CN104849267A - Method for determining content of silicon in fluosilicic acid volumetric method - Google Patents
Method for determining content of silicon in fluosilicic acid volumetric method Download PDFInfo
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- CN104849267A CN104849267A CN201510234698.8A CN201510234698A CN104849267A CN 104849267 A CN104849267 A CN 104849267A CN 201510234698 A CN201510234698 A CN 201510234698A CN 104849267 A CN104849267 A CN 104849267A
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- mixed solution
- silicon
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000002253 acid Substances 0.000 title claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 13
- 239000010703 silicon Substances 0.000 title claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 16
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000835 fiber Substances 0.000 claims abstract description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- 239000001103 potassium chloride Substances 0.000 claims abstract description 8
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 8
- 238000004448 titration Methods 0.000 claims abstract description 7
- 235000003270 potassium fluoride Nutrition 0.000 claims abstract description 6
- 239000011698 potassium fluoride Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical class [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 4
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 10
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 238000004364 calculation method Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 11
- 239000000243 solution Substances 0.000 abstract description 4
- 239000011259 mixed solution Substances 0.000 abstract 6
- 238000001816 cooling Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000000207 volumetry Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for determining content of silicon in a fluosilicic acid volumetric method. The method comprises the following steps: step 1: dissolving a sample; step 2: adding 40ml to 50ml of a mixed solution of nitric acid and hydrochloric acid, wherein the mixed solution comprises 60 percent by weight of nitric acid, 5 percent by weight of hydrochloric acid and the balance of water, and cooling the mixed solution to the room temperature; step 3: adding potassium chloride until the potassium chloride is saturated, adding 10ml of potassium fluoride with 20% concentration and 0.1g of polytetrafluoroethylene fibers, slightly stirring, and then standing the mixed solution for 5 to 8 minutes, wherein the diameter of each polytetrafluoroethylene fiber is 1 to 5 filaments; step 4: adding the mixed solution into a 100ml centrifugal bottle, centrifuging the mixed solution for 1 minute at a speed of 10000 turns per minute in a centrifugal machine, removing liquid supernatant, washing solids by utilizing a saturated potassium nitrate solution, then dissolving the solids by utilizing boiled water which is neutralized, carrying out the titration by utilizing NaOH, and calculating the content of silicon according to the consumption of sodium hydroxide. The invention aims at providing the method capable of accurately measuring the content of silicon in the fluosilicic acid volumetric method.
Description
Technical field
The present invention relates to detection field, particularly a kind of method of hydrofluosilicic acid volumetric determination silicone content.
Background technology
In glass, the mensuration of the content of silicon adopts hydrofluosilicic acid volumetric determination mostly, the method mainly utilizes the potassium fluosilicate feature that solubleness is extremely low in the aqueous solution of normal temperature, react with potassium fluoride the precipitation generating potassium fluosilicate after silicon in glass being converted to hydrofluosilicic acid, then make potassium fluosilicate precipitate hydrolysis and measure the amount that hydrofluoric content obtains silicon, said method Problems existing is potassium fluosilicate is cotton-shaped, adopt the method duration filtered, adopt centrifugal method centrifuging not thorough.
Summary of the invention
The object of the present invention is to provide a kind of can the method for hydrofluosilicic acid volumetric determination silicone content of Measurement accuracy.
Technical scheme of the present invention is: a kind of method of hydrofluosilicic acid volumetric determination silicone content, comprises the following steps:
Step 1: sample dissolution; What take 0.1g is crushed to the siliceous sample of 500 object, adds 1.5-2.5g NaOH, is heated to 600-650 DEG C of melting 15-20 minute;
Step 2: the mixed liquor adding 40ml-50ml nitric acid and hydrochloric acid, the water wherein containing the nitric acid of 60wt%, the hydrochloric acid of 5wt% and surplus in mixed liquor, is cooled to room temperature;
Step 3: add potassium chloride until potassium chloride is saturated, adds potassium fluoride and 0.1g polytetrafluoroethylene fibre that 10ml concentration is 20wt%, slightly mixes rear standing 5-8 minute; The diameter of described polytetrafluoroethylene fibre is 1-5 silk;
Step 4: be added in the centrifugal bottle of 100ml, in centrifuges with the centrifugation 1 minute of 10000 revs/min, abandoning supernatant, by solid first with after the washing of saturated potassium nitrate solution, then dissolve with being neutralized to neutral boiling water, use NaOH titration, according to the amount of the Dosage calculation silicon of NaOH.
In the method for above-mentioned hydrofluosilicic acid volumetric determination silicone content, in described step 4, the volume of boiling water is 200-250ml, and the indicator of described titration operation is phenolphthalein.
Beneficial effect of the present invention is as follows:
The present invention adopts the content of silicon in hydrofluosilicic acid volumetric determination sample, wherein adopts polytetrafluoroethylene fibre to join in solution centrifugal, facilitate the precipitation of cotton-shaped potassium fluosilicate, and its deposition efficiency is high, equal with traditional filtration method measuring accuracy.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in further detail, but does not form any limitation of the invention.
