CN105158406A - Method for measuring silica content in ferromanganese iron by utilizing potassium fluosilicate volumetric method - Google Patents
Method for measuring silica content in ferromanganese iron by utilizing potassium fluosilicate volumetric method Download PDFInfo
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- CN105158406A CN105158406A CN201510549209.8A CN201510549209A CN105158406A CN 105158406 A CN105158406 A CN 105158406A CN 201510549209 A CN201510549209 A CN 201510549209A CN 105158406 A CN105158406 A CN 105158406A
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Abstract
A method for measuring silica content in ferromanganese iron by utilizing a potassium fluosilicate volumetric method comprises the steps of adopting nitric acid-hydrochloric acid-hydrofluoric acid to dissolve a ferromanganese iron sample, adding hydrogen peroxide to remove the color of high valence manganese to remove the interference during titration after the sample is dissolved completely, adding saturated potassium nitrate to form potassium fluosilicate sediment, so as to enable silicon to exist in a complete sediment form, separating the sediment through suction filtration, then dissolving the sediment by using hot water to form hydrofluoric acid, and finally, adopting hydrofluoric acid formed by titration of a sodium hydroxide standard solution, so as to calculate the silica content. The method has the characteristics of high efficiency, high accuracy and low cost.
Description
Technical field
The present invention relates to a kind of assay method of content of silicon in ferromanganese, have and relate to a kind of method utilizing silicon fluoro acid potassium volumetric determination content of silicon in ferromanganese.
Background technology
Ferromanganese is the ferroalloy of manganese and iron composition, mainly contains high carbon ferromanganese, mid-carbon fe-mn, low-carbon ferromanganese, manganese metal, spiegel, silicomangan etc.In steel-making, manganeisen is important deoxidizer and alloy addition, plays the effect of component controlling, so ferromanganese has a wide range of applications in smelter STEELMAKING PRODUCTION.Wherein, silicone content is one of leading indicator evaluating ferromanganese quality, and be also the main authority that ferromanganese enters that factory's quality is checked on and price is settled accounts, therefore, the content measuring Silicon in Ferromanganese is exactly significant.
At present, the method for the silicon measured in ferromanganese mainly contains perchloric acid determination, inductively coupled plasma emission spectrography, x ray fluorescence spectrometry, absorption photometry and silicon molybdenum blues photometry etc.Wherein, accurately and stable, but medicine adds that kind is many and consumption large, complicated operation, long flow path for perchloric acid determination measurement result, and cost is high, and energy consumption is large, is not suitable for the Fast Measurement demand in producing.Inductively coupled plasma emission spectrography adopts large-scale instrument to measure, and cost of determination is higher.Though x ray fluorescence spectrometry can meet the requirement of express-analysis, the accuracy of result often depends on the preparation method of sample, and equipment cost is high, and environmental requirement is strict.Absorption photometry needs to join corresponding standard solution and does curve, simultaneously inapplicable for high-carbon sample, high-carbon sample has the sample interference colorimetric that cannot dissolve, the not special treatment step for high-carbon sample, such as, silicon in Their Determination by Spectrophotometry ferromanganese, Wang Shengli, Wang Shuhua, " analysis and test ", 2007,9th phase P57-58.Silicon molybdenum blues photometry measures silicon and cannot once open for high-carbon sample, and needs to carry out complicated residue treatment step, also needs to do corresponding typical curve in company with sample simultaneously, relatively loaded down with trivial details; Moreover the problem that the data that during silicon molybdenum blues photometry mensuration, high-carbon sample often occurs are on the low side.Such as CN201410463003.9 discloses a kind of assay method of content of silicon in ferromanganese, needs drawing standard curve method, and the reagent type of adding is more, and cost is higher.Silicon in prior art silicon molybdenum blues photometry Fast Measurement silicomanganese, Wang Huiqing, " Laigang science and technology " phase Dec the 6th in 2011, P57-59, the method needs drawing standard curve equally, and is only applicable to the mensuration of the lower Silicon in Ferromanganese of carbon content, and the ferromanganese sample high for carbon content has insolubles, cannot accurate colorimetric, measurement result is easily on the low side.
Summary of the invention
Technical matters to be solved by this invention is, provides a kind of and utilizes that silicon fluoro acid potassium volumetric method is efficient, the method for the mensuration content of silicon in ferromanganese of the high and low cost of accuracy.
