CN102890081A - Method for measuring phosphorus content in nitriding reinforcing agent - Google Patents
Method for measuring phosphorus content in nitriding reinforcing agent Download PDFInfo
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- CN102890081A CN102890081A CN2012103542826A CN201210354282A CN102890081A CN 102890081 A CN102890081 A CN 102890081A CN 2012103542826 A CN2012103542826 A CN 2012103542826A CN 201210354282 A CN201210354282 A CN 201210354282A CN 102890081 A CN102890081 A CN 102890081A
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- nitrogenize
- phosphorus content
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Abstract
The invention relates to a method for measuring phosphorus content in a nitriding reinforcing agent. The method comprises the steps of: adding nitric acid and hydrofluoric acid in a sample to be measured for dissolving the sample to be measured, adding perchloric acid until smoking and adding acid for dissolving a test solution to obtain a sample liquid to be measured. The phosphorus content in the nitriding reinforcing agent can be directly measured after the sample to be measured is dissolved, so that the method has the advantages of convenience for operation, high accuracy rate of the measured phosphorus content and good stability, reproducibility and accuracy of a measurement result, and can fully meet the demand on daily measurement of the phosphorus content in the nitriding reinforcing agent.
Description
Technical field
The invention belongs to analysis and testing technology, especially relate to the assay method technical field of phosphorus content in a kind of nitrogenize reinforcing agent.
Background technology
The mensuration of phosphorus content in the nitrogenize reinforcing agent, also there is not at present the national standard analytical approach, measuring phosphorus content in other samples such as the steel is to adopt spectrophotometric method, operate loaded down with trivial details, analyze, measure long flow path, method need to consume a large amount of chemical reagent in addition, not only contaminated environment but also endanger the healthy of operating personnel.The employing ICP-AES is measured; although just can measure P elements after the dissolution sample; time saving and energy saving; and need not consume a large amount of chemical reagent; can reduce the pollution to environment, the protection operating personnel's is healthy, but larger because measuring difficulty; therefore, also there is not at present effective method to measure phosphorus content in the nitrogenize reinforcing agent.
Summary of the invention
The purpose of this invention is to provide a kind of can Accurate Determining nitrogenize reinforcing agent in the method for phosphorus content.
The present invention is achieved through the following technical solutions:
The assay method of phosphorus content in a kind of nitrogenize reinforcing agent, comprise line strength of measuring test liquid with conventional ICP-AES, in the standard working curve of phosphorus, obtain corresponding phosphorus content value according to this line strength, the present invention is characterised in that, test liquid makes through the following step:
A, the amount of pressing 150～250mL/g sample, in nitrogenize reinforcing agent sample, add nitric acid, in nitrogenize reinforcing agent sample, add hydrofluorite by the amount of 5～15mL/g sample, under 100～150 ℃ of temperature, slow heating for dissolving gets the lysate of 40～50mL/g sample;
B, the amount by 1～2mL/mL lysate in the lysate of steps A add perchloric acid, under 300～350 ℃, are heated to the perchloric acid cigarette and emit continuation heating 5～10min when bottleneck, and cooling gets lysate;
C, the amount of pressing 10～15mL/mL lysate in step B gained lysate add watery hydrochloric acid, are heated to 100～150 ℃ and treat the salt dissolving, and hot-cold lysis liquid is to room temperature, and dilute with water concentration is 0.001g/mL, shakes up, and gets sample to be tested liquid.
The nitric acid of described steps A and hydrofluorite are commercial analysis net product.
The perchloric acid of described step B is commercial analysis net product.
The watery hydrochloric acid of described step C is following volume ratio: HCl:H
2O=1:1.
The present invention compared with prior art has following advantages and effect: after adopting such scheme to make sample to be tested liquid, it is available ICP-AES of the prior art, directly measure phosphorus content in the nitrogenize reinforcing agent, not only easy to operate, and the phosphorus content accuracy rate of measuring is high, its measurement result has good stability, reappearance and accuracy, and evidence the inventive method is reliable, practical, can satisfy the needs of phosphorus content in the daily mensuration nitrogenize reinforcing agent.
Embodiment
Below in conjunction with embodiment the present invention is described further.
