CN102749319A - Method for detecting contents of silicon, manganese and phosphorus in vanadium-nitrogen alloy - Google Patents
Method for detecting contents of silicon, manganese and phosphorus in vanadium-nitrogen alloy Download PDFInfo
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- CN102749319A CN102749319A CN2012102552515A CN201210255251A CN102749319A CN 102749319 A CN102749319 A CN 102749319A CN 2012102552515 A CN2012102552515 A CN 2012102552515A CN 201210255251 A CN201210255251 A CN 201210255251A CN 102749319 A CN102749319 A CN 102749319A
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Abstract
The invention provides a method for detecting contents of silicon, manganese and phosphorus in a vanadium-nitrogen alloy. The method comprises the following steps of: adding nitric acid, hydrochloric acid and water to a sample; heating the sample until the sample is completely dissolved, so as to obtain a sample solution to be detected; detecting spectral line intensity of the sample solution to be detected by using a traditional inductively coupled plasma atomic emission spectrometry; and obtaining corresponding contents of the silicon, the manganese and the phosphorus in a standard working curve of the silicon, the manganese and the phosphorus according to the spectral line intensity. The method for detecting the contents of the silicon, the manganese and the phosphorus in the vanadium-nitrogen alloy, provided by the invention, has the advantages of convenience in operation, high accuracies of the detected contents of the silicon, the manganese and the phosphorus; a detecting result has the advantages of good stability, reproducibility and accuracy; and requirements on daily content detections of the silicon, the manganese and the phosphorus in the vanadium-nitrogen alloy can be completely satisfied.
Description
Technical field
The present invention relates to the assay method of silicon, manganese and phosphorus content in a kind of VN alloy, belong to the analysis and testing technology field.
Background technology
At present standard GB/T25483.8-2009 adopts ICP-AES, comes the silicon in the VN alloy, manganese and phosphorus content are measured.Specifically be with the most of VN alloy test portion of nitric acid heating for dissolving; Filter; The residue that filtration is obtained is used hydrochloric acid leaching again with the fusion in muffle furnace of mixed with little amount flux, after the filtrating that obtains with above-mentioned filtration merges; Constant volume becomes sample solution, adopts ICP-AES to measure again.This method adopts nitric acid heating for dissolving VN alloy test portion, causes the silica test result on the low side easily, in addition; This method is used the nitric acid heating for dissolving earlier, uses alkali fusion again, uses hydrochloric acid leaching again; Complex operation not only causes also that salt content increases in the solution, and easy blocking torch pipe.In addition, though just can measure after the sample dissolution silicon, manganese and P elements, time saving and energy saving; And need not consume a large amount of chemical reagent; Can reduce pollution to environment, the protection health of operators, but bigger because of measuring difficulty; Therefore, also there is not efficient ways to measure at present to silicon, manganese and phosphorus content in the VN alloy.
Summary of the invention
The object of the present invention is to provide a kind of method that can accurately measure silicon in the VN alloy, manganese and phosphorus content.
The present invention realizes through following technical scheme: the assay method of silicon, manganese and phosphorus content in a kind of VN alloy; Comprise line strength of measuring test liquid with conventional ICP-AES; In the standard working curve of silicon, manganese and phosphorus, obtain corresponding silicon, manganese and 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 15～25mL/g sample; In the VN alloy sample, add nitric acid, and in the VN alloy sample, add hydrochloric acid, press the amount of 150～170mL/g sample again by the amount of 40～50mL/g sample; In the VN alloy sample, add entry; Under 100～120 ℃ of temperature, be heated to the VN alloy sample and dissolve fully, get the lysate of 100～110mL/g sample;
The lysate of B, cooling step A is to room temperature, and this lysate of dilute with water to concentration is 0.002 g/mL, shakes up, and gets sample to be tested liquid.
The nitric acid of said steps A, hydrochloric acid are commercial analysis net product.
The present invention compared with prior art has advantage and effect: after adopting such scheme to process sample to be tested liquid; It is available ICP-AES of the prior art; Directly measure silicon, manganese and phosphorus content in the VN alloy; Not only operation is very easy, and the silicon of measuring, manganese and phosphorus content accuracy rate are high, and it measures the result has good stable property, reappearance and accuracy.The inventive method is reliable, practical, convenient, fast, can satisfy the needs of silicon, manganese and phosphorus content in the daily mensuration VN alloy fully.
