CN110779916A - Method for determining manganese content in manganese carbonate ore by ammonium nitrate method - Google Patents
Method for determining manganese content in manganese carbonate ore by ammonium nitrate method Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention belongs to the technical field of chemical detection, and relates to a method for determining manganese content in manganese carbonate ore by using an ammonium nitrate method. The method comprises 1, weighing a sample; 2. adding phosphoric acid and nitric acid, and heating to completely dissolve the sample until slight smoke is emitted; 3. adding ammonium nitrate, completely blowing yellow flue gas, adding distilled water when the yellow flue gas is cooled to 60-70 ℃, and cooling to room temperature; 4. titrate with standard solution. The invention effectively shortens the analysis and measurement period, ensures the determination precision and accuracy, is easier and safer in the temperature control process, and is simple and easy to master in the operation method.
Description
Technical Field
The invention belongs to the technical field of chemical detection, and relates to a method for determining manganese content in manganese carbonate ore by using an ammonium nitrate method.
Background
The traditional method for measuring the manganese content in manganese carbonate ore is an ammonium nitrate oxidation titration method, and specifically comprises the steps of dissolving an ore sample by nitric acid, hydrochloric acid and phosphoric acid, adding ammonium nitrate into a phosphoric acid medium, oxidizing bivalent manganese in the sample into trivalent manganese, adding N-phenyl-substituted anthranilic acid as an indicator, titrating by using a ferrous ammonium sulfate standard solution, and calculating to measure the manganese content in the ore.
The existing method for determining the manganese content in manganese ore by using an ammonium nitrate method has a plurality of defects: the hydrochloric acid is needed to be added when the sample is decomposed, so that the smoking time is longer, and the measurement time is longer; the temperature control requirement is high, solid ammonium nitrate needs to be rapidly added when the wall of the bottle has no backflow and the liquid temperature is about 220 ℃, yellow nitrogen oxide gas is completely removed, and in the operation, if too many samples are used, the result is lower or higher, because the reinforced solid ammonium nitrate is too early and phosphate is not completely converted, but if the sample is delayed, the phosphate is crystallized, and the analysis result is influenced; in addition, when nitric acid is added, if the temperature is high and the speed is too high, part of the sample can be splashed out, so that the sample is not completely dissolved, the analysis error is increased, and meanwhile, the potential safety hazard is large.
At present, the assessment requirements of various manganese plants on slag are higher and higher, in order to more accurately master the analysis data of the slag and enable production units to timely make control over various key points of a chemical combination process, the most original method is still adopted, and more samples are taken and made, so that the personnel in a quality inspection part are stressed, and the analysis cost is increased; therefore, it is necessary to develop a more effective analysis and test method for the manganese content in manganese ore and manganese slag.
Disclosure of Invention
The invention aims to provide a method for determining the manganese content in manganese carbonate ore by an ammonium nitrate method, which reduces determination errors, shortens determination time, reduces operation difficulty and effectively ensures measurement accuracy.
The technical scheme of the invention for solving the technical problems is as follows.
A method for determining the manganese content in manganese carbonate ore by an ammonium nitrate method comprises the following steps:
(1) weighing 0.1g of sample and placing the sample in a conical flask; wherein the granularity of the sample is less than or equal to 0.125 mm;
(2) adding 15mL of phosphoric acid and 3mL of nitric acid, placing the conical flask on an electric furnace for heating to completely dissolve the sample until slight smoke is emitted, and taking down the conical flask; wherein, the concentration of the phosphoric acid is more than or equal to 85 percent, and the preparation method of the nitric acid is that 50mL of concentrated nitric acid is measured and dissolved in 50mL of water;
(3) adding 2g of ammonium nitrate, fully shaking, simultaneously blowing out yellow flue gas, adding 50mL of distilled water when cooling to 60-70 ℃, fully dissolving the ammonium nitrate, and cooling to room temperature;
(4) titrating with an ammonium ferrous sulfate standard solution to be light red, adding 3-4 drops of N-phenyl-o-aminobenzoic acid indicator, and continuously titrating until the liquid to be detected becomes bright yellow, namely the end point; wherein the concentration of the ammonium ferrous sulfate standard solution is 0.02 mol/L.
