CN103175824A - Method for measuring content of silicon and phosphorus in ferromanganese iron by inductively coupled plasma spectrum emission instrument - Google Patents
Method for measuring content of silicon and phosphorus in ferromanganese iron by inductively coupled plasma spectrum emission instrument Download PDFInfo
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Abstract
The invention discloses a method for measuring the content of silicon and phosphorus in ferromanganese iron by an inductively coupled plasma spectrum emission instrument. The method comprises the following steps of: preparing an atomized solution of a ferromanganese iron sample and standard solutions comprising a manganese standard solution, a phosphorus standard solution and a silicon standard solution; and introducing the atomized solution into an inductively coupled plasma atomic emission spectrometer, and measuring the spectral line intensity of an element to be measured, thus obtaining the content of silicon and phosphorus in the ferromanganese iron sample according to the spectral line intensity measured via the standard solutions with given concentrations. Due to the technical scheme disclosed by the invention, the content of silicon and phosphorus in ferromanganese iron can be rapidly and accurately measured.
Description
Technical field
The present invention relates to technical field of ferrous metallurgical analysis, particularly relate to a kind of method that inductively coupled plasma spectrometry transmitter is measured the Silicon in Ferromanganese phosphorus content.
Background technology
Ferromanganese is one of important alloy raw material that uses in converter steelmaking process, along with the raising to smelting new steel grade quality requirements, the requirement that smelting process is controlled also improves accordingly, therefore all kinds of raw materials that use in smelting process no longer are satisfied with the check of major component, analyze quickly and accurately the content of other Related Components in raw material, seem and become more and more important thereby control to smelt more accurately composition.
At present, the chemical analysis method of domestic existing Silicon in Ferromanganese and phosphorus, silicon adopts gravimetric determination in GB/T5686.2-2008 more, phosphorus adopts alkalim-etry mensuration in GB/T5686.4-2008 more, two kinds of chemicals and complex operation step that method consumption is a large amount of, especially silicon adopt sample of gravimetric method test to need the time of 2-3 days.
Inductively coupled plasma spectrometry transmitter (Inductive Coupled Plasma EmissionSpectrometer, ICP), take inductively coupled plasma as excitation source, have that detection limit is low, the range of linearity is wide, ionization and chemistry disturbs less, accuracy and precision advanced analysis performance.
Summary of the invention
The purpose of this invention is to provide a kind of inductively coupled plasma spectrometry transmitter and measure the method for Silicon in Ferromanganese phosphorus content, can measure quickly and accurately the content of Silicon in Ferromanganese and phosphorus.
Technical scheme is specific as follows:
A kind of inductively coupled plasma spectrometry transmitter is measured the method for Silicon in Ferromanganese phosphorus content, comprising:
The atomized soln of preparation ferromanganese sample, preparing standard solution, described standard solution comprise manganese standard solution, phosphorus standard solution and silicon standard solution;
Atomized soln is introduced inductively coupled plasma atomic emission spectrometer, measure element spectral line intensity to be measured, according to line strength that the described standard solution of concentration known records, draw the content of silicon and phosphorus in described ferromanganese sample.
Further: in the atomized soln process of preparation ferromanganese sample, 0.2500g ferromanganese sample is placed in the 250mL beaker, add sal prunella nitration mixture 20mL heating for dissolving, after 10 ~ 30min, filter in the 200mL beaker with Medium speed filter paper, with salt pickling beaker 3-4 time, washing precipitation 5-6 time, filter, filtrate is preserved as main liquid; Precipitation is put into platinum crucible, after carbonization, ashing, in 900 ℃ of calcination 10min, takes out coolingly, adds 1～2g mixed flux melting 10min again, and is cooling; Platinum crucible is put into the beaker that adds in advance 50ml water, boiled to emitting air pocket, be cooled to room temperature, clean platinum crucible, extract and mother liquor are merged, transfer to that in the 250ml volumetric flask, constant volume shakes up, the atomized soln of acquisition ferromanganese sample.
Further: in the sal prunella nitration mixture, hydrochloric acid, nitric acid, water volume ratio are 1:1:3, and hydrochloric acid density is 1.19g/ml.
