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 PDFInfo
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- 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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- CN
- China
- Prior art keywords
- pyrolusite
- sulfuric acid
- acid
- ammonium sulfate
- assay method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000011572 manganese Substances 0.000 title claims abstract description 16
- 238000003556 assay Methods 0.000 title claims abstract description 12
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 34
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZLXPLDLEBORRPT-UHFFFAOYSA-M [NH4+].[Fe+].[O-]S([O-])(=O)=O Chemical compound [NH4+].[Fe+].[O-]S([O-])(=O)=O ZLXPLDLEBORRPT-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 230000008719 thickening Effects 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 7
- 238000004448 titration Methods 0.000 claims abstract description 6
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 241000208125 Nicotiana Species 0.000 claims abstract description 4
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 16
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 16
- 239000011698 potassium fluoride Substances 0.000 claims description 8
- 235000003270 potassium fluoride Nutrition 0.000 claims description 8
- 239000008236 heating water Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- ALYNCZNDIQEVRV-UHFFFAOYSA-N 4-aminobenzoic acid Chemical compound NC1=CC=C(C(O)=O)C=C1 ALYNCZNDIQEVRV-UHFFFAOYSA-N 0.000 claims description 2
- 229960004050 aminobenzoic acid Drugs 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract description 2
- -1 o-amino benzoyl Chemical group 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
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
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710963583.1A CN107607670B (en) | 2017-10-16 | 2017-10-16 | Method for determining tetravalent manganese in pyrolusite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710963583.1A CN107607670B (en) | 2017-10-16 | 2017-10-16 | Method for determining tetravalent manganese in pyrolusite |
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| CN107607670A true CN107607670A (en) | 2018-01-19 |
| CN107607670B CN107607670B (en) | 2019-12-31 |
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| CN201710963583.1A Expired - Fee Related CN107607670B (en) | 2017-10-16 | 2017-10-16 | Method for determining tetravalent manganese in pyrolusite |
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Citations (6)
| 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 |
-
2017
- 2017-10-16 CN CN201710963583.1A patent/CN107607670B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (4)
| 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》 * |
| 韦文业等: "盐酸溶样-硫酸亚铁铵容量法测定软锰矿中锰含量", 《化工技术与开发》 * |
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| CN107607670B (en) | 2019-12-31 |
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Granted publication date: 20191231 |