Embodiment
Below in conjunction with embodiment the present invention is done and to further describe.
Embodiment 1
Prepare silicon, manganese and phosphorus standard solution by routine:
1, the preparation of silicon standard solution:
1A, with commercial silicon dioxide (more than 99.9%) in 1000 ℃ of following calcination 1h, the cooling, drying;
1B, the amount of pressing 10 g mixed flux/g sample take by weighing the dry silicon dioxide of 0.4279g step 1A, add 4.3 g mixed fluxs; This mixed flux is following mass ratio: natrium carbonicum calcinatum: boric acid=2:1, and mixing gets potpourri; Potpourri is placed in the platinum crucible in 150 ℃ of heating down, place again to be heated to potpourri under 1000 ℃ of temperature and to melt to transparently, continue heating and melting 5min; Cooling gets the molten sample;
1C, the molten sample of step 1B is put into 100 mL70 ℃ hot water, heating for dissolving molten sample is limpid to solution, is cooled to room temperature, is diluted with water to the silicon solution of 200 μ g/mL, the silicon standard solution, place plastic bottle subsequent use this standard solution;
2, the preparation of manganese standard solution:
2A, commercial electrolytic manganese (content is more than 99.9%) is cleaned to surperficial non-oxidation manganese with dilute sulfuric acid, the volume ratio of this dilute sulfuric acid is: H
2SO
4: H
2O=5:95, water is cleaned repeatedly again, puts into absolute ethyl alcohol and embathes air dry 4～5 times;
2B, the amount of pressing 40mL/g electrolytic manganese, the dry electrolytic manganese that takes by weighing 0.5000g step 2A is put into the rare nitric acid of 20mL, and the volume ratio of this rare nitric acid is: HNO
3: H
2O=1:3; The heating for dissolving electrolytic manganese, cools off to drive most oxides of nitrogen to boiling, and thin up to 500 μ g/mL gets the manganese standard solution;
The 20.00 mL manganese standard solution that 2C, removing step 2B make place 500 mL volumetric flasks, are diluted with water to scale, shake up, and this solution contains 20 μ g/mL manganese;
3, the preparation of phosphorus titer:
3A, commercial potassium dihydrogen phosphate (content is more than 99.99%) is dried to constant weight under 105 ℃, and in exsiccator, be cooled to room temperature;
3B, the amount of pressing 10 mL/g potassium dihydrogen phosphates take by weighing the dry potassium dihydrogen phosphate of 2.1968g step 3A and put into 200mL water to dissolving fully, are diluted with water to 500 μ g/mL, get the phosphorus standard solution;
The 20.00 mL phosphorus standard solution that 3C, removing step 3B make are diluted with water to scale in 500 mL volumetric flasks, shake up, and this solution contains the phosphorus of 20 μ g/mL;
4, the preparation of vanadium standard solution:
4A, with commercial vanadium pentoxide in 105 ℃ of following oven dry 2 h, and in exsiccator, be cooled to room temperature;
4B, the amount of pressing 30 mL/g vanadium pentoxide take by weighing the dry vanadium pentoxide of 4.463g step 4A, and adding concentration is the sodium hydroxide solution 134mL of 50g/L, and the heating for dissolving vanadium pentoxide gets lysate;
4C, in the lysate of step 4B, add in the dilute sulfuric acid with lysate to acid and excessive 20mL, this dilute sulfuric acid is following volume ratio: H
2SO
4: H
2O=1:1, heating evaporation is to emitting the sulfuric acid cigarette, and cooling adds 100mL water, is heated to 100～150 ℃, with dissolved salts, cooling, thin up becomes the vanadium solution of 25mg/mL, gets the vanadium standard solution;
5, contain the preparation of silicon, manganese and the phosphorus standard solution of vanadium:
5A, the massfraction of listing by table 1; Silicon, manganese and phosphorus standard solution that step 1C, 2C, 3C are obtained place 7 100 mL volumetric flasks respectively; Add 6.00 mL vanadium standard solution and 5 mL dilute sulfuric acids that step 4C makes respectively, this dilute sulfuric acid is following volume ratio: H
2SO
4: H
2O=1:9 is diluted with water to scale, and mixing obtains seven parts of silicon, manganese and phosphorus standard solution that 100 mL faintly acids contain vanadium respectively;
5B, with conventional ICP-AES of the prior art; Line strength of silicon, manganese and phosphorus in seven parts of standard solution of difference determination step 5A; Measure condition of work and see table 1, the wavelength and the progression of the silicon in the standard solution, manganese and P elements are seen table 2;
5C, the massfraction with listed silicon, manganese and phosphorus standard solution among the step 5A is a horizontal ordinate respectively, is ordinate with line strength of silicon, manganese and phosphorus in the step 5B gained standard solution, draws out the standard working curve of silicon, manganese and phosphorus.
