CN111830194A - Chemical analysis method for zinc in high-manganese and high-zinc material - Google Patents
Chemical analysis method for zinc in high-manganese and high-zinc material Download PDFInfo
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- CN111830194A CN111830194A CN202010441984.2A CN202010441984A CN111830194A CN 111830194 A CN111830194 A CN 111830194A CN 202010441984 A CN202010441984 A CN 202010441984A CN 111830194 A CN111830194 A CN 111830194A
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Abstract
The invention relates to a chemical analysis method for zinc in a high-manganese and high-zinc material, which adopts concentrated hydrochloric acid as a complexing reducing agent to reduce high-valence manganese ions in a solution after triacid decomposition, thereby ensuring that the manganese ions are completely separated when ferric hydroxide is used as a carrier for separation. Hydrochloric acid-nitric acid-sulfuric acid is adopted to dissolve high-manganese and high-zinc materials, concentrated hydrochloric acid is used as a complexing reducing agent to reduce high-valence manganese ions in the solution after the triacid decomposition, and complete separation of the manganese ions is ensured when ferric hydroxide is used as a carrier for separation. The method has the advantages of high precision, good accuracy, reliable result and the like.
Description
Technical Field
The invention belongs to a chemical analysis technology, in particular to a chemical analysis method for zinc in a high-manganese and high-zinc material.
Background
With the continuous reduction of high-grade zinc ores, the development and utilization of secondary resources containing zinc become more and more important, so that the resources can be fully utilized, the sustainable development of the resources is realized, the policies of energy conservation and emission reduction, green metallurgy development and industry upgrade in China are met, the production cost can be reduced, the secondary zinc resources become important raw materials for zinc production, and 30% of the zinc in the whole world comes from the secondary zinc resources. The zinc-containing secondary resources are more in variety, and zinc-containing soot waste and the like are also available besides the zinc-plated materials, zinc alloys and zinc-manganese dry batteries. The zinc-containing soot waste is formed by volatilizing zinc in a gas state in the processes of blast furnace iron making and waste steel regeneration smelting, iron ore concentrate and a steel zinc coating, is cooled and collected and accumulated along with flue gas entering a dust collecting system, is simultaneously accompanied with enrichment of elements such as Pb, Mn, Cd and the like, and is increasingly valued by people as a main zinc-containing secondary resource.
According to the literature, the determination method for the content of zinc in the zinc-containing material is more, relevant national standards exist, but the chemical analysis method for zinc in the high-manganese and high-zinc material is almost free of relevant literature, compared with the common zinc-containing material, manganese in the high-manganese and high-zinc material has multiple valence states and more complex components, the sample is decomposed by utilizing the traditional triacid, the hot nitric-sulfuric mixed acid has stronger oxidizability, and due to the fact that the concentration of manganese ions is higher and the complexation of coordination ions of the manganese ions is higher, the low-valence manganese ions are more easily oxidized to the valence state more than trivalent. In the process of separating manganese ions by taking ferric hydroxide as a carrier, partial manganese ions are oxidized to be in a higher valence state due to the oxidation property of ammonium persulfate, wherein compounds of manganese except manganese dioxide are water-soluble, so that the manganese ions in the solution can not be completely separated when the ferric hydroxide is taken as the carrier to separate the manganese ions, and the manganese ions form precipitates to enable the solution to be turbid and an indicator to be incapable of obviously indicating an end point when zinc is titrated by subsequent EDTA (ethylene diamine tetraacetic acid), so that the titration end point judgment of the zinc is seriously influenced, the existing analysis conditions and analysis methods of the zinc have certain limitations, and the accuracy of a test result is greatly influenced.
Disclosure of Invention
The invention aims to provide a chemical analysis method for zinc in a high-manganese and high-zinc material, which is simple to operate, efficient and reliable, can completely separate manganese in the material after dissolving of triacid, and does not generate any interference on the titration result of zinc.