Further: the measuring bottle of trying to please pipettes respectively 30ml manganese standard solution, pipette the mixed standard solution of at least two variable concentrations of silicon standard solution and phosphorus standard solution preparation, each mixed standard solution is introduced respectively the inductively coupled plasma spectrometry transmitter, measure emitted luminescence intensity, the drawing curve; Each atomized soln is introduced the inductively coupled plasma spectrometry transmitter, measure silicon and the corresponding emitted luminescence intensity of phosphorus, determine the content of silicon and phosphorus according to working curve; The analysis of line wavelength of element to be measured is: phosphorus 213.617nm, silicon 251.612nm.
Further: in the process for preparation of described manganese standard solution, take the 5.000g electrolytic manganese in the 250mL beaker, add the 50mL aqueous solution of nitric acid, heating for dissolving is boiled and eliminated oxides of nitrogen, and is cooling, move in the 1000mL volumetric flask, be diluted with water to scale, shake up, concentration be the manganese standard solution of 5mg/mL.
Further: in aqueous solution of nitric acid, nitric acid and water volume ratio are 2:3.
Further: in the process for preparation of described phosphorus standard solution, choose the benchmark potassium dihydrogen phosphate, through 105 ℃ of baking 1h, be placed in exsiccator in advance, be cooled to room temperature; Take 1.0985g drying schedule potassium dihydrogen phosphate, be placed in the 500mL beaker, with the suitable quantity of water dissolving, boil, cooling, move in the 1000mL volumetric flask, be diluted with water to scale, mixing, concentration be the phosphorus standard solution of 250 μ g/mL, dilute again 10 times, concentration be the phosphorus standard solution of 25 μ g/mL.
Further: in the process for preparation of described silicon standard solution, choosing purity is 99.99% silicon dioxide, after 1000 ℃ of calcination 1h, is placed in exsiccator and is chilled to room temperature in advance; Take the silicon dioxide of 0.5349g drying, be placed in the platinum crucible that is added with the 3g natrium carbonicum calcinatum, the above covers 1～2g natrium carbonicum calcinatum again, with platinum crucible prior to the heating of low temperature place, being placed in 950 ℃ of high-temperature heatings melts to transparent again, time is 20 ~ 40min, continue again heating and melting 3min, cooling after, put into the plastic beaker that fills cold water and leach frit, after the frit dissolving, take out after platinum crucible is cleaned, all solution are moved in the 1000mL volumetric flask, be diluted with water to scale, shake up, concentration be 250 μ g/mL silicon standard solution.Dilute again 10 times, store in plastic bottle, concentration be 25 μ g/mL silicon standard solution.
Beneficial effect of the present invention:
1, molten sample is abundant; Sample is used hydrochloric acid extraction with sal prunella nitration mixture dissolving, the residue of filtration after processing with sodium carbonate and boric acid mixed flux again, and twice solution is merged, and the method is dissolution sample fully, thereby improves the accuracy of measuring.
2, can measure quickly and accurately the content of Silicon in Ferromanganese and phosphorus; Dissolution sample of ICP method can be measured the content of Silicon in Ferromanganese and phosphorus simultaneously, and classic method can only once be measured a kind of element, and traditional more complex operation of chemical method step.
3, environmental protection; Adopt traditional analysis need to use more chemicals, will use the perchloric acid of easily blasting when analyzing silicon, and the present invention only uses a small amount of sal prunella nitration mixture and mixed flux, has advantages of energy-saving and environmental protection.
Embodiment
The total thinking of the present invention is: the ferromanganese sample with the dissolving of sal prunella nitration mixture, is filtered and uses hydrochloric acid extraction after rear residue is processed with sodium carbonate boric acid mixed flux, be diluted to certain volume after twice solution is merged, obtain the atomized soln of ferromanganese sample; Atomized soln is introduced inductively coupled plasma atomic emission spectrometer, measure element spectral line intensity to be measured, according to line strength that the concentration known standard substance records, obtain the concentration of test substance corresponding element.
In the present invention, agents useful for same is preferred:
Hydrochloric acid: density is 1.19g/ml;
Aqueous hydrochloric acid solution: hydrochloric acid: water volume ratio is 5:95;
Aqueous solution of nitric acid: nitric acid: water volume ratio is 2:3;
Sal prunella nitration mixture: hydrochloric acid: nitric acid: water volume ratio is 1:1:3;
Mixed flux: sodium carbonate: the boric acid mass ratio is 2:1.