Embodiment 2
The mensuration of silicon, manganese and phosphorus in the VN alloy to be measured:
1, the preparation of VN alloy test liquid to be measured:
1A, the amount of pressing the 15mL/g sample; In 0.2000g VN alloy sample, add the pure nitric acid 3mL of commercial analysis, and the amount of pressing the 40mL/g sample adds commercial analysis pure hydrochloric acid 8mL, the amount of pressing the 150mL/g sample again in the VN alloy sample; In the VN alloy sample, add entry 30 mL; Under 100 ℃ of temperature, slowly be heated to the VN alloy sample and dissolve fully, get the lysate of 20 mL;
1B, hot-cold lysis liquid are to room temperature, and dilute with water lysate to concentration is 100 mL, shake up, and get sample to be tested liquid;
2, the mensuration of silicon, manganese and phosphorus in the VN alloy sample:
2A, with the identical condition of work of embodiment 1 step 5B under; Measure line strength of present embodiment 2 step 1B gained sample to be tested liquid; According to measured line strength, on the working curve of embodiment 1 step 5C, once obtain silicon in the sample, manganese and phosphorus content and be respectively: 0.22%; 0.010%, 0.023%.
Embodiment 3
The mensuration of silicon, manganese and phosphorus in the VN alloy to be measured:
1, the preparation of VN alloy test liquid to be measured:
1A, the amount of pressing the 25mL/g sample; In 0.2000g VN alloy sample, add the pure nitric acid 5mL of commercial analysis, and the amount of pressing the 50mL/g sample adds commercial analysis pure hydrochloric acid 10mL, the amount of pressing the 170mL/g sample again in the VN alloy sample; In the VN alloy sample, add entry 34 mL; Under 120 ℃ of temperature, slowly be heated to the VN alloy sample and dissolve fully, get the lysate of 22 mL;
1B, hot-cold lysis liquid are to room temperature, and dilute with water lysate to concentration is 100 mL, shake up, and get sample to be tested liquid;
2, the mensuration of silicon, manganese and phosphorus in the VN alloy sample:
2A, with the identical condition of work of embodiment 1 step 5B under; Measure line strength of present embodiment 3 step 1B gained sample to be tested liquid; According to measured line strength, on the working curve of embodiment 1 step 5C, once obtain silicon in the sample, manganese and phosphorus content and be respectively: 0.22%; 0.010%, 0.023%.
Embodiment 4
The mensuration of silicon, manganese and phosphorus in the VN alloy to be measured:
1, the preparation of VN alloy test liquid to be measured:
1A, the amount of pressing the 20mL/g sample; In 0.2000g VN alloy sample, add the pure nitric acid 4mL of commercial analysis, and the amount of pressing the 45mL/g sample adds commercial analysis pure hydrochloric acid 9mL, the amount of pressing the 160mL/g sample again in the VN alloy sample; In the VN alloy sample, add entry 32 mL; Under 110 ℃ of temperature, slowly be heated to the VN alloy sample and dissolve fully, get the lysate of 21 mL;
1B, hot-cold lysis liquid are to room temperature, and dilute with water lysate to concentration is 100 mL, shake up, and get sample to be tested liquid;
2, the mensuration of silicon, manganese and phosphorus in the VN alloy sample:
2A, with the identical condition of work of embodiment 1 step 5B under; Measure line strength of present embodiment 4 step 1B gained sample to be tested liquid; According to measured line strength, on the working curve of embodiment 1 step 5C, once obtain silicon in the sample, manganese and phosphorus content and be respectively: 0.22%; 0.010%, 0.023%.
