CN113433115A - Method for measuring lead and zinc content in direct reduced iron - Google Patents
Method for measuring lead and zinc content in direct reduced iron Download PDFInfo
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- CN113433115A CN113433115A CN202110630919.9A CN202110630919A CN113433115A CN 113433115 A CN113433115 A CN 113433115A CN 202110630919 A CN202110630919 A CN 202110630919A CN 113433115 A CN113433115 A CN 113433115A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a method for measuring the content of lead and zinc in direct reduced iron, which comprises the steps of sample treatment, working curve standard solution preparation and sample measurement. The method adopts the plasma atomic emission spectrometry to measure the contents of lead and zinc in the direct reduced iron, so that two elements are simultaneously measured, the chemical reagent is saved, the pollution to the environment is reduced, the labor cost is reduced, and the working efficiency is improved. The method can rapidly and accurately analyze the content of lead and zinc in the direct reduced iron, is beneficial to the production of direct reduced iron products and the good application of the direct reduced iron products in steel smelting, avoids the generation of waste products, and plays a good role in supervision and risk control for saving resources.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and particularly relates to a method for measuring the content of lead and zinc in direct reduced iron.
Background
In the steel smelting process, direct reduced iron is sometimes added into molten iron to accelerate the steel smelting and improve the quality of steel. However, with the research and development and production of the direct reduced iron product, analytical research on a plurality of chemical components in the direct reduced iron is carried out by the Kunzi steel technology center by applying the existing detection technology and means, and researches find that some chemical components have good influence on the quality of the direct reduced iron and some chemical components are harmful elements of the direct reduced iron. Lead and zinc are harmful elements of the direct reduced iron, so that the content of lead and zinc in the direct reduced iron needs to be accurately analyzed so as to monitor the quality of the direct reduced iron and prevent unqualified direct reduced iron products from being produced.
At present, no national standard and industrial standard are made for measuring the content of lead and zinc in the direct reduced iron. In the prior art, the content of lead and zinc is measured by different methods and different reagents by a photometric method, and the content of lead and zinc cannot be measured simultaneously by the photometric method. In addition, the photometric method uses a large amount of chemical reagents and glassware, and has the disadvantages of long analysis time, high cost, low working efficiency and environmental pollution. In addition, as atomic absorption spectrometry has a narrow linear range, a sample with a high content is often subjected to liquid separation and dilution, which is prone to cause errors. In addition, the atomic absorption spectrometry is also used for separately measuring the contents of lead and zinc twice, and cannot simultaneously measure the contents of lead and zinc. Therefore, it is very necessary to develop a method for measuring the content of lead and zinc in direct reduced iron that can solve the above problems.
Disclosure of Invention
The invention aims to provide a method for measuring the content of lead and zinc in direct reduced iron, which has the advantages of high analysis accuracy, high analysis speed, low labor cost and small environmental pollution.
The invention aims to provide a method for measuring the content of lead and zinc in direct reduced iron, which comprises the steps of sample treatment, working curve standard solution preparation and sample measurement, and specifically comprises the following steps:
1) sample processing
Weighing the sample to be measured in a steel measuring flask according to the ratio of 50-600ml/gTest specimenAdding hydrochloric acid, heating to dissolve to obtain a mixed solution, adding 1/6-1/2 volume of nitric acid into the mixed solution, continuously dissolving until the nitric acid smoke is exhausted, and large bubbles appear on the liquid surface, taking down, cooling, and shaking to a constant volume to obtain a sample solution to be tested;
2) preparation of working curve standard solution
A. Dissolving 7 parts of sample blank solution according to the sample treatment process in the step 1;
B. respectively adding 0mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL and 10.00mL of lead and zinc standard stock solutions into the 7 sample blank solutions in the step A;
3) sample measurement
And (3) measuring the spectral intensity of the lead and zinc standard solutions by using a plasma atomic emission spectrometer, and sequentially measuring the element contents of lead and zinc in the sample to be measured according to a working curve drawn by the emission intensity and the concentration of the lead and the zinc.
