CN103389239A - Mixed flux and method for measuring silicon content of silicon iron by perchloric acid dehydration gravimetric method - Google Patents
Mixed flux and method for measuring silicon content of silicon iron by perchloric acid dehydration gravimetric method Download PDFInfo
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- CN103389239A CN103389239A CN2013103496983A CN201310349698A CN103389239A CN 103389239 A CN103389239 A CN 103389239A CN 2013103496983 A CN2013103496983 A CN 2013103496983A CN 201310349698 A CN201310349698 A CN 201310349698A CN 103389239 A CN103389239 A CN 103389239A
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Abstract
The invention discloses a mixed flux and a method for measuring the silicon content of silicon iron by a perchloric acid dehydration gravimetric method and applied to decomposition of an early-stage sample, and belongs to the field of chemistry. The mixed flux consists of anhydrous sodium carbonate and nitrate potash, wherein the weight ratio of the anhydrous sodium carbonate to the nitrate potash is (6-11):1. The method for measuring the silicon content of the silicon iron comprises the following steps: a, mixing a silicon iron sample to be measured and the mixed flux uniformly, wrapping the mixture by using filter paper into a spherical sample, and placing the sample into a porcelain crucible with graphite powder; b, placing the porcelain crucible with the sample into a muffle furnace, slowly heating to 900 DEG +/-10 DEG C and preserving heat for 15-20 minutes; c, taking out the porcelain crucible subjected to heat preservation in the step b and cooling to below 50 DEG C, wherein the sample is shaped like a button; and d, placing the button-shaped sample into hydrochloric acid and leaching, and in the subsequent steps, operating the leaching liquid according to an analysis method in national standard GB4333.1-84. According to the mixed flux and the method, the sample can be fused and decomposed effectively, so that the measuring result is more accurate.
Description
Technical field
The invention belongs to the analytical chemistry field, be specifically related to a kind of perchloric acid determination and measure sample decomposition in early stage mixed flux and the method for Silicon in Ferrosilicon content.
Background technology
Present GB GB4333.1-84 " ferrosilicon chemical analysis method perchloric acid determination is measured the silicon amount ", early stage, the processing of sample operated mixed flux sodium carbonate used: sodium peroxide=1:2(mass ratio) can not well sample be decomposed, and very easily produce sample and splash phenomenon, make Lower result, the method is difficult to operation.Application number is 200810149787.2 Chinese patents: the disclosed flux of a kind of fusion metallurgy sample analysis fusing agent and preparation and application thereof, adopt boric acid in reality: sodium carbonate=1:2(mass ratio) test, found that and can be well sample be melted, but because the existence of boron makes measurement result all the time higher 1.5%～2.0%.Use the mixed flux of mensuration Silicon in Ferrosilicon content provided by the present invention, can avoid the phenomenon that splashes of sample, melt well sample, make measurement result accurate, and easy and simple to handle.
By literature search, in the analytical chemistry field, also there is no the flux that directly adopts natrium carbonicum calcinatum and potassium nitrate to be mixed at present, do not have flux provided by the present invention to be used for the mensuration of ferrosilicon sample silicone content yet.
Summary of the invention
Technical matters to be solved by this invention be to provide a kind of can be effectively with sample melted decompose, make measurement result more accurately the perchloric acid determination decomposition sample of measuring Silicon in Ferrosilicon content with mixed flux and method.
The technical solution adopted for the present invention to solve the technical problems is: the perchloric acid determination is measured the mixed flux of Silicon in Ferrosilicon content, natrium carbonicum calcinatum and potassium nitrate, consists of, and the weight ratio of natrium carbonicum calcinatum and potassium nitrate is 6～11 ︰ 1.
Further, the weight ratio of natrium carbonicum calcinatum and potassium nitrate is 7～10 ︰ 1.
Wherein, in above-mentioned mixed flux, natrium carbonicum calcinatum and potassium nitrate are Powdered.
Wherein, in above-mentioned mixed flux, it is pure that natrium carbonicum calcinatum and potassium nitrate are analysis.
The perchloric acid determination is measured the method for Silicon in Ferrosilicon content, comprises the steps:
A, ferrosilicon sample to be measured is mixed with above-mentioned any one mixed flux, then, with filter paper parcel glomeration ball sample, put into the porcelain crucible that fills dag;
B, the porcelain crucible that will fill sample are put into muffle furnace, slowly are warming up to 900 ℃ ± 10 ℃, are incubated 15～20 minutes;
Porcelain crucible after c, taking-up step b insulation, be cooled to below 50 ℃, and sample becomes the button shape;
D, button shape sample is put into hydrochloric acid leach, subsequent step, according to analytical approach operation in GB GB4333.1-84, namely records the content of Silicon in Ferrosilicon with leaching liquid.
Wherein, in said method, the weight ratio of mixed solvent and ferrosilicon sample to be measured is: 20～30 ︰ 1.
Wherein, in said method step a, the addition of mixed flux is 4～6g.