The method for determining the manganese content in manganese carbonate ore by using the ammonium nitrate method has the beneficial effects that:
(1) the phosphoric acid and the nitric acid are directly used for dissolving the sample, so that not only can the ore sample be completely dissolved, but also the temperature can be controlled to be about 220 ℃, and the temperature control process is easier and safer;
(2) after the sample is dissolved, the sample is oxidized in a heated concentrated phosphoric acid medium, and then titration measurement is carried out, so that the error generated when the reagent is added again is reduced, the measurement effect is ensured, the operation difficulty is effectively reduced, and the measurement time is shortened;
(3) the ammonium nitrate is added when the sample to be measured smokes, so that the reaction is more violent, the sample to be measured is more completely oxidized, and the accuracy of the measurement result is improved;
(4) the method effectively shortens the analysis and measurement period, ensures the determination precision and accuracy, has simple operation method, is easy to master, and can meet the daily analysis requirement.
Detailed Description
Example 1
Main apparatus and reagents:
electronic analytical balance (parts per million);
phosphoric acid: the concentration is not less than 85%;
nitric acid (1+ 1): measuring 50mL of concentrated nitric acid and dissolving in 50mL of water;
ammonium nitrate: an AR solid reagent;
standard solution of ferrous ammonium sulfate: 0.02mol/L, the preparation method is that 8g of ferrous ammonium sulfate is weighed and dissolved in 1000mL of sulfuric acid (5+95), and the solution is stored in a brown bottle.
In addition, reagents used in the experiment are all analytically pure; the experimental water is distilled water or water with the purity equivalent to that of the distilled water; the calibration method is consistent with the analysis method.
Example 2
A method for determining the manganese content in manganese carbonate ore by an ammonium nitrate method comprises the following steps:
(1) weighing 0.1000g of sample with the granularity not more than 0.125mm in a 300mL conical flask;
(2) adding 15mL of phosphoric acid and 3mL of nitric acid (1+1), wherein the conical flask is placed on an electric furnace for heating, and meanwhile, continuously shaking the conical flask to fully disperse and dissolve the sample until slight smoke is emitted, and taking down the conical flask; wherein, the concentration of the phosphoric acid is more than or equal to 85 percent, and the preparation method of the nitric acid is that 50mL of concentrated nitric acid is measured and dissolved in 50mL of water;
(3) adding 2g of ammonium nitrate, fully shaking, simultaneously blowing out yellow flue gas, adding 50mL of distilled water when cooling to 60-70 ℃ (cooling to the outer wall of the conical flask without scalding hands), fully dissolving the ammonium nitrate, and cooling to room temperature;
(4) titrating with an ammonium ferrous sulfate standard solution to be light red, adding 3-4 drops of N-phenyl-o-aminobenzoic acid indicator, and continuously titrating until the liquid to be detected becomes bright yellow, namely the end point; wherein the concentration of the ammonium ferrous sulfate standard solution is 0.02 mol/L.
Example 3
After the manganese carbonate ore is measured by the method, the analysis result is calculated according to the following formula;
Mn％＝C*V*M/m*100％
in the formula:
c-concentration of standard titration solution of ferrous ammonium sulfate, unit: mol/L;
m-relative atomic mass of manganese: 54.94 of the total weight of the powder;
v is volume of ammonium ferrous sulfate standard titration solution consumed by titration test solution, unit: mL;
m-weighed sample mass, unit: g.
specifically, manganese ore standards GSB 03-2587-.
As can be seen from the above table, the precision of the results measured by the method of the present application was 0.031% and 0.071%, respectively, and the analysis requirements were completely satisfied.
Meanwhile, the manganese ore sample and slag are analyzed and compared by the method of example 2 and the existing measuring method, and the results are shown in the following table.
| Numbering | Example 2/%) | Existing assay methods/%) | Relative error |
| 1 | 22.50 | 22.46 | 0.04 |
| 2 | 22.10 | 22.00 | 0.10 |
| 3 | 15.74 | 15.61 | 0.13 |
| 4 | 1.97 | 1.91 | 0.06 |
As can be seen from the above table, the result of the measurement of the manganese content in the manganese ore by using the method of example 2 of the present application is substantially the same as that of the measurement by using the existing measurement method, which indicates that the precision and accuracy requirements for the measurement of the manganese content in the manganese carbonate ore can be met by using the improved method.