The method adopts the plasma atomic emission spectrometry to measure the contents of lead and zinc in the direct reduced iron, leads the two elements to be measured simultaneously, has strong innovation, saves chemical reagents, reduces the pollution to the environment, reduces the labor cost, improves the working efficiency, can quickly and accurately analyze the contents of lead and zinc in the direct reduced iron, is beneficial to the production of direct reduced iron products and the good application of the direct reduced iron products in the steel smelting, avoids the generation of waste products, and plays a good role in monitoring and controlling risks for saving resources.
Compared with the prior art, the invention has the following advantages:
(1) compared with the conventional photometric method, the analysis method can simultaneously determine the content of lead and zinc, uses less chemical reagents, has high analysis speed and little environmental pollution, and reduces the labor intensity of analysis operators.
(2) Compared with an atomic absorption spectrometry, the analysis method adopted by the invention can simultaneously determine the elements of lead and zinc, has wide linear range, only needs to increase more high-content points of the standard solution in the working curve for a high-content sample, and does not need to take, separate and dilute the sample, thereby reducing the determination error.
(3) Repeated tests prove that the measuring result obtained by the method has good stability, reproducibility and accuracy.
(4) Practice proves that the method is reliable and practical, and can meet the requirement of measuring the content of lead and zinc in the daily direct reduced iron.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to be limiting in any way, and any variations or modifications which are based on the teachings of the present invention are intended to fall within the scope of the present invention.
The reagents adopted by the invention are all analytical pure reagents, and the water is deionized water.
The invention relates to a method for measuring the content of lead and zinc in direct reduced iron, which comprises the steps of sample treatment, working curve standard solution preparation and sample measurement, and specifically comprises the following steps:
1) sample processing
Weighing the sample to be measured in a steel measuring flask according to the ratio of 50-600ml/gTest specimenAdding hydrochloric acid, heating to dissolve to obtain a mixed solution, adding 1/6-1/2 volume of nitric acid into the mixed solution, continuously dissolving until the nitric acid smoke is exhausted, and large bubbles appear on the liquid surface, taking down, cooling, and shaking to a constant volume to obtain a sample solution to be tested;
2) preparation of working curve standard solution
A. Dissolving 7 parts of sample blank solution according to the sample treatment process in the step 1;
B. respectively adding 0mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL and 10.00mL of lead and zinc standard stock solutions into the 7 sample blank solutions in the step A;
3) sample measurement
And (3) measuring the spectral intensity of the lead and zinc standard solutions by using a plasma atomic emission spectrometer, and sequentially measuring the element contents of lead and zinc in the sample to be measured according to a working curve drawn by the emission intensity and the concentration of the lead and the zinc.
In the step 1, the density of the hydrochloric acid is 1.19 g/mL.
In the step 1, the heating dissolution is carried out for 5-15min at the temperature of 80-100 ℃.
In the step 2, the concentration of the lead standard stock solution is 100 mug/ml, and the preparation method comprises the following steps: weighing 0.1000g of pure lead with the purity of more than 99.9 percent, dissolving the pure lead with 20mL of 1+1 nitric acid, boiling to remove nitrogen oxide, cooling to room temperature, transferring the solution into a 1000mL volumetric flask, fixing the volume with distilled water or pure water, and shaking up to obtain a lead standard stock solution.
In the step 2, the concentration of the zinc standard stock solution is 100 mug/ml, and the preparation method comprises the following steps: 0.1245g of pure zinc with the purity of more than 99.9 percent is weighed, the reference zinc oxide which is burned to a constant amount at 1000 ℃ in advance and cooled in a dryer is dissolved by 30mL of 1+1 hydrochloric acid, diluted by 30mL of water and transferred into a 1000mL volumetric flask, and the volume is constant by using distilled water or pure water and shaken uniformly to obtain the zinc standard stock solution.
In the step 2, the mass percentage concentrations of lead and zinc in 7 parts of standard solution are respectively 0, 0.10%, 0.20%, 0.40%, 0.60%, 0.80% and 1.00%.
