CN106802297A - The method that ammonium nitrate oxidation ferrometry determines manganese content in nitrogen manganese alloy - Google Patents
The method that ammonium nitrate oxidation ferrometry determines manganese content in nitrogen manganese alloy Download PDFInfo
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Abstract
The invention discloses a kind of method that ammonium nitrate oxidation ferrometry determines manganese content in nitrogen manganese alloy, including：Nitrogen manganese alloy sample solution is weighed, increases chloric acid；Heating smoke, oxidation trivalent chromium is Cr VI, hydrochloric acid is added dropwise and catches up with yellow smog；Filtering, precipitation is transferred in platinum crucible together with filter paper, and cooling is taken out in 800~850 DEG C of high temperature furnaces after burning in after low temperature dry ashing, being placed in；Add mixed flux to be melted in high temperature furnace, platinum crucible is put into the beaker of correspondence filtrate, boil to air pocket is emitted, be cooled to room temperature, clean platinum crucible；Phosphoric acid, nitric acid are added, is heated to being removed when just emitting phosphoric acid cigarette, add ammonium nitrate solid, shake and blow away nitrogen oxide, plus sulfuric acid shakes up；When being titrated to blush with iron ammonium sulfate standard titration solution, plus N benzene is for o-amino benzoyl acid indicator, is titrated to bright green for terminal, draws manganese content in nitrogen manganese alloy.The present invention have the degree of accuracy is high, precision is good, quick, accurate, it is practical the characteristics of.
Description
Technical field
The present invention relates to a kind of chemical analysis technology, specifically, it is related to a kind of ammonium nitrate oxidation ferrometry to determine nitrogen
The method of manganese content in manganese alloy.
Background technology
Due to nitrogen, the various effects of manganese, need to add manganese, nitrogen two simultaneously when high strength steel, stainless steel, heat resisting steel is refined
During kind of element, exist as the solubility of nitrogen is low, density is small, be difficult to add and nitrogen addition it is whard to control the shortcomings of.However, with
When nitrogen manganese compound form is added, it is not only easy to add, and the utilization rate of manganese, nitrogen is also high, therefore it is each in research nitrogen manganese alloy
The content important in inhibiting of element.
Manganese plays deoxidation, denitrogenation and alloying action in steel-making.The presence of manganese can be eliminated or weakened because of the heat that sulphur causes
Fragility, so as to improve the hot-working character of steel.Manganese and iron form solid solution, improve the hardness of ferrite and austenite in steel and strong
Degree, manganese is also the formation element of carbide, and a part of iron atom is replaced into cementite.Manganese reduces critical transitions temperature in steel
Degree, refines pearlitic grain and improves the intensity of pearlitic steel.The content that therefore, it can manganese in Accurate Determining nitrogen manganese alloy is very heavy
Will.
But the content of manganese cannot be detected when in the prior art, chromium content is higher in nitrogen manganese alloy.
The content of the invention
Technical problem solved by the invention is to provide a kind of ammonium nitrate oxidation ferrometry and determines manganese in nitrogen manganese alloy
The method of content, with the degree of accuracy it is high, precision is good, quick, accurate, it is practical the characteristics of.
Technical scheme is as follows：
A kind of method that ammonium nitrate oxidation ferrometry determines manganese content in nitrogen manganese alloy, including：
Nitrogen manganese alloy sample is weighed, chloroazotic acid, hydrofluoric acid is added and is heated to being completely dissolved, increase chloric acid；
Heating smoke, oxidation trivalent chromium is Cr VI, hydrochloric acid is added dropwise and catches up with yellow smog, then smoke, then hydrochloric acid is added dropwise；
Filtering, cleans beaker, precipitation is transferred in platinum crucible together with filter paper, in after low temperature dry ashing, being placed in 800~850 DEG C
Cooling is taken out after being burnt in high temperature furnace；
Add mixed flux to be melted in high temperature furnace, take out cooling；Platinum crucible is put into the beaker of correspondence filtrate, is boiled
To air pocket is emitted, room temperature is cooled to, cleans platinum crucible；
Phosphoric acid, nitric acid are added, is heated to being removed when just emitting phosphoric acid cigarette, add ammonium nitrate solid, shake and blow away the oxygen of nitrogen
Compound, plus sulfuric acid shakes up, and is cooled to room temperature；
When being titrated to blush with iron ammonium sulfate standard titration solution, plus N- benzene is for o-amino benzoyl acid indicator, after
The continuous bright green that is titrated to draws manganese content in nitrogen manganese alloy for terminal.