Table 1 silicon, manganese and the % of phosphorus standard serial solution unit (massfraction)
| Standard name | Si | Mn | P |
| Blank1 | 0.00 | 0.00 | 0.00 |
| STD1 | 0.050 | 0.005 | 0.005 |
| STD2 | 0.10 | 0.010 | 0.010 |
| STD3 | 0.20 | 0.020 | 0.020 |
| STD4 | 0.30 | 0.030 | 0.030 |
| STD5 | 0.40 | 0.040 | 0.040 |
| STD6 | 0.50 | 0.050 | 0.050 |
Table 2 instrument condition of work
| Power (W) | Atomizing pressure (psi) | Secondary air amount (L/min) | Pump speed (rpm) | Integral time (s) |
| 1150 | 26.06 | 0.5 | 130 | 10 |
Table 3 element wavelength to be measured and progression
| Element | Wavelength (nm) | Level |
| Si | 251.611 | 134 |
| Mn | 279.482 | 120 |
| P | 177.499 | 490 |
Claims (1)
1. the assay method of silicon, manganese and phosphorus content in the VN alloy; Comprise line strength of measuring test liquid with conventional ICP-AES; In the standard working curve of silicon, manganese and phosphorus, obtain corresponding silicon, manganese and 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 15～25mL/g sample; In the VN alloy sample, add nitric acid, and in the VN alloy sample, add hydrochloric acid, press the amount of 150～170mL/g sample again by the amount of 40～50mL/g sample; In the VN alloy sample, add entry; Under 100～120 ℃ of temperature, be heated to the VN alloy sample and dissolve fully, get the lysate of 100～110mL/g sample;
The lysate of B, cooling step A is to room temperature, and this lysate of dilute with water to concentration is 0.002 g/mL, shakes up, and gets sample to be tested liquid.
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| CN104807806A (en) * | 2015-04-30 | 2015-07-29 | 武汉钢铁(集团)公司 | Method for measuring content of phosphorus in sintered flux |
| CN105223188A (en) * | 2014-05-29 | 2016-01-06 | 上海梅山钢铁股份有限公司 | A kind of steel-making assay method of elemental silicon content in siliceous exothermic mixture |
| CN105300975A (en) * | 2015-11-11 | 2016-02-03 | 武钢集团昆明钢铁股份有限公司 | Detecting method for phosphorus content in vanadium slag |
| CN106596522A (en) * | 2017-02-28 | 2017-04-26 | 武钢集团昆明钢铁股份有限公司 | Determination method for contents of silicon, manganese and phosphorus in natural microalloy iron powder |
| CN110823868A (en) * | 2019-10-21 | 2020-02-21 | 南京钢铁股份有限公司 | Analysis method for determining primary and secondary components in composite vanadium-nitrogen alloy |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105223188A (en) * | 2014-05-29 | 2016-01-06 | 上海梅山钢铁股份有限公司 | A kind of steel-making assay method of elemental silicon content in siliceous exothermic mixture |
| CN104807806A (en) * | 2015-04-30 | 2015-07-29 | 武汉钢铁(集团)公司 | Method for measuring content of phosphorus in sintered flux |
| CN105300975A (en) * | 2015-11-11 | 2016-02-03 | 武钢集团昆明钢铁股份有限公司 | Detecting method for phosphorus content in vanadium slag |
| CN105300975B (en) * | 2015-11-11 | 2018-04-24 | 武钢集团昆明钢铁股份有限公司 | The detection method of phosphorus content in a kind of vanadium slag |
| CN106596522A (en) * | 2017-02-28 | 2017-04-26 | 武钢集团昆明钢铁股份有限公司 | Determination method for contents of silicon, manganese and phosphorus in natural microalloy iron powder |
| CN110823868A (en) * | 2019-10-21 | 2020-02-21 | 南京钢铁股份有限公司 | Analysis method for determining primary and secondary components in composite vanadium-nitrogen alloy |
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