CN103743617A - Rapid exact stable reliable silicon iron sample digestion method - Google Patents
Rapid exact stable reliable silicon iron sample digestion method Download PDFInfo
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- CN103743617A CN103743617A CN201310716601.8A CN201310716601A CN103743617A CN 103743617 A CN103743617 A CN 103743617A CN 201310716601 A CN201310716601 A CN 201310716601A CN 103743617 A CN103743617 A CN 103743617A
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Abstract
The invention discloses a rapid exact stable reliable silicon iron sample digestion method, and belongs to the technical field of test analysis sample pretreatment. The method comprises the steps of firstly placing 0.0800-0.1200g of silicon iron sample into a plastic digestion bottle, successively adding 9-11ml of nitric acid and 4-6ml of hydrofluoric acid, and sealing the digestion bottle; placing the digestion bottle into a heater to heat for 4-6 min under the temperature of 55-65 DEG C after the sample is dissolved, and then cooling the sample to 20-25 DEG C; successively adding 4-6ml of urea solution, 9-11ml of potassium fluoride solution and 2-3g of potassium nitrate, sealing and shaking up, and cooling for 12-18min; filtering a sample solution in a sample bottle, washing the digestion bottle and sedimentation by using the 9-11ml of potassium fluoride solution; shifting the sedimentation and a filter material into a plastic sample bottle, and adding 12-18ml of potassium chloride-ethanol solution. The digestion method provided by the invention has the advantages that various losses in the sample treatment are effectively prevented, the stability, reproducibility and veracity of a testing result are improved, the dissolution is rapid, the sample manufacturing time is shortened, a sample solution is directly used for measuring silicon content, the method is simple and rapid, and the popularization and application value is good.
Description
Technical field
The invention belongs to test analysis sample pretreatment technical field, be specifically related to a kind of quick and precisely, reliable and stable ferrosilicon sample digestion method.
Background technology
The conventional chemical analysis of measuring silicone content in Antaciron mainly contains two kinds of gravimetric method and potassium fluosilicate titrimetrys.Wherein, adopt gravimetric determination silicone content accuracy rate high, but the running time is long, is unfavorable for the quantitative detection of batch samples.Adopt potassium fluosilicate titrimetry to have easy and simple to handle, advantage that can Fast Measurement batch samples, but in conventional detection operation, owing to clearing up reaction too violent, silicon react with hydrofluorite that the silicon tetrafluoride generating is very easy to volatilize, and causes measurement result on the low side.Therefore, research and development one can rapid-digestion ferrosilicon sample, and little, the reliable and stable method for sample pretreatment of volatilization loss during sample preparation, for improving accuracy, the reappearance that in ferrosilicon sample, element silicon quantitatively detects, is a technical matters urgently to be resolved hurrily.
Summary of the invention
The object of the present invention is to provide a kind of quick and precisely, reliable and stable ferrosilicon sample digestion method.
The object of the present invention is achieved like this: a kind of quick and precisely, reliable and stable ferrosilicon sample digestion method, comprise dissolving, precipitation and filter progress, specifically comprise:
A, dissolving: ferrosilicon sample 0.0800 ~ 0.1200g to be cleared up is placed in to plastics and clears up bottle, add successively 9 ~ 11ml nitric acid, 4 ~ 6ml hydrofluorite, airtight with being about to clear up bottle; Sample will be cleared up bottle and be placed in well heater after dissolving, at 55 ~ 65 ℃, heat 4 ~ 6min, then sample solution will be cooled to 20 ~ 25 ℃;
B, precipitation: after the sample solution in steps A is cooling, add successively 4 ~ 6ml urea liquid, 9 ~ 11ml potassium fluoride solution and 2 ~ 3g potassium nitrate, after airtight shaking up, cooling 12 ~ 18min;
C, filtration: sample solution cooling in step B is filtered in plastic sample bottle with filter material, and wash and clear up bottle and precipitation with 9 ~ 11ml Klorvess Liquid, to precipitate and filter material moves in plastic sample bottle, add 12 ~ 18ml potassium chloride-ethanolic solution, obtain testing sample solution.