The working conditions of the plasma atomic emission spectrometer are as follows: the RF power of the high-frequency generator is 1100-1200W, the atomization pressure is 26.08PSi, the auxiliary gas flow is 0.5L/min, the flushing pump speed is 50rpm/min, the sample flushing time is 3s, the exposure time is 15s, the wavelength of the lead analysis line is 220.353, the series is 453, and the wavelength of the zinc analysis line is 206.200 and the series is 463.
The present invention is further illustrated by the following examples.
EXAMPLE 1 Standard stock solution preparation
Lead standard stock solution preparation: weighing 0.1000g of pure lead with the purity of more than 99.9 percent, dissolving the pure lead with 20mL of 1+1 nitric acid, boiling to remove nitrogen oxide, cooling to room temperature, transferring the solution into a 1000mL volumetric flask, fixing the volume with distilled water or pure water, and shaking up to obtain a 100 mu g/mL lead standard stock solution.
Preparation of zinc standard stock solution: 0.1245g of pure zinc with the purity of more than 99.9 percent is weighed, the reference zinc oxide which is burned to a constant amount at 1000 ℃ in advance and cooled in a dryer is dissolved by 30mL of 1+1 hydrochloric acid, diluted by 30mL of water, transferred into a 1000mL volumetric flask, and is subjected to constant volume by using distilled water or pure water and shaking up to obtain 100 mu g/mL of zinc standard stock solution.
Example 2
Weighing 0.1000g of sample into a 100mL steel measuring flask, adding 20mL of hydrochloric acid (rho 1.19g/mL) to dissolve for 10min on an electric furnace at 100 ℃, adding 8mL of nitric acid (rho 1.42g/mL), continuously dissolving until the nitric acid smoke is exhausted, taking down the sample until large bubbles appear on the liquid level, cooling, and carrying out constant volume shaking uniformly to obtain the sample liquid to be tested.
Adding 20mL of hydrochloric acid into 7 100mL steel measuring bottles, heating and dissolving for 10min on an electric furnace at 100 ℃, adding 8mL of nitric acid, continuously dissolving until the nitric acid smoke is exhausted, and large bubbles appear on the liquid surface, taking down, cooling, and shaking up to constant volume; then 0mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL and 10.00mL of the standard stock solution of lead and zinc prepared in example 1 are respectively added into 7 parts of the blank solution of the sample and shaken to obtain the standard solution series of lead and zinc respectively, the spectral intensity of lead and zinc is measured by a plasma atomic emission spectrometer, the spectral intensity-mass fraction working curve of the element to be measured is drawn by taking the element content as the abscissa and the spectral intensity as the ordinate, and the correlation coefficient of each working curve is more than 0.999.
And (3) introducing the sample solution to be tested into a plasma atomic emission spectrometer to measure the spectral intensity of lead and zinc, and finding out that the content of lead and the content of zinc in the direct reduced iron sample to be tested are 0.20% and 0.35% respectively on the working curve.
The operating conditions of the plasma atomic emission spectrometer in this example are shown in tables 1 and 2.
TABLE 1 working conditions of the apparatus
TABLE 2 wavelength of the element to be measured and the spectral line
| Element(s) | Wavelength (nm) |
| Pb | 220.353 |
| Zn | 206.200 |
Example 3
Weighing 0.1000g of sample into a 100mL steel measuring flask, adding 60mL of hydrochloric acid (rho 1.19g/mL) to dissolve for 15min on an electric furnace at 90 ℃, adding 30mL of nitric acid (rho 1.42g/mL), continuously dissolving until the nitric acid smoke is exhausted, taking down the sample until large bubbles appear on the liquid level, cooling, and carrying out constant volume shaking uniformly to obtain the sample liquid to be tested.
The sample solution to be tested was introduced into a plasma atomic emission spectrometer to measure the spectral intensity of lead and zinc, and the content of lead and the content of zinc in the directly reduced iron sample to be tested were found to be 0.21% and 0.34% respectively on the working curve in example 2.
The working conditions of the plasma atomic emission spectrometer in this example are the same as in example 2.
