CN105223146A - A kind of method adopting silicone content in silicon molybdenum blue colorimetric method for determining ferro-silico aluminium - Google Patents
A kind of method adopting silicone content in silicon molybdenum blue colorimetric method for determining ferro-silico aluminium Download PDFInfo
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- CN105223146A CN105223146A CN201510629435.7A CN201510629435A CN105223146A CN 105223146 A CN105223146 A CN 105223146A CN 201510629435 A CN201510629435 A CN 201510629435A CN 105223146 A CN105223146 A CN 105223146A
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Abstract
The invention discloses a kind of method adopting silicone content in silicon molybdenum blue colorimetric method for determining ferro-silico aluminium, its object is to provide one quicker, accurately, the method of silicone content in efficient mensuration ferro-silico aluminium, the inventive method adopts sodium hydroxide solution to dissolve most of sample, then watery hydrochloric acid-nitric acid dissolve residue sample is added, heat and dissolve completely until sample, be cooled to room temperature, be transferred to volumetric flask, divide and get solution in another volumetric flask, add ammonium molybdate and generate molybdenum yellow, add oxalic acid and shelter interference element, add iron ammonium sulfate and generate silicon molybdenum blue, use spectrophotometric determination solution absorbance.In company with the standard specimen conversion sample content value of the close content of sample strip same breed.
Description
Technical field
The present invention relates to ferroalloy analysis technical field, be specifically related to a kind of method adopting silicone content in silicon molybdenum blue colorimetric method for determining ferro-silico aluminium.
Background technology
Alsimin is for a kind of double deoxidizer in STEELMAKING PRODUCTION, Alsimin density ratio fine aluminium density is large, more easily enter molten steel, for improving inclusion morphology, reduce elemental gas content in molten steel, be improve steel quality, reduce costs, economize on effective new technology of aluminium, in steelmaking process, using Alsimin ratio to be used alone fine aluminium, to make deoxidizer efficiency higher.The product of low melting point can be formed with Alsimin deoxidation, easily float and then improve steel quality, being specially adapted to continuous casting steel deoxidation requirement.Facts have proved, it not only meets deoxidation in steel making requirement, also has desulfurization performance and has than great, the advantages such as penetration power is strong.
In ferro-silico aluminium, the mensuration of silicon has gravimetric method usually, silicon fluoro acid potassium volumetric method etc.Gravimetric method operating process is long, is not suitable for the Fast Measurement in production, and silicon fluoro acid potassium volumetric method needs sample to dissolve completely under the condition do not heated, and the Specimen Determination opened for difficulty is inaccurate.
Summary of the invention
When the present invention measures silicon in ferro-silico aluminium to solve existing method, long flow path, operates slow problem, and speed operations speed simultaneously, reduces costs, the invention provides a kind of more fast, measure the method for silicone content in ferro-silico aluminium accurately and efficiently.
For reaching above-mentioned purpose, a kind of method adopting silicone content in silicon molybdenum blue colorimetric method for determining ferro-silico aluminium of the present invention, comprises the following steps:
Take the sample that quality is m, add sodium hydroxide solution heating for dissolving major part sample, then add watery hydrochloric acid, nitric acid dissolve residue sample, heat and dissolve completely until sample, be cooled to room temperature, be transferred to volumetric flask, divide and get part in another volumetric flask, add ammonium molybdate solution and generate molybdenum yellow, add oxalic acid solution and shelter interference element, add l ferrous ammonium sulfate solution and generate silicon molybdenum blue, be diluted to scale with water, shake up;
Separately get portion and do reference solution: add oxalic acid solution, ammonium molybdate solution, l ferrous ammonium sulfate solution, be diluted to scale with water, shake up;
Select applicable cuvette and light damping plate according to the height of silicone content in sample, select wavelength to be 650nm, use 721 type spectrophotometers to carry out the mensuration of solution absorbance, in company with the standard specimen conversion sample content value of the close content of sample strip same breed;
Analysis result calculation:
In formula:
W (Si): the percentage of the siliceous quality of sample;
W marks (%): the siliceous mass percent of standard specimen;
A sample: the absorbance of Specimen Determination;
A marks: the absorbance that standard specimen measures.
Wherein said nitric acid density is 1.42g/mL.
Wherein said hydrochloric acid density is 1.19g/mL, and hydrochloric acid and water volume ratio are 1:1.
Wherein said concentration of sodium hydroxide solution is 200g/L.
Wherein said ammonium molybdate solution concentration is 50g/L.
Wherein said oxalic acid solution concentration is 50g/L.
Wherein said l ferrous ammonium sulfate solution concentration is 60g/L, and containing the 10mL concentrated sulphuric acid in often liter of solution, described concentrated sulphuric acid density is 1.84g/mL.
