CN103175824B - Inductively coupled plasma spectrometry transmitter measures the method for Silicon in Ferromanganese phosphorus content - Google Patents
Inductively coupled plasma spectrometry transmitter measures the method for Silicon in Ferromanganese phosphorus content Download PDFInfo
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Abstract
The invention discloses a kind of method that inductively coupled plasma spectrometry transmitter measures Silicon in Ferromanganese phosphorus content, comprise: the atomized soln of preparation ferromanganese sample, preparing standard solution, described standard solution comprises manganese standard solution, phosphorus standard solution and silicon standard solution; Atomized soln is introduced inductively coupled plasma atomic emission spectrometer, measures 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.Utilize technical solution of the present invention can measure the content of Silicon in Ferromanganese and phosphorus quickly and accurately.
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 measures Silicon in Ferromanganese phosphorus content.
Background technology
Ferromanganese is one of important alloy raw material used in converter steelmaking process, along with the raising to smelting new steel grade quality requirements, the requirement that smelting process controls also is improved accordingly, therefore all kinds of raw materials used in smelting process are no longer satisfied with to the inspection of major component, analyze the content of other Related Components in raw material quickly and accurately, thus control to smelt composition more accurately and then seem and become more and more important.
At present, the chemical analysis method of domestic existing Silicon in Ferromanganese and phosphorus, gravimetric determination in silicon many employings GB/T5686.2-2008, in phosphorus many employings GB/T 5686.4-2008, alkalim-etry measures, the time that the chemicals that two kinds of method consumption is a large amount of and complex operation step, especially silicon adopt gravimetric method to test a sample to need 2-3 days.
Inductively coupled plasma spectrometry transmitter (Inductive Coupled Plasma EmissionSpectrometer, ICP), be excitation source with inductively coupled plasma, have that detection limit is low, the range of linearity wide, ionization and chemistry disruption is few, accuracy and precision advanced analysis performance.
Summary of the invention
The object of this invention is to provide a kind of method that inductively coupled plasma spectrometry transmitter measures Silicon in Ferromanganese phosphorus content, the content of Silicon in Ferromanganese and phosphorus can be measured quickly and accurately.
Technical scheme is specific as follows:
Inductively coupled plasma spectrometry transmitter measures a method for Silicon in Ferromanganese phosphorus content, comprising:
The atomized soln of preparation ferromanganese sample, preparing standard solution, described standard solution comprises manganese standard solution, phosphorus standard solution and silicon standard solution; In the atomized soln process of preparation ferromanganese sample, 0.2500g ferromanganese sample is placed in 250mL beaker, adds sal prunella nitration mixture 20mL heating for dissolving, after 10 ~ 30min, filter in 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 puts into platinum crucible, after carbonization, ashing, in 900 DEG C of calcination 10min, takes out cooling, adds 1 ~ 2g mixed flux melting 10min again, cooling; Platinum crucible is put into the beaker adding 50ml water and 10ml hydrochloric acid in advance, boiling to emitting air pocket, being cooled to room temperature, clean platinum crucible, extract and mother liquor are merged, transfers to constant volume in 250ml volumetric flask and shake up, obtain the atomized soln of ferromanganese sample;
Measuring bottle of trying to please pipettes 30ml manganese standard solution respectively, pipette the mixed standard solution of silicon standard solution and phosphorus standard solution preparation at least two variable concentrations, each mixed standard solution is introduced inductively coupled plasma spectrometry transmitter respectively, measures emitted luminescence intensity, drawing curve; Each atomized soln is introduced inductively coupled plasma spectrometry transmitter, measures silicon and the emitted luminescence intensity corresponding to phosphorus, according to the content of working curve determination silicon and phosphorus; The analysis of line wavelength of element to be measured is: phosphorus 213.617nm, silicon 251.612nm.
Further: in sal prunella nitration mixture, hydrochloric acid, nitric acid, water volume ratio are 1:1:3, and hydrochloric acid density is 1.19g/ml.
Further: in the process for preparation of described manganese standard solution, take 5.000g electrolytic manganese in 250mL beaker, add 50mL aqueous solution of nitric acid, heating for dissolving, boils and eliminates oxides of nitrogen, cooling, move in 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 benchmark potassium dihydrogen phosphate, dry 1h through 105 DEG C in advance, be placed in exsiccator, be cooled to room temperature; Take 1.0985g drying schedule potassium dihydrogen phosphate, be placed in 500mL beaker, dissolve by suitable quantity of water, boil, cooling, move in 1000mL volumetric flask, be diluted with water to scale, mixing, concentration be the phosphorus standard solution of 250 μ g/mL, dilute 10 times again, 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, in advance after 1000 DEG C of calcination 1h, is placed in exsiccator and is chilled to room temperature; Take the silicon dioxide of 05349g drying, be placed in the platinum crucible being added with 3g natrium carbonicum calcinatum, cover 1 ~ 2g natrium carbonicum calcinatum more above, platinum crucible is heated prior to low temperature place, being placed in 950 DEG C of high-temperature heatings again melts to transparent, time is 20 ~ 40min, continue heating and melting 3min again, after cooling, the plastic beaker put into filling cold water leaches frit, after frit dissolves, take out after platinum crucible is cleaned, all solution is moved in 1000mL volumetric flask, is diluted with water to scale, shake up, concentration be 250 μ g/mL silicon standard solution.Dilute 10 times again, 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 sal prunella nitration mixture dissolves, and uses hydrochloric acid extraction again after the residue sodium carbonate of filtration and the process of boric acid mixed flux, twice solution is merged, and the method can abundant sample dissolution, thus improves the accuracy of measurement.