Embodiment 1
A method for hydrofluosilicic acid volumetric determination silicone content, comprises the following steps:
Step 1: sample dissolution; What take 0.1g is crushed to 500 object simple glasses, adds 1.5-2.5g NaOH, is heated to 600-650 DEG C of melting 15-20 minute;
Step 2: the mixed liquor adding 40ml-50ml nitric acid and hydrochloric acid, the water wherein containing the nitric acid of 60wt%, the hydrochloric acid of 5wt% and surplus in mixed liquor, is cooled to room temperature;
Step 3: add potassium chloride until potassium chloride is saturated, adds potassium fluoride and 0.1g polytetrafluoroethylene fibre that 10ml concentration is 20wt%, slightly mixes rear standing 5-8 minute; The diameter of described polytetrafluoroethylene fibre is 1-5 silk;
Step 4: be added in the centrifugal bottle of 100ml, in centrifuges with the centrifugation 1 minute of 10000 revs/min, abandoning supernatant, by solid first with after the washing of saturated potassium nitrate solution, then dissolve with being neutralized to neutral 230ml boiling water, with the NaOH titration of 0.15mol/L, the indicator of described titration operation is phenolphthalein, according to the amount of the Dosage calculation silicon of NaOH.
Adopt the simple glass of same batch, replicate determination 10 times, the silicone content in the simple glass of this batch is 72.5wt%.
Comparative example 1
Adopt the method that scientific and technical literature " glass " the 7th phase in the 2010th total 226th phase " potassium fluoride volumetry surveys silicon error analysis and countermeasure " records, the silicone content of the simple glass of test and embodiment 1 same batch, the mean value of the silicon measured is 72.4w%, the method used time in filter process is longer, general needs 30 minutes to 1 hour, because flocculent deposit easily blocks filter paper hole, filtration time is extended.
Above-describedly be only preferred embodiment of the present invention, all do within the scope of the spirit and principles in the present invention any amendment, equivalently to replace and improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. a method for hydrofluosilicic acid volumetric determination silicone content, is characterized in that, comprises the following steps:
Step 1: sample dissolution; What take 0.1g is crushed to the siliceous sample of 500 object, adds 1.5-2.5g NaOH, is heated to 600-650 DEG C of melting 15-20 minute;
Step 2: the mixed liquor adding 40ml-50ml nitric acid and hydrochloric acid, the water wherein containing the nitric acid of 60wt%, the hydrochloric acid of 5wt% and surplus in mixed liquor, is cooled to room temperature;
Step 3: add potassium chloride until potassium chloride is saturated, adds potassium fluoride and 0.1g polytetrafluoroethylene fibre that 10ml concentration is 20wt%, slightly mixes rear standing 5-8 minute; The diameter of described polytetrafluoroethylene fibre is 1-5 silk;
Step 4: be added in the centrifugal bottle of 100ml, in centrifuges with the centrifugation 1 minute of 10000 revs/min, abandoning supernatant, by solid first with after the washing of saturated potassium nitrate solution, then dissolve with being neutralized to neutral boiling water, use NaOH titration, according to the amount of the Dosage calculation silicon of NaOH.
2. the method for hydrofluosilicic acid volumetric determination silicone content according to claim 1, is characterized in that, in described step 4, the volume of boiling water is 200-250ml, and the indicator of described titration operation is phenolphthalein.
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| CN201510234698.8A CN104849267B (en) | 2015-05-11 | 2015-05-11 | The method of fluosilicic acid volumetric determination silicone content |
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| CN201510234698.8A CN104849267B (en) | 2015-05-11 | 2015-05-11 | The method of fluosilicic acid volumetric determination silicone content |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105158406A (en) * | 2015-08-31 | 2015-12-16 | 内蒙古包钢钢联股份有限公司 | Method for measuring silica content in ferromanganese iron by utilizing potassium fluosilicate volumetric method |
| CN105588833A (en) * | 2015-12-17 | 2016-05-18 | 吴志强 | Method for detecting silicon dioxide in silica sand through potassium fluosilicate volumetric method |
| 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 |
| CN109030711A (en) * | 2018-06-28 | 2018-12-18 | 四川龙蟒钛业股份有限公司 | The measuring method of silicon in a kind of Phosphorus Slag |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103159218A (en) * | 2011-12-14 | 2013-06-19 | 常熟市新华化工有限公司 | Production method of potassium fluosilicate |
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2015
- 2015-05-11 CN CN201510234698.8A patent/CN104849267B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103159218A (en) * | 2011-12-14 | 2013-06-19 | 常熟市新华化工有限公司 | Production method of potassium fluosilicate |
Non-Patent Citations (4)
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| 唐锦坤等: "AV絮凝剂沉淀法测定硅锰合金中硅", 《大众科技》 * |
| 王贤: "氟硅酸钾容量法测硅误差分析及对策", 《玻璃》 * |
| 聂淑兰: "氟硅酸钾容量法测定硅石中二氧化硅的含量", 《铁合金》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105158406A (en) * | 2015-08-31 | 2015-12-16 | 内蒙古包钢钢联股份有限公司 | Method for measuring silica content in ferromanganese iron by utilizing potassium fluosilicate volumetric method |
| CN105588833A (en) * | 2015-12-17 | 2016-05-18 | 吴志强 | Method for detecting silicon dioxide in silica sand through potassium fluosilicate volumetric method |
| 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 |
| 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 |
| CN109030711A (en) * | 2018-06-28 | 2018-12-18 | 四川龙蟒钛业股份有限公司 | The measuring method of silicon in a kind of Phosphorus Slag |
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| CN104849267B (en) | 2017-10-24 |
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Application publication date: 20150819 Assignee: RONGXIAN RUNDA FURNITURE CO.,LTD. Assignor: WUZHOU CITY PRODUCT QUALITY INSPECTION Contract record no.: X2023980045114 Denomination of invention: Method for determining silicon content using fluorosilicic acid volumetric method Granted publication date: 20171024 License type: Common License Record date: 20231031 |