Adopt digestion procedure of the present invention dissolves silicon ferroelectric sample fast, effectively shorten the pretreatment time of sample, improve analysis speed.For making measurement result more accurately and reliably, the method for the invention is to medicament composition, proportioning and clear up, precipitation, filtering technique etc. all adjust.The closed processes adopting can effectively prevent the volatilization loss of silicon in violent acidolysis reaction.In the apolegamy of acid mixture and the regulation and control of addition, the method for the invention is realizing on the basis that sample fully clears up, and can not decompose precipitation, accessory substance generates and residual acid is removed and be brought impact.For preventing precipitation decomposition, the method for the invention has been adjusted cooling velocity, precipitation temperature and the filtration time of sample solution, has improved stability, reappearance and the accuracy of analyzing measurement result.In addition, potassium chloride-ethanolic solution that the method for the invention in the end adds in step also has the effect that reduces sediment solubility and remove residual acid, thereby has further improved the reliability of testing result.Through clearing up, process the testing sample solution that obtains and can directly measure silicone content by titrimetry of the prior art, simple and efficient to handle, there is good application value.
Embodiment
The present invention is further illustrated below, but never in any form the present invention is limited, and any conversion or the replacement based on training centre of the present invention, done, all fall into protection scope of the present invention.
Quick and precisely, a reliable and stable ferrosilicon sample digestion method, comprise dissolving, precipitation and filter progress, specifically comprise:
A, dissolving: ferrosilicon sample 0.0800 ~ 0.1200g to be cleared up is placed in to plastics and clears up bottle, add successively 9 ~ 11ml nitric acid, 4 ~ 6ml hydrofluorite, airtight with being about to clear up bottle; Sample will be cleared up bottle and be placed in well heater after dissolving, at 55 ~ 65 ℃, heat 4 ~ 6min, then sample solution will be cooled to 20 ~ 25 ℃;
B, precipitation: after the sample solution in steps A is cooling, add successively 4 ~ 6ml urea liquid, 9 ~ 11ml potassium fluoride solution and 2 ~ 3g potassium nitrate, after airtight shaking up, cooling 12 ~ 18min;
C, filtration: sample solution cooling in step B is filtered in plastic sample bottle with filter material, and wash and clear up bottle and precipitation with 9 ~ 11ml Klorvess Liquid, to precipitate and filter material moves in plastic sample bottle, add 12 ~ 18ml potassium chloride-ethanolic solution, obtain testing sample solution.
It can be any in polyethylene bottle or teflon bottle that described plastics are cleared up bottle.
The density of described nitric acid is 1.42g/ml, and the density of described hydrofluorite is 1.15g/ml.
Described well heater can be any in water-bath, electric jacket, insulation can or microwave generator.
Described microwave generator can be any in micro-wave oven or microwave dissolver.
The concentration of described urea liquid is 5%, and the concentration of described potassium fluoride solution is 15%.
The described cooling flowing water cooling method that refers to, is about to the airtight bottle of clearing up and with chilled water, washes away cooling.
The described cooling cooling bath cooling method that also can adopt.
Described filter material is quantitative filter paper.
Described plastic sample bottle can be teflon bottle or polytetrafluoroethylene beaker.
Describedly with Klorvess Liquid washing, clear up bottle and precipitation, refer to and clear up bottle and precipitate each 2 ~ 4 times with Klorvess Liquid washing.
The concentration of described Klorvess Liquid is 4 ~ 6%, and the concentration of described potassium chloride-ethanolic solution is 4 ~ 6%.
embodiment 1
A, dissolving: ferrosilicon sample 0.1000g to be cleared up is placed in to teflon and clears up bottle, add successively 10ml red fuming nitric acid (RFNA), 5ml hydrofluorite, with being about to clear up a bottle airtight and shake gently; Sample will be cleared up bottle and be placed in water-bath after dissolving, at 60 ℃, heat 5min, then sample solution flowing water will be cooled to 23 ℃.
B, precipitation: after the sample solution in steps A is cooling, add successively the urea liquid of 5ml 5%, potassium fluoride solution and the 2.5g potassium nitrate of 10ml 15%, after airtight shaking up, the cooling 15min of flowing water.
