CN103149196A - Method for determining content of silicon, phosphor and aluminium in ferrocolumbium through inductive coupling plasma emission spectroscopy - Google Patents
Method for determining content of silicon, phosphor and aluminium in ferrocolumbium through inductive coupling plasma emission spectroscopy Download PDFInfo
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- CN103149196A CN103149196A CN2013100585063A CN201310058506A CN103149196A CN 103149196 A CN103149196 A CN 103149196A CN 2013100585063 A CN2013100585063 A CN 2013100585063A CN 201310058506 A CN201310058506 A CN 201310058506A CN 103149196 A CN103149196 A CN 103149196A
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Abstract
The invention discloses a method for determining the content of silicon, phosphor and aluminium in ferrocolumbium through inductive coupling plasma emission spectroscopy. The method comprises the following steps of: weighing a ferrocolumbium sample, and dissolving the ferrocolumbium sample in acid to obtain a solution to be tested; preparing a standard solution, and determining standard working curves needed for the content of the silicon, phosphorous and aluminium in the ferrocolumbium sample; and introducing the solution to be tested into an inductive coupling plasma emission spectrograph, and determining the content of the silicon, phosphorous and aluminium according to the standard working curves. The method can be used for simultaneously determining multiple elements, is simple and convenient in operation, rapid in analysis speed, short in time needed for testing and high in accuracy and has the advantages of energy conservation and environmental-friendliness.
Description
Technical field
The present invention relates to technical field of ferrous metallurgical analysis, specifically, relate to the method that a kind of inductively coupled plasma atomic emission (Inductively coupled plasma emission spectrum, ICP) is measured silicon phosphorus aluminium content in ferro-niobium.
Background technology
Ferrocolumbium is very important niobium goods, and it is widely used in low alloy steel, structural steel, stainless refractory steel, antiwear cast iron alloy etc.But niobium is crystal grain thinning in steel, reduces superheated susceptivity and the temper brittleness of steel, improves intensity and the toughness of steel, improves the austenite corrosion among crystalline grains.Add with the ferrocolumbium form that in steel, alloying is the method that generally adopts.Therefore, know that accurately silicon in ferro-niobium, phosphorus, aluminium content tool are of great significance.
In ferro-niobium, silicon, manganese, phosphorus, aluminum content tests have x-fluorescence spectrophotometer method to measure at present, but the x-fluorescent spectrometry has certain difficulty when sample prepares, and other method is mainly chemical gauging.Wherein phosphorus adopts national standard method mensuration need to use a large amount of chemical reagent and need the time of 2-3 days just can complete, and silicon adopts the method for colorimetric to measure, and aluminium adopts EDTA coordination method to measure.Need a large amount of chemical reagent to need many people to operate simultaneously during each element of chemical gauging and detection time longer.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of method that inductively coupled plasma atomic emission is measured silicon phosphorus aluminium content in ferro-niobium, and the method can be measured a plurality of elements simultaneously.
Technical scheme of the present invention is as follows:
A kind of inductively coupled plasma atomic emission is measured the method for silicon phosphorus aluminium content in ferro-niobium, comprises the following steps: take the ferro-niobium sample, with the described ferro-niobium sample of acid dissolving, obtain solution to be measured; Preparation standard solution is determined silicon, phosphorus and the required standard working curve of aluminium content in described ferro-niobium sample; Described solution to be measured is introduced inductive coupling plasma emission spectrograph, measure the content of silicon, phosphorus and aluminium in described ferro-niobium sample according to described standard working curve.
Further, the described ferro-niobium sample that takes, with the described ferro-niobium sample of acid dissolving, the step that obtains solution to be measured comprises: take 0.2g ferro-niobium sample and be placed in the 250ml polytetrafluoroethylene beaker; Add 10ml nitric acid in described ferro-niobium sample; Drip 5ml hydrofluorite in described ferro-niobium sample, then at room temperature placed 1 hour, described ferro-niobium sample is dissolved fully; Described ferro-niobium sample after dissolving is fully transferred to that in 100ml plastics volumetric flask, constant volume shakes up.
Further, described preparation standard solution determines that the step of the standard working curve that silicon, phosphorus and aluminium content in described ferro-niobium sample is required comprises: the ferro-niobium standard sample of different quality is placed in respectively 5 250ml polytetrafluoroethylene beakers; Add 10ml nitric acid in described ferro-niobium standard sample; Drip 5ml hydrofluorite in described ferro-niobium standard sample, then at room temperature placed 1 hour, described ferro-niobium standard sample is dissolved fully; Described ferro-niobium standard sample after dissolving is fully transferred to that in 100ml plastics volumetric flask, constant volume shakes up; Draw described standard working curve according to the light intensity of each element in described ferro-niobium standard sample.