Compared with the existing determination method, the method for determining the manganese content in manganese carbonate ore by adopting the ammonium nitrate method has the following differences and advantages.
(1) In the existing ammonium nitrate method, hydrochloric acid and phosphoric acid are adopted to dissolve an ore sample, however, as a liquid to be detected is generally heated to 300 ℃ at a high temperature, nitric acid is added, and after nitric acid smoke is removed, the liquid is cooled to 220 ℃ (at the moment, phosphoric acid also emits micro smoke); by the operation, the operation difficulty is increased, the determination time is prolonged, and the determination process is not easy to master. Multiple test analysis shows that the improved determination method can be used for directly dissolving the sample by using phosphoric acid and nitric acid, can also meet the requirement of completely dissolving the ore sample, is easy to control the temperature (about 220 ℃), only needs about ten minutes of dissolution compared with the traditional dissolution method for half a hour, obviously shortens the analysis time, and saves a large amount of detection time for laboratories for detecting large quantities of ore samples.
(2) When the ammonium nitrate is added, the sample dissolving temperature is not too high or too low; when the concentration is too high, pyrophosphate which is adhered to the bottom of the conical flask and is not dissolved is easily generated, so that the measurement result is low; if the amount is too low, the sample is not completely dissolved. The correct method is as follows: when the sample to be detected smokes (the temperature is about 220 ℃), ammonium nitrate is added, so that the sample to be detected can be better oxidized, and the reaction is more severe and should be carried out in a fume hood.
(3) The improvement of the traditional ammonium nitrate determination method can well shorten the analysis and measurement period and can keep better determination precision and accuracy; the method is simple to operate and easy to master, and can meet the daily analysis requirement.
In addition, if the determined ore sample is pyrolusite or pyrolusite, the ore sample contains manganese dioxide, so that a small amount of hydrochloric acid is required to be added for reduction during sample dissolution, and the manganese dioxide can be analyzed and measured; however, since the Mn content of pyrolusite is not constant, it is likely to cause inaccurate measurement results, and thus, it is not recommended to measure the Mn content of pyrolusite using a nitric acid method.
Claims (5)
1. A method for determining the manganese content in manganese carbonate ore by an ammonium nitrate method is characterized by comprising the following steps:
(1) weighing 0.1g of sample and placing the sample in a conical flask;
(2) adding 15mL of phosphoric acid and 3mL of nitric acid, placing the conical flask on an electric furnace for heating to completely dissolve the sample until slight smoke is emitted, and taking down the conical flask;
(3) adding 2g of ammonium nitrate, fully shaking, simultaneously blowing out yellow flue gas, adding 50mL of distilled water when cooling to 60-70 ℃, fully dissolving the ammonium nitrate, and cooling to room temperature;
(4) titrating with an ammonium ferrous sulfate standard solution to light red, adding 3-4 drops of N-phenyl-o-aminobenzoic acid indicator, and continuously titrating until the liquid to be detected becomes bright yellow, namely the end point.
2. The method of claim 1, wherein in step (1), the sample has a particle size of 0.125mm or less.
3. The method according to claim 1, wherein the concentration of phosphoric acid in the step (2) is 85% or more.
4. The method according to claim 1, wherein in the step (2), the nitric acid is prepared by measuring 50mL of concentrated nitric acid dissolved in 50mL of water.
5. The method according to claim 1, wherein in the step (4), the concentration of the standard solution of ferrous ammonium sulfate is 0.02 mol/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| 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 |
| CN104807813A (en) * | 2015-05-13 | 2015-07-29 | 湖南瑞铨冶金有限公司 | Rapid analysis method for content of manganese in ferromanganese iron |
| 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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104807813A (en) * | 2015-05-13 | 2015-07-29 | 湖南瑞铨冶金有限公司 | Rapid analysis method for content of manganese in ferromanganese iron |
| 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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| 刘亮 等: "硝酸铵法测定菱锰矿中锰含量方法的改进", 《化学分析计量》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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Application publication date: 20200211 |