Embodiment 1
Preparation phosphorus standard solution:
1, the preparation of phosphorus titer:
1A, commercial potassium dihydrogen phosphate (content is more than 99.99%) dried under 105 ℃ be cooled to room temperature to constant weight and in exsiccator;
1B, the amount of pressing 10 mL/g potassium dihydrogen phosphates are put into water to fully dissolving with the potassium dihydrogen phosphate of above-mentioned drying, are diluted with water to 500 μ g/mL, get the phosphorus titer;
1C, pipette the 10.00 mL phosphorus standard solution that the 2B step makes and place 500 mL volumetric flasks, be diluted with water to scale, shake up, this solution contains 10 μ g/mL phosphorus;
2, the preparation of manganese solution:
2A, be that 4.9% sulfuric acid liquid cleans to surperficial non-oxidation manganese with commercial electrolytic manganese (content is more than 99.9%) with mass concentration, water is cleaned repeatedly again, puts into absolute ethyl alcohol and embathes drying 4～5 times;
2B, the amount of pressing 40mL/g electrolytic manganese are put into rare nitric acid with the electrolytic manganese of above-mentioned drying, and wherein the volume ratio of rare nitric acid is: HNO
3: H
2O=1:3; Heating for dissolving, is cooled off to drive most oxides of nitrogen to boiling, and thin up gets the manganese titer to 10mg/mL;
3, contain the preparation of the phosphorus standard solution of manganese:
3A, 0.00 mL, 1.00 mL, 3.00 mL, 5.00 mL, 7.00 mL, 9.00 mL, the 15.00 mL gallium standard solution (massfraction is respectively 0.00%, 0.010%, 0.030%, 0.050%, 0.070%, 0.090%, 0.15%) that make of removing step 1C respectively, place respectively 7 100mL volumetric flasks, add respectively 5.00 mL manganese solutions and 5 mL watery hydrochloric acid that the 2B step makes, be diluted with water to scale, mixing, obtain respectively seven parts of standard solution that 100 mL faintly acids contain manganese, wherein watery hydrochloric acid is following volume ratio: HCl:H
2O=1:1;
3B, with conventional ICP-AES of the prior art, phosphorus line strength in seven parts of standard solution of determination step 3A is measured condition of work and is seen Table 1 respectively, wavelength and the progression of the element phosphor in the standard solution see Table 2;
3C, the massfraction of listed phosphorus standard solution is as horizontal ordinate in the 3A respectively, and phosphorus line strength is ordinate in the step 3B gained standard solution, draws out the standard working curve of phosphorus.
Embodiment 2
The mensuration of phosphorus in the nitrogenize reinforcing agent to be measured:
1, the preparation of nitrogenize reinforcing agent test liquid to be measured:
A, the amount of pressing the 150mL/g sample, the amount of add nitric acid 15mL in 0.1000 g nitrogenize reinforcing agent sample, press the 5mL/g sample adds hydrofluorite 0.5mL in nitrogenize reinforcing agent sample, and under 100 ℃ of temperature, slow heating for dissolving gets the lysate of 4mL;
B, the amount of pressing the 1mL/mL lysate in the lysate of steps A add perchloric acid 4mL, under 300 ℃, are heated to the perchloric acid cigarette and emit continue heating 5min when bottleneck, and cooling gets lysate 1mL;
C, the amount of pressing the 10mL/mL lysate in step B gained lysate add watery hydrochloric acid 10mL, are heated to 100 ℃ and treat the salt dissolving, and hot-cold lysis liquid is to room temperature, and dilute with water concentration is 100mL, shakes up, and gets sample to be tested liquid.
2, the mensuration of phosphorus in the nitrogenize reinforcing agent sample:
2A, with the identical condition of work of embodiment 1 step 3B under, line strength of determination step 1C gained test solution to be measured according to measured line strength, on the working curve of embodiment 1 step 3C, obtains that phosphorus content is in the sample: 0.081%.
Embodiment 3
The mensuration of phosphorus in the nitrogenize reinforcing agent to be measured:
1, the preparation of nitrogenize reinforcing agent test liquid to be measured:
A, the amount of pressing the 250mL/g sample, the amount of add nitric acid 25mL in 0.1000 g nitrogenize reinforcing agent sample, press the 15mL/g sample adds hydrofluorite 1.5mL in nitrogenize reinforcing agent sample, and under 150 ℃ of temperature, slow heating for dissolving gets the lysate of 5mL;
B, the amount of pressing the 2mL/mL lysate in the lysate of steps A add perchloric acid 10mL, under 350 ℃, are heated to the perchloric acid cigarette and emit continue heating 10min when bottleneck, and cooling gets lysate 2mL;
C, the amount of pressing the 15mL/mL lysate in step B gained lysate add watery hydrochloric acid 30mL, are heated to 150 ℃ and treat the salt dissolving, and hot-cold lysis liquid is to room temperature, and dilute with water concentration is 100mL, shakes up, and gets sample to be tested liquid.
2, the mensuration of phosphorus in the nitrogenize reinforcing agent sample:
2A, with the identical condition of work of embodiment 1 step 3B under, line strength of determination step 1C gained test solution to be measured according to measured line strength, on the working curve of embodiment 1 step 3C, obtains that phosphorus content is in the sample: 0.081%.