Further, the analysis of line wavelength of silicon, phosphorus and the aluminium in described ferro-niobium sample is respectively: silicon 251.612nm, phosphorus 213.617nm, aluminium 396.153nm.
Technique effect of the present invention is as follows:
1, method of the present invention only needs dissolved samples once, can measure simultaneously the content of silicon, phosphorus, aluminium in the ferro-niobium sample, and easy and simple to handle, analysis speed is fast, the test required time is short, accuracy is high.
2, method of the present invention is only used a small amount of nitric acid and hydrofluorite, has advantages of energy-saving and environmental protection.
Embodiment
Preferred embodiment of the invention ICP spectrometer used is entirely to compose the direct-reading plasma-speetrometer by the OPTIMA5300DV Bidirectional observation type that U.S. PE company produces.The software of this spectrometer adopts Winlab32 software, has multispectral match function, and atomizer adopts the hydrofluoric acid resistant atomizer.The running parameter of this spectrometer is as shown in table 1.
The running parameter of table 1 spectrometer of the present invention
The flow process that ICP method of the present invention is measured the method for silicon, phosphorus and aluminium content in ferro-niobium is as follows:
Step S1: take the ferro-niobium sample, with the described ferro-niobium sample of acid dissolving, obtain solution to be measured;
Preferred embodiment of the invention nitric acid used is that top grade is pure, and density is 1.42g/ml; Hydrofluorite is that top grade is pure, and density is 1.15g/ml.
Take 0.2g ferro-niobium sample and be placed in the 250ml polytetrafluoroethylene beaker.Add 10ml nitric acid in this ferro-niobium sample.Slowly drip 5ml hydrofluorite in this ferro-niobium sample.Constantly shake beaker when dripping hydrofluorite, controlling reaction can not be too fast, avoids silicon to form silicon tetrafluoride gas and overflows.Then at room temperature placed 1 hour, during need to shake beaker, this ferro-niobium sample is dissolved fully.This ferro-niobium sample after dissolving is fully transferred to that in 100ml plastics volumetric flask, constant volume shakes up.
Step S2: preparation standard solution, determine silicon, phosphorus and the required standard working curve of aluminium content in the ferro-niobium sample.
The ferro-niobium standard sample of different quality is placed in respectively 5 250ml polytetrafluoroethylene beakers.Add 10ml nitric acid in this ferro-niobium standard sample.Slowly drip 5ml hydrofluorite in this ferro-niobium standard sample, constantly shake beaker when dripping hydrofluorite, controlling reaction can not be too fast, avoids silicon to form silicon tetrafluoride gas and overflows.Then at room temperature placed 1 hour, during need to shake beaker, this ferro-niobium standard sample is dissolved fully.Ferro-niobium standard sample after dissolving is fully transferred to that in 100ml plastics volumetric flask, constant volume shakes up.This ferro-niobium standard sample is incorporated in the ICP spectrometer, starts this ICP spectrometer this ferro-niobium standard sample is tested.Wherein, the analysis of line wavelength of silicon, phosphorus and aluminium is respectively: silicon 251.612nm, phosphorus 213.617nm and aluminium 396.153nm.Light intensity drawing standard working curve according to each element in this ferro-niobium standard sample of test gained.The content of each element is as horizontal ordinate in this ferro-niobium standard sample, take the light intensity of each element of recording as ordinate, and the drawing standard working curve.The related coefficient of standard working curve: phosphorus 0.992, silicon are 0.998, aluminium is 0.999.
Step S3: solution to be measured is introduced the ICP spectrometer, measure the content of silicon, phosphorus and aluminium in the ferro-niobium sample according to standard working curve.
With atomized solution after solution atomization to be measured, this atomized soln is introduced the ICP spectrometer, start the ICP spectrometer this atomized soln is tested, obtain the light intensity of silicon, phosphorus and aluminium.Wherein, the analysis of line wavelength of silicon, phosphorus and aluminium is respectively: silicon 251.612nm, phosphorus 213.617nm and aluminium 396.153nm.Obtain the content of corresponding silicon, phosphorus and aluminium according to the light intensity on standard working curve.
Under identical experiment condition, measure the light intensity of a reagent blank solvent, with the impact on experimental result of environment, the experiment of getting rid of experiment medicine used, experimental implementation.
To compare with silicon, phosphorus and aluminium content in the ferro-niobium sample of ICP method mensuration with silicon, phosphorus and aluminium content in the ferro-niobium sample of chemical analysis method mensuration, as shown in table 2.
Adopt as can be seen from Table 2 the ICP method can measure exactly silicon in the ferro-niobium sample, phosphorus and aluminium content.
