CN102621030A - Method for determining silicon dioxide in limestone and dolomite by using gravimetric method - Google Patents
Method for determining silicon dioxide in limestone and dolomite by using gravimetric method Download PDFInfo
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- CN102621030A CN102621030A CN2012100926843A CN201210092684A CN102621030A CN 102621030 A CN102621030 A CN 102621030A CN 2012100926843 A CN2012100926843 A CN 2012100926843A CN 201210092684 A CN201210092684 A CN 201210092684A CN 102621030 A CN102621030 A CN 102621030A
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Abstract
The invention provides a method for determining silicon dioxide in limestone and dolomite by using a gravimetric method. A method for quickly dissolving in acid and fusing residue by using a small amount of mixed flux is employed, a frit in filtrate and washing liquid is leached, the silicon dioxide in a test solution is determined by using a perchloric acid dehydration gravimetric method, and the accurate content of the silicon dioxide in a test sample is obtained. The method has the advantages that long-time heating of the limestone and the dolomite in a high-temperature furnace is not required, energy consumption is reduced, and time is saved; all test samples can be completely decomposed by recovering the residue which is dissolved in the acid, and analysis accuracy is ensured; and silicic acid is coagulated by one-time perchloric acid smoking, the aim of completely coagulating the silicic acid can be completely fulfilled, and analysis time is shortened.
Description
Technical field
The present invention relates to the method for silicon dioxide in gravimetric determination lime stone, the rauhkalk.
Background technology
Along with development of modern industry; More and more be deep in the every field to metallurgy, building materials, chemical industry with the development and application of raw material limestone, rauhkalk; Lime stone, rauhkalk have become the mineral resources with important economic worth, therefore also its grade quality are had higher requirement.The whether accurate purposes and the product quality that directly influences lime stone, rauhkalk of its major component dioxide-containing silica analysis.
At present for dioxide-containing silica greater than 2% lime stone, rauhkalk sample; The middle perchloric acid dehydrated weight methods of standard GB/T3286.2-1998 " mensuration of lime stone, rauhkalk chemical analysis method silica volume " that adopt are measured more; The platinum crucible that will fill test portion in the primary standard places furnace temperature to be lower than 300 ℃ high temperature furnace; Cover the platinum lid, make between platinum crucible and platinum lid and stay a gap.Furnace temperature is warming up to 1000 ℃ gradually, and under this temperature, keeps 30min.After again the calcination thing being added a large amount of hydrochloric acid decomposition, add a large amount of perchloric acid and smolder, make through filtration, washing, calcination, impure silicon dioxide to be added sulfuric acid, hydrofluorite by silicate condensation, wave silicon, calculate the content of silicon dioxide.First low temperature begins calcination in the former method, and the retention time is longer, though follow the hydrochloric acid content that adds the decomposition test portion bigger, some lime stone that is difficult to decompose, rauhkalk analysis is not still decomposed fully, makes analysis result on the low side.
Summary of the invention
Technical matters to be solved by this invention provides the method for silicon dioxide in a kind of gravimetric determination lime stone, the rauhkalk, decomposes slow and not exclusively and bring sample analysis problem of lower as a result to overcome in the existing in prior technology measuring process sample.
For solving the problems of the technologies described above; The present invention adopts a kind of fast acid to dissolve, and residue leaches frit with the method for mixed with little amount flux fusion in filtrating and washing lotion; Test solution is measured silicon dioxide in the test solution with perchloric acid dehydrated weight method again, thereby obtains the accurate content of silicon dioxide in the sample.It is characterized in that, may further comprise the steps:
Step 1, test portion are directly used the appropriate hydrochloric acid heating and decomposition, and filtrating is left and taken in filtered while hot test solution, washing;
Step 2, the residue use ratio after hydrochloric acid decomposed are 1.5: 1～3: 1 natrium carbonicum calcinatum and the fusion of boric acid mixed flux, and it is extremely complete in the former beaker that fills filtrating and washing lotion, to leach frit with hydrochloric acid;
Step 3, low-temperature evaporation to 10～20ml, adding ethanol or methyl alcohol are evaporated to dried, catch up with most boric acid, add hydrochloric acid heating for dissolving salt again,
Step 4, adding perchloric acid cover upper surface ware, the backflow of smoldering makes silicate condensation; Wash out silicic acid; Filtration, washing, calcination, wave silicon, divided by sample mass, promptly calculate the dioxide-containing silica in the sample with the difference of deposition before and after the hydrofluoric acid treatment and the gross mass of platinum crucible.
Preferably, said natrium carbonicum calcinatum is 2 to 1 with the ratio of boric acid mixed flux.
