A method for detecting nickel in steelmaking dust.

Abstract

This invention discloses a method for detecting nickel in steelmaking dust. The equipment used in this analytical method is an inductively coupled plasma atomic emission spectrometer (ICP). The process steps are simple and clear, requiring the dust to be analyzed to be prepared into a solution, and then the equipment is set to automatic analysis. The breakthrough in this invention is the dissolution of the dust sample. This method has few interfering factors during the determination process, is simple and fast to operate, has good accuracy and precision, and low labor intensity, making it suitable for industrial production. It is particularly suitable for operation using an inductively coupled plasma atomic emission spectrometer. By accurately determining the nickel content of the dust, the treatment and use of the dust can be based on evidence, reducing environmental pressure and making full and complete use of secondary resources, thus maximizing economic benefits.

Description

Technical Field

[0001] This invention belongs to the field of metallurgical technology, specifically relating to a method for detecting nickel in steelmaking dust, specifically an analytical method using inductively coupled plasma atomic emission spectrometry (ICP). Background Technology

[0002] Currently, there is no national standard method for the analysis of dust ash composition, and no relevant patents or literature have been published by various testing centers. In the paper "Research on Smelting Process of Stainless Steel Dust Ash" (document number 1672-4461(2013)01-0057-04), Jiuquan Iron & Steel Tianfeng Stainless Steel Co., Ltd. used an X-ray derivatization instrument to analyze the composition of dust ash. After our company used the analysis method in the literature and performed XRD analysis, the results showed a large discrepancy compared with those of the Shanghai Materials Research Institute.

[0003] Invention CN103278505A discloses a method for analyzing the composition of blast furnace dust based on multi-feature analysis. It employs a digital camera to acquire images and then utilizes a computer image processing system to analyze the composition of the blast furnace dust. This invention's method uses a computer system to process images and classify the components of blast furnace dust, demonstrating that a good automatic classification method can be found for blast furnace dust, thereby accurately and automatically analyzing its composition. Summary of the Invention

[0004] The carbon circular economy is a new model of sustainable development promoted by the international community today, emphasizing the most efficient use of resources and environmental protection. Steelmaking processes generate a large amount of dust, which is a valuable secondary resource. Reuse of this resource should be based on accurate compositional analysis. Our company's smelting process is EAF+VOD, which differs from traditional blast furnace carbon steel production. The proportions of elements in the dust collected are significantly different, with Ni being a crucial indicator for evaluating the grade of steelmaking dust.

[0005] The purpose of this invention is to provide an analytical method for Ni element in steelmaking dust. The analytical method uses an inductively coupled plasma atomic emission spectrometer (ICP). The process steps are simple and clear. It requires preparing the dust to be analyzed into a solution and then setting the equipment for automatic analysis. The breakthrough of this invention is the dissolution of the dust sample. This method has few interfering factors during the determination process, is simple and fast to operate, has good accuracy and precision, and has low labor intensity.

[0006] To achieve the above-mentioned objectives, the present invention provides the following technical solution: a method for detecting nickel in steelmaking dust, the technical solution of which is as follows:

[0007] S1. Standard sample used in the scheme: Dust collection ash No. 138-1; Inspection standard sample used in the scheme: Dust collection ash No. 137-6; Unless otherwise specified, all reagents used in the scheme are analytical grade solutions.

[0008] S2. Weigh 0.05g, 0.10g, and 0.20g of standard samples, weigh 0.10g of inspection sample, and weigh 0.10g of dust sample to be analyzed. Place each sample in a 250mL beaker, for a total of 5 samples.

[0009] S3. Weigh 10 mL of deionized water into a beaker, add 5 mL of concentrated nitric acid and 15 mL of concentrated hydrochloric acid, heat to dissolve for 50-60 minutes, set the heating plate to 350℃, rinse the watch glass and beaker walls twice with deionized water, and heat to concentrate the solution to 25 mL.

