CN111257258A - Method for detecting zinc in dust mud based on atomic absorption spectrum - Google Patents
Method for detecting zinc in dust mud based on atomic absorption spectrum Download PDFInfo
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- CN111257258A CN111257258A CN202010233941.5A CN202010233941A CN111257258A CN 111257258 A CN111257258 A CN 111257258A CN 202010233941 A CN202010233941 A CN 202010233941A CN 111257258 A CN111257258 A CN 111257258A
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- sample
- zinc
- dust mud
- test solution
- atomic absorption
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 46
- 239000011701 zinc Substances 0.000 title claims abstract description 46
- 239000000428 dust Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000000862 absorption spectrum Methods 0.000 title description 4
- 238000001514 detection method Methods 0.000 claims abstract description 18
- 238000001479 atomic absorption spectroscopy Methods 0.000 claims abstract description 16
- 239000012085 test solution Substances 0.000 claims description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 229910052799 carbon Inorganic materials 0.000 claims description 19
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 12
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 230000031700 light absorption Effects 0.000 claims description 6
- 230000005855 radiation Effects 0.000 claims description 5
- 238000002835 absorbance Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 239000012086 standard solution Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- 239000000779 smoke Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 2
- 238000000889 atomisation Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000003113 dilution method Methods 0.000 abstract description 3
- 229910052729 chemical element Inorganic materials 0.000 abstract description 2
- 239000000126 substance Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 229960001484 edetic acid Drugs 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- JUWSSMXCCAMYGX-UHFFFAOYSA-N gold platinum Chemical compound [Pt].[Au] JUWSSMXCCAMYGX-UHFFFAOYSA-N 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 235000013980 iron oxide Nutrition 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The invention belongs to the technical field of chemical element detection, and provides a method for detecting zinc in dust mud based on atomic absorption spectroscopy, wherein the atomic absorption spectroscopy has the advantages of less detection interference, high accuracy, low detection limit and high detection speed, and can be used for detecting samples with higher content by a dilution method, and is suitable for detecting samples with more complex dust mud components. The method can simplify the detection means of the zinc element in the dust and mud, reduce the reagents used for detection, and improve the efficiency, and is a simple and efficient detection method.
Description
Technical Field
The invention belongs to the technical field of chemical element detection, and provides a method for detecting zinc in dust mud based on atomic absorption spectroscopy.
Background
The high converter steelmaking process can generate a large amount of dust and mud, and the dust and mud contains a large amount of elements such as iron, carbon, calcium, zinc and the like, so that the recycling value is high. Before recycling, the contents of various elements in the dust and mud are firstly determined, and reliable data support is provided for recycling the dust and mud, so that the resource can be utilized to the maximum extent. Because the types of dust and mud are more, the content difference of various elements is larger, and no national standard method is used for detecting various elements in the dust and mud at present. In addition, the components of dust and mud samples are complex, the existing detection method of zinc element is mainly based on a chemical titration method, the main operations are that the samples are dissolved by acid, masking agent is added to mask interfering ions, EDTA (ethylene diamine tetraacetic acid) (with known accurate concentration) is used for titration, the percentage content of the zinc element is calculated, the procedure for detecting the zinc element in the dust and mud by a wet method is complicated, the consumed time is long, the types of added medicine reagents are many, and certain influence is caused on the environment.
Disclosure of Invention
In view of the above problems, the present invention provides a method for detecting zinc in dust mud based on atomic absorption spectroscopy, which is characterized in that: comprises the following steps of (a) carrying out,
step 1: weighing a sample, heating a muffle furnace to 800 ℃, putting the sample into the muffle furnace, volatilizing carbon elements in the sample in a high-temperature heating mode, heating for 30min to enable all carbon elements to be volatilized after carbon is completely leaked, taking out, and placing in a dryer for cooling. Adding acid solution to dissolve the solution to obtain dust mud test solution;
step 2: preparing a zinc standard solution with the diluted zinc content of 0.1-5.0%;
and step 3: and respectively measuring the absorbance of the zinc standard test solution and the dust mud test solution by adopting atomic absorption spectroscopy, and calculating the concentration of zinc in the dust mud test solution by taking a light absorption curve based on the concentration of the zinc standard test solution as a standard curve.
Further, in step 3, the light absorption curves of the zinc standard test solution and the dust mud test solution are respectively obtained by displaying the following operations, firstly, the dust mud test solution to be tested enters an atomizer, and enters air-acetylene flame after being atomized, wherein the temperature is 2300 ℃; the zinc hollow cathode lamp is adopted to emit monochromatic light with specific wavelength to pass through flame, zinc atoms absorb the monochromatic light with the specific wavelength, unabsorbed characteristic radiation light enters a spectrometer detection system through a monochromator and a slit, the residual characteristic radiation light is converted into an electric signal in a photomultiplier, and a light absorption curve of the electric signal is displayed on a reading device.