The content of silicon, phosphorus and aluminium that table 2 ICP method of the present invention and chemical analysis method are measured
Claims (4)
1. an inductively coupled plasma atomic emission is measured the method for silicon phosphorus aluminium content in ferro-niobium, it is characterized in that, comprises the following steps:
Take the ferro-niobium sample, with the described ferro-niobium sample of acid dissolving, obtain solution to be measured;
Preparation standard solution is determined silicon, phosphorus and the required standard working curve of aluminium content in described ferro-niobium sample;
Described solution to be measured is introduced inductive coupling plasma emission spectrograph, measure the content of silicon, phosphorus and aluminium in described ferro-niobium sample according to described standard working curve.
2. inductively coupled plasma atomic emission as claimed in claim 1 is measured the method for silicon phosphorus aluminium content in ferro-niobium, it is characterized in that, and the described ferro-niobium sample that takes, with the described ferro-niobium sample of acid dissolving, the step that obtains solution to be measured comprises:
Take 0.2g ferro-niobium sample and be placed in the 250ml polytetrafluoroethylene beaker;
Add 10ml nitric acid in described ferro-niobium sample;
Drip 5ml hydrofluorite in described ferro-niobium sample, then at room temperature placed 1 hour, described ferro-niobium sample is dissolved fully;
Described ferro-niobium sample after dissolving is fully transferred to that in 100ml plastics volumetric flask, constant volume shakes up.
3. inductively coupled plasma atomic emission as claimed in claim 2 is measured the method for silicon phosphorus aluminium content in ferro-niobium, it is characterized in that, described preparation standard solution, determine that the step of the standard working curve that silicon, phosphorus and aluminium content in described ferro-niobium sample is required comprises:
The ferro-niobium standard sample of different quality is placed in respectively 5 250ml polytetrafluoroethylene beakers;
Add 10ml nitric acid in described ferro-niobium standard sample;
Drip 5ml hydrofluorite in described ferro-niobium standard sample, then at room temperature placed 1 hour, described ferro-niobium standard sample is dissolved fully;
Described ferro-niobium standard sample after dissolving is fully transferred to that in 100ml plastics volumetric flask, constant volume shakes up;
Draw described standard working curve according to the light intensity of each element in described ferro-niobium standard sample.
4. inductively coupled plasma emission spectrography as claimed in claim 3 is measured the method for silicon, phosphorus and aluminium content in ferro-niobium, it is characterized in that, the analysis of line wavelength of silicon, phosphorus and aluminium in described ferro-niobium sample is respectively: silicon 251.612nm, phosphorus 213.617nm, aluminium 396.153nm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103575723A (en) * | 2013-11-14 | 2014-02-12 | 内蒙古第一机械集团有限公司 | Method for testing content of phosphorus in nickel-phosphorus alloy plating layer |
| CN103940807A (en) * | 2014-04-29 | 2014-07-23 | 从化钽铌冶炼厂 | Method for determining content of silicon in potassium fluotantalate |
| CN104122219A (en) * | 2014-07-31 | 2014-10-29 | 攀钢集团江油长城特殊钢有限公司 | Method for determining content of phosphorus in ferroniobium |
| CN104697984A (en) * | 2015-03-30 | 2015-06-10 | 西部新锆核材料科技有限公司 | Method for measuring magnesium content in nuclear-grade sponge zirconium particles |
| CN104949926A (en) * | 2015-05-27 | 2015-09-30 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of aluminum in manganese-iron alloy |
| CN104977290A (en) * | 2015-06-25 | 2015-10-14 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of aluminium in ferrophosphorous |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103575723A (en) * | 2013-11-14 | 2014-02-12 | 内蒙古第一机械集团有限公司 | Method for testing content of phosphorus in nickel-phosphorus alloy plating layer |
| CN103940807A (en) * | 2014-04-29 | 2014-07-23 | 从化钽铌冶炼厂 | Method for determining content of silicon in potassium fluotantalate |
| CN103940807B (en) * | 2014-04-29 | 2015-06-10 | 从化钽铌冶炼厂 | Method for determining content of silicon in potassium fluotantalate |
| CN104122219A (en) * | 2014-07-31 | 2014-10-29 | 攀钢集团江油长城特殊钢有限公司 | Method for determining content of phosphorus in ferroniobium |
| CN104122219B (en) * | 2014-07-31 | 2016-11-23 | 攀钢集团江油长城特殊钢有限公司 | The assay method of phosphorus content in ferro-niobium |
| CN104697984A (en) * | 2015-03-30 | 2015-06-10 | 西部新锆核材料科技有限公司 | Method for measuring magnesium content in nuclear-grade sponge zirconium particles |
| CN104949926A (en) * | 2015-05-27 | 2015-09-30 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of aluminum in manganese-iron alloy |
| CN104977290A (en) * | 2015-06-25 | 2015-10-14 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of aluminium in ferrophosphorous |
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Application publication date: 20130612 |