CN107607670A - The assay method of tetravalent manganese in a kind of pyrolusite - Google Patents

The assay method of tetravalent manganese in a kind of pyrolusite Download PDF

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Publication number
CN107607670A
CN107607670A CN201710963583.1A CN201710963583A CN107607670A CN 107607670 A CN107607670 A CN 107607670A CN 201710963583 A CN201710963583 A CN 201710963583A CN 107607670 A CN107607670 A CN 107607670A
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pyrolusite
sulfuric acid
acid
ammonium sulfate
assay method
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CN201710963583.1A
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CN107607670B (en
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展宗波
刘世聪
陶青
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Baiyin Nonferrous Group Co Ltd
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Baiyin Nonferrous Group Co Ltd
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Abstract

The present invention relates to a kind of assay method of tetravalent manganese in pyrolusite.The Mn that the present invention obtains to pyrolusite to processing4+Secondary precipitate be ashed, calcination is cleared up by the concentrated sulfuric acid, concentrated nitric acid and concentrated phosphoric acid, ammonium nitrate is added into the thickening thing after resolution, stirring to tobacco disperses, and adds sulfuric acid and stirs to thickening thing dissolving, is cooled to room temperature, using iron ammonium sulfate standard liquid volumetric soiutions to pale red, adding N benzene, it is titration end-point to continue iron ammonium sulfate standard liquid volumetric soiutions and be changed into yellow green from pink, by the way that Mn is calculated for o-amino benzoyl acid indicator4+Content.Tetravalent manganese in pyrolusite is measured using the assay method of the present invention, with the advantages that high accuracy, favorable reproducibility, precision is high.

Description

The assay method of tetravalent manganese in a kind of pyrolusite
Technical field
The present invention relates to a kind of assay method of tetravalent manganese in pyrolusite.
Background technology
Pyrolusite is a kind of important additives in zinc abstraction production process, main chemical MnO2, its property is steady Fixed, content is 50%~60%, and density be 4.23g/ml ~ 4.36g/ml, and hardness is 2 ~ 2.5;In zinc leaching process, add Enter appropriate pyrolusite powder, can be by Fe in solution2+It is oxidized to Fe3+, its reaction equation is as follows:2 Fe2++MnO2+ 4H+= 2Fe3++Mn2++2H2O;From reaction equation as can be seen that pyrolusite in Fe2+It is Mn to react4+, and Mn2+、Mn3+ And it is not involved in reacting;Therefore the assay method of pyrolusite is established, the quality of pyrolusite can be effectively monitored, cost is reduced and disappear Consumption, more intuitively reflects production technology situation, has important directive function to production.
The content of the invention
The purpose of the present invention is that a kind of assay method of tetravalent manganese in pyrolusite is provided the problem of presence for prior art.
Concrete technical scheme of the present invention is as follows:
The assay method of tetravalent manganese, comprises the following steps in a kind of pyrolusite:
A, pyrolusite style is put into beaker after weighing, and concentration 400g/L ammonium sulfate and concentration 5mol/L are sequentially added into beaker Sulfuric acid, 10~40min of heating water bath dissolving, obtain containing Mn3+And Mn4+Primary sedimentation thing and contain Mn2+Once filter Liquid, primary sedimentation thing is put into beaker, the mixed solution of sulfuric acid, hydrofluoric acid and potassium fluoride, heating water bath are added into beaker 30min, obtain containing Mn4+Secondary precipitate and contain Mn3+Secondary filtrate;
B, the obtained secondary precipitates of step a are ashed, sequentially add the concentrated sulfuric acid, concentrated nitric acid and concentrated phosphoric acid and calcination is entered Row resolution, adds ammonium nitrate into the thickening thing after resolution, stirs to tobacco and disperse, and adds concentration 4mol/L sulfuric acid, stirring To thickening thing dissolving, room temperature is cooled to, using iron ammonium sulfate standard liquid volumetric soiutions to pale red, it is adjacent to add for 2~4 drop N benzene generations Aminobenzoic acid indicator, it is titration end-point to continue iron ammonium sulfate standard liquid volumetric soiutions and be changed into yellow green from pink;
C, to Mn in pyrolusite4+Cubage:
The mol ratio of each component is in the mixed solution of the sulfuric acid, hydrofluoric acid and potassium fluoride:
Sulfuric acid:Hydrofluoric acid:Potassium fluoride=4:11.5:3.4.
The invention has the advantages that:
Precision test:Precision weighs 10 parts of equivalent pyrolusite, is determined simultaneously using the method for the present invention, measurement result Mn4+ Content average value be 27.94%, relative standard deviation (RSD) be 1.46%, result of the test shows, this method favorable reproducibility, Precision is high, complies fully with the quality control requirement of assay.
The measure of recovery of standard addition:Recovery of standard addition has been carried out to the tetravalent manganese in pyrolusite using the method for the present invention Measure, the rate of recovery demonstrate the accuracy of method more than 95%.
Embodiment
To the assay method of tetravalent manganese in pyrolusite, comprise the following steps:
A, m is weighed0=0.1000g pyrolusite style is put into beaker, and concentration 400g/L ammonium sulfate is sequentially added into beaker 20ml and concentration 5mol/L sulfuric acid 1ml, 10~40min of heating water bath dissolve, and obtain containing Mn3+And Mn4+Primary sedimentation thing With contain Mn2+First-time filtrate, primary sedimentation thing is put into beaker, adds into beaker sulfuric acid, hydrofluoric acid and potassium fluoride Mixed solution, the mol ratio of the mixed solution is sulfuric acid:Hydrofluoric acid:Potassium fluoride=4:11.5:3.4, heating water bath 30min, obtain Contain Mn4+Secondary precipitate and contain Mn3+Secondary filtrate;
B, the obtained secondary precipitates of step a are ashed, sequentially add the 5ml concentrated sulfuric acid, 10ml concentrated nitric acid and 15ml Concentrated phosphoric acid calcination is cleared up, into the thickening thing after resolution plus ammonium nitrate 2g, stir to tobacco and disperse, add concentration 4mol/L sulfuric acid 10ml, stirring are cooled to room temperature, using iron ammonium sulfate standard liquid volumetric soiutions to light red to thickening thing dissolving Color, 2~4 drop N benzene are added for o-amino benzoyl acid indicator, continues iron ammonium sulfate standard liquid volumetric soiutions and is changed into yellow from pink Green is titration end-point, actual concentrations C=0.04850mol/L of iron ammonium sulfate standard titration solution, consumes iron ammonium sulfate The ml of the volume V of standard titration solution=23.05;
C, above-mentioned numerical value is substituted into following formula to Mn in pyrolusite4+Cubage:

Claims (2)

1. the assay method of tetravalent manganese in a kind of pyrolusite, it is characterised in that comprise the following steps:
A, pyrolusite style is put into beaker after weighing, and concentration 400g/L ammonium sulfate and concentration 5mol/L are sequentially added into beaker Sulfuric acid, 10~40min of heating water bath dissolving, obtain containing Mn3+And Mn4+Primary sedimentation thing and contain Mn2+Once filter Liquid, primary sedimentation thing is put into beaker, the mixed solution of sulfuric acid, hydrofluoric acid and potassium fluoride, heating water bath are added into beaker 30min, obtain containing Mn4+Secondary precipitate and contain Mn3+Secondary filtrate;
B, the obtained secondary precipitates of step a are ashed, sequentially add the concentrated sulfuric acid, concentrated nitric acid and concentrated phosphoric acid and calcination is entered Row resolution, adds ammonium nitrate into the thickening thing after resolution, stirs to tobacco and disperse, and adds concentration 4mol/L sulfuric acid, stirring To thickening thing dissolving, room temperature is cooled to, using iron ammonium sulfate standard liquid volumetric soiutions to pale red, it is adjacent to add for 2~4 drop N benzene generations Aminobenzoic acid indicator, it is titration end-point to continue iron ammonium sulfate standard liquid volumetric soiutions and be changed into yellow green from pink;
C, to Mn in pyrolusite4+Cubage:
2. the assay method of tetravalent manganese in a kind of pyrolusite as claimed in claim 1, it is characterised in that:
The mol ratio of each component is in the mixed solution of the sulfuric acid, hydrofluoric acid and potassium fluoride:
Sulfuric acid:Hydrofluoric acid:Potassium fluoride=4:11.5:3.4.
CN201710963583.1A 2017-10-16 2017-10-16 Method for determining tetravalent manganese in pyrolusite Expired - Fee Related CN107607670B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU715614A1 (en) * 1978-10-03 1980-02-15 Научно-Исследовательский И Проектный Институт По Обогащению И Агломерации Руд Черных Металлов Method of manganese determination in pyrolusite
SU722846A1 (en) * 1978-05-03 1980-03-25 Научно-Исследовательский И Проктный Институт По Обогащению И Агломерации Руд Черных Металлов Method of magnanine magnanese determination
CN102128836A (en) * 2010-12-06 2011-07-20 天津钢铁集团有限公司 Method for detecting manganese in carbon manganese alloy
CN104502345A (en) * 2014-12-01 2015-04-08 武钢集团昆明钢铁股份有限公司 Method for accurately and quickly detecting manganese content in nitridation reinforcer
CN106290705A (en) * 2016-07-21 2017-01-04 本钢板材股份有限公司 Utilize the method for manganese amount in volumetric determination ferrous ammonium sulfate carbon manganese ball
CN106802297A (en) * 2016-12-29 2017-06-06 内蒙古包钢钢联股份有限公司 The method that ammonium nitrate oxidation ferrometry determines manganese content in nitrogen manganese alloy

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* Cited by examiner, † Cited by third party
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SU722846A1 (en) * 1978-05-03 1980-03-25 Научно-Исследовательский И Проктный Институт По Обогащению И Агломерации Руд Черных Металлов Method of magnanine magnanese determination
SU715614A1 (en) * 1978-10-03 1980-02-15 Научно-Исследовательский И Проектный Институт По Обогащению И Агломерации Руд Черных Металлов Method of manganese determination in pyrolusite
CN102128836A (en) * 2010-12-06 2011-07-20 天津钢铁集团有限公司 Method for detecting manganese in carbon manganese alloy
CN104502345A (en) * 2014-12-01 2015-04-08 武钢集团昆明钢铁股份有限公司 Method for accurately and quickly detecting manganese content in nitridation reinforcer
CN106290705A (en) * 2016-07-21 2017-01-04 本钢板材股份有限公司 Utilize the method for manganese amount in volumetric determination ferrous ammonium sulfate carbon manganese ball
CN106802297A (en) * 2016-12-29 2017-06-06 内蒙古包钢钢联股份有限公司 The method that ammonium nitrate oxidation ferrometry determines manganese content in nitrogen manganese alloy

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* Cited by examiner, † Cited by third party
Title
周方钦等: "软锰矿中二氧化锰含量的快速滴定", 《冶金分析》 *
彭洪等: "碘量法测定软锰矿中的二氧化锰", 《铀矿冶》 *
林顺增等: "软锰矿锰含量分析测定研究", 《三明职业大学学报》 *
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