Wherein, in the said method steps d, the 40mL hydrochloric acid of button shape sample being put into 1+1 leaches.
Wherein, the hydrochloric acid solution after the hydrochloric acid of 1+1 refers to the water that concentration is the concentrated hydrochloric acid use equal volume of 35-37% is diluted.
Wherein, in said method step b, the porcelain crucible that fills sample is put into temperature lower than the muffle furnace of 300 ℃, and then heat temperature raising.
The invention has the beneficial effects as follows: the mixed flux component that the present invention measures Silicon in Ferrosilicon content is few, prepare simple and fast, it is convenient to store, consumption is few, cost is low, effective to the decomposition of ferrosilicon sample, make measurement result more accurate, also can be generalized to silicon and other constituent analyses decomposition use of sample in earlier stage in other alloy, raw material.The inventive method is easy and simple to handle, and measurement result is accurate.
Embodiment
The present invention is further described below by embodiment.
Perchloric acid determination of the present invention is measured the mixed flux of Silicon in Ferrosilicon content, natrium carbonicum calcinatum and potassium nitrate, consists of, and the weight ratio of natrium carbonicum calcinatum and potassium nitrate is 6～11 ︰ 1.
Preferably, in order to make final measurement result more accurate, the weight ratio of natrium carbonicum calcinatum and potassium nitrate is 7～10 ︰ 1.
Wherein, in above-mentioned mixed flux, natrium carbonicum calcinatum and potassium nitrate are Powdered.
Wherein, in above-mentioned mixed flux, it is pure that natrium carbonicum calcinatum and potassium nitrate are analysis.
The preparation method of mixed flux of the present invention: first take and analyze pure potassium nitrate pulverize in mortar, then take in proportion and analyze pure natrium carbonicum calcinatum and mix with potassium nitrate, bottle standby.
Perchloric acid determination of the present invention is measured the method for Silicon in Ferrosilicon content, comprises the steps:
A, ferrosilicon sample to be measured is mixed with the described mixed flux of above-mentioned any one, then (it will be understood by those skilled in the art that herein and should pack tightly as far as possible with filter paper parcel glomeration ball sample, and more tight better), put into the porcelain crucible that fills dag (it will be appreciated by persons skilled in the art that dag should 800～900 ℃ of calcinations);
B, the porcelain crucible that will fill sample are put into muffle furnace, slowly are warming up to 900 ℃ ± 10 ℃, are incubated 15～20 minutes;
Porcelain crucible after c, taking-up step b insulation, be cooled to below 50 ℃, and sample becomes the button shape;
D, button shape sample is put into hydrochloric acid leach, subsequent step, according to analytical approach operation in GB GB4333.1-84, namely records the content of Silicon in Ferrosilicon with leaching liquid.
In steps d, subsequent step is about to leaching liquid and starts operation according to the step that obtains hydrochloric acid leaching liquid in GB GB4333.1-84 " ferrosilicon chemical analysis method perchloric acid determination measure silicon amount " and get final product.
Preferably, in order to make final measurement result more accurate, the weight ratio of mixed solvent and ferrosilicon sample to be measured is: 20～30 ︰ 1.
Further preferred, in order to make final measurement result more accurate, in said method step a, the addition of mixed flux is 4～6g.
Preferably, in the said method steps d, the 40mL hydrochloric acid of button shape sample being put into 1+1 leaches.
Preferably,, in order to make final measurement result more accurate, in said method step b, the porcelain crucible that fills sample is put into temperature lower than the muffle furnace of 300 ℃, and then heat temperature raising.Sample is jumped to be spattered.
Below by embodiment, the specific embodiment of the present invention is described further, but therefore protection scope of the present invention is not limited among embodiment.
Embodiment one
Get same ferrosilicon standard specimen YSB11601-99(Si%=72.95) adopt natrium carbonicum calcinatum: the mixed flux decomposition sample that potassium nitrate is respectively (weight ratio) 5:1,7:1,8:1,10:1,15:1 carries out three replicate determinations, check the precision of its assay method, method is as follows, and acquired results is in Table 1.
A with diameter be 12.5cm at a slow speed quantitative filter paper divide two halves equally, get half and be folded into funnel-form, be put on the 30ml crucible, b adds 5 gram mixed fluxs of the present invention to folding in filter paper in a, the ferrosilicon sample 0.2000g to be measured that c will take sweeps in mixed flux in b, sample is fully mixed with mixed flux, and d is with a, b, the described filter paper packaging glomeration of c sample ball.F is put in the described sample ball of d to fill dag and grind in smooth smooth 100ml porcelain crucible.G puts into muffle furnace lower than 300 ℃ with the described porcelain crucible that fills sample of f, slowly heats up, and about 30～40 minutes, furnace temperature rose to 900 ℃ ± 10 ℃, was incubated 15～20 minutes.H takes out the described crucible of g, is cooled to approximately below 50 ℃, and the sample ball becomes button-type, puts into and fills the leaching of (1+1) 40mL hydrochloric acid 500mL beaker, and subsequent step, by the operation of GB GB4333.1-84 analytical approach, is measured the content of Silicon in Ferrosilicon.
