CN-120271835-B - Iron ion detection fluorescent probe, application and fluorescent detection method

Abstract

The invention relates to a fluorescent probe for detecting iron ions, application and a fluorescent detection method, belongs to the technical field of iron content detection, and solves the technical problems of complex operation, time consumption and the like in iron content detection in magnesium oxide. The preparation method of the fluorescent probe comprises the steps of firstly weighing pyrazine-2, 3,5, 6-tetracarboxylic acid and Zn (NO) 3 , dissolving in a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide, stirring to obtain a mixed solution, secondly, placing the mixed solution obtained in the first step into an oven for continuous heating to obtain white transparent bulk crystals, and washing, filtering, drying and grinding the white transparent bulk crystals to obtain the fluorescent probe. The invention synthesizes a novel zinc-based compound by a solvothermal method, and can be used as a fluorescent probe for fluorescent detection of iron ions in magnesium oxide, so that trace detection of the iron ions can be realized, and low-magnetism magnesium oxide with iron content meeting the requirements of industry standards can be screened out.

Inventors

• DING BO
• YAO WEI
• GAO ENJUN

Assignees

• 山西山川新材料有限公司

Dates

Publication Date

20260508

Application Date

20250407

Claims (5)

1. 1. An iron ion detection fluorescent probe, characterized in that the molecular formula of the fluorescent probe is (Zn 2 (C 8 O 8 N 2 H 2 )·DMSO·HCOOH) n ; the preparation method of the fluorescent probe comprises the following steps: Weighing pyrazine-2, 3,5, 6-tetracarboxylic acid and Zn (NO 3 ) 2 is dissolved in a mixed solvent of N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO), stirring to obtain a mixed solution, wherein the mass ratio of pyrazine-2, 3,5, 6-tetracarboxylic acid to Zn (NO 3 ) 2 is 1:6, and the volume ratio of N, N-Dimethylformamide (DMF) to dimethyl sulfoxide (DMSO) is 3:1; And step two, placing the mixed solution obtained in the step one in a 90 ℃ plus or minus 5 ℃ oven, continuously heating for 4-6 days to obtain white transparent blocky crystals, and washing, filtering, drying and grinding the white transparent blocky crystals to obtain the fluorescent probe.
2. 2. The ferric ion detection fluorescent probe of claim 1, wherein the agitation time in step one is 30min-60min.
3. 3. Use of the iron ion detection fluorescent probe according to claim 1 for rapid detection of iron content in magnesium oxide.
4. 4. A fluorescence detection method for rapidly detecting the iron content in magnesium oxide is characterized by comprising the following steps: Weighing dried 0.5g of magnesium oxide into a platinum crucible, adding 4.0g of anhydrous sodium carbonate and 2.7g of boric acid into the platinum crucible, uniformly mixing, covering a platinum cover, slightly leaving a gap, putting into a high-temperature furnace, slowly heating, gradually heating to 1100 ℃ plus or minus 25 ℃ for 10min, taking out the crucible, covering the platinum cover or a surface dish, after the crucible is slightly cold, adding 55mL of sulfuric acid solution while stirring, heating in a steam bath until a sample is completely dissolved, cooling, and transferring to a volumetric flask for constant volume to obtain a magnesium oxide solution; Taking 1mg of the iron ion detection fluorescent probe in the claim 1, adding 3mL of the magnesium oxide solution prepared in the step one, uniformly mixing, and measuring the fluorescence intensity of the iron ion detection fluorescent probe at the excitation wavelength of 290 nm.
5. 5. The fluorescence detection method for rapidly detecting iron content in magnesium oxide according to claim 4, wherein in the first step, the volume ratio of sulfuric acid in the sulfuric acid solution to water is 1:9.

