CN101397126A - Method for preparing primary standard reagent potash iodate - Google Patents
Method for preparing primary standard reagent potash iodate Download PDFInfo
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- CN101397126A CN101397126A CNA2007100612811A CN200710061281A CN101397126A CN 101397126 A CN101397126 A CN 101397126A CN A2007100612811 A CNA2007100612811 A CN A2007100612811A CN 200710061281 A CN200710061281 A CN 200710061281A CN 101397126 A CN101397126 A CN 101397126A
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Abstract
The invention relates to a method for preparing standard reagent of potassium iodate, comprising the preparation steps as follows: (1) industrial potassium iodate is dissolved in deioned water and heated till being dissolved; potassium carbonate is then added in the solution; the solution is then mixed and reacts for 0.5-1.5 hours; subsequently, the temperature is kept for 1.5-2.5 hours; (2) hydrogen peroxide is added in the solution, the temperature is kept for 0.5-1.5 hours and the solution is filtrated subsequently; (3) pH value is adjusted to 5.5-6.5 by using potassium acid iodate; (4) pH value of the filtrated solution is adjusted to 4-5 by iodic acid and the solution reacts for 1.5-2.5 hours; (5) the filtrated solution is kept still and the temperature is kept; the filtrated solution is filtrated by active carbon and statically arranged and the crystal is suction-filtrated, washed by water and dehydrated by a dehydration machine; the dehydrated crystal is arranged in a drying box and dried and parched with the constant temperature of 90-110 DEG C for 7-9 hours, thus obtaining the standard reagent of potassium iodate. The preparation method can thoroughly remove the impurity metal element, effectively improves the purity of the product, and improves the content under a condition that the clarity is ensured to be qualified, with the content reaching 99.95-100.05%.
Description
Technical field
The invention belongs to the chemical reagent field, especially a kind of preparation method of primary standard reagent potash iodate.
Background technology
Potassium Iodate is applied in as standard reagent in the chemical analytical standard solution of all trades and professions, uses very extensive.Potassium Iodate as standard reagent is preparation so at present: industrial Potassium Iodate is dissolved in the deionized water, uses activated carbon filtration, and content is generally on the low side, does not reach 99.95%-100.05%, thereby has influenced the precise results of analyzing other standardized solution.And our preparation method to be industrial Potassium Iodate be dissolved in the deionized water, solution is transferred to alkalescence with potassium hydroxide, add salt of wormwood again to form carbonate deposition, remove impurity metallic elements, again with the potassium acid iodate neutralization, add acid iodide again to improve the content of Potassium Iodate.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, the preparation method of the higher primary standard reagent potash iodate of a kind of Potassium Iodate content is provided.
The technical scheme that the present invention takes is:
A kind of preparation method of primary standard reagent potash iodate, the step of its preparation method is:
(1). industrial Potassium Iodate is dissolved in the deionized water, is heated to dissolving, transferring the Ph value with potassium hydroxide then is 8.5～9.5, adds salt of wormwood again, stirring reaction, temperature of reaction are 75～85 ℃, and the reaction times is 0.5～1.5 hour, be incubated 1.5～2.5 hours then, the impurity metallic elements that settles out filters;
(2). add hydrogen peroxide in above-mentioned filtrate, its addition is so that ferrous ion is oxidized to high ferro promptly hydrolysis reaction takes place and be precipitated out to be as the criterion, and is incubated 0.5～1.5 hour after-filtration;
(3). use in the potassium acid iodate and above-mentioned filtrate, transferring the Ph value is 5.5～6.5;
(4). transferring the Ph value of filtrate with acid iodide is 4～5, in temperature is to react 1.5～2.5 hours under 85～95 ℃ the temperature condition;
(5). with the static insulation of filtrate 1.5～2.5 hours, use activated carbon filtration, static 18～20 hours, the crystallization that suction strainer is separated out, and wash with water, dewater with water extracter, loft drier freeze-day with constant temperature, oven dry are put in crystallization after the dehydration, bake out temperature is 90～110 ℃, and drying time is 7～9 hours, promptly gets the primary standard reagent potash iodate finished product.
