easily removable substances such as carbon dioxide and water. In summary, ammonium fluoride, hydrobromic acid, hydrochloric acid, nitric acid and perchloric acid mixed acids effectively remove the interference of silicon, sulfur and carbon impurities through their respective specific mechanisms of action, providing accurate results for chemical analysis.

[0019] The technical solution provided by this application may have the following beneficial effects:

[0020] 1) This method is simple to operate, can quickly obtain the zinc content in the ore sample, effectively improves the detection efficiency of the ore sample, has low requirements on equipment during the detection process, and the test results are reliable and stable. It does not require a lot of chemical reagents, and effectively reduces the detection cost.

[0021] 2) The present application effectively removes the interference of silicon, sulfur and carbon impurities by adding a mixture of ammonium fluoride, hydrobromic acid, hydrochloric acid, nitric acid and perchloric acid to the zinc-containing ore sample, and can accurately detect the high content of zinc in the ore.

[0022] 3) This application sets the working parameters of the inductively coupled plasma emission spectrometer as follows: RF power of 1200 W, auxiliary gas (Ar) flow rate of 10 L / min, nebulizer flow rate of 0.65 L / min, sample lifting time of 15 s, stabilization time of 10 s, integration time of 5 s, injection pump speed of 80 r / min, zinc analysis line of 472.215 nm, which can accurately detect high content of zinc in ore.

[0023] 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

[0024] 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.

[0025] Figure 1 It is a schematic diagram of the zinc standard working curve shown in this application. DETAILED DESCRIPTION

[0026] 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.

[0027] Example 1

[0028] A method for detecting high-content zinc in ore, comprising the following steps:

[0029] S1: Place the zinc-containing ore sample that has passed through a 0.100 mm sieve in a 250 ml beaker;

[0030] S2: Add 2 mL of ammonium fluoride solution, 10 mL of hydrobromic acid, 10 mL of hydrochloric acid, 10 mL of nitric acid and 1 mL of perchloric acid into a beaker. The mass fraction of ammonium fluoride is 18.5%, the mass fraction of hydrobromic acid is 28.85%, the mass fraction of hydrochloric acid is 36.5%, the mass fraction of nitric acid is 63.0%, and the mass fraction of perchloric acid is 71.2%. It dissolves clearly at low temperature, and the temperature is 200-250°C;

[0031] S3: Continue to steam with a high-temperature electric heating plate until perchloric acid smoke is emitted to remove carbon for 5 minutes, then remove the plate. The continuous heating temperature is 180-380℃;

[0032] S4: Add 20ml of hydrochloric acid and cool; wash the sample solution remaining on the conical flask. Slightly heat to completely dissolve the precipitate, the temperature is 200-250℃, after cooling, transfer to a 500ml volumetric flask, dilute to the scale with deionized water, shake well, and obtain the test solution;

[0033] S5: Prepare standard solutions of different concentrations according to the zinc content in the ore sample, the concentrations of the zinc standard solutions are 0.00ug / L, 30.00ug / L, 60.00ug / L, 90.00ug / L, 120.00ug / L, 150.00ug / L, and 200.00ug / L, respectively, put each standard solution into an inductively coupled plasma emission spectrometer, measure the fluorescence intensity of the standard solution, and draw a zinc standard working curve with the standard solution concentration as the abscissa and the corresponding intensity as the ordinate; the linear regression equation of the working standard curve is: y=0.0026X-0.0021, and the linear regression coefficient r=0.9999.

[0034] S6: placing the solution to be tested in step S4 into an inductively coupled plasma emission spectrometer to obtain the fluorescence intensity of the solution to be tested, and calculating the zinc content on a zinc standard working curve according to the fluorescence intensity value.

[0035] The operating parameters of the inductively coupled plasma optical emission spectrometer are shown in Table 1.

[0036] Table 1 Operating parameters of inductively coupled plasma emission spectrometer

[0037]

[0038] Comparative Example 1: Determination of zinc content in ore by precipitation separation Na2EDTA titration method

[0039] Weigh 0.2000g of the sample, accurate to 0.0001g, place it in a 400ml beaker, add a small amount of water to moisten it, add 10ml of hydrochloric acid, cover the watch glass and dissolve it at low temperature to drive out hydrogen sulfide for 5min-10min, add 5ml of nitric acid until the sample is completely decomposed, and remove the watch glass. Add 5ml of sulfuric acid (1+1), continue to heat until it is wet salt, remove and cool, add 20ml of sulfuric acid (1+9,), cover the watch glass, heat to dissolve the salts, and cool slightly. Blow the watch glass and the wall of the cup with water, and dilute the volume to about 60ml, filter with slow quantitative filter paper, collect the filtrate in a beaker, wash the beaker and precipitate with sulfuric acid (2+28) 5 times each, wash the beaker and precipitate with water once each, and retain the filtrate. Boil the filtrate and concentrate it to a volume of about 100ml to completely destroy the excess ammonium persulfate, remove and cool. Add 0.1g ascorbic acid, 1 drop of methyl orange indicator, adjust with ammonia and hydrochloric acid until the solution just turns red, add 20ml acetic acid-sodium acetate buffer solution, 5ml potassium fluoride solution, 10ml sodium thiosulfate solution, add 2 drops of dimethyl orange indicator, and titrate the solution with Na2EDTA standard until the solution changes from purple-red to bright yellow, which is the end point. Calculate the amount of zinc based on the volume of Na2EDTA consumed.