C, filtration: sample solution cooling in step B is filtered in teflon sample bottle with quantitative filter paper, and wash and clear up bottle and precipitate each three times with the Klorvess Liquid of 10ml 15%, to precipitate and filter paper moves in teflon sample bottle, potassium chloride-the ethanolic solution that adds 15ml 5%, obtains testing sample solution.
D, detection: in testing sample solution, drip the phenolphthalein indicator of 5 1%, with sour with remnants in 4% sodium hydroxide solution, filter paper is mashed, carefully clean wall of cup surrounding, be neutralized to and occur pink.Then add 200ml boiling water, use at once standard solution of sodium hydroxide titration, when approaching terminal, add the phenolphthalein indicator of 5 1%, continue to be titrated to the rose pink terminal that is.In company with sample, doing blank test compares, calculates.
embodiment 2
A, dissolving: ferrosilicon sample 0.1200g to be cleared up is placed in to tygon and clears up bottle, add successively 11ml red fuming nitric acid (RFNA), 6ml hydrofluorite, with being about to clear up a bottle airtight and shake gently; Sample will be cleared up bottle and be placed in electric jacket after dissolving, at 55 ℃, heat 6min, then sample solution will be cooled to 20 ℃ with cooling bath.
B, precipitation: after the sample solution in steps A is cooling, add successively the urea liquid of 6ml 5%, potassium fluoride solution and the 3g potassium nitrate of 11ml 15%, after airtight shaking up, with the cooling 18min of cooling bath.
C, filtration: sample solution cooling in step B is filtered in teflon sample bottle with quantitative filter paper, and wash and clear up bottle and precipitate each four times with the Klorvess Liquid of 11ml 15%, to precipitate and filter paper moves in teflon sample bottle, potassium chloride-the ethanolic solution that adds 18ml 5%, obtains testing sample solution.
D, detection: in testing sample solution, drip the phenolphthalein indicator of 5 1%, with sour with remnants in 4% sodium hydroxide solution, filter paper is mashed, carefully clean wall of cup surrounding, be neutralized to and occur pink.Then add 200ml boiling water, use at once standard solution of sodium hydroxide titration, when approaching terminal, add the phenolphthalein indicator of 5 1%, continue to be titrated to the rose pink terminal that is.In company with sample, doing blank test compares, calculates.
embodiment 3
A, dissolving: ferrosilicon sample 0.0800g to be cleared up is placed in to teflon and clears up bottle, add successively 9ml red fuming nitric acid (RFNA), 4ml hydrofluorite, with being about to clear up a bottle airtight and shake gently; Sample will be cleared up bottle and be placed in microwave dissolver after dissolving, at 65 ℃, heat 4min, then sample solution flowing water will be cooled to 25 ℃.
B, precipitation: after the sample solution in steps A is cooling, add successively the urea liquid of 4ml 5%, potassium fluoride solution and the 2g potassium nitrate of 9ml 15%, after airtight shaking up, the cooling 12min of flowing water.
C, filtration: sample solution cooling in step B is filtered in polytetrafluoroethylene beaker with quantitative filter paper, and wash and clear up bottle and precipitate each twice with the Klorvess Liquid of 9ml 15%, to precipitate and filter paper moves in polytetrafluoroethylene beaker, potassium chloride-the ethanolic solution that adds 12ml 5%, obtains testing sample solution.
D, detection: in testing sample solution, drip the phenolphthalein indicator of 5 1%, with sour with remnants in 4% sodium hydroxide solution, filter paper is mashed, carefully clean wall of cup surrounding, be neutralized to and occur pink.Then add 200ml boiling water, use at once standard solution of sodium hydroxide titration, when approaching terminal, add the phenolphthalein indicator of 5 1%, continue to be titrated to the rose pink terminal that is.In company with sample, doing blank test compares, calculates.