And described industrial Potassium Iodate is 125:1 with the weight ratio of the salt of wormwood that is added.
Advantage of the present invention and positively effect are:
1. the present invention is transferred to alkalescence to industrial potassium iodate solution with potassium hydroxide, adds salt of wormwood again and forms carbonate deposition, uses activated carbon filtration again, removes impurity metallic elements so completely, can effectively improve the purity of product.
2. the present invention adds in the potassium acid iodate and basic solution, adds an amount of acid iodide again, guaranteeing to improve content under the qualified prerequisite of clarity, reaches 99.95-100.05%.
Embodiment
Below in conjunction with embodiment technology contents of the present invention is described further; Following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1:
A kind of preparation method of primary standard reagent potash iodate the steps include:
(1). 25 kilograms of industrial Potassium Iodates are dissolved in the 125L deionized water, are heated to dissolving, transferring the Ph value with potassium hydroxide is 9; Add 200g salt of wormwood again, stirring reaction, temperature of reaction is 80 ℃, and the reaction times is 1 hour, is incubated 2 hours, and the impurity such as metallic element Ca, Mg that settle out filter.
(2). in filtrate, add a little hydrogen peroxide, ferrous ion is oxidized to high ferro promptly hydrolysis reaction takes place and be precipitated out, be incubated 1 hour after-filtration.
(3). use in the potassium acid iodate and above filtrate, transferring the Ph value is 6.
(4). transferring solution Ph value with acid iodide again is 4.5, and temperature of reaction is 90 ℃, and the reaction times is 2 hours.
(5). static insulation 2 hours, use activated carbon filtration, static 20 hours, the crystallization that suction strainer is separated out, and use the 10L cold water washing, with the water extracter dehydration, loft drier freeze-day with constant temperature, oven dry are put in the crystallization after the dehydration, temperature is 100 ℃, and drying time is 8 hours, promptly gets the primary standard reagent potash iodate finished product.
Embodiment 2:
A kind of preparation method of primary standard reagent potash iodate the steps include:
(1). 50 kilograms of industrial Potassium Iodates are dissolved in the 250L deionized water, are heated to dissolving, transferring the Ph value with potassium hydroxide is 9; Add 400g salt of wormwood again, stirring reaction, temperature of reaction is 85 ℃, and the reaction times is 0.5 hour, is incubated 2 hours, and the metallic element that settles out filters.
(2). in filtrate, add a little hydrogen peroxide, ferrous ion is oxidized to high ferro promptly hydrolysis reaction takes place and be precipitated out, be incubated 1.5 hours after-filtration.
(3). use in the potassium acid iodate and above filtrate, transferring the Ph value is 6.
(4). transferring solution Ph value with acid iodide again is 4, and temperature of reaction is 95 ℃, and the reaction times is 1.5 hours.
(5). static insulation 2.5 hours, use activated carbon filtration, static 18 hours, the crystallization that suction strainer is separated out, and use the 20L cold water washing, dewater with water extracter, loft drier freeze-day with constant temperature, oven dry are put in crystallization after the dehydration, temperature is 90 ℃, and drying time is 9 hours, promptly gets the primary standard reagent potash iodate finished product.
By experiment, obtain a result as follows:
Acidity (Ph) content (%) clarity
1 100 muddinesses
4 99.98 No. 4
4.5 99.95 No. 2
More than experiment shows, it is 4.5 to be the best that acid iodide is transferred Ph value.