Example 4
Weighing 0.1000g of sample into a 100mL steel measuring flask, adding 5mL of hydrochloric acid (rho 1.19g/mL) to dissolve for 5min on an electric furnace at 80 ℃, adding 1mL of nitric acid (rho 1.42g/mL), continuously dissolving until the nitric acid smoke is exhausted, taking down the sample until large bubbles appear on the liquid level, cooling, and carrying out constant volume shaking uniformly to obtain the sample liquid to be tested.
The sample solution to be tested is introduced into a plasma atomic emission spectrometer to measure the spectral intensity of lead and zinc, and the content of lead and the content of zinc in the direct reduced iron sample to be tested are respectively found to be 0.20% and 0.36% on the working curve in the embodiment 2.
The working conditions of the plasma atomic emission spectrometer in this example are the same as in example 2.
Claims (7)
1. A method for measuring the content of lead and zinc in direct reduced iron is characterized by comprising the steps of sample treatment, working curve standard solution preparation and sample measurement, and specifically comprises the following steps:
1) sample processing
Weighing the sample to be measured in a steel measuring flask according to the ratio of 50-600ml/gTest specimenAdding hydrochloric acid, heating to dissolve to obtain mixed solution, adding 1/6-1/2 volume of nitric acid, and dissolvingDissolving until the nitric acid smoke is exhausted, taking down the liquid surface and cooling the liquid surface when large bubbles appear, and performing constant volume shaking to obtain a sample liquid to be tested;
2) preparation of working curve standard solution
A. Dissolving 7 parts of sample blank solution according to the sample treatment process in the step 1;
B. respectively adding 0mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL and 10.00mL of lead and zinc standard stock solutions into the 7 sample blank solutions in the step A;
3) sample measurement
And (3) measuring the spectral intensity of the lead and zinc standard solutions by using a plasma atomic emission spectrometer, and sequentially measuring the element contents of lead and zinc in the sample to be measured according to a working curve drawn by the emission intensity and the concentration of the lead and the zinc.
2. The assay method according to claim 1, wherein in step 1, the density of hydrochloric acid is 1.19 g/mL.
3. The method according to claim 1, wherein the dissolution by heating in step 1 is carried out at 80 to 100 ℃ for 5 to 15 minutes.
4. The determination method according to claim 1, wherein in the step 2, the concentration of the lead standard stock solution is 100 μ g/ml, and the configuration method comprises the following steps: weighing 0.1000g of pure lead with the purity of more than 99.9 percent, dissolving the pure lead with 20mL of 1+1 nitric acid, boiling to remove nitrogen oxide, cooling to room temperature, transferring the solution into a 1000mL volumetric flask, fixing the volume with distilled water or pure water, and shaking up to obtain a lead standard stock solution.
5. The determination method according to claim 1, wherein in the step 2, the concentration of the zinc standard stock solution is 100 μ g/ml, and the configuration method comprises the following steps: 0.1245g of pure zinc with the purity of more than 99.9 percent is weighed, the reference zinc oxide which is burned to a constant amount at 1000 ℃ in advance and cooled in a dryer is dissolved by 30mL of 1+1 hydrochloric acid, diluted by 30mL of water and transferred into a 1000mL volumetric flask, and the volume is constant by using distilled water or pure water and shaken uniformly to obtain the zinc standard stock solution.
6. The method according to claim 1, wherein in the step 2, the lead and zinc concentrations in 7 parts of the standard solution are 0, 0.10%, 0.20%, 0.40%, 0.60%, 0.80%, and 1.00% by mass, respectively.
7. The method of claim 1, wherein the plasma atomic emission spectrometer is operated under the following conditions: the RF power of the high-frequency generator is 1100-1200W, the atomization pressure is 26.08PSi, the auxiliary gas flow is 0.5L/min, the flushing pump speed is 50rpm/min, the sample flushing time is 3s, the exposure time is 15s, the wavelength of the lead analysis line is 220.353, the series is 453, and the wavelength of the zinc analysis line is 206.200 and the series is 463.
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2021
- 2021-06-07 CN CN202110630919.9A patent/CN113433115A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102565025A (en) * | 2010-12-15 | 2012-07-11 | 鞍钢股份有限公司 | Method for measuring content of aluminum, silicon and zinc in coating of aluminum-plated zinc plate |
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