Method for detecting zinc element in zinc-containing waste residue

Abstract

The invention discloses a method for detecting metal zinc in zinc-containing waste residues. The method comprises the following steps: preparing the zinc-containing waste residues into a sample of which the particle size is less than 0.09 mm; the method comprises the following steps: weighing a sample, putting the sample into a dried conical flask, adding a ferric trichloride solution, plugging a bottle opening with a plug, stirring, taking down, filtering, filtering into a 200mL volumetric flask with filter paper, washing the conical flask and the filter paper, discarding the filter paper, and retaining filtrate; making the volume constant to the scale by using ultrapure water, and uniformly mixing to obtain a solution to be detected; taking a zinc element standard solution, obtaining a zinc element standard curve solution by adopting a dilution method, detecting the zinc element standard curve solution by using an inductively coupled plasma atomic emission spectrometer to obtain a zinc element standard curve, and detecting the solution to be detected under the same conditions to obtain a zinc element standard curve. And calculating according to the zinc element standard curve to obtain the content of metal zinc in the zinc-containing waste residue. The detection method provided by the invention is accurate and reliable, is simple and convenient to operate, can improve the detection efficiency and detection precision of the metal zinc content, and also reduces the operation difficulty of sample preparation and sample detection.

Description

Technical Field

[0001] The present invention relates to the technical field of analytical chemistry, and more particularly to a method for detecting metallic zinc in zinc-containing waste slag. Background Art

[0002] Zinc-containing slag generated during steelmaking (such as electric furnace ash and converter ash) is a typical zinc-containing solid waste in the steel industry. Its treatment and resource utilization are important issues in environmental protection and the circular economy. It primarily comes from the dust formed by the condensation of zinc volatilization during the smelting of zinc-containing scrap steel (such as galvanized steel sheets and automotive scrap steel), as well as residual zinc compounds in the slag. Zinc-containing slag is primarily composed of metallic zinc, zinc compounds, and other components. Recycling, treating, and reusing zinc-containing slag is a relatively scientific approach to waste slag treatment.

[0003] During the entire process, the components of zinc-containing waste slag need to be measured to determine its value, among which the content of metallic zinc is an important indicator.

[0004] Therefore, it is currently necessary to provide a method for detecting metallic zinc in zinc-containing waste slag to provide a technical basis for the treatment and utilization of zinc-containing waste slag. Summary of the Invention

[0005] The purpose of the present invention is to overcome the above-mentioned defects of the prior art, provide a method for detecting metallic zinc in zinc-containing waste slag, and provide a technical basis for the treatment and utilization of zinc-containing waste slag.

[0006] To achieve the above object, the technical solution of the present invention is as follows:

[0007] A method for detecting metallic zinc in zinc-containing waste slag comprises the following steps:

[0008] (1) Prepare a sample with a particle size of less than 0.09 mm from zinc-containing waste slag;

[0009] (2) Weigh 0.1g to 0.2g of sample into a dried conical flask, add 100mL to 120mL of ferric chloride solution, plug the flask with a stopper, stir for 30min to 40min, remove the solution, filter it with filter paper into a 200mL volumetric flask, rinse the conical flask and filter paper, discard the filter paper, and retain the filtrate. Dilute to the mark with ultrapure water and mix well to obtain the test solution.

[0010] (3) taking a zinc standard solution, using a dilution method to obtain a zinc standard curve solution, using an inductively coupled plasma atomic emission spectrometer to detect the zinc standard curve solution to obtain a zinc standard curve, detecting the test solution under the same conditions, and calculating the content of metallic zinc in the zinc-containing waste slag according to the zinc standard curve.

[0011] Optionally, in step (3), the calculation formula is as follows:

[0012]

[0013] Where: w zn : metallic zinc content, in %; c: zinc content obtained from the zinc element standard curve, in μg / mL; V: volume of the solution to be tested, in mL; m: mass of the sample, in g.

[0014] Optionally, in step (2), the mass concentration of the ferric chloride solution is 3% to 5%.

[0015] Optionally, in step (3), the parameters of the inductively coupled plasma atomic emission spectrometer are: high-frequency emission power is 1150W; peristaltic pump speed is 60r / min; nebulizing gas flow rate is 0.6L / min; auxiliary gas flow rate is 0.5L / min; detector measurement temperature is -47°C; optical chamber temperature is 38°C; observation height is 15mm; integration time long wave is 10s, and short wave is 10s.