Further, transferring the sample after carbon leakage and cooling to a polytetrafluoroethylene beaker, adding hydrochloric acid according to the mass volume ratio of the sample to the hydrochloric acid of 0.01g/mL, adding hydrofluoric acid according to 0.02g/mL, adding perchloric acid according to 0.02g/mL after the sample is completely dissolved, removing the hydrofluoric acid until white dense smoke is emitted, stopping heating when the sample is viscous, and cooling the sample; adding hydrochloric acid into the cooled sample according to the volume ratio of the sample to the hydrochloric acid of 0.01g/mL, heating to dissolve salts in the sample, cooling, transferring the sample into a 100mL volumetric flask, and performing constant volume to obtain a dust mud test solution;
further, the monochromator separates other light radiation that does not need to be detected.
Further, the sample is placed in a porcelain boat and heated in a muffle furnace.
The invention has the advantages that:
the method has the advantages of less detection interference of atomic absorption spectrometry, high accuracy, low detection limit (the detection limit refers to the minimum concentration or minimum amount of a substance to be detected which can be detected from a sample by a certain analysis method within a given reliability degree), high detection speed, capability of detecting a sample with higher content by a dilution method, suitability for detecting a sample with more complex dust and mud components, capability of simplifying detection means of zinc in dust and mud, reduction of used reagents, cost saving, efficiency improvement, capability of detecting a dust and mud sample with higher zinc content by the dilution method, wide detection range, less generated waste and reduction of environmental pollution.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a method for detecting zinc in dust mud by utilizing atomic absorption spectroscopy. The dust and mud are produced by the process that molten steel is turned over and airflow on the surface of the melt is burst in the oxygen blowing smelting process of the converter, so that a certain amount of iron and iron oxides are evaporated and escape with the furnace gas, and fine particles of bulk materials are also brought into a flue by the furnace gas in the charging process. The flue gas is wetted by water and collected, and then is concentrated into converter dust mud. The method for detecting the zinc in the dust and mud by using the atomic absorption spectrum comprises the following specific steps:
step 1: sampling dust mud
Weigh 0.1000g (+ -0.0002 g), place in porcelain boat, run carbon in 800 degree muffle furnace for 30min, cool. Carbon running for 30 minutes is the most ideal carbon running time obtained by repeated experiments. The carbon element can not be volatilized completely in a short time, and the carbon element can be volatilized completely in a long time, but resources are wasted.
And volatilizing carbon elements in the dust mud sample by using high temperature. The acid-soluble sample is not allowed to have carbon element, and if the sample contains a certain amount of carbon element, the effect of next acid-soluble sample is influenced, so that the detection result is influenced.
Transferring to a polytetrafluoroethylene beaker (or a platinum gold beaker), adding 10ml of hydrochloric acid and 5ml of hydrofluoric acid, and heating on a high-temperature electric furnace to dissolve the sample. And after the sample is basically dissolved, adding 5ml of perchloric acid into the sample, continuing heating to further dissolve the sample and simultaneously driving hydrofluoric acid smoke. And (3) when the sample is completely dissolved and perchloric acid is completely volatilized, stopping heating, cooling the sample, keeping the sample in a small volume, and controlling the acidity. To the cooled sample, 10ml of hydrochloric acid (1+1) was added, and the sample was heated to dissolve salts in the sample. And (6) cooling. The sample was transferred to a 100ml volumetric flask and the volume was fixed.
Hydrochloric acid and hydrofluoric acid are added in the operation step to dissolve the sample, and perchloric acid is added to drive the hydrofluoric acid. Hydrochloric acid and hydrofluoric acid must be added firstly, and perchloric acid is added after the sample is dissolved. The adding amount is based on the corresponding optimal proportion amount after the muffle furnace runs carbon for 30min at 800 ℃ and is cooled, so that the sample can be fully dissolved, and the medicine is not wasted. Occasionally, 800 ℃ is found to be the most ideal carbon running temperature, the temperature is too low to reach the carbon volatilization temperature, and the surface layer of the sample is hardened by too high temperature, but the carbon in the sample cannot volatilize and escape.
Step 2: preparation of Standard solution
Taking 1000 mu g/ml of national standard test solution of zinc, diluting the national standard test solution of zinc step by step to obtain standard test solutions of 50 mu g/ml,25 mu g/ml,10 mu g/ml, 5 mu g/ml and 2.5 mu g/ml, and preparing a zinc standard solution with the diluted zinc content of 0.1-5.0% according to experimental needs.
