CN115950717A - Method for detecting nickel element in steelmaking dust-collecting ash - Google Patents

Abstract

The invention discloses a method for detecting nickel element in steelmaking dust-collecting ash, wherein the device used in the method is an inductively coupled plasma emission spectrometer (ICP), the process steps are simple and clear, the dust to be analyzed is required to be prepared into solution, and then the device is set for automatic analysis.

Description

Method for detecting nickel element in steelmaking dust-collecting ash

Technical Field

The invention belongs to the technical field of smelting, and particularly relates to a method for detecting nickel elements in steelmaking dust-collecting ash, in particular to an analysis method by utilizing an inductively coupled plasma emission spectrometer (ICP).

Background

At present, no national standard corresponding method exists for analyzing the components of the fly ash, no relevant patent and literature are published in each detection center, the components of the fly ash are analyzed by an X-ray derivative instrument by wine steel Tianfeng stainless steel Limited company in document number 1672-4461 (2013) 01-0057-04 stainless steel fly ash smelting process research, and the deviation of the analysis result of the document analysis method analyzed by XRD and the analysis result of Shanghai material research institute is larger.

The invention of CN103278505A is a blast furnace dust-removal ash component analysis method based on multi-feature analysis, which adopts a digital camera to collect images and then utilizes a computer image processing system to analyze the blast furnace dust-removal ash component. The method of the invention processes the image through the computer system to obtain the blast furnace dust component classification, which shows that the blast furnace dust can completely find a good automatic classification method, thereby accurately and automatically analyzing the components of the dust.

Disclosure of Invention

Carbon recycling economy is a new mode of practice for the sustainable development of today's international society push, emphasizing the most efficient use of resources and environmental protection. A large amount of dust removal products are generated in the steelmaking process of steel enterprises, the dust removal products are precious secondary resources, the reutilization of resources is on the premise of accurate component analysis, the smelting process is EAF + VOD, the method is different from the traditional blast furnace carbon steel production, the element proportion in the dust is greatly different, and the Ni element is an important index for evaluating the grade of the steelmaking dust.

The invention aims to provide an analysis method of Ni element in steelmaking fly ash, the equipment used in the analysis method is an inductively coupled plasma emission spectrometer (ICP), the process steps are simple and clear, the fly ash to be analyzed needs to be prepared into solution, and then the equipment is set for automatic analysis.

In order to achieve the above object, the present invention provides the following technical solutions: a method for detecting nickel element in steelmaking dust-collecting ash, which adopts the technical scheme as follows:

s1, standard sample used in the scheme: dust collection number 138-1, protocol used inspection standard: the number of the dust collection ash is 137-6. Reagents used in the scheme are not indicated to be analytically pure solutions;

s2, weighing standard samples with the weights of 0.05g, 0.10g and 0.20g respectively, weighing 0.10g of an inspection sample and 0.10g of a dust collection sample to be analyzed, respectively placing the samples in 250mL beakers, and weighing 5 parts of samples in total;

s3, weighing 10mL of deionized water in a measuring cup, adding the deionized water into the beaker, weighing 5mL of concentrated nitric acid, weighing 15mL of concentrated hydrochloric acid, heating and dissolving for 50-60min, setting the temperature of a heating plate at 350 ℃, washing a surface dish and the wall of the beaker with the deionized water twice, and heating and concentrating the volume of the solution to 25mL.

And S4, filtering the solution dissolved in the beaker into a 100mL volumetric flask, and if sample residues are adhered to the wall of the beaker, scraping the sample residues with a glass rod and washing the sample residues with deionized water. And putting the filter residue and the filter paper into a platinum crucible.

S5, putting the platinum crucible into a high-temperature furnace at 1000 ℃, ashing for 30min, adding 1g of fluxing agent, and melting for 30min.

S6, after the platinum crucible is taken out of the high-temperature furnace and cooled, the crucible and the crucible cover are placed into an original corresponding beaker, 20mL1 hydrochloric acid is added, a surface dish is covered, the beaker is held by hand to be inclined, a small amount of hydrochloric acid in the crucible flows out, the crucible cover is guaranteed to be soaked and heated and pyrolyzed, after a large amount of bubbles are formed in hydrochloric acid reaction in the crucible, the crucible becomes clear yellow solution, heating is stopped, the beaker is taken down, the crucible cover is lifted up by a glass rod to be vertically placed, the crucible cover and the crucible are taken out, deionized water is used for purging, and the volume of the concentrated solution is heated to about 25mL.

S7, cooling the solution, wherein the concentration of the standard sample in the bottle is as follows

Examination of standard 137-7 composition: ni:3.94 percent.

And S8, transferring the solution in the beaker to a volumetric flask after the solution is cooled, and metering the volume to a scale.

S9, the type of an analytical instrument: a German Spack full-spectrum direct-reading plasma emission spectrometer; generator parameters: the plasma power is 1400W, the pump rotating speed is 30Rpm, the cooling gas flow is 13L/min, and the atomizer flow is 0.8L/min.

Under the working condition of a selected instrument, introducing the standard series solution into an inductively coupled plasma atomic emission spectrometer, measuring the analysis line intensity of nickel elements in the standard series solution from low to high, and drawing a working curve by taking the mass fraction of the nickel elements as a horizontal coordinate and the analysis line intensity as a vertical coordinate; and analyzing the result according to the dust collection ash sample after checking the calibration of the sample.

Compared with the prior art, the invention has the beneficial effects that: the method has the advantages of simple steps, easy operation, few interference factors in the determination process, small influence of manual operation, high determination precision, low labor intensity, suitability for industrial production, particular suitability for operation of an atomic emission spectrometry instrument utilizing inductively coupled plasma, reliable determination of the nickel component in the dust-collecting ash, complete and sufficient utilization of secondary resources on the basis of reducing environmental protection pressure and maximization of economic benefit, and is suitable for operation of an atomic emission spectrometry instrument utilizing the dust-collecting ash.