The technical scheme that the present invention solves the employing of its technical matters is that a kind of method utilizing silicon fluoro acid potassium volumetric determination content of silicon in ferromanganese, comprises the following steps:
(1) dissolve: first add nitric acid, hydrochloric acid, hydrofluoric acid dissolution ferromanganese sample;
(2) color of value Mn is eliminated: after ferromanganese sample dissolution is complete, add 5 ~ 15, the hydrogen peroxide of 25% ~ 35%;
(3) precipitation and separation: then add saturated sylvite, ambient temperatare puts 20 ~ 40min, then filtering-depositing, washing precipitation 3 ~ 5 times, cleans the acid solution remained on filter paper simultaneously;
(4) dissolution precipitation: then precipitation is put into container in the lump together with filter paper, utilizes hot water dissolving to precipitate, and forms hydrofluorite;
(5) titration: finally adopt the hydrofluorite formed in standard solution of sodium hydroxide titration step (4) is terminal by yellow to blueness, namely can be regarded as to obtain the content of silicon.
Further, in step (3), add saturated potassium nitrate, ambient temperatare puts 30min, and then filtered off with suction precipitation, utilizes potassium nitrate-ethanol wash liquid to precipitate 4 times, cleans the acid solution remained on filter paper simultaneously;
Further, described potassium nitrate-ethanol washing lotion is dissolved in 90mL water by 6g potassium nitrate, adds 10mL ethanol formulated.
Further, in step (4), described hot water is the distilled water boiled.
Further, in step (5), described Concentration of Sodium Hydroxide Solution Standard is 0.1000mol/L.
Compared with prior art, the present invention has following useful technique effect:
(1) efficient: to adopt silicon fluoro acid potassium volumetric determination content of silicon in ferromanganese to substantially reduce operating process compared to the gravimetric method in GB and colourimetry, shorten minute, improve production efficiency, thus easy, quick, the easy to operate demand be more suitable for basic, normal, high carbon ferromanganese rapid assay methods in enterprise's production of the present invention.
(2) accuracy is high: adopt silicon fluoro acid potassium volumetric method can open sample fast, adopt acid base titration, reaction velocity is fast, and terminal is obviously easily grasped, and measurement result is stablized, and accurately and reliably, experiment proves data, and relative standard deviation is all less than 5%.
(3) low cost: low to equipment, environmental requirement, decreases the service time of high temperature furnace and electric hot plate, has saved energy cost; And greatly reduce use kind and the addition of medicine, reduce material cost.
Embodiment
Below in conjunction with embodiment, the present invention is illustrated further.
One, reagent
1, nitric acid (density is 1.42g/mL)
2, hydrochloric acid (density is 1.19g/mL)
3, hydrofluorite (density is ρ 1.15g/mL)
4, hydrogen peroxide (30%)
5, saturated potassium nitrate
6, potassium nitrate-ethanol washing lotion (6g potassium nitrate is dissolved in 90mL water, adds 10mL ethanol)
7, neutral water: (distilled water boils emptying carbon dioxide)
8, bromothymol blue (density is 1g/L ethanolic solution)
9, Standard Volumetric Solutions for Sodium Hydroxide (concentration is 0.1000mol/L)
Embodiment 1
1, the mensuration of content of silicon in ferromanganese: take ferromanganese sample 0.5000g in 300mL polytetrafluoroethylene beaker, add 10mL nitric acid (density is the red fuming nitric acid (RFNA) of 1.42g/mL), 5mL hydrofluorite (density is ρ 1.15g/mL), 10mL hydrochloric acid (density is 1.19g/mL) molten sample, dissolve completely until sample, add (30%) 5 ~ 15, hydrogen peroxide to eliminate the color of value Mn, then the saturated potassium nitrate of 20mL is added, ambient temperatare puts 30min, precipitation and fluid separation applications is made by filtered off with suction, eliminate interference, by potassium nitrate-ethanol washing lotion, (6g potassium nitrate is dissolved in 90mL water, add 10mL ethanol) wash beaker and precipitation several, clean the acid solution remained on filter paper, precipitation after suction filtration is put into 500mL triangular flask in the lump together with filter paper, add neutral water (distilled water boils emptying carbon dioxide) the dissolution precipitation formation hydrofluorite that 120mL boils, finally adopt the hydrofluorite that Standard Volumetric Solutions for Sodium Hydroxide (concentration is 0.1000mol/L) titration is formed, be terminal by yellow to blueness, by calculating the content of silicon.
2, sample analysis result calculates:
In formula:
W (Si): the percentage of the siliceous quality of sample.