Beneficial effect of the present invention is:
(1) reduced in the high temperature furnace that the furnace temperature that prior art adopted is lower than 300 ℃, covered the platinum lid, made platinum crucible and platinum stay a gap between covering.Furnace temperature is warming up to 1000 ℃ gradually, and under this temperature, keeps the process of 30min, reduced energy consumption, practiced thrift the time simultaneously.
(2) the molten residue of acid reclaims all samples can be decomposed fully, has guaranteed the accuracy of analyzing.
(3) once emit perchloric acid cigarette cohesion silicic acid, can reach silicate condensation purpose completely fully, another has reduced analysis time.
Below in conjunction with embodiment technical scheme of the present invention is further specified.
Embodiment
(1) take by weighing 0.5g～1.0g test portion, be accurate to 0.0001g, place beaker, add 15mL～30mL hydrochloric acid (1+1), heating decomposes to no bubble with test portion and produces.
(2) with the test solution filtered while hot; Residue is placed platinum crucible; After dry in high temperature furnace, the ashing, add 1g～2g natrium carbonicum calcinatum and boric acid flux fusion 10～25min, the taking-up crucible to mix at 1.5: 1; Cooling adds 2mL～10mL hydrochloric acid (1+1) and leaches frit in the beaker that fills filtrating and washing lotion.
(3) continue to be heated to the about 20mL of volume, add 10mL～25mL ethanol or methyl alcohol, low-temperature evaporation adds 20mL hydrochloric acid (1+1) to doing; The heating for dissolving salt adds 10mL～30mL perchloric acid, cover upper surface ware (staying a gap); Be heated to and emit the white cigarette of perchloric acid, and keep smoldering backflow 10min～25min, subsequent step washes out silicic acid; Filtration, washing, calcination, to wave silicon identical with former method, but only need once emit the cohesion of perchloric acid cigarette, can reach silicate condensation purpose completely fully.
Embodiment 1
(1) take by weighing the 0.5005g test portion, place beaker, add 20mL hydrochloric acid (1+1), heating decomposes to no bubble with test portion and produces.
(2) with the test solution filtered while hot, residue is placed platinum crucible, after dry in high temperature furnace, the ashing; Add 1g natrium carbonicum calcinatum and boric acid with 2 to the 1 flux fusion 10min that mix; Take out crucible, cooling adds 2mL hydrochloric acid (1+1) and leaches frit in the beaker that fills filtrating and washing lotion.
(3) continue to be heated to the about 20mL of volume, add 25mL ethanol or methyl alcohol, low-temperature evaporation is to doing; Add 10mL hydrochloric acid (1+1), the heating for dissolving salt adds 30mL perchloric acid; Cover upper surface ware (staying a gap) is heated to and emits the white cigarette of perchloric acid, and keeps smoldering backflow 25min; Subsequent step washes out silicic acid; Filtration, washing, calcination, to wave silicon identical with former method, and deposition respectively is 32.8906g and 32.8413g with the gross mass of platinum crucible before and after the hydrofluoric acid treatment, and the dioxide-containing silica that result of calculation draws in the sample is 9.85%.
Example 2:
(1) take by weighing the 0.8004g test portion, place beaker, add 15mL hydrochloric acid (1+1), heating decomposes to no bubble with test portion and produces.
(2) with the test solution filtered while hot, residue is placed platinum crucible, after dry in high temperature furnace, the ashing; Add 1.5g natrium carbonicum calcinatum and boric acid with 3 to the 1 flux fusion 15min that mix; Take out crucible, cooling adds 6mL hydrochloric acid (1+1) and leaches frit in the beaker that fills filtrating and washing lotion.
(3) continue to be heated to the about 20mL of volume, add 16mL ethanol or methyl alcohol, low-temperature evaporation is to doing; Add 18mL hydrochloric acid (1+1), the heating for dissolving salt adds 10mL perchloric acid; Cover upper surface ware (staying a gap) is heated to and emits the white cigarette of perchloric acid, and keeps smoldering backflow 10min; Subsequent step washes out silicic acid; Filtration, washing, calcination, to wave silicon identical with former method, and deposition respectively is 31.1637g and 31.1218g with the gross mass of platinum crucible before and after the hydrofluoric acid treatment, and the dioxide-containing silica that result of calculation draws in the sample is 5.23%.
Example 3
(1) take by weighing the 1.0010g test portion, place beaker, add 30mL hydrochloric acid (1+1), heating decomposes to no bubble with test portion and produces.
(2) with the test solution filtered while hot, residue is placed platinum crucible, after dry in high temperature furnace, the ashing; Add 2g natrium carbonicum calcinatum and boric acid with 2 to the 1 flux fusion 25min that mix; Take out crucible, cooling adds 10mL hydrochloric acid (1+1) and leaches frit in the beaker that fills filtrating and washing lotion.