[0040] Comparative Example 2: Determination of zinc content in ore by titration with Na2EDTA extraction

[0041] Weigh 2.5000g of the sample, accurate to 0.0001g, place it in a 300ml conical beaker, moisten it with 20ml water, add 2-3ml liquid bromine, react at room temperature for 15min and shake it from time to time, add 15ml nitric acid, leave it for 15min, put the conical flask on the hot plate to heat, boil to drive out the bromine vapor, cool and add 100ml water, heat and boil and cool. Transfer the sample to a 500ml volumetric flask, dilute to scale with water, wash the insoluble residue on the filter paper with water, place the filtered insoluble residue and filter paper in a 25ml platinum crucible, put it in a muffle furnace at 800℃ for ashing, add 2ml sulfuric acid, 2ml nitric acid and 2ml hydrofluoric acid, evaporate the solution to dryness, and cool. Add a small amount of water to dissolve the soluble salt. Filter with medium-speed filter paper, combine the filtrate and the washing liquid into the same volumetric flask mentioned above, and dilute to scale with water. Pipette 50ml solution into the separatory funnel of 250ml, drip ammonia water until a small amount of turbidity is produced, add 5ml hydrochloric acid, 50ml concealing agent, mix.Add 80ml methyl isobutyl copper methyl, shake 1min, after phase separation, slowly put lower aqueous phase into another separatory funnel, add 20ml methyl isobutyl copper methyl, extract for the second time, after phase separation, discard aqueous phase, merge twice with base phase, put into 400ml beaker, add 1ml hydrochloric acid and 70ml ethanol to two separatory funnels respectively, shake, and the liquid in two separatory funnels is put into above-mentioned beaker.Add 10ml sodium fluoride solution, 10ml thiourea solution, 20ml buffer solution, 5ml potassium iodide solution, 0.1g xylenol orange, use Na2EDTA standard titration solution to solution from purple red to bright yellow is terminal point, according to the volume of consuming Na2EDTA, calculate zinc amount.Implementation comparison example is shown in Table 3 below:

[0042] Table 3 Comparison table of Example 1, Comparative Example 1 and Comparative Example 2

[0043]

[0044] As shown in Table 2, the error between the test results obtained by the method of the present technical solution and the results of the precipitation separation Na2EDTA titration method and the extraction separation Na2EDTA titration method is small, so it is feasible to use the present technical solution to determine the content of zinc in the ore. The present method is simple to operate, can quickly obtain the zinc content in the ore sample, effectively improves the detection efficiency of the ore sample, has low requirements for equipment during the detection process, and has reliable and stable test results, does not require expensive auxiliary reagents, and effectively reduces the detection cost.

[0045] 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 high-content zinc in ore, characterized in that: The following steps are involved: S1: Add a mixture of ammonium fluoride, hydrobromic acid, hydrochloric acid, nitric acid and perchloric acid to the zinc-containing ore sample, dissolve it at low temperature until it becomes clear, and then continue to heat; S2: adding hydrochloric acid to the heated solution and cooling; S3: Slightly heat the cooled solution, cool it down, and shake it to make it uniform to obtain the solution to be tested; S4: Prepare standard solutions of different concentrations according to the zinc content in the ore sample, put each standard solution into an inductively coupled plasma emission spectrometer, measure the fluorescence intensity of the standard solution, and draw a zinc standard working curve with the standard solution concentration as the abscissa and the corresponding fluorescence intensity as the ordinate; The analytical line wavelength of zinc is 472.215nm; The operating parameters of the inductively coupled plasma emission spectrometer were as follows: RF power was 1200 W, auxiliary gas (Ar) flow rate was 10 L / min, nebulizer flow rate was 0.65 L / min, sample lifting time was 15 s, stabilization time was 10 s, integration time was 5 s, and sample pump speed was 80 r / min; S5: placing the solution to be tested in step S3 into an inductively coupled plasma emission spectrometer to obtain the fluorescence intensity of the solution to be tested, and calculating the zinc content value on the zinc standard working curve according to the fluorescence intensity value.

2. The detection method according to claim 1, characterized in that: In the step S1, the mass fraction of ammonium fluoride is 18.5%, the mass fraction of hydrobromic acid is 28.85%, the mass fraction of hydrochloric acid is 36.5%, the mass fraction of nitric acid is 63.0%, and the mass fraction of perchloric acid is 71.2%.

3. The detection method according to claim 2, characterized in that: In step S1, the volume ratio of ammonium fluoride, hydrobromic acid, hydrochloric acid, nitric acid and perchloric acid is 2:10:10:10:

1.

4. The detection method according to claim 1, characterized in that: In the step S1, the temperature during low temperature dissolution is 200°C-250°C.

5. The detection method according to claim 1, characterized in that: In the step S1, the continuous heating temperature is 180-380° C., and the heating time is 5 minutes.

6. The detection method according to claim 1, characterized in that: In step S3, the temperature during slight heating is 200-250°C.

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