Description

Iron ion detection fluorescent probe, application and fluorescent detection method Technical Field The invention belongs to the technical field of iron content detection, and particularly relates to an iron ion detection fluorescent probe, application and a fluorescent detection method. Background Magnesium oxide, also known as magnesia, is a white hygroscopic solid mineral that exists in nature in the form of periclase and is the raw material for smelting magnesium (or oxide). Magnesium oxide is used as a refractory material and has physical and chemical stability at high temperature, is used as a building material and has excellent properties of fire resistance, termite resistance, moisture resistance, mildew resistance, high strength and the like, and can be used as antacid, magnesium supplement and short-term laxative, and can also be used for relieving heartburn and dyspepsia in the medical field. As the purity of magnesium oxide increases, the application performance of the magnesium oxide is improved, so that the impurity content of the high-purity magnesium oxide is monitored. The impurity content of the high-purity magnesium oxide needs to be strictly controlled, and according to different customer requirements, the calcium, the iron, the silicon, the aluminum and the heavy metal all need to meet specific standards so as to ensure the quality and the performance of the product. Wherein, iron is used as a common impurity in magnesium oxide, and the content of the iron is clearly required in industry standards. For example HG/T-6066-2022 specifies that iron ions should be 0.5% or less in magnesium oxide for mineral insulated cables. The general conventional detection means of iron ions generally follow the chemical analysis method of GB/T5069-2015 magnesium aluminum refractory materials, namely an o-phenanthroline photometry. The principle is that sodium carbonate-boric acid mixed flux is used for melting and dilute hydrochloric acid leaching is carried out. Fe (III) was reduced to Fe (II) with hydroxylamine hydrochloride, and in a weakly acidic solution, fe (II) formed an orange-red complex with phenanthroline, and its absorbance was measured at a spectrophotometer wavelength of 510 nm. The method has the advantages of accuracy, but also has the defects of being unfavorable for enterprise application, such as complex operation, long time consumption, complex required reagent and the like. Therefore, it is highly desirable to develop a method for rapidly detecting the iron impurity content that meets the magnesium oxide industry standards. Disclosure of Invention The invention aims to overcome the defects of the prior art, provides a fluorescent probe for detecting iron ions, application and a fluorescent detection method, and solves the technical problems of complex operation, time consumption and the like in the aspect of detecting the iron content in magnesium oxide. In order to solve the problems, the technical scheme of the invention is that the fluorescent probe for detecting the iron ions has a molecular formula (Zn 2(C8O8N2H2)·DMSO·HCOOH)n). Preferably, the preparation steps of the fluorescent probe are as follows: Weighing pyrazine-2, 3,5, 6-tetracarboxylic acid and Zn (NO) 3, dissolving in a mixed solvent of N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO), and stirring to obtain a mixed solution, wherein the mass ratio of pyrazine-2, 3,5, 6-tetracarboxylic acid to Zn (NO) 3 is 1:6, and the volume ratio of N, N-Dimethylformamide (DMF) to dimethyl sulfoxide (DMSO) is 3:1; and step two, placing the mixed solution obtained in the step one in a 90 ℃ plus or minus 5 ℃ oven, continuously heating for 4-6 days to obtain white transparent blocky crystals, and washing, filtering, drying and grinding the white transparent blocky crystals to obtain the fluorescent probe. Preferably, the stirring time in the first step is 30min-60min. The invention also aims to provide an application of the iron ion detection fluorescent probe in rapid detection of the iron content in magnesium oxide. Another object of the present invention is to provide a fluorescence detection method for rapidly detecting iron content in magnesium oxide, comprising the steps of: Weighing dried 0.5g of magnesium oxide into a platinum crucible, adding 4.0g of anhydrous sodium carbonate and 2.7g of boric acid into the platinum crucible, uniformly mixing, covering a platinum cover, slightly leaving a gap, putting into a high-temperature furnace, slowly heating, gradually heating to 1100 ℃ plus or minus 25 ℃ for 10min, taking out the crucible, covering the platinum cover or a surface dish, after the crucible is slightly cold, adding 55mL of sulfuric acid solution while stirring, heating in a steam bath until a sample is completely dissolved, cooling, and transferring to a volumetric flask for constant volume to obtain a magnesium oxide solution; And step two, taking 1mg of the iron ion detection fluorescent probe, adding 3mL of t