Further：Manganese contentC：Ferrous sulfate concentration of standard solution, V：Drop
Surely ferrous sulfate standard liquid volume, m are consumed：Sample weighting amount, M (Mn)：The molal weight of manganese.
Further：
0.1000g samples are weighed in 300mL conical flasks, plus 15mL chloroazotic acid, few drops hydrofluoric acid is added dropwise, it is heated to completely molten
Solution, plus 10mL perchloric acid；
Heating smoke, oxidation trivalent chromium is Cr VI, hydrochloric acid is added dropwise and catches up with yellow smog, then smoke, then a small amount of dropwise addition salt
Acid, 4~5 times repeatedly, removes slightly cold, adds 5mL hydrochloric acid and 5mL water, heating for dissolving salt；
Filtered in 300mL beakers with Medium speed filter paper, beaker is cleaned with hydrochloric acid, wash precipitation 3~4 times, washed 5~6 times, will
Precipitation is transferred in platinum crucible together with filter paper, is taken out in after low temperature dry ashing, being placed in 800~850 DEG C of high temperature furnaces to burn 10 minutes, cold
But；
1~2g, the mixed flux of+1 part of boric acid of 2 parts of sodium carbonate are added, is melted 15 minutes in 900 DEG C of high temperature furnaces, taken out
Cooling；Platinum crucible is put into the 300mL beakers of correspondence filtrate, is boiled to air pocket is emitted, be cooled to room temperature, clean platinum crucible；
Heating concentrates filtrate to 20mL, plus 15mL phosphoric acid, 3~4mL nitric acid；Continue to be heated to be removed when just having emitted phosphoric acid cigarette,
1~2g ammonium nitrate is added immediately, nitrogen oxide, plus 50mL sulfuric acid is shaken and blow away, shaken up, be cooled to room temperature；
When being titrated to blush with iron ammonium sulfate standard titration solution, drop N- benzene is indicated for ortho-aminobenzoic acid plus three
Agent, continues to be titrated to bright green for terminal.
Further：The step of also including evaluation testing result, evaluation criteria includes the degree of accuracy, precision and tolerance.
Compared with prior art, the technology of the present invention effect includes：
The present invention have the degree of accuracy is high, precision is good, quick, accurate, it is practical the characteristics of.
(1) it is quick, efficient.
The method that the present invention is used is volumetric method, with fast and efficiently feature.
(2) it is accurate, stabilization.
When chromium content is higher in ferromanganese, there is certain influence on the Accurate Determining of manganese, the present invention not only eliminates chromium to result
Influence, and solve the problems, such as that sample is not readily dissolved.
(3) it is cost-effective.
The invention belongs to conventional capacity method, simple glassware and reagent are only needed, purchase large-scale instrument can be saved
Cost.
Specific embodiment
Technical solution of the present invention is elaborated below with reference to example embodiment.However, example embodiment can
Implement in a variety of forms, and be not understood as limited to implementation method set forth herein；Conversely, thesing embodiments are provided so that
The design of example embodiment more comprehensively and completely, and is comprehensively conveyed to those skilled in the art by the present invention.
In the present invention, in the presence of a large amount of phosphoric acid complexing agents, after adding excessive solid ammonium nitrate, manganese is oxidized to trivalent
State, then titrates manganic with ferrous standard titration solution, and the percentage composition of manganese is sought according to ferrous consumption.Using chlorine high
The methods such as chromium, treatment residue are caught up with sour smoke, hydrochloric acid, and the nitrogen manganese alloy that will can be not readily dissolved all dissolves.It is situated between in phosphoric acid afterwards
Bivalent manganese is oxidized to manganic with ammonium nitrate in matter, with N- benzene for ortho-aminobenzoic acid as indicator, use iron ammonium sulfate mark
Quasi- solution titration manganic analyzes manganese in nitrogen manganese alloy.Suitable for production upper nitrogen manganese alloy and other less soluble manganese systems
The measure of manganese in ferroalloy.
The method that ammonium nitrate oxidation ferrometry determines manganese content in nitrogen manganese alloy, specifically includes following steps：
Step 1：Nitrogen manganese alloy sample is weighed, chloroazotic acid, hydrofluoric acid is added and is heated to being completely dissolved, increase chloric acid；
0.1000g samples are weighed in 300mL conical flasks, plus 15mL chloroazotic acid, few drops hydrofluoric acid is added dropwise, it is heated to completely molten
Solution, plus 10mL perchloric acid.