[0016] Optionally, in step (3), the concentration range of the zinc element standard curve solution is 0 μg / mL to 50 μg / mL.

[0017] Optionally, in step (2), the specific process of flushing the conical flask and filter paper is: aiming the water column of the bottle washing nozzle at the inner wall of the conical flask to flush all the liquid on the inner wall into the receiving container; the same operation is performed to flush all the ions to be tested in the filter paper into the receiving container.

[0018] Optionally, in step (2), the diameter of the filter paper is 12.5 cm.

[0019] Optionally, in step (1), the mass fraction of metallic zinc in the sample is 1% to 8%.

[0020] The implementation of the present invention will have the following beneficial effects:

[0021] 1. The sample processing cost of this method is low.

[0022] 2. This method has simple sample processing steps, uses fewer chemical reagents, and has less impact on the environment.

[0023] 3. This method only requires basic laboratory reagents and is suitable for use in most laboratories.

[0024] 4. The detection method of the present invention is accurate, reliable, and simple to operate. It can not only improve the detection efficiency and detection accuracy of zinc content, but also reduce the difficulty of sample preparation and sample detection operations, overcoming the shortcomings of traditional inspection methods such as complex operation, high cost, low efficiency, and narrow measurement range. It is suitable for the determination of metallic zinc content in zinc-containing waste slag and has important promotion value and practical value. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is the standard curve of zinc element in Example 1 of the present invention. DETAILED DESCRIPTION

[0026] The present invention is further described below with reference to specific examples, but is not intended to limit the present invention in any way.

[0027] The present invention discloses a method for detecting metallic zinc in zinc-containing waste slag, comprising the following steps:

[0028] (1) Prepare zinc-containing waste slag into samples with a particle size of less than 0.09 mm.

[0029] In a specific embodiment, in step (1), the mass fraction of metallic zinc in the sample is 1% to 8%.

[0030] (2) Weigh 0.1g to 0.2g of sample into a dried conical flask, add 100mL to 120mL of ferric chloride solution, plug the flask, stir for 30min to 40min, remove the flask, filter, and transfer the solution to a 200mL volumetric flask using filter paper. Rinse the conical flask and filter paper, discard the filter paper, and retain the filtrate. Dilute to the mark with ultrapure water and mix thoroughly to obtain the test solution.

[0031] In a specific embodiment, in step (2), the mass concentration of the ferric chloride solution is 3% to 5%.

[0032] In a specific embodiment, in step (2), the specific process of rinsing the conical flask and the filter paper is as follows: aiming the water column of the washing bottle nozzle at the inner wall of the conical flask to flush all the liquid on the inner wall into the receiving container; and the same operation is performed to flush all the ions to be measured in the filter paper into the receiving container.

[0033] In one specific embodiment, in step (2), the diameter of the filter paper is 12.5 cm.

[0034] (3) Taking a zinc standard solution, using a dilution method to obtain a zinc standard curve solution, using an inductively coupled plasma atomic emission spectrometer to detect the zinc standard curve solution to obtain a zinc standard curve, detecting the test solution under the same conditions, and calculating the content of metallic zinc in the zinc-containing waste slag according to the zinc standard curve.

[0035] In one specific embodiment, in step (3), the calculation formula is as follows:

[0036]

[0037] Where: w zn : metallic zinc content, in %; c: zinc content obtained from the zinc element standard curve, in μg / mL; V: volume of the solution to be tested, in mL; m: mass of the sample, in g.

[0038] In a specific embodiment, in step (3), the parameters of the inductively coupled plasma atomic emission spectrometer are as follows: high-frequency emission power is 1150 W; peristaltic pump speed is 60 r / min; nebulizing gas flow rate is 0.6 L / min; auxiliary gas flow rate is 0.5 L / min; detector measurement temperature is -47°C; light chamber temperature is 38°C; observation height is 15 mm; integration time is 10 s for long wave and 10 s for short wave.

[0039] In a specific embodiment, in step (3), the concentration range of the zinc standard curve solution is 0 μg / mL to 50 μg / mL.