Preferred ICP spectrometer is that U.S. PE company produces, and OPTIMA5300DV Bidirectional observation type is composed the direct-reading plasma-speetrometer entirely, Winlab32 software, and Instrument working parameter is as shown in table 1.
Table 1
| Parameter | The high frequency frequency | Power | Cooling gas flow | The assisted gas flow | Carrier gas flux | The solution elevating amount |
| Numerical value | 40.68MHZ | 1300W | 15L/min | 0.2L/min | 0.8L/min | 1.5mL/min |
| Parameter | Flush time | Preburn time | Integral time | The reading time-delay | Observed altitude | Observed pattern |
| Numerical value | 8s | 45s | 2～10s is automatic | 30s | 15mm | Axially |
The analysis of line wavelength of element to be measured is: phosphorus 213.617nm, silicon 251.612nm.
Step 1: the atomized soln of preparation ferromanganese sample;
In the present invention, the ferromanganese sample has been got 7 kinds, is respectively: ferromanganese YSBC18602-08, high carbon ferromanganese YSB C11602-99, mid-carbon fe-mn YSBC41601-99, mid-carbon fe-mn GBW01421, mid-carbon fe-mn YSBC25614-96, mid-carbon fe-mn GSB03-1361-2001, mid-carbon fe-mn GSB03-1358-2001.
0.2500g ferromanganese sample is placed in the 250mL beaker, adds sal prunella nitration mixture 20mL heating for dissolving, after 10 ~ 30min, the most of dissolving of sample is filtered in the 200mL beaker with Medium speed filter paper, with salt pickling beaker 3-4 time, precipitate 5-6 time, filter, filtrate is preserved as main liquid.Precipitation is put into platinum crucible, after carbonization, ashing, in 900 ℃ of calcination 10min, takes out coolingly, adds 1～2g mixed flux melting 10min again, and is cooling.Platinum crucible is put into the beaker that adds in advance 50ml water and 10ml hydrochloric acid, boiled to emitting air pocket, be cooled to room temperature, clean platinum crucible, extract and mother liquor are merged, transfer to that in the 250ml volumetric flask, constant volume shakes up, the atomized soln of acquisition ferromanganese sample.
Like this, just can obtain seven kinds of atomized solns of ferromanganese YSBC18602-08, high carbon ferromanganese YSB C11602-99, mid-carbon fe-mn YSBC41601-99, mid-carbon fe-mn GBW01421, mid-carbon fe-mn YSBC25614-96, mid-carbon fe-mn GSB03-1361-2001, mid-carbon fe-mn GSB03-1358-2001.
Step 2: the preparation of standard solution;
The preparation of manganese standard solution: take the 5.000g electrolytic manganese in the 250mL beaker, add the 50mL aqueous solution of nitric acid, heating for dissolving, boil and eliminate oxides of nitrogen, cooling, move in the 1000mL volumetric flask, be diluted with water to scale, shake up, concentration be the manganese standard solution of 5mg/mL.
The preparation of phosphorus standard solution: the benchmark potassium dihydrogen phosphate, through 105 ℃ of baking 1h, be placed in exsiccator in advance, be cooled to room temperature.Take 4.3936g drying schedule potassium dihydrogen phosphate, be placed in the 500mL beaker, with suitable quantity of water dissolving, boil, cooling, move in the 1000mL volumetric flask, be diluted with water to scale, mixing, then dilute 10 times, concentration be the phosphorus standard solution of 100 μ g/mL.
The preparation of silicon standard solution: silicon dioxide, purity after 1000 ℃ of calcination 1h, are placed in exsiccator and are chilled to room temperature in advance more than 99.99%.take the silicon dioxide of 0.4279g drying, be placed in the platinum crucible that is added with the 3g natrium carbonicum calcinatum, the above covers 1～2g natrium carbonicum calcinatum again, with platinum crucible prior to the heating of low temperature place, being placed in 950 ℃ of high-temperature heatings melts to transparent again, time is 20 ~ 40min, continue again heating and melting 3min, after cooling, put into the plastic beaker that fills cold water and leach frit, after the frit dissolving, taking out platinum crucible carefully cleans, all solution are moved in the 200mL volumetric flask, be diluted with water to scale, shake up, dilute again 10 times, store in plastic bottle, concentration be 100 μ g/mL silicon standard solution.