Step 2：Heating smoke, oxidation trivalent chromium is Cr VI, hydrochloric acid is added dropwise and catches up with yellow smog, then smoke, then be added dropwise
Hydrochloric acid；
Heating smoke, oxidation trivalent chromium is Cr VI, hydrochloric acid is added dropwise and catches up with yellow smog, then smoke, then a small amount of dropwise addition salt
Acid, 4~5 times repeatedly, removes slightly cold, adds 5mL hydrochloric acid and 5mL water, heating for dissolving salt.
Step 3：Filtering, cleans beaker, and precipitation is transferred in platinum crucible together with filter paper, in after low temperature dry ashing, being placed in 800~
Cooling is taken out after being burnt in 850 DEG C of high temperature furnaces；
Filtered in 300mL beakers with Medium speed filter paper, beaker is cleaned with hydrochloric acid (1+100), wash precipitation 3~4 times, washing 5
~6 times, precipitation is transferred in platinum crucible together with filter paper, is burnt 10 points in after low temperature dry ashing, being placed in 800~850 DEG C of high temperature furnaces
Clock takes out, cooling.
Step 4：Add mixed flux to be melted in high temperature furnace, take out cooling；Platinum crucible is put into the beaker of correspondence filtrate
In, boil to air pocket is emitted, room temperature is cooled to, clean platinum crucible；
1~2g mixed fluxs (+1 part of boric acid of 2 parts of sodium carbonate) is added, is melted 15 minutes in 900 DEG C of high temperature furnaces, taken out cold
But.Platinum crucible is put into the 300mL beakers of correspondence filtrate, is boiled to air pocket is emitted, be cooled to room temperature, clean platinum crucible.
Step 5：Phosphoric acid, nitric acid are added, is heated to being removed when just emitting phosphoric acid cigarette, add ammonium nitrate solid, shaken and blow away
Nitrogen oxide, plus sulfuric acid shakes up, and is cooled to room temperature；
Heating concentrates filtrate to 20mL, plus 15mL phosphoric acid, 3~4mL nitric acid.Continue to be heated to be removed when just having emitted phosphoric acid cigarette,
Add immediately 1~2g ammonium nitrate (Gu), shake and blow away nitrogen oxide, plus 50mL sulfuric acid (5+95), shake up, be cooled to room
Temperature.
Step 6：When being titrated to blush with iron ammonium sulfate standard titration solution, plus N- benzene is indicated for ortho-aminobenzoic acid
Agent, continues to be titrated to bright green for terminal.
When being titrated to blush with iron ammonium sulfate standard titration solution, plus three and drip N- benzene for ortho-aminobenzoic acid (2g/L)
Indicator, continues to be titrated to bright green for terminal.
Step 7：Draw manganese content in nitrogen manganese alloy.
The calculating of analysis result, manganese content：
In formula：C：Ferrous sulfate concentration of standard solution (mol/L).
V：Titration consumption ferrous sulfate standard liquid volume (mL)
m：Sample weighting amount (g)
M(Mn)：The molal weight (54.94g/mol) of manganese.
Step 8：Measurement result and discussion.
1st, the degree of accuracy and precision.
In order to verify the accuracy of this method, 2 mid-carbon fe-mn standard samples are randomly choosed, with the measured value and mark of this law
Quasi- value is compareed.It is shown in Table 1.From the result in table 1, measurement error very little, in the error range that national standard is allowed,
Requirement can be fully met.
The degree of accuracy of table 1
Method precision experiment carries out 5 parallel molten samples using same sample, is measured on same calibration curve, comes
The reappearance of verification method, as a result as shown in table 2.
The precision of table 2
2nd, tolerance.
From table 3 it can be seen that under the operation of not homogeneous, collimation as a result very well, is illustrated using molten sample effect of the invention
Very well, sample dissolves the complete and free of losses during molten sample to fruit.
The tolerance of table 3
Term used herein is explanation and exemplary and nonrestrictive term.Because the present invention can be with various
Form specific implementation without deviating from invention it is spiritual or substantive, it should therefore be appreciated that above-described embodiment be not limited to it is any foregoing
Details, and widely being explained in the spirit and scope that should be limited in appended claims, thus fall into claim or its etc.
Whole changes and remodeling in the range of effect all should be appended claims and covered.