The invention difference from existing technology is that the present invention achieves following technique effect:
1) fast, efficient: to substantially reduce operating process compared to gravimetric determination, saved medicine, decrease manpower expenditure, improve production efficiency;
2) accurate, stable: molten sample have employed first Sodium Hydroxide Alkaline and dissolved early stage, after add acid-soluble two course of dissolutions of acid solution, ensure that sample is opened completely, carry out colorimetric after sheltering interfering material by screening agent, result is stablized, and data are accurately and reliably.
Embodiment
Below in conjunction with embodiment, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.
1. method summary:
This method adopts sodium hydroxide solution to dissolve most of sample, then watery hydrochloric acid-nitric acid dissolve residue sample is added, heat and dissolve completely until sample, be cooled to room temperature, be transferred to 250mL volumetric flask, divide and get 10mL in 100mL volumetric flask, add ammonium molybdate and generate molybdenum yellow, add oxalic acid and shelter interference element, add iron ammonium sulfate and generate silicon molybdenum blue, use spectrophotometric determination solution absorbance.In company with the standard specimen conversion sample content value of the close content of sample strip same breed.
2. reagent:
2.1 nitric acid (density is 1.42g/mL)
2.2 hydrochloric acid (density is the hydrochloric acid of 1.19g/mL and water volume ratio is 1:1)
2.3 sodium hydroxide solutions (concentration is 200g/L)
2.4 ammonium molybdate solutions (concentration is 50g/L)
2.5 oxalic acid solutions (concentration is 50g/L)
2.6 l ferrous ammonium sulfate solution (concentration is 60g/L, containing the 10mL concentrated sulphuric acid (density is 1.84g/mL) in often liter of solution)
3. sampling and sample preparation
4. sample size
Take sample 0.1000g.
5. analytical procedure
Take sample 0.1000g, add 20mL sodium hydroxide solution (concentration is 200g/L) heating for dissolving major part sample, then 40mL watery hydrochloric acid (density is the hydrochloric acid of 1.19g/mL and water volume ratio is 1:1) is added, 2mL nitric acid (density is 1.42g/mL) dissolves residue sample, heat and dissolve completely until sample, be cooled to room temperature, be transferred to 250mL volumetric flask, divide and get 10mL in 100mL volumetric flask, add 5mL ammonium molybdate solution (concentration is 50g/L) and generate molybdenum yellow, add 10mL oxalic acid solution (concentration is 50g/L) and shelter interference element, (concentration is 60g/L to add 10mL l ferrous ammonium sulfate solution, containing the 10mL concentrated sulphuric acid (density is 1.84g/mL) in often liter of solution) generate silicon molybdenum blue, scale is diluted to water, shake up.
Separately get portion and do reference solution: add oxalic acid solution (concentration is 50g/L) 10mL, ammonium molybdate solution (concentration is 50g/L) 5mL, l ferrous ammonium sulfate solution (concentration is 60g/L, containing the 10mL concentrated sulphuric acid (density is 1.84g/mL) in often liter of solution) 10mL.Be diluted to scale with water, shake up.
Select applicable cuvette and light damping plate according to the height of silicone content in sample, select wavelength to be 650nm, use 721 type spectrophotometers to carry out the mensuration of solution absorbance.In company with the standard specimen conversion sample content value of the close content of sample strip same breed.
6. Analysis result calculation:
In formula: W (Si): the percentage of the siliceous quality of sample;
W marks (%): the siliceous mass percent of standard specimen;
A sample: the absorbance of Specimen Determination;
A marks: the absorbance that standard specimen measures.
7. sample analysis contrast
Table one standard specimen accuracy test
Table two compares with gravimetric method
As can be seen from the above table, adopt the data that in silicon molybdenum blue colorimetric method for determining ferro-silico aluminium, silicone content obtains accurate, fast and convenient, stability is better, and operating process is shorter, and method is easily grasped, fast, efficiently.