Embodiment 4
The mensuration of phosphorus in the nitrogenize reinforcing agent to be measured:
1, the preparation of nitrogenize reinforcing agent test liquid to be measured:
A, the amount of pressing the 200mL/g sample, the amount of add nitric acid 20mL in 0.1000 g nitrogenize reinforcing agent sample, press the 10mL/g sample adds hydrofluorite 1mL in nitrogenize reinforcing agent sample, and under 120 ℃ of temperature, slow heating for dissolving gets the lysate of 4.5mL;
B, the amount of pressing the 1.5mL/mL lysate in the lysate of steps A add perchloric acid 6.75mL, under 320 ℃, are heated to the perchloric acid cigarette and emit continue heating 7min when bottleneck, and cooling gets lysate 1.5mL;
C, the amount of pressing the 12mL/mL lysate in step B gained lysate add watery hydrochloric acid 18mL, are heated to 120 ℃ and treat the salt dissolving, and hot-cold lysis liquid is to room temperature, and dilute with water concentration is 100mL, shakes up, and gets sample to be tested liquid.
2, the mensuration of phosphorus in the nitrogenize reinforcing agent sample:
2A, with the identical condition of work of embodiment 1 step 3B under, line strength of determination step 1C gained test solution to be measured according to measured line strength, on the working curve of embodiment 1 step 3C, obtains that phosphorus content is in the sample: 0.081%.
Table 1 instrument condition of work
Table 2 element wavelength to be measured and progression
Claims (4)
1. the assay method of phosphorus content in the nitrogenize reinforcing agent, comprise line strength of measuring test liquid with conventional ICP-AES, in the standard working curve of phosphorus, obtain corresponding phosphorus content value according to this line strength, it is characterized in that, test liquid makes through the following step:
A, the amount of pressing 150～250mL/g sample, in nitrogenize reinforcing agent sample, add nitric acid, in nitrogenize reinforcing agent sample, add hydrofluorite by the amount of 5～15mL/g sample, under 100～150 ℃ of temperature, slow heating for dissolving gets the lysate of 40～50mL/g sample;
B, the amount by 1～2mL/ml lysate in the lysate of steps A add perchloric acid, under 300～350 ℃, are heated to the perchloric acid cigarette and emit continuation heating 5～10min when bottleneck, and cooling gets lysate;
C, the amount of pressing 10～15mL/mL lysate in step B gained lysate add watery hydrochloric acid, are heated to 100～150 ℃ and treat the salt dissolving, and hot-cold lysis liquid is to room temperature, and dilute with water concentration is 0.001g/mL, shakes up, and gets sample to be tested liquid.
2. the assay method of phosphorus content in the nitrogenize reinforcing agent sample as claimed in claim 1 is characterized in that the nitric acid of described steps A and hydrofluorite are commercial analysis net product.
3. the assay method of phosphorus content in the nitrogenize reinforcing agent sample as claimed in claim 1, the perchloric acid that it is characterized in that described step B is commercial analysis net product.
4. the assay method of phosphorus content in the nitrogenize reinforcing agent sample as claimed in claim 1 is characterized in that the watery hydrochloric acid among the described step C is following volume ratio: HCl:H
2O=1:1.
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| CN2012103542826A CN102890081A (en) | 2012-09-21 | 2012-09-21 | Method for measuring phosphorus content in nitriding reinforcing agent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105092496A (en) * | 2015-08-14 | 2015-11-25 | 武钢集团昆明钢铁股份有限公司 | Method for detecting content of phosphorus in nitrification intensifier |
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| JPH05231996A (en) * | 1992-02-20 | 1993-09-07 | Sumitomo Metal Ind Ltd | Method of manufactureing intermetallic compound estimation test piece and reagent |
| JP3832204B2 (en) * | 2000-07-28 | 2006-10-11 | 株式会社Ｓｕｍｃｏ | Method for analyzing trace impurities in silicon substrates |
| CN101750406A (en) * | 2008-12-15 | 2010-06-23 | 鞍钢股份有限公司 | Method for measuring Ti content in low-carbon ferrophosphorus |
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2012
- 2012-09-21 CN CN2012103542826A patent/CN102890081A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05231996A (en) * | 1992-02-20 | 1993-09-07 | Sumitomo Metal Ind Ltd | Method of manufactureing intermetallic compound estimation test piece and reagent |
| JP3832204B2 (en) * | 2000-07-28 | 2006-10-11 | 株式会社Ｓｕｍｃｏ | Method for analyzing trace impurities in silicon substrates |
| CN101750406A (en) * | 2008-12-15 | 2010-06-23 | 鞍钢股份有限公司 | Method for measuring Ti content in low-carbon ferrophosphorus |
Non-Patent Citations (2)
| Title |
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| 陈菲菲: "ICP 光谱法测定硅锰合金中的磷", 《山东冶金》 * |
| 黄梅: "电感耦合等离子体原子发射光谱法测定硅锰合金中磷", 《化学研究与应用》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105092496A (en) * | 2015-08-14 | 2015-11-25 | 武钢集团昆明钢铁股份有限公司 | Method for detecting content of phosphorus in nitrification intensifier |
| CN105092496B (en) * | 2015-08-14 | 2017-12-15 | 武钢集团昆明钢铁股份有限公司 | The detection method of phosphorus content in a kind of nitridation reinforcing agent |
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