Claims (9)
1. quick and precisely, a reliable and stable ferrosilicon sample digestion method, it is characterized in that comprising dissolving, precipitation and filter progress, specifically comprise:
A, dissolving: ferrosilicon sample 0.0800 ~ 0.1200g to be cleared up is placed in to plastics and clears up bottle, add successively 9 ~ 11ml nitric acid, 4 ~ 6ml hydrofluorite, airtight with being about to clear up bottle; Sample will be cleared up bottle and be placed in well heater after dissolving, at 55 ~ 65 ℃, heat 4 ~ 6min, then sample solution will be cooled to 20 ~ 25 ℃;
B, precipitation: after the sample solution in steps A is cooling, add successively 4 ~ 6ml urea liquid, 9 ~ 11ml potassium fluoride solution and 2 ~ 3g potassium nitrate, after airtight shaking up, cooling 12 ~ 18min;
C, filtration: sample solution cooling in step B is filtered in plastic sample bottle with filter material, and wash and clear up bottle and precipitation with 9 ~ 11ml Klorvess Liquid, to precipitate and filter material moves in plastic sample bottle, add 12 ~ 18ml potassium chloride-ethanolic solution, obtain testing sample solution.
As claimed in claim 1 quick and precisely, reliable and stable ferrosilicon sample digestion method, it is characterized in that it can be any in polyethylene bottle or teflon bottle that described plastics are cleared up bottle.
As claimed in claim 1 quick and precisely, reliable and stable ferrosilicon sample digestion method, the density that it is characterized in that described nitric acid is 1.42g/ml, the density of described hydrofluorite is 1.15g/ml.
As claimed in claim 1 quick and precisely, reliable and stable ferrosilicon sample digestion method, it is characterized in that described well heater can be any in water-bath, electric jacket, insulation can or microwave generator.
As claimed in claim 1 quick and precisely, reliable and stable ferrosilicon sample digestion method, the concentration that it is characterized in that described urea liquid is 5%, the concentration of described potassium fluoride solution is 15%.
As claimed in claim 1 quick and precisely, reliable and stable ferrosilicon sample digestion method, it is characterized in that described filter material is quantitative filter paper.
As claimed in claim 1 quick and precisely, reliable and stable ferrosilicon sample digestion method, it is characterized in that described plastic sample bottle is teflon bottle.
As claimed in claim 1 quick and precisely, reliable and stable ferrosilicon sample digestion method, it is characterized in that describedly with Klorvess Liquid washing, clearing up bottle and precipitation, refer to and clear up bottle and precipitate each 2 ~ 4 times with Klorvess Liquid washing.
As claimed in claim 1 quick and precisely, reliable and stable ferrosilicon sample digestion method, the concentration that it is characterized in that described Klorvess Liquid is 4 ~ 6%, the concentration of described potassium chloride-ethanolic solution is 4 ~ 6%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104502179A (en) * | 2014-12-01 | 2015-04-08 | 武钢集团昆明钢铁股份有限公司 | Test sample treatment method for simultaneously measuring content of silicon and phosphor in silicon-manganese alloy by ICP |
| CN105986137B (en) * | 2016-06-15 | 2018-08-14 | 贵州铝城铝业原材料研究发展有限公司 | A kind of technique and intermediate producing alloy aluminum |
| 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 |
| CN113866254A (en) * | 2021-09-14 | 2021-12-31 | 河南省地质矿产勘查开发局第一地质矿产调查院 | Method for determining silicon content in plant-derived primary agricultural product, microwave digestion solution and application thereof |
| CN114720627A (en) * | 2022-04-06 | 2022-07-08 | 江苏南大光电材料股份有限公司 | Method for detecting relative content of halogen in silicon precursor by titration |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104502179A (en) * | 2014-12-01 | 2015-04-08 | 武钢集团昆明钢铁股份有限公司 | Test sample treatment method for simultaneously measuring content of silicon and phosphor in silicon-manganese alloy by ICP |
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| 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 |
| CN113866254A (en) * | 2021-09-14 | 2021-12-31 | 河南省地质矿产勘查开发局第一地质矿产调查院 | Method for determining silicon content in plant-derived primary agricultural product, microwave digestion solution and application thereof |
| CN114720627A (en) * | 2022-04-06 | 2022-07-08 | 江苏南大光电材料股份有限公司 | Method for detecting relative content of halogen in silicon precursor by titration |
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Application publication date: 20140423 |