8. conclusion
By this method, the content of silicon in ferro-silico aluminium can be determined accurately.That has saved medicine compared to gravimetric method adds kind and addition, substantially reduces the running time, has saved cost of drugs, reduced energy consumption.This method molten sample step is simple and quick, and determination data accurately and reliably, is applicable to being applied to the Fast Measurement producing silicon in upper ferro-silico aluminium.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (7)
1. adopt a method for silicone content in silicon molybdenum blue colorimetric method for determining ferro-silico aluminium, it is characterized in that comprising the following steps:
Take the sample that quality is m, add sodium hydroxide solution heating for dissolving major part sample, then add watery hydrochloric acid, nitric acid dissolve residue sample, heat and dissolve completely until sample, be cooled to room temperature, be transferred to volumetric flask, divide and get part in another volumetric flask, add ammonium molybdate solution and generate molybdenum yellow, add oxalic acid solution and shelter interference element, add l ferrous ammonium sulfate solution and generate silicon molybdenum blue, be diluted to scale with water, shake up;
Separately get portion and do reference solution: add oxalic acid solution, ammonium molybdate solution, l ferrous ammonium sulfate solution, be diluted to scale with water, shake up;
Select applicable cuvette and light damping plate according to the height of silicone content in sample, select wavelength to be 650nm, use 721 type spectrophotometers to carry out the mensuration of solution absorbance, in company with the standard specimen conversion sample content value of the close content of sample strip same breed;
Analysis result calculation:
In formula:
W (Si): the percentage of the siliceous quality of sample;
W marks (%): the siliceous mass percent of standard specimen;
A sample: the absorbance of Specimen Determination;
A marks: the absorbance that standard specimen measures.
2. the method for silicone content in employing silicon molybdenum blue colorimetric method for determining ferro-silico aluminium according to claim 1, is characterized in that: described nitric acid density is 1.42g/mL.
3. the method for silicone content in employing silicon molybdenum blue colorimetric method for determining ferro-silico aluminium according to claim 1, it is characterized in that: described hydrochloric acid density is 1.19g/mL, hydrochloric acid and water volume ratio are 1:1.
4. the method for silicone content in employing silicon molybdenum blue colorimetric method for determining ferro-silico aluminium according to claim 1, is characterized in that: described concentration of sodium hydroxide solution is 200g/L.
5. the method for silicone content in employing silicon molybdenum blue colorimetric method for determining ferro-silico aluminium according to claim 1, is characterized in that: described ammonium molybdate solution concentration is 50g/L.
6. the method for silicone content in employing silicon molybdenum blue colorimetric method for determining ferro-silico aluminium according to claim 1, is characterized in that: described oxalic acid solution concentration is 50g/L.
7. the method for silicone content in employing silicon molybdenum blue colorimetric method for determining ferro-silico aluminium according to claim 1, is characterized in that: described l ferrous ammonium sulfate solution concentration is 60g/L, and containing the 10mL concentrated sulphuric acid in often liter of solution, described concentrated sulphuric acid density is 1.84g/mL.
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Cited By (6)
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| CN108931484A (en) * | 2016-09-30 | 2018-12-04 | 罗斯蒙特分析公司 | Colorimetric analysis instrument with reagent diagnosis |
| CN109374546A (en) * | 2018-11-07 | 2019-02-22 | 内蒙古第机械集团股份有限公司 | The measuring method of silicone content in a kind of ferrotianium |
| CN111458330A (en) * | 2020-04-28 | 2020-07-28 | 今麦郎饮品股份有限公司 | Method for semi-quantitatively detecting content of metasilicic acid in mineral water and detection reagent thereof |
| CN113406022A (en) * | 2021-01-29 | 2021-09-17 | 郑州机械研究所有限公司 | Method for rapidly judging silicon content in alloy |
| CN113607878A (en) * | 2021-07-29 | 2021-11-05 | 北京首钢股份有限公司 | Assay method for concentration of free acid and ferrous ion in pickling waste hydrochloric acid and application |
| CN113624703A (en) * | 2021-08-24 | 2021-11-09 | 郑州机械研究所有限公司 | Method for quickly judging silicon content in aluminum alloy |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108931484A (en) * | 2016-09-30 | 2018-12-04 | 罗斯蒙特分析公司 | Colorimetric analysis instrument with reagent diagnosis |
| CN109374546A (en) * | 2018-11-07 | 2019-02-22 | 内蒙古第机械集团股份有限公司 | The measuring method of silicone content in a kind of ferrotianium |
| CN111458330A (en) * | 2020-04-28 | 2020-07-28 | 今麦郎饮品股份有限公司 | Method for semi-quantitatively detecting content of metasilicic acid in mineral water and detection reagent thereof |
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| CN113607878A (en) * | 2021-07-29 | 2021-11-05 | 北京首钢股份有限公司 | Assay method for concentration of free acid and ferrous ion in pickling waste hydrochloric acid and application |
| CN113607878B (en) * | 2021-07-29 | 2024-06-07 | 北京首钢股份有限公司 | Assay method and application of free acid and ferrous ion concentration in pickling waste hydrochloric acid |
| CN113624703A (en) * | 2021-08-24 | 2021-11-09 | 郑州机械研究所有限公司 | Method for quickly judging silicon content in aluminum alloy |
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Application publication date: 20160106 |