And step 3: atomic absorption spectroscopy
The atomic absorption spectrum is used for determining the content of an element to be detected based on the absorption degree of ground state atoms in a sample to a characteristic spectral line of the element. When the experimental conditions such as temperature, absorption optical path, sample introduction mode and the like are fixed, the element phase fundamental state atoms generated by the sample absorb monochromatic light radiated by the hollow cathode lamp of the element serving as an acute line light source, and the absorbance (A) of the monochromatic light is in direct proportion to the concentration (C) of the element in the sample. That is, in the formula, a ═ KC, K is a constant. Therefore, the concentration of zinc in the test solution prepared from the dust mud can be obtained by measuring the absorbance of the zinc standard test solution and the test solution prepared from the dust mud and knowing the concentration of the zinc standard test solution.
Firstly, the zinc standard test solution is measured one by one, and the instrument automatically makes a zinc standard curve. And measuring the sample test solution of the dust mud, and obtaining the content of zinc in the dust mud according to a standard curve. If the zinc content in the dust mud is higher and exceeds the range of the zinc standard curve, diluting the sample and then measuring.
The experimental result data are as follows:
| serial number | Sample 1 (%) | Sample 2 (%) | Sample 3 (%) |
| Chemical titration method | 4.28 | 8.23 | 15.37 |
| Atomic absorption spectroscopy | 4.42 | 8.42 | 15.22 |
| Error of the measurement | 0.14 | 0.19 | 0.15 |
The accuracy of the measurement result is good, and the requirement of chemical analysis errors is met.
Comparing the zinc element in the mud by atomic absorption spectrometry with the zinc element in the mud by wet method, the obtained result is as follows:
from the comparison results, it can be found that the atomic absorption spectrometry uses less chemical drugs and has short analysis time, thus being an accurate and efficient analysis method.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (4)
1. A method for detecting zinc in dust mud based on atomic absorption spectroscopy is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
step 1: weighing a sample, heating a muffle furnace to 800 ℃, placing the sample in the furnace, heating for 30min to completely volatilize carbon elements, taking out the sample, placing the sample in a dryer for cooling, and adding an acid solution for dissolving to obtain a dust mud test solution;
step 2: preparing a zinc standard solution with the diluted zinc content of 0.1-5.0%;
and step 3: and respectively measuring the absorbance of the zinc standard test solution and the dust mud test solution by adopting atomic absorption spectroscopy, and calculating the concentration of zinc in the dust mud test solution by taking a light absorption curve based on the concentration of the zinc standard test solution as a standard curve.
2. The method for detecting zinc in dust mud based on atomic absorption spectroscopy as claimed in claim 1, wherein: in step 3, the light absorption curves of the zinc standard test solution and the dust mud test solution are respectively obtained by the following operation display, firstly, the liquid to be tested enters an atomizer, and enters air-acetylene flame after atomization, wherein the temperature is 2300 ℃; the zinc hollow cathode lamp is adopted to emit monochromatic light with specific wavelength to pass through flame, zinc atoms absorb the monochromatic light with the specific wavelength, unabsorbed characteristic radiation light enters a spectrometer detection system through a monochromator and a slit, the residual characteristic radiation light is converted into an electric signal in a photomultiplier, and a light absorption curve of the electric signal is displayed on a reading device.
3. The method for detecting zinc in dust mud based on atomic absorption spectroscopy as claimed in claim 1, wherein: transferring the sample after carbon leakage and cooling to a polytetrafluoroethylene beaker, adding hydrochloric acid according to the mass-to-volume ratio of the sample to the hydrochloric acid of 0.01g/mL, adding hydrofluoric acid according to 0.02g/mL, adding perchloric acid according to 0.02g/mL when the sample is completely dissolved, stopping heating until white dense smoke is emitted and the sample is sticky, and cooling; and adding hydrochloric acid into the sample according to the volume ratio of the sample to the hydrochloric acid of 0.01g/mL, heating, dissolving and cooling, transferring the sample into a 100mL volumetric flask, and performing constant volume to obtain a dust mud test solution.
4. The method for detecting zinc in dust mud based on atomic absorption spectroscopy as claimed in claim 1, wherein: the sample is placed in a porcelain boat and heated in a muffle furnace.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010233941.5A CN111257258A (en) | 2020-03-30 | 2020-03-30 | Method for detecting zinc in dust mud based on atomic absorption spectrum |
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| CN202010233941.5A CN111257258A (en) | 2020-03-30 | 2020-03-30 | Method for detecting zinc in dust mud based on atomic absorption spectrum |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112147093A (en) * | 2020-07-29 | 2020-12-29 | 特康药业集团有限公司 | Method for detecting mineral elements in formula food with special medical application |
| RU2767313C1 (en) * | 2020-10-26 | 2022-03-17 | федеральное государственное бюджетное образовательное учреждение высшего образования "Алтайский государственный университет" | Low-melting extractant and method for extracting zinc (ii) from acidic aqueous solutions |
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| RU2767313C1 (en) * | 2020-10-26 | 2022-03-17 | федеральное государственное бюджетное образовательное учреждение высшего образования "Алтайский государственный университет" | Low-melting extractant and method for extracting zinc (ii) from acidic aqueous solutions |
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