[0010] S4. Filter the dissolved solution from the beaker into a 100mL volumetric flask. If any sample residue adheres to the beaker wall, scrape it off with a glass rod and rinse thoroughly with deionized water. Place the filter residue along with the filter paper into a platinum crucible.

[0011] S5. Place the platinum crucible in a high-temperature furnace at 1000℃, ashing for 30 minutes, add 1g of flux, and melt for 30 minutes.

[0012] S6. After the platinum crucible is removed from the high-temperature furnace and cooled, place the crucible and its lid into the corresponding beaker, add 20 mL of 1:1 hydrochloric acid, cover with a watch glass, and tilt the beaker to allow a small amount of hydrochloric acid to flow out of the crucible, ensuring that the lid is soaked. Heat for pyrolysis. After a large number of bubbles are produced by the hydrochloric acid reaction in the crucible, the solution inside the crucible will become a clear yellow solution. Stop heating and remove the beaker. Use a glass rod to lift the lid of the crucible so that it stands upright. Remove the lid and the crucible, rinse them with deionized water, and heat to concentrate the solution to approximately 25 mL.

[0013] S7. Cooling solution, the concentrations in the standard sample bottle are as follows:

[0014]

[0015] The composition of standard sample 137-7 was as follows: Ni: 3.94%.

[0016] S8. After the solution in the beaker has cooled, transfer it to a volumetric flask and bring it to the mark.

[0017] S9. Analytical instrument model: Spark full-spectrum direct-reading plasma emission spectrometer (Germany); Generator parameters: plasma power 1400W, pump speed 30Rpm, cooling gas flow rate 13L / min, nebulizer flow rate 0.8 L / min.

[0018] Under the selected instrument operating conditions, a series of standard solutions were introduced into the inductively coupled plasma atomic emission spectrometer (ICP-AES). The analytical line intensities of nickel in the standard solutions were measured from low to high. A working curve was plotted with the mass fraction of nickel as the abscissa and the analytical line intensity as the ordinate. The results were obtained from the dust sample after calibration based on the inspection sample.

[0019] Compared with the prior art, the beneficial effects of the present invention are: simple steps, easy operation, fewer interference factors during the measurement process, less impact from human operation, high measurement accuracy, low labor intensity, suitable for industrial production, especially suitable for operation using inductively coupled plasma atomic emission spectrometry. Through accurate determination of the nickel composition of dust collection ash, the treatment and use of dust collection ash are based on evidence, reducing environmental pressure, and fully utilizing the value of secondary resources, maximizing economic benefits. Detailed Implementation

[0020] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Example

[0021] S1. Standard sample used in the scheme: Dust collection ash, No. 138-1; Inspection standard sample used in the scheme: Dust collection ash, No. 137-6. All reagents used in the scheme, unless otherwise specified, are analytical grade solutions.

[0022] S2. Weigh 0.05g, 0.10g, and 0.20g of standard samples, weigh 0.10g of inspection sample, and weigh 0.10g of dust sample to be analyzed. Place each sample in a 250mL beaker, for a total of 5 samples.

[0023] S3. Weigh 10 mL of deionized water into a beaker, add 5 mL of concentrated nitric acid and 15 mL of concentrated hydrochloric acid, heat to dissolve for 50-60 minutes, set the heating plate to 350℃, rinse the watch glass and beaker walls twice with deionized water, and heat to concentrate the solution to 25 mL.

[0024] S4. Filter the dissolved solution from the beaker into a 100mL volumetric flask. If any sample residue adheres to the beaker wall, scrape it off with a glass rod and rinse thoroughly with deionized water. Place the filter residue along with the filter paper into a platinum crucible.

[0025] S5. Place the platinum crucible in a high-temperature furnace at 1000℃, ashing for 30 minutes, add 1g of flux, and melt for 30 minutes.