(3) continue to be heated to the about 20mL of volume, add 10mL ethanol or methyl alcohol, low-temperature evaporation is to doing; Add 25mL hydrochloric acid (1+1), the heating for dissolving salt adds 20mL perchloric acid; Cover upper surface ware (staying a gap) is heated to and emits the white cigarette of perchloric acid, and keeps smoldering backflow 15min; Subsequent step washes out silicic acid; Filtration, washing, calcination, to wave silicon identical with former method, and deposition respectively is 31.1637g and 31.1351g with the gross mass of platinum crucible before and after the hydrofluoric acid treatment, and the dioxide-containing silica that result of calculation draws in the sample is 2.86%.
It should be noted last that; Above embodiment is only unrestricted in order to technical scheme of the present invention to be described; Although with reference to preferred embodiment the present invention is specified, those of ordinary skill in the art should be appreciated that and can make amendment or be equal to replacement technical scheme of the present invention; And not breaking away from the spirit and the scope of technical scheme of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (2)
1. the method for silicon dioxide in a gravimetric determination lime stone, the rauhkalk is characterized in that may further comprise the steps:
Step 1, test portion are directly used the appropriate hydrochloric acid heating and decomposition, and filtrating is left and taken in filtered while hot test solution, washing;
Step 2, the residue use ratio after hydrochloric acid decomposed are 1.5: 1～3: 1 natrium carbonicum calcinatum and the fusion of boric acid mixed flux, and it is extremely complete in the former beaker that fills filtrating and washing lotion, to leach frit with hydrochloric acid;
Step 3, low-temperature evaporation to 10～20ml, adding ethanol or methyl alcohol are evaporated to dried, catch up with most boric acid, add hydrochloric acid heating for dissolving salt again,
Step 4, adding perchloric acid cover upper surface ware, the backflow of smoldering makes silicate condensation; Wash out silicic acid; Filtration, washing, calcination, wave silicon, divided by sample mass, promptly calculate the dioxide-containing silica in the sample with the difference of deposition before and after the hydrofluoric acid treatment and the gross mass of platinum crucible.
2. the method for silicon dioxide is characterized in that in gravimetric determination lime stone according to claim 1, the rauhkalk, and said natrium carbonicum calcinatum is 2 to 1 with the ratio of boric acid mixed flux.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103389239A (en) * | 2013-08-12 | 2013-11-13 | 攀枝花学院 | Mixed flux and method for measuring silicon content of silicon iron by perchloric acid dehydration gravimetric method |
| CN103528912A (en) * | 2013-09-18 | 2014-01-22 | 刘俊菊 | Rapid system analysis for limestone and dolomite |
| CN104634641A (en) * | 2015-03-04 | 2015-05-20 | 四川西冶新材料有限公司 | Method for separating and purifying quartz in soldering flux or coating |
| CN105388084A (en) * | 2015-11-07 | 2016-03-09 | 武钢集团昆明钢铁股份有限公司 | Detection method for silicon content in manganese-rich slag |
| CN106124356A (en) * | 2016-06-14 | 2016-11-16 | 华电莱州发电有限公司 | Dioxide-containing silica abbreviated analysis method in limestone |
| CN111678835A (en) * | 2020-06-22 | 2020-09-18 | 浙江天能电池(江苏)有限公司 | Method for measuring content of silicon dioxide in silica sol for storage battery |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103389239A (en) * | 2013-08-12 | 2013-11-13 | 攀枝花学院 | Mixed flux and method for measuring silicon content of silicon iron by perchloric acid dehydration gravimetric method |
| CN103528912A (en) * | 2013-09-18 | 2014-01-22 | 刘俊菊 | Rapid system analysis for limestone and dolomite |
| CN104634641A (en) * | 2015-03-04 | 2015-05-20 | 四川西冶新材料有限公司 | Method for separating and purifying quartz in soldering flux or coating |
| CN104634641B (en) * | 2015-03-04 | 2017-05-10 | 四川西冶新材料股份有限公司 | Method for separating and purifying quartz in soldering flux or coating |
| CN105388084A (en) * | 2015-11-07 | 2016-03-09 | 武钢集团昆明钢铁股份有限公司 | Detection method for silicon content in manganese-rich slag |
| CN106124356A (en) * | 2016-06-14 | 2016-11-16 | 华电莱州发电有限公司 | Dioxide-containing silica abbreviated analysis method in limestone |
| CN111678835A (en) * | 2020-06-22 | 2020-09-18 | 浙江天能电池(江苏)有限公司 | Method for measuring content of silicon dioxide in silica sol for storage battery |
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Application publication date: 20120801 |