Claims (2)
1. the preparation method of a primary standard reagent potash iodate is characterized in that:
The step of its preparation method is:
(1). industrial Potassium Iodate is dissolved in the deionized water, is heated to dissolving, transferring the Ph value with potassium hydroxide then is 8.5～9.5, adds salt of wormwood again, stirring reaction, temperature of reaction are 75～85 ℃, and the reaction times is 0.5～1.5 hour, be incubated 1.5～2.5 hours then, the impurity metallic elements that settles out filters;
(2). add hydrogen peroxide in above-mentioned filtrate, its addition is so that ferrous ion is oxidized to high ferro promptly hydrolysis reaction takes place and be precipitated out to be as the criterion, and is incubated 0.5～1.5 hour after-filtration;
(3). use in the potassium acid iodate and above-mentioned filtrate, transferring the Ph value is 5.5～6.5;
(4). transferring the Ph value of filtrate with acid iodide is 4～5, in temperature is to react 1.5～2.5 hours under 85～95 ℃ the temperature condition;
(5). with the static insulation of filtrate 1.5～2.5 hours, use activated carbon filtration, static 18～20 hours, the crystallization that suction strainer is separated out, and wash with water, dewater with water extracter, loft drier freeze-day with constant temperature, oven dry are put in crystallization after the dehydration, bake out temperature is 90～110 ℃, and drying time is 7～9 hours, promptly gets the primary standard reagent potash iodate finished product.
2. the preparation method of primary standard reagent potash iodate according to claim 1 is characterized in that: described industrial Potassium Iodate is 125:1 with the weight ratio of the salt of wormwood that is added.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100612811A CN101397126B (en) | 2007-09-28 | 2007-09-28 | Method for preparing primary standard reagent potash iodate |
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| CN2007100612811A CN101397126B (en) | 2007-09-28 | 2007-09-28 | Method for preparing primary standard reagent potash iodate |
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| CN101397126A true CN101397126A (en) | 2009-04-01 |
| CN101397126B CN101397126B (en) | 2012-01-25 |
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| CN2007100612811A Expired - Fee Related CN101397126B (en) | 2007-09-28 | 2007-09-28 | Method for preparing primary standard reagent potash iodate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583252A (en) * | 2012-04-10 | 2012-07-18 | 自贡市金典化工有限公司 | Method for producing sodium periodate |
| CN108593838A (en) * | 2018-03-26 | 2018-09-28 | 河北省农林科学院农业资源环境研究所 | It is a kind of to titrate the primary standard substance for absorbing the ammonium salt in boric acid solution |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034410C (en) * | 1994-09-03 | 1997-04-02 | 连云港市化工研究所 | Industrial method for preparation of pure iodic acid solution and its salts |
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2007
- 2007-09-28 CN CN2007100612811A patent/CN101397126B/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583252A (en) * | 2012-04-10 | 2012-07-18 | 自贡市金典化工有限公司 | Method for producing sodium periodate |
| CN108593838A (en) * | 2018-03-26 | 2018-09-28 | 河北省农林科学院农业资源环境研究所 | It is a kind of to titrate the primary standard substance for absorbing the ammonium salt in boric acid solution |
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| CN101397126B (en) | 2012-01-25 |
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Assignee: TIANJIN KERMEL CHEMICAL REAGENT Co.,Ltd. Assignor: Tianjin Chemical Reagent Research Institute Contract record no.: 2012120000027 Denomination of invention: Method for preparing primary standard reagent potash iodate Granted publication date: 20120125 License type: Exclusive License Open date: 20090401 Record date: 20120509 |
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Address after: 300240 Tianjin Admiralty street Dongli District Xu Zhuangzi Patentee after: TIANJIN CHEMICAL REAGENT RESEARCH INSTITUTE Co.,Ltd. Address before: 300240 Xu Zhuangzi, Dongli District, Tianjin Patentee before: Tianjin Chemical Reagent Research Institute |
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Application publication date: 20090401 Assignee: TIANJIN KERMEL CHEMICAL REAGENT Co.,Ltd. Assignor: Tianjin Chemical Reagent Research Institute Contract record no.: 2012120000027 Denomination of invention: Method for preparing primary standard reagent potash iodate Granted publication date: 20120125 License type: Exclusive License Record date: 20120509 |
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