Step 3: atomized soln is introduced inductively coupled plasma atomic emission spectrometer, measure element spectral line intensity to be measured, according to line strength that the concentration known standard solution records, draw the content of silicon and phosphorus in the ferromanganese sample.
Get 8 250mL volumetric flasks and pipette respectively 30ml manganese standard solution, pipette the mixed standard solution of silicon and a plurality of variable concentrations of phosphorus standard solution preparation according to table 2, each mixed standard solution is introduced respectively the ICP emission spectrometer, measure emitted luminescence intensity, the drawing curve.
Table 2
| Label | Silicon mark liquid | Silicone content % | Phosphorus mark liquid | Phosphorus content % |
| 0 | 0ml | 0.00 | 0ml | 0.00 |
| 1 | 5ml（25μg/mL） | 0.050 | 5ml（25μg/mL） | 0.050 |
| 2 | 10ml（25μg/mL） | 0.100 | 10ml（25μg/mL） | 0.100 |
| 3 | 20ml（25μg/mL） | 0.200 | 20ml（25μg/mL） | 0.200 |
| 4 | 5ml（250μg/mL） | 0.500 | 30ml（25μg/mL） | 0.300 |
| 5 | 10ml（250μg/mL） | 1.00 | 4ml（250μg/mL） | 0.400 |
| 6 | 20ml（250μg/mL） | 2.00 | 5ml（250μg/mL） | 0.500 |
| 7 | 50ml（250μg/mL） | 5.00 | 10ml（250μg/mL） | 1.00 |
The lysate of each sample is introduced the ICP emission spectrometer, measure silicon, the corresponding emitted luminescence intensity of phosphorus, determine the content of silicon, phosphorus according to working curve, result is as shown in table 3.
Table 3
Can find out by above-mentioned steps, by the inventive method, can utilize plasma emission spectrometry to measure fast and accurately the content of Silicon in Ferromanganese and phosphorus.
Claims (8)
1. an inductively coupled plasma spectrometry transmitter is measured the method for Silicon in Ferromanganese phosphorus content, comprising:
The atomized soln of preparation ferromanganese sample, preparing standard solution, described standard solution comprise manganese standard solution, phosphorus standard solution and silicon standard solution;
Atomized soln is introduced inductively coupled plasma atomic emission spectrometer, measure element spectral line intensity to be measured, according to line strength that the described standard solution of concentration known records, draw the content of silicon and phosphorus in described ferromanganese sample.
2. inductively coupled plasma spectrometry transmitter as claimed in claim 1 is measured the method for Silicon in Ferromanganese phosphorus content, it is characterized in that: in the atomized soln process of preparation ferromanganese sample, 0.2500g ferromanganese sample is placed in the 250mL beaker, add sal prunella nitration mixture 20mL heating for dissolving, after 10 ~ 30min, filter in the 200mL beaker with Medium speed filter paper, with salt pickling beaker 3-4 time, precipitate 5-6 time, filter, filtrate is preserved as main liquid; Precipitation is put into platinum crucible, after carbonization, ashing, in 900 ℃ of calcination 10min, takes out coolingly, adds 1～2g mixed flux melting 10min again, and is cooling; Platinum crucible is put into the beaker that adds in advance 50ml water and 10ml hydrochloric acid, boiled to emitting air pocket, be cooled to room temperature, clean platinum crucible, extract and mother liquor are merged, transfer to that in the 250ml volumetric flask, constant volume shakes up, the atomized soln of acquisition ferromanganese sample.
3. inductively coupled plasma spectrometry transmitter as claimed in claim 2 is measured the method for Silicon in Ferromanganese phosphorus content, and it is characterized in that: in the sal prunella nitration mixture, hydrochloric acid, nitric acid, water volume ratio are 1:1:3, and hydrochloric acid density is 1.19g/ml.