Claims (4)
1. a kind of method that ammonium nitrate oxidation ferrometry determines manganese content in nitrogen manganese alloy, including：
Nitrogen manganese alloy sample is weighed, chloroazotic acid, hydrofluoric acid is added and is heated to being completely dissolved, increase chloric acid；
Heating smoke, oxidation trivalent chromium is Cr VI, hydrochloric acid is added dropwise and catches up with yellow smog, then smoke, then hydrochloric acid is added dropwise；
Filtering, cleans beaker, precipitation is transferred in platinum crucible together with filter paper, in after low temperature dry ashing, being placed in 800~850 DEG C of high temperature
Cooling is taken out after being burnt in stove；
Add mixed flux to be melted in high temperature furnace, take out cooling；Platinum crucible is put into the beaker of correspondence filtrate, is boiled to emitting
Air pocket, is cooled to room temperature, cleans platinum crucible；
Phosphoric acid, nitric acid are added, are heated to being removed when just emitting phosphoric acid cigarette, add ammonium nitrate solid, shake and blow away nitrogen oxide,
Plus sulfuric acid shakes up, room temperature is cooled to；
When being titrated to blush with iron ammonium sulfate standard titration solution, plus N- benzene is for o-amino benzoyl acid indicator, continues to drip
Fixed is terminal to bright green, draws manganese content in nitrogen manganese alloy.
2. the method that ammonium nitrate oxidation ferrometry as claimed in claim 1 determines manganese content in nitrogen manganese alloy, its feature exists
In：Manganese contentC：Ferrous sulfate concentration of standard solution, V：Titration consumption sulfuric acid is sub-
Iron standard liquid volume, m：Sample weighting amount, M (Mn)：The molal weight of manganese.
3. the method that the ammonium nitrate oxidation ferrometry as described in claims 1 or 2 determines manganese content in nitrogen manganese alloy, it is special
Levy and be：
0.1000g samples are weighed in 300mL conical flasks, plus 15mL chloroazotic acid, few drops hydrofluoric acid is added dropwise, it is heated to being completely dissolved,
Plus 10mL perchloric acid；
Heating smoke, oxidation trivalent chromium is Cr VI, hydrochloric acid is added dropwise and catches up with yellow smog, then smoke, then a small amount of dropwise addition hydrochloric acid, instead
It is multiple 4~5 times, remove slightly cold, add 5mL hydrochloric acid and 5mL water, heating for dissolving salt；
Filtered in 300mL beakers with Medium speed filter paper, beaker is cleaned with hydrochloric acid, wash precipitation 3~4 times, washed 5~6 times, will precipitated
It is transferred in platinum crucible together with filter paper, is taken out in after low temperature dry ashing, being placed in 800~850 DEG C of high temperature furnaces to burn 10 minutes, cooling；
1~2g, the mixed flux of+1 part of boric acid of 2 parts of sodium carbonate are added, is melted 15 minutes in 900 DEG C of high temperature furnaces, take out cooling；
Platinum crucible is put into the 300mL beakers of correspondence filtrate, is boiled to air pocket is emitted, be cooled to room temperature, clean platinum crucible；
Heating concentrates filtrate to 20mL, plus 15mL phosphoric acid, 3~4mL nitric acid；Continue to be heated to be removed when just having emitted phosphoric acid cigarette, immediately
1~2g ammonium nitrate is added, nitrogen oxide, plus 50mL sulfuric acid is shaken and blow away, shaken up, be cooled to room temperature；
When being titrated to blush with iron ammonium sulfate standard titration solution, drop N- benzene of plus three for o-amino benzoyl acid indicator, after
The continuous bright green that is titrated to is for terminal.
4. the method that the ammonium nitrate oxidation ferrometry as described in claims 1 or 2 determines manganese content in nitrogen manganese alloy, it is special
Levy and be：The step of also including evaluation testing result, evaluation criteria includes the degree of accuracy, precision and tolerance.
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| CN107607670A (en) * | 2017-10-16 | 2018-01-19 | 白银有色集团股份有限公司 | The assay method of tetravalent manganese in a kind of pyrolusite |
| CN110779916A (en) * | 2019-11-22 | 2020-02-11 | 宁夏天元锰业集团有限公司 | Method for determining manganese content in manganese carbonate ore by ammonium nitrate method |
| CN112858571A (en) * | 2021-01-13 | 2021-05-28 | 广东韶钢松山股份有限公司 | Method for detecting manganese content in rare earth nitrogen alloy |
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