2, the content of Silicon in Ferromanganese and phosphorus can be measured quickly and accurately; ICP method sample dissolution can the content of Simultaneously test Silicon in Ferromanganese and phosphorus, and classic method once can only measure a kind of element, and traditional more complex operation of chemical method step.
3, environmental protection; Adopt traditional analysis to need to use more chemicals, the perchloric acid of easily blasting will be used when analyzing silicon, and the present invention only uses a small amount of sal prunella nitration mixture and mixed flux, has the advantage of energy-saving and environmental protection.
Embodiment
The total thinking of the present invention is: dissolved by ferromanganese sample sal prunella nitration mixture, after filtering residue with after the process of sodium carbonate boric acid mixed flux with hydrochloric acid extraction, be diluted to certain volume after being merged by twice solution, obtain the atomized soln of ferromanganese sample; Atomized soln is introduced inductively coupled plasma atomic emission spectrometer, measures element spectral line intensity to be measured, according to line strength that 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: boric acid mass ratio is 2:1.
Preferred ICP spectrometer is that PE company of the U.S. produces, and direct-reading plasma-speetrometer composed entirely by OPTIMA5300DV Bidirectional observation type, and Winlab32 software, Instrument working parameter is as shown in table 1.
Table 1
| Parameter | Higher frequency | Power | Cooling gas flow | Assisted gas flow | Carrier gas flux | 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 | 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, ferromanganese sample has got 7 kinds, is respectively: ferromanganese YSBC18602-08, high carbon ferromanganese YSB C 11602-99, mid-carbon fe-mn YSBC41601-99, mid-carbon fe-mn GBW 01421, mid-carbon fe-mn YSBC 25614-96, mid-carbon fe-mn GSB 03-1361-2001, mid-carbon fe-mn GSB03-1358-2001.
0.2500g ferromanganese sample is placed in 250mL beaker, adds sal prunella nitration mixture 20mL heating for dissolving, after 10 ~ 30min, sample major part is dissolved, and filters in 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 puts into platinum crucible, after carbonization, ashing, in 900 DEG C of calcination 10min, takes out cooling, adds 1 ~ 2g mixed flux melting 10min again, cooling.Platinum crucible is put into the beaker adding 50ml water and 10ml hydrochloric acid in advance, boiling to emitting air pocket, being cooled to room temperature, clean platinum crucible, extract and mother liquor are merged, transfers to constant volume in 250ml volumetric flask and shake up, obtain the atomized soln of ferromanganese sample.
Like this, seven kinds of atomized solns of ferromanganese YSBC18602-08, high carbon ferromanganese YSB C 11602-99, mid-carbon fe-mn YSBC41601-99, mid-carbon fe-mn GBW 01421, mid-carbon fe-mn YSBC 25614-96, mid-carbon fe-mn GSB 03-1361-2001, mid-carbon fe-mn GSB 03-1358-2001 can just be obtained.
Step 2: the preparation of standard solution;
The preparation of manganese standard solution: take 5.000g electrolytic manganese in 250mL beaker, add 50mL aqueous solution of nitric acid, heating for dissolving, boil and eliminate oxides of nitrogen, cooling, move in 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: benchmark potassium dihydrogen phosphate, dries 1h through 105 DEG C in advance, is placed in exsiccator, is cooled to room temperature.Take 4.3936g drying schedule potassium dihydrogen phosphate, be placed in 500mL beaker, dissolve by suitable quantity of water, boil, cooling, move in 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, more than 99.99%, in advance after 1000 DEG C of calcination 1h, is placed in exsiccator and is chilled to room temperature.Take the silicon dioxide of 0.4279g drying, be placed in the platinum crucible being added with 3g natrium carbonicum calcinatum, cover 1 ~ 2g natrium carbonicum calcinatum more above, platinum crucible is heated prior to low temperature place, being placed in 950 DEG C of high-temperature heatings again melts to transparent, time is 20 ~ 40min, continue heating and melting 3min again, after cooling, the plastic beaker put into filling cold water leaches frit, after frit dissolves, take out platinum crucible carefully to clean, all solution is moved in 200mL volumetric flask, be diluted with water to scale, shake up, dilute 10 times again, 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, measures element spectral line intensity to be measured, according to line strength that concentration known standard solution records, draws the content of silicon and phosphorus in ferromanganese sample.