4. inductively coupled plasma spectrometry transmitter as claimed in claim 1 is measured the method for Silicon in Ferromanganese phosphorus content, it is characterized in that: the measuring bottle of trying to please pipettes respectively 30ml manganese standard solution, pipette the mixed standard solution of at least two variable concentrations of silicon standard solution and phosphorus standard solution preparation, each mixed standard solution is introduced respectively the inductively coupled plasma spectrometry transmitter, measure emitted luminescence intensity, the drawing curve; Each atomized soln is introduced the inductively coupled plasma spectrometry transmitter, measure silicon and the corresponding emitted luminescence intensity of phosphorus, determine the content of silicon and phosphorus according to working curve; The analysis of line wavelength of element to be measured is: phosphorus 213.617nm, silicon 251.612nm.
5. inductively coupled plasma spectrometry transmitter as claimed in claim 1 is measured the method for Silicon in Ferromanganese phosphorus content, it is characterized in that: in the process for preparation of described manganese standard solution, take the 5.000g electrolytic manganese in the 250mL beaker, add the 50mL aqueous solution of nitric acid, heating for dissolving, boil and eliminate oxides of nitrogen, cooling, move in the 1000mL volumetric flask, be diluted with water to scale, shake up, concentration be the manganese standard solution of 5mg/mL.
6. inductively coupled plasma spectrometry transmitter as claimed in claim 5 is measured the method for Silicon in Ferromanganese phosphorus content, and it is characterized in that: in aqueous solution of nitric acid, nitric acid and water volume ratio are 2:3.
7. inductively coupled plasma spectrometry transmitter as claimed in claim 1 is measured the method for Silicon in Ferromanganese phosphorus content, it is characterized in that: in the process for preparation of described phosphorus standard solution, choose the benchmark potassium dihydrogen phosphate, in advance through 105 ℃ of baking 1h, be placed in exsiccator, be cooled to room temperature; Take 4.3936g drying schedule potassium dihydrogen phosphate, be placed in the 500mL beaker, with suitable quantity of water dissolving, boil, cooling, move in the 1000mL volumetric flask, be diluted with water to scale, mixing, then dilute 10 times, concentration be the phosphorus standard solution of 100 μ g/mL.
8. inductively coupled plasma spectrometry transmitter as claimed in claim 1 is measured the method for Silicon in Ferromanganese phosphorus content, it is characterized in that: in the process for preparation of described silicon standard solution, choosing purity is 99.99% silicon dioxide, after 1000 ℃ of calcination 1h, is placed in exsiccator and is chilled to room temperature in advance, take the silicon dioxide of 0.4279g drying, be placed in the platinum crucible that is added with the 3g natrium carbonicum calcinatum, the above covers 1～2g natrium carbonicum calcinatum again, with platinum crucible prior to the heating of low temperature place, being placed in 950 ℃ of high-temperature heatings melts to transparent again, time is 20 ~ 40min, continue again heating and melting 3min, after cooling, put into the plastic beaker that fills cold water and leach frit, after the frit dissolving, taking out platinum crucible carefully cleans, all solution are moved in the 200mL volumetric flask, be diluted with water to scale, shake up, dilute again 10 times, store in plastic bottle, concentration be 100 μ g/mL silicon standard solution.
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| CN106979944A (en) * | 2017-03-27 | 2017-07-25 | 山东钢铁集团日照有限公司 | The detection method of silicon and phosphorus content in a kind of measure manganeisen |
| CN107607522A (en) * | 2017-08-29 | 2018-01-19 | 东旭科技集团有限公司 | A kind of method of phosphorus content in measure glass |
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| CN108709882A (en) * | 2018-08-14 | 2018-10-26 | 武汉钢铁有限公司 | Measure the method for element silicon and phosphorus element content in low-silicon nodulizer |
| CN110967335A (en) * | 2019-07-11 | 2020-04-07 | 包钢勘察测绘研究院 | Method for measuring content of free silicon dioxide in iron-containing dust mud |
| CN111208116A (en) * | 2020-02-27 | 2020-05-29 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring silicon content in non-oriented silicon steel environment-friendly coating liquid |
| CN113390857A (en) * | 2021-06-07 | 2021-09-14 | 武钢集团昆明钢铁股份有限公司 | Method for measuring contents of manganese oxide, calcium oxide and phosphorus in manganese pellets |
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