[0040] The following are specific embodiments

[0041] Example 1

[0042] Take 1 # Zinc-containing waste slag was measured.

[0043] The samples were processed into specimens with a particle size less than 0.09 mm.

[0044] Weigh 0.1 (± 0.0002) g of sample and place it in a dried conical flask. Add 100 mL of ferric chloride solution (3%, dissolve ferric chloride in distilled water and filter before use). Stopper the bottle mouth with a stopper, place it on a magnetic stirrer and stir for 30 min. Remove it and filter the solution in the conical flask into a 200 mL volumetric flask using medium-speed filter paper with a diameter of 12.5 cm. Wash the conical flask and filter paper, make up to volume, and mix thoroughly to obtain the solution to be tested.

[0045] The zinc standard solution was diluted stepwise to obtain calibration solutions with concentrations of 0 μg / mL, 1 μg / mL, 3 μg / mL, 5 μg / mL, 7 μg / mL, and 10 μg / mL. The calibration solutions were measured using an inductively coupled plasma atomic emission spectrometer (ICP-AES) to obtain a calibration curve. The ICP-AES parameters were as follows: high-frequency transmission power of 1150 W; peristaltic pump speed of 60 r / min; atomizing gas flow rate of 0.6 L / min; auxiliary gas flow rate of 0.5 L / min; detector measurement temperature of -47°C; light chamber temperature of 38°C; observation height of 15 mm; integration time of 10 s for long wave and 10 s for short wave. Under the same conditions, the metallic zinc content of the test solution was 6.7 μg / mL. The metallic zinc content in the zinc slag was calculated using the following formula:

[0046]

[0047] Where: w zn : metallic zinc content, in %; c: zinc content obtained from the zinc element standard curve, in μg / mL; V: volume of the solution to be tested, in mL; m: mass of the sample, in g.

[0048] Calculated to be 1 # The content of metallic zinc in the zinc-containing waste slag is 1.34%.

[0049] Example 2

[0050] Take 2 # Zinc-containing waste slag was measured.

[0051] The samples were processed into specimens with a particle size less than 0.09 mm.

[0052] Weigh 0.2 (± 0.0002) g of sample and place it in a dried conical flask. Add 100 mL of ferric chloride solution (5%, dissolve ferric chloride in distilled water and filter before use). Stopper the bottle mouth with a stopper, place it on a magnetic stirrer and stir for 30 min. Remove it and filter the solution in the conical flask into a 200 mL volumetric flask using medium-speed filter paper with a diameter of 12.5 cm. Wash the conical flask and filter paper, make up to volume, and mix well to obtain the solution to be tested.

[0053] The zinc standard solution was diluted stepwise to obtain calibration solutions with concentrations of 0 μg / mL, 2 μg / mL, 6 μg / mL, 10 μg / mL, 14 μg / mL, and 20 μg / mL. The calibration solutions were measured using an inductively coupled plasma atomic emission spectrometer (ICP-AES) to obtain a calibration curve. The ICP-AES parameters were as follows: high-frequency transmission power of 1150 W; peristaltic pump speed of 60 r / min; atomizing gas flow rate of 0.6 L / min; auxiliary gas flow rate of 0.5 L / min; detector measurement temperature of -47°C; light chamber temperature of 38°C; observation height of 15 mm; integration time of 10 s for long wave and 10 s for short wave. Under the same conditions, the test solution was tested and the metallic zinc content was 15.6 μg / mL. The metallic zinc content in the zinc slag was calculated using the following formula:

[0054]

[0055] Where: w zn : metallic zinc content, in %; c: zinc content obtained from the zinc element standard curve, in μg / mL; V: volume of the solution to be tested, in mL; m: mass of the sample, in g.

[0056] Calculated to be 2 # The content of metallic zinc in the zinc-containing waste slag is 1.56%.

[0057] Example 3

[0058] Take 3 # Zinc-containing waste slag was measured.

[0059] The samples were processed into specimens with a particle size less than 0.09 mm.

[0060] Weigh 0.1 (± 0.0002) g of sample and place it in a dried conical flask. Add 120 mL of ferric chloride solution (4%, dissolve ferric chloride in distilled water and filter before use). Stopper the bottle mouth with a stopper, place it on a magnetic stirrer and stir for 40 min. Remove it and filter the solution in the conical flask into a 200 mL volumetric flask using medium-speed filter paper with a diameter of 12.5 cm. Wash the conical flask and filter paper, make up to volume, and mix thoroughly to obtain the solution to be tested.