In order to achieve the purpose, the invention discloses a chemical analysis method of zinc in a high-manganese high-zinc material, which is characterized by comprising the following steps of:
step 1, weighing 0.1000-0.2000g of high-manganese and high-zinc material, placing the material in a glass beaker, wetting the material with a small amount of water, adding 10-20mL of hydrochloric acid, 3-7mL of nitric acid and 5-15mL of sulfuric acid, heating the material until dense smoke is emitted, steaming the material to a small volume, taking down the material and cooling the material;
step 2, adding 3-5mL of concentrated hydrochloric acid, heating to dissolve a sample to regulate a wet salt state, taking down and cooling;
step 3, adding 60-90mL of distilled water, heating to dissolve soluble salts, and cooling; adding ammonium chloride and ammonium persulfate, neutralizing with ammonia water until ferric hydroxide precipitate appears, adding excessive solution until pH is 9.0, boiling, breaking excessive ammonium persulfate, filtering, separating, and titrating.
In the technical scheme of the chemical analysis method for zinc in the high-manganese and high-zinc material, the further preferable technical scheme is characterized in that:
1. weighing 0.2000g of high-manganese and high-zinc substances in the step 1;
2. adding 15mL of hydrochloric acid, 5mL of nitric acid and 10mL of sulfuric acid in the step 1;
3. 4mL of concentrated hydrochloric acid is added in the step 2;
4. 75mL of distilled water was added in step 3.
Compared with the prior art, the invention has the beneficial effects that:
1. the separation technology is simple to operate, the separation efficiency is high, and the result is reliable;
2. aiming at the analysis method that the zinc in the high-manganese and high-zinc material is difficult to accurately measure, the manganese in the material after the triacid is dissolved can be completely separated, and the titration result of the zinc is not interfered.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1, a chemical analysis method for zinc in a high manganese and high zinc material, comprising the steps of: step 1, weighing 0.1000-0.2000g of high-manganese and high-zinc material, placing the material in a glass beaker, wetting the material with a small amount of water, adding 10-20mL of hydrochloric acid, 3-7mL of nitric acid and 5-15mL of sulfuric acid, heating the material until dense smoke is emitted, steaming the material to a small volume, taking down the material and cooling the material; step 2, adding 3-5mL of concentrated hydrochloric acid, heating to dissolve a sample to regulate a wet salt state, taking down and cooling; step 3, adding 60-90mL of distilled water, heating to dissolve soluble salts, and cooling; adding ammonium chloride and ammonium persulfate, neutralizing with ammonia water until ferric hydroxide precipitate appears, adding excessive solution until pH is 9.0, boiling, breaking excessive ammonium persulfate, filtering, separating, and titrating. The invention adopts hydrochloric acid-nitric acid-sulfuric acid to dissolve high-manganese and high-zinc materials, uses concentrated hydrochloric acid as a complexing reducing agent to reduce high-valence manganese ions in the solution after the triacid decomposition, and ensures that the manganese ions are completely separated when ferric hydroxide is used as a carrier for separation. The chemical reagents used in the test method adopted by the invention are all analytical pure reagents.
Example 2, according to the chemical analysis method of zinc in the high-manganese high-zinc material described in example 1, 0.2000g of the high-manganese high-zinc material is weighed in the step 1.
Example 3, according to the chemical analysis method of zinc in high manganese and high zinc material of example 1 or 2, 15mL of hydrochloric acid, 5mL of nitric acid and 10mL of sulfuric acid are added in step 1.
Example 4, in the chemical analysis method for zinc in high manganese and high zinc material according to example 1, 2 or 3, 4mL of concentrated hydrochloric acid is added in the step 2.
Example 5, the chemical analysis method for zinc in a high manganese and high zinc material according to any one of examples 1 to 4: 75mL of distilled water was added in step 3.
Example 6, the method for chemical analysis of zinc in a high manganese and high zinc material according to any one of examples 1 to 5, comprising the steps of: (1) 0.2000g of high-manganese and high-zinc materials with different manganese contents are respectively and accurately weighed and placed in a glass beaker, moistened by a small amount of water, added with 15mL of hydrochloric acid, 5mL of nitric acid and 10mL of (1 + 1) sulfuric acid, heated until dense smoke is emitted and steamed to a small volume, and then taken down for cooling. (2) Adding 4mL of hydrochloric acid, heating to dissolve the sample to restore the wet salt state, taking down and cooling. (3) Then, 75mL of distilled water was added, and the mixture was heated to dissolve soluble salts and cooled. Adding ammonium chloride and ammonium persulfate, neutralizing with ammonia water until ferric hydroxide precipitate appears, adding excessive solution until pH is 9.0, boiling, breaking excessive ammonium persulfate, filtering, separating, and titrating.