V: the milliliter number consuming Standard Volumetric Solutions for Sodium Hydroxide during sample titration
V
0: in company with the milliliter number consuming Standard Volumetric Solutions for Sodium Hydroxide during blank titration
M
si/4: 1/4 of Si relative atomic mass
C: the concentration (0.1000mol/L) of Standard Volumetric Solutions for Sodium Hydroxide
M: the quality taking sample
Result of calculation is in table 1.
The contrast of table 1-sample analysis
As shown in Table 1, no matter all can open fast for low-carbon (LC) sample or high-carbon sample, molten sample is complete, and determination data accurately and reliably, and does not need drawing standard curve, operating process is shorter, terminal is easily observed, and assay method is easily grasped, fast, efficiently, be applicable to being applied to the Fast Measurement producing upper Silicon in Ferromanganese.
Claims (5)
1. utilize a method for silicon fluoro acid potassium volumetric determination content of silicon in ferromanganese, it is characterized in that, comprise the following steps:
(1) dissolve: first add nitric acid, hydrochloric acid, hydrofluoric acid dissolution ferromanganese sample;
(2) color of value Mn is eliminated: after ferromanganese sample dissolution is complete, add 5 ~ 15, the hydrogen peroxide of 25% ~ 35%;
(3) precipitation and separation: then add saturated sylvite, ambient temperatare puts 20 ~ 30min, then filtering-depositing, washing precipitation 2 ~ 4 times, cleans the acid solution remained on filter paper simultaneously;
(4) dissolution precipitation: then precipitation is put into container in the lump together with filter paper, utilizes hot water dissolving to precipitate, and forms hydrofluorite;
(5) titration: finally adopt the hydrofluorite formed in standard solution of sodium hydroxide titration step (4) is terminal by yellow to blueness, namely can be regarded as to obtain the content of silicon.
2. the method utilizing silicon fluoro acid potassium volumetric determination content of silicon in ferromanganese according to claim 1, it is characterized in that, in step (3), add saturated potassium nitrate, ambient temperatare puts 30min, then filtered off with suction precipitation, utilizes potassium nitrate-ethanol wash liquid to precipitate 3 times, cleans the acid solution remained on filter paper simultaneously.
3. the method utilizing silicon fluoro acid potassium volumetric determination content of silicon in ferromanganese according to claim 2, is characterized in that, described potassium nitrate-ethanol washing lotion is dissolved in 90mL water by 6g potassium nitrate, adds 10mL ethanol formulated.
4. the method utilizing silicon fluoro acid potassium volumetric determination content of silicon in ferromanganese according to claim 1 and 2, is characterized in that, in step (4), described hot water is the distilled water boiled.
5. the method utilizing silicon fluoro acid potassium volumetric determination content of silicon in ferromanganese according to claim 1,2 or 4, is characterized in that, in step (5), described Concentration of Sodium Hydroxide Solution Standard is 0.1000mol/L.
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Cited By (5)
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| CN106226303A (en) * | 2016-08-23 | 2016-12-14 | 内蒙古包钢钢联股份有限公司 | A kind of assay method of silicone content in low-carbon ferrochromium |
| 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 |
| CN109387597A (en) * | 2017-08-04 | 2019-02-26 | 中车大同电力机车有限公司 | The method for decomposing dioxide-containing silica in potassium fluoride volumetry detection quartz sand using hydrofluoric acid |
| CN109991362A (en) * | 2019-03-26 | 2019-07-09 | 南京钢铁股份有限公司 | The measuring method of silicone content in a kind of silicon vanadium iron |
| CN111377474A (en) * | 2020-04-21 | 2020-07-07 | 深圳市考拉生态科技有限公司 | Method and equipment for purifying calcium fluoride from carbonate-removed fluorine-containing solid waste |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106226303A (en) * | 2016-08-23 | 2016-12-14 | 内蒙古包钢钢联股份有限公司 | A kind of assay method of silicone content in low-carbon ferrochromium |
| 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 |
| CN109387597A (en) * | 2017-08-04 | 2019-02-26 | 中车大同电力机车有限公司 | The method for decomposing dioxide-containing silica in potassium fluoride volumetry detection quartz sand using hydrofluoric acid |
| CN109991362A (en) * | 2019-03-26 | 2019-07-09 | 南京钢铁股份有限公司 | The measuring method of silicone content in a kind of silicon vanadium iron |
| CN111377474A (en) * | 2020-04-21 | 2020-07-07 | 深圳市考拉生态科技有限公司 | Method and equipment for purifying calcium fluoride from carbonate-removed fluorine-containing solid waste |
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