[0061] The zinc standard solution was diluted stepwise to obtain calibration solutions with concentrations of 0 μg / mL, 10 μg / mL, 20 μg / mL, 30 μg / mL, 40 μg / mL, and 50 μg / mL. The calibration solutions were measured using an inductively coupled plasma atomic emission spectrometer (ICP-AES) to obtain a calibration curve. The ICP-AES parameters were as follows: high-frequency transmission power of 1150 W; peristaltic pump speed of 60 r / min; atomizing gas flow rate of 0.6 L / min; auxiliary gas flow rate of 0.5 L / min; detector measurement temperature of -47°C; light chamber temperature of 38°C; observation height of 15 mm; integration time of 10 s for long wave and 10 s for short wave. Under the same conditions, the metallic zinc content of the test solution was 37.05 μg / mL. The metallic zinc content in the zinc slag was calculated using the following formula:

[0062]

[0063] Where: w zn : metallic zinc content, in %; c: zinc content obtained from the zinc element standard curve, in μg / mL; V: volume of the solution to be tested, in mL; m: mass of the sample, in g.

[0064] Calculated to be 3 # The content of metallic zinc in the zinc-containing waste slag is 7.41%.

[0065] The experimental results of spike recovery of Examples 1-3 are shown in the following table:

[0066]

[0067] The above-described embodiments merely represent several implementation methods of the present invention. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent application. It should be noted that a person skilled in the art would be able to make various modifications and improvements without departing from the spirit of the present invention, all of which fall within the scope of protection of the present invention. Therefore, the scope of protection of the patent for this invention shall be determined by the appended claims.

Claims

1. A method for detecting metallic zinc in zinc-containing waste slag, characterized in that: The following steps are involved: (1) Prepare a sample with a particle size of less than 0.09 mm from zinc-containing waste slag; (2) Weigh 0.1g to 0.2g of sample into a dried conical flask, add 100mL to 120mL of ferric chloride solution, plug the flask with a stopper, stir for 30min to 40min, remove the solution, filter it with filter paper into a 200mL volumetric flask, rinse the conical flask and filter paper, discard the filter paper, and retain the filtrate. Dilute to the mark with ultrapure water and mix well to obtain the test solution. (3) taking a zinc standard solution, using a dilution method to obtain a zinc standard curve solution, using an inductively coupled plasma atomic emission spectrometer to detect the zinc standard curve solution to obtain a zinc standard curve, detecting the test solution under the same conditions, and calculating the content of metallic zinc in the zinc-containing waste slag according to the zinc standard curve.

2. The method for detecting metallic zinc in zinc-containing waste slag according to claim 1, wherein In step (3), the calculation formula is as follows: Where: w zn : metallic zinc content, in %; c: zinc content obtained from the zinc element standard curve, in μg / mL; V: volume of the solution to be tested, in mL; m: mass of the sample, in g.

3. The method for detecting metallic zinc in zinc-containing waste slag according to claim 1, wherein In step (2), the mass concentration of the ferric chloride solution is 3% to 5%.

4. The method for detecting metallic zinc in zinc-containing waste slag according to claim 1, wherein In step (3), the parameters of the inductively coupled plasma atomic emission spectrometer are: high-frequency emission power of 1150 W; peristaltic pump speed of 60 r / min; atomizing gas flow rate of 0.6 L / min; auxiliary gas flow rate of 0.5 L / min; detector measurement temperature of -47°C; light chamber temperature of 38°C; observation height of 15 mm; integration time long wave of 10 s, short wave of 10 s.

5. The method for detecting metallic zinc in zinc-containing waste slag according to claim 1, wherein The concentration range of the zinc element standard curve solution is 0 μg / mL to 50 μg / mL.

6. The method for detecting metallic zinc in zinc-containing waste slag according to claim 1, wherein In step (2), the diameter of the filter paper is 12.5 cm.

7. The method for detecting metallic zinc in zinc-containing waste slag according to claim 1, wherein In step (1), the mass fraction of metallic zinc in the sample is 1% to 8%.

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