The table shows the accuracy and precision of samples treated according to example 6.
The table above shows the control assay for samples not treated according to the invention.
Example 7 the method for chemical analysis of zinc in a high manganese and high zinc material according to any one of examples 1 to 6, comprising the steps of: (1) accurately weighing 0.2000g of sample standard-1 and standard-2 (two zinc standard samples (BY 0110-1 and YSS-30-2006) which are respectively selected, adding a certain amount of manganese sulfate reagent to be used as a simulated high-manganese and high-zinc material sample which is marked as sample standard-1 and standard-2) and placing the sample standard-1 and standard-2 in a glass beaker, wetting the sample standard-1 and standard-2 with a small amount of water, adding 15mL of hydrochloric acid, 5mL of nitric acid and 10mL of (1 + 1) sulfuric acid, heating until dense smoke is generated, steaming to a small volume, taking down and cooling. (2) Adding 4mL of hydrochloric acid, heating to dissolve the sample to restore the wet salt state, taking down and cooling. (3) Then, 75mL of distilled water was added, and the mixture was heated to dissolve soluble salts and cooled. Adding ammonium chloride and ammonium persulfate, neutralizing with ammonia water until ferric hydroxide precipitate appears, adding excessive solution until pH is 9.0, boiling, breaking excessive ammonium persulfate, filtering, separating, and titrating.
The table shows the analytical results and precision of the synthesized high manganese and high zinc sample treated according to example 7.
The table above shows the comparative analysis results for the synthesized high manganese and high zinc samples that were not treated by the method of the present invention.
Example 8, the method for chemical analysis of zinc in a high manganese and high zinc material according to any one of examples 1 to 7, comprising the steps of: (1) respectively and accurately weighing 0.2000g of high-manganese and high-zinc material and standard-2, placing the material and the standard-2 in a glass beaker, then adding a certain mass of zinc-based standard high-purity zinc, wetting the material by using a small amount of water, adding 15mL of hydrochloric acid, 5mL of nitric acid and 10mL of (1 + 1) sulfuric acid, heating until dense smoke is emitted, steaming to a small volume, taking down and cooling. (2) Adding 4mL of hydrochloric acid, heating to dissolve the sample to restore the wet salt state, taking down and cooling. (3) Then, 75mL of distilled water was added, and the mixture was heated to dissolve soluble salts and cooled. Adding ammonium chloride and ammonium persulfate, neutralizing with ammonia water until ferric hydroxide precipitate appears, adding excessive solution until pH is 9.0, boiling, breaking excessive ammonium persulfate, filtering, separating, and titrating.
The table above shows the results of the measurement and the standard recovery test of the sample after the treatment of example 8.
The table above is a control experiment for samples that were not treated by the method of the present invention.
According to the method, a traditional triacid decomposition sample is utilized, the hot nitric-sulfuric mixed acid has strong oxidizability, and due to the fact that the concentration of manganese ions is high and the complexation of coordination ions of the manganese ions, low-valence manganese ions are easily oxidized to a valence state more than three valence states. In the process of separating manganese ions by taking ferric hydroxide as a carrier, part of the manganese ions are oxidized to a higher valence state due to the oxidation of ammonium persulfate, wherein the manganese compounds except manganese dioxide are water-soluble, so that the manganese ions in the solution cannot be completely separated when the ferric hydroxide is taken as the carrier to separate the manganese ions. In order to completely separate the manganese ions in the solution during the precipitation separation by taking ferric hydroxide as a carrier, the manganese ions in the solution are completely kept in a divalent state before the ammonium persulfate is oxidized. Therefore, the method adopts concentrated hydrochloric acid as a complexing reducing agent to reduce high-valence manganese ions in the solution after the triacid decomposition, and ensures that the manganese ions are completely separated when ferric hydroxide is used as a carrier for separation. As can be seen from the sample precision test and the standard recovery rate test, the method has the advantages of good precision, high recovery rate, reliable result and the like.