Table 1 different proportion mixed flux test findings
By data in table 1 as seen, the mixed flux of pressing three kinds of proportionings of the present invention is used for measuring Silicon in Ferrosilicon content, and measurement result reappearance and accuracy are all better; Show that the mixed flux of several proportionings of the present invention all can meet the decomposition requirement of ferrosilicon sample; The mixed flux measurement result of proportioning outside the present invention: ratio is that the mean value of 5:1 seems and can meet the demands, but reappearance is obviously poor; Find in experiment, molten sample splashes more, and three samples splash degree varies and cause, and has carried out certain recovery in operation; Ratio is that the measurement result of 15:1 is generally on the low side, and reappearance is also poor, may be because the potassium nitrate amount is few, and the oxidizing substance quantity not sufficient can not make due to ferrosilicon decomposes fully.Laboratory can select the proportioning of natrium carbonicum calcinatum and potassium nitrate that analysis cost is reduced according to price.
Embodiment two
Get three ferrosilicon sample masses and be 0.2000 gram, according to the procedure of embodiment one, the mixed flux of getting anhydrous carbon sodium: potassium nitrate=10:1 decomposes sample, carries out three replicate determinations, checks the precision of its assay method, and acquired results is in Table 2.
The analysis result of the same mixed flux of table 2 to the Different Silicon iron sample
By data in table 1 as seen, by mixed flux of the present invention, be used for measuring Silicon in Ferrosilicon content, the measurement result reappearance is better; Extreme difference is less than 0.3%.Blank value is very low, can ignore.
Claims (9)
1. the perchloric acid determination is measured the mixed flux of Silicon in Ferrosilicon content, it is characterized in that being comprised of natrium carbonicum calcinatum and potassium nitrate, and the weight ratio of natrium carbonicum calcinatum and potassium nitrate is 6～11 ︰ 1.
2. perchloric acid determination according to claim 1 is measured the mixed flux of Silicon in Ferrosilicon content, and it is characterized in that: the weight ratio of natrium carbonicum calcinatum and potassium nitrate is 7～10 ︰ 1.
3. perchloric acid determination according to claim 1 and 2 is measured the mixed flux of Silicon in Ferrosilicon content, and it is characterized in that: natrium carbonicum calcinatum and potassium nitrate are Powdered.
4. perchloric acid determination according to claim 1 and 2 is measured the mixed flux of Silicon in Ferrosilicon content, it is characterized in that: it is pure that natrium carbonicum calcinatum and potassium nitrate are analysis.
5. the perchloric acid determination is measured the method for Silicon in Ferrosilicon content, it is characterized in that comprising the steps:
A, ferrosilicon sample to be measured is mixed with the described mixed flux of any one in claim 1～4, then, with filter paper parcel glomeration ball sample, put into the porcelain crucible that fills dag;
B, the porcelain crucible that will fill sample are put into muffle furnace, slowly are warming up to 900 ℃ ± 10 ℃, are incubated 15～20 minutes;
Porcelain crucible after c, taking-up step b insulation, be cooled to below 50 ℃, and sample becomes the button shape;
D, button shape sample is put into hydrochloric acid leach, subsequent step, according to analytical approach operation in GB GB4333.1-84, namely records the content of Silicon in Ferrosilicon with leaching liquid.
6. perchloric acid determination according to claim 5 is measured the method for Silicon in Ferrosilicon content, and it is characterized in that: the weight ratio of mixed solvent and ferrosilicon sample to be measured is: 20～30 ︰ 1.
7. perchloric acid determination according to claim 6 is measured the method for Silicon in Ferrosilicon content, and it is characterized in that: in step a, the addition of mixed flux is 4～6g.
8. perchloric acid determination according to claim 7 is measured the method for Silicon in Ferrosilicon content, and it is characterized in that: in steps d, the 40mL hydrochloric acid of button shape sample being put into 1+1 leaches.
9. according to claim 5 to 8, the described perchloric acid determination of any one is measured the method for Silicon in Ferrosilicon content, it is characterized in that: in step b, the porcelain crucible that fills sample is put into temperature lower than the muffle furnace of 300 ℃, and then heat temperature raising.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106556615A (en) * | 2016-11-21 | 2017-04-05 | 厦门出入境检验检疫局检验检疫技术中心 | The detection method of silicon doping situation in a kind of iron scale |
| CN111721598A (en) * | 2020-06-19 | 2020-09-29 | 内蒙古第一机械集团股份有限公司 | Chemical flux for determining rare earth magnesium silicon iron alloy |
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| CN106556615B (en) * | 2016-11-21 | 2019-03-05 | 厦门出入境检验检疫局检验检疫技术中心 | The detection method of silicon doping situation in a kind of iron scale |
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