Detailed Description

The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.

Examples

S1, standard samples used in the scheme: dust collection number 138-1, protocol used inspection standard: the number of the dust collection ash is 137-6. Reagents used in the scheme are not indicated to be analytically pure solutions;

s2, weighing standard samples with the weight of 0.05g, 0.10g and 0.20g respectively, weighing 0.10g of inspection sample and 0.10g of dust collection ash sample to be analyzed, and placing the samples in 250mL beakers for 5 parts in total;

s3, weighing 10mL of deionized water in a measuring cup, adding the deionized water into the beaker, weighing 5mL of concentrated nitric acid, weighing 15mL of concentrated hydrochloric acid, heating and dissolving for 50-60min, setting the temperature of a heating plate at 350 ℃, washing a surface dish and the wall of the beaker with the deionized water twice, and heating and concentrating the volume of the solution to 25mL.

And S4, filtering the solution dissolved in the beaker to a 100mL volumetric flask, and if sample residues are adhered to the wall of the beaker, scraping the sample residues with a glass rod and washing the sample residues with deionized water. And putting the filter residue and the filter paper into a platinum crucible.

S5, putting the platinum crucible into a high-temperature furnace at 1000 ℃, ashing for 30min, adding 1g of fluxing agent, and melting for 30min.

S6, after the platinum crucible is taken out of the high-temperature furnace and cooled, the crucible and the crucible cover are placed into an original corresponding beaker, 20mL1 hydrochloric acid is added, a surface dish is covered, the beaker is held by hand to be inclined, a small amount of hydrochloric acid in the crucible flows out, the crucible cover is guaranteed to be soaked and heated and pyrolyzed, after a large amount of bubbles are formed in hydrochloric acid reaction in the crucible, the crucible becomes clear yellow solution, heating is stopped, the beaker is taken down, the crucible cover is lifted up by a glass rod to be vertically placed, the crucible cover and the crucible are taken out, deionized water is used for purging, and the volume of the concentrated solution is heated to about 25mL.

S7, cooling the solution, wherein the concentration in the standard sample bottle is as follows

Examination of standard 137-7 composition: ni:3.94 percent.

And S8, transferring the solution in the beaker to a volumetric flask after the solution is cooled, and fixing the volume to the scale.

S9, the type of an analytical instrument: a German Spack full-spectrum direct-reading plasma emission spectrometer; generator parameters: the plasma power is 1400W, the pump rotating speed is 30Rpm, the cooling gas flow is 13L/min, and the atomizer flow is 0.8L/min.

Under the working condition of a selected instrument, introducing the standard series solution into an inductively coupled plasma atomic emission spectrometer, measuring the analysis line intensity of nickel elements in the standard series solution from low to high, and drawing a working curve by taking the mass fraction of the nickel elements as a horizontal coordinate and the analysis line intensity as a vertical coordinate; the dust ash sample analyzed the results after checking the sample calibration.

Claims (1)

1. A method for detecting nickel element in steelmaking dust-collecting ash is characterized by comprising the following steps: the method for detecting the nickel element in the steelmaking dust-collecting ash comprises the following specific steps:

s1, standard samples used in the scheme: dust collection number 138-1, protocol used inspection standard: the number of the dust collection ash is 137-6, and reagents used in the scheme are not all analytical pure solutions;

s2, weighing standard samples with the weights of 0.05g, 0.10g and 0.20g respectively, weighing 0.10g of an inspection sample and 0.10g of a dust collection sample to be analyzed, respectively placing the samples in 250mL beakers, and weighing 5 parts of samples in total;

s3, weighing 10mL of deionized water in a measuring cup, adding the deionized water into the beaker, weighing 5mL of concentrated nitric acid, weighing 15mL of concentrated hydrochloric acid, heating and dissolving for 50 to 60min, setting the temperature of a heating plate at 350 ℃, washing a watch glass and the wall of the beaker with the deionized water twice, and heating and concentrating the volume of the solution to 25mL;

s4, filtering the solution dissolved in the beaker into a 100mL volumetric flask, if sample slag is adhered to the wall of the beaker, scraping the sample slag with a glass rod, washing the sample slag with deionized water, and putting filter residues and filter paper into a platinum crucible;

s5, putting the platinum crucible into a high-temperature furnace at 1000 ℃, ashing for 30min, adding 1g of fluxing agent, and melting for 30min;

s6, after the platinum crucible is taken out of the high-temperature furnace and cooled, placing the crucible and a crucible cover into an original corresponding beaker, adding 20mL1 hydrochloric acid, covering a surface dish, holding the beaker to incline, enabling a small amount of hydrochloric acid in the crucible to flow out, so as to ensure that the crucible cover is soaked, heating and pyrolyzing, after a large amount of bubbles are formed in the hydrochloric acid reaction in the crucible, changing the crucible into a clear yellow solution, stopping heating and taking off the beaker, picking up the crucible cover with a glass rod to enable the crucible cover to stand, taking out the crucible cover and the crucible, purging with deionized water, and heating the volume of the concentrated solution to about 25mL;

s7, cooling the solution;

s8, transferring the solution in the beaker to a volumetric flask after the solution is cooled, and fixing the volume to a scale;

s9, introducing the standard series solution into an inductively coupled plasma atomic emission spectrometer under the selected working condition of the instrument, measuring the analysis line intensity of the nickel element in the standard series solution from low to high, and drawing a working curve by taking the mass fraction of the nickel element as a horizontal coordinate and the analysis line intensity as a vertical coordinate; and analyzing the result according to the dust collection ash sample after checking the calibration of the sample.