The above description is only for the preferred embodiments of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution of the present invention and the inventive concept thereof within the scope of the present invention.
Claims (5)
1. A chemical analysis method for zinc in a high-manganese and high-zinc material is characterized by comprising the following steps:
step 1, weighing 0.1000-0.2000g of high-manganese and high-zinc material, placing the material in a glass beaker, wetting the material with a small amount of water, adding 10-20mL of hydrochloric acid, 3-7mL of nitric acid and 5-15mL of sulfuric acid, heating the material until dense smoke is emitted, steaming the material to a small volume, taking down the material and cooling the material;
step 2, adding 3-5mL of concentrated hydrochloric acid, heating to dissolve a sample to regulate a wet salt state, taking down and cooling;
step 3, adding 60-90mL of distilled water, heating to dissolve soluble salts, and cooling; adding ammonium chloride and ammonium persulfate, neutralizing with ammonia water until ferric hydroxide precipitate appears, adding excessive solution until pH is 9.0, boiling, breaking excessive ammonium persulfate, filtering, separating, and titrating.
2. The chemical analysis method for zinc in the high-manganese and high-zinc material according to claim 1, characterized in that: in the step 1, 0.2000g of high manganese and high zinc compound is weighed.
3. The chemical analysis method for zinc in the high-manganese and high-zinc material according to claim 1, characterized in that: in the step 1, 15mL of hydrochloric acid, 5mL of nitric acid and 10mL of sulfuric acid are added.
4. The chemical analysis method for zinc in the high-manganese and high-zinc material according to claim 1, characterized in that: 4mL of concentrated HCl was added in step 2.
5. The chemical analysis method for zinc in the high-manganese and high-zinc material according to claim 1, characterized in that: 75mL of distilled water was added in step 3.
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Citations (6)
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| CN102645432A (en) * | 2012-04-19 | 2012-08-22 | 白银有色集团股份有限公司 | Analysis method for quickly and accurately measuring zinc in zinc electrolyte |
| CN104089952A (en) * | 2014-07-17 | 2014-10-08 | 云南磷化集团有限公司 | Method for determining content of magnesium oxide in manganese ore |
| CN104316643A (en) * | 2014-10-10 | 2015-01-28 | 荆门市格林美新材料有限公司 | Three-element determination method of nickel-cobalt-manganese ternary material |
| CN108037237A (en) * | 2017-11-24 | 2018-05-15 | 昭通市鼎安科技有限公司 | The method of Zn content in EDTA volumetric determination zinc ores |
| CN108872468A (en) * | 2018-04-25 | 2018-11-23 | 长春黄金研究院有限公司 | The measuring method of copper content in a kind of high manganese ore |
| CN109030710A (en) * | 2018-05-31 | 2018-12-18 | 长春黄金研究院有限公司 | A method of being simple and efficient Zn content in the complicated sample ore of measurement |
-
2020
- 2020-05-22 CN CN202010441984.2A patent/CN111830194A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102645432A (en) * | 2012-04-19 | 2012-08-22 | 白银有色集团股份有限公司 | Analysis method for quickly and accurately measuring zinc in zinc electrolyte |
| CN104089952A (en) * | 2014-07-17 | 2014-10-08 | 云南磷化集团有限公司 | Method for determining content of magnesium oxide in manganese ore |
| CN104316643A (en) * | 2014-10-10 | 2015-01-28 | 荆门市格林美新材料有限公司 | Three-element determination method of nickel-cobalt-manganese ternary material |
| CN108037237A (en) * | 2017-11-24 | 2018-05-15 | 昭通市鼎安科技有限公司 | The method of Zn content in EDTA volumetric determination zinc ores |
| CN108872468A (en) * | 2018-04-25 | 2018-11-23 | 长春黄金研究院有限公司 | The measuring method of copper content in a kind of high manganese ore |
| CN109030710A (en) * | 2018-05-31 | 2018-12-18 | 长春黄金研究院有限公司 | A method of being simple and efficient Zn content in the complicated sample ore of measurement |
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