Get 8 250mL volumetric flasks and pipette 30ml manganese standard solution respectively, the mixed standard solution that silicon and phosphorus standard solution prepare multiple variable concentrations is pipetted according to table 2, each mixed standard solution is introduced ICP emission spectrometer respectively, measures emitted luminescence intensity, 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 ICP emission spectrometer, and measure silicon, emitted luminescence intensity corresponding to phosphorus, according to the content of working curve determination silicon, phosphorus, result is as shown in table 3.
Table 3
Can be found out by above-mentioned steps, by the inventive method, plasma emission spectrometry can be utilized to measure the content of Silicon in Ferromanganese and phosphorus fast and accurately.
Claims (6)
1. inductively coupled plasma spectrometry transmitter measures a method for Silicon in Ferromanganese phosphorus content, comprising:
The atomized soln of preparation ferromanganese sample, preparing standard solution, described standard solution comprises manganese standard solution, phosphorus standard solution and silicon standard solution; In the atomized soln process of preparation ferromanganese sample, 0.2500g ferromanganese sample is placed in 250mL beaker, adds sal prunella nitration mixture 20mL heating for dissolving, after 10 ~ 30min, filter in 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 puts into platinum crucible, after carbonization, ashing, in 900 DEG C of calcination 10min, takes out cooling, adds 1 ~ 2g mixed flux melting 10min again, cooling; Platinum crucible is put into the beaker adding 50ml water and 10ml hydrochloric acid in advance, boiling to emitting air pocket, being cooled to room temperature, clean platinum crucible, extract and mother liquor are merged, transfers to constant volume in 250ml volumetric flask and shake up, obtain the atomized soln of ferromanganese sample;
Measuring bottle of trying to please pipettes 30ml manganese standard solution respectively, pipette the mixed standard solution of silicon standard solution and phosphorus standard solution preparation at least two variable concentrations, each mixed standard solution is introduced inductively coupled plasma spectrometry transmitter respectively, measures emitted luminescence intensity, drawing curve; Each atomized soln is introduced inductively coupled plasma spectrometry transmitter, measures silicon and the emitted luminescence intensity corresponding to phosphorus, according to the content of working curve determination silicon and phosphorus; The analysis of line wavelength of element to be measured is: phosphorus 213.617nm, silicon 251.612nm.
2. inductively coupled plasma spectrometry transmitter as claimed in claim 1 measures the method for Silicon in Ferromanganese phosphorus content, it is characterized in that: in sal prunella nitration mixture, hydrochloric acid, nitric acid, water volume ratio are 1:1:3, and hydrochloric acid density is 1.19g/ml.
3. inductively coupled plasma spectrometry transmitter as claimed in claim 1 measures the method for Silicon in Ferromanganese phosphorus content, it is characterized in that: in the process for preparation of described manganese standard solution, take 5.000g electrolytic manganese in 250mL beaker, add 50mL aqueous solution of nitric acid, heating for dissolving, boil and eliminate oxides of nitrogen, cooling, moves in 1000mL volumetric flask, is diluted with water to scale, shake up, concentration be the manganese standard solution of 5mg/mL.
4. inductively coupled plasma spectrometry transmitter as claimed in claim 3 measures the method for Silicon in Ferromanganese phosphorus content, it is characterized in that: in aqueous solution of nitric acid, nitric acid and water volume ratio are 2:3.
5. inductively coupled plasma spectrometry transmitter as claimed in claim 1 measures the method for Silicon in Ferromanganese phosphorus content, it is characterized in that: in the process for preparation of described phosphorus standard solution, choose benchmark potassium dihydrogen phosphate, dry 1h through 105 DEG C in advance, be placed in exsiccator, be cooled to room temperature; Take 4.3936g drying schedule potassium dihydrogen phosphate, be placed in 500mL beaker, dissolve by suitable quantity of water, boil, cooling, move in 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.
6. inductively coupled plasma spectrometry transmitter as claimed in claim 1 measures 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, in advance after 1000 DEG C of calcination 1h, be placed in exsiccator and be chilled to room temperature, take the silicon dioxide of 0.4279g drying, be placed in the platinum crucible being added with 3g natrium carbonicum calcinatum, cover 1 ~ 2g natrium carbonicum calcinatum more above, platinum crucible is heated prior to low temperature place, being placed in 950 DEG C of high-temperature heatings again melts to transparent, time is 20 ~ 40min, continue heating and melting 3min again, after cooling, the plastic beaker put into filling cold water leaches frit, after frit dissolves, take out platinum crucible carefully to clean, all solution is moved in 200mL volumetric flask, be diluted with water to scale, shake up, dilute 10 times again, store in plastic bottle, concentration be 100 μ g/mL silicon standard solution.
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