[0026] S6. After the platinum crucible is removed from the high-temperature furnace and cooled, place the crucible and its lid into the corresponding beaker, add 20 mL of 1:1 hydrochloric acid, cover with a watch glass, and tilt the beaker to allow a small amount of hydrochloric acid to flow out of the crucible, ensuring that the lid is soaked. Heat for pyrolysis. After a large number of bubbles are produced by the hydrochloric acid reaction in the crucible, the solution inside the crucible will become a clear yellow solution. Stop heating and remove the beaker. Use a glass rod to lift the lid of the crucible so that it stands upright. Remove the lid and the crucible, rinse them with deionized water, and heat to concentrate the solution to approximately 25 mL.

[0027] S7. Cooling solution, the concentrations in the standard sample bottle are as follows:

[0028]

[0029] The composition of standard sample 137-7 was as follows: Ni: 3.94%.

[0030] S8. After the solution in the beaker has cooled, transfer it to a volumetric flask and bring it to the mark.

[0031] S9. Analytical instrument model: Spark full-spectrum direct-reading plasma emission spectrometer (Germany); Generator parameters: plasma power 1400W, pump speed 30Rpm, cooling gas flow rate 13L / min, nebulizer flow rate 0.8 L / min.

[0032] Under the selected instrument operating conditions, a series of standard solutions were introduced into the inductively coupled plasma atomic emission spectrometer (ICP-AES). The analytical line intensities of nickel in the standard solutions were measured from low to high. A working curve was plotted with the mass fraction of nickel as the abscissa and the analytical line intensity as the ordinate. The results were obtained from the dust sample after calibration based on the inspection sample.

Claims

1. A method for detecting nickel element in steelmaking dust, characterized in that: The detection method of the nickel element in the steelmaking dust collecting ash is specifically as follows: S1, the sample used in the scheme: dust collecting ash No. 138-1, the sample used in the scheme: dust collecting ash No. 137-6, and the reagent used in the scheme is not marked as an analytical pure solution; S2, weigh the sample weight of 0.05g, 0.10g, 0.20g, weigh the sample weight of 0.10g, weigh the sample weight of 0.10g, and place them in a 250mL beaker, a total of 5 test samples; S3, measure 10mL of deionized water and add it to the beaker, measure 5mL of concentrated nitric acid and 15mL of concentrated hydrochloric acid, heat and dissolve for 50-60min, set the heating plate temperature to 350℃, rinse the surface dish and beaker wall with deionized water twice, and heat and concentrate the solution volume to 25mL; S4, filter the dissolved solution in the beaker to a 100mL volumetric flask, if there is sample residue adhering to the beaker wall, use a glass rod to scrape it clean and rinse it with deionized water, and put the filter residue together with the filter paper into a platinum crucible; S5, place the platinum crucible in a high-temperature furnace at 1000℃, ash for 30min, add 1g of flux, and melt for 30min; S6, after cooling, place the crucible and the cover in the corresponding beaker, add 20mL of 1:1 hydrochloric acid, cover the surface dish, tilt the beaker, and let the hydrochloric acid in the crucible flow out a little to ensure that the cover is soaked, heat and decompose, and when the hydrochloric acid in the crucible reacts and a large amount of bubbles are generated, the solution in the crucible becomes clear and yellow, stop heating and remove the beaker, use a glass rod to lift the cover and make it stand, remove the cover and the crucible, and rinse them with deionized water, and heat and concentrate the solution volume to about 25mL; S7, cool the solution; S8, after the solution in the beaker cools down, transfer it to a volumetric flask and dilute to the scale; S9, under the selected instrument working conditions, introduce the standard series solution into the inductively coupled plasma atomic emission spectrometer, measure the analysis line intensity of the nickel element in the standard series solution from low to high, take the mass fraction of the nickel element as the horizontal coordinate and the analysis line intensity as the vertical coordinate, and draw a working curve; According to the calibration of the sample, the dust collecting ash sample is analyzed and the results are obtained.

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