CN103048318B - Content of iodine fast quantitative measurement method for detecting in well mine salt - Google Patents
Content of iodine fast quantitative measurement method for detecting in well mine salt Download PDFInfo
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- CN103048318B CN103048318B CN201210558766.2A CN201210558766A CN103048318B CN 103048318 B CN103048318 B CN 103048318B CN 201210558766 A CN201210558766 A CN 201210558766A CN 103048318 B CN103048318 B CN 103048318B
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Abstract
The present invention is content of iodine fast quantitative measurement method for detecting in a kind of well mine salt, comprising: (1) takes appropriate salt compounded of iodine, is placed in bottle, is dissolved in water; (2) in described bottle, the mixing of appropriate phosphoric acid solution is first added, to provide acid condition; Add appropriate liquor natrii hypochloritis mixing again, for iodide ion is oxidized to iodate ion; Then add appropriate oxalic acid solution, react rear remaining sodium hypochlorite to eliminate with iodide ion; (3) in described bottle, add appropriate liquor kalii iodide, make described potassium iodide and iodate ion occur fully to react; (4) by sodium thiosulfate solution titrated, to described bottle, solution is faint yellow; (5) in described bottle, add starch indicator solution, after shaking up, continue to use described sodium thiosulfate solution titrated, to described bottle, solution colour disappears just; (6) according to the consumption of hypo solution, the content of iodine in salt compounded of iodine is conversed.Therefore, the present invention can measure the total content of iodine in well mine salt quickly and accurately.
Description
Technical field
The present invention relates to a kind of salt iodine fast quantitative measurement method for detecting, be applicable to the fast quantitative analysis of content of iodine in well mine salt.
Background technology
Supplementation of iodine salt is the most effective way of prevention and control of iodine deficient disease, and Iodine Salt Surveillance is the main work in preventing and controlling.Frequent routine, a large amount of Iodine Salt Surveillances require that detection method should be accurate simply again.But existing salt compounded of iodine quantitative detecting method is more loaded down with trivial details, detect sample length consuming time, speed is slow, can not adapt to large sample amount and Site Detection requirements of one's work.
For this situation, the applicant of the application once have submitted application for a patent for invention to State Intellectual Property Office: CN201210180708.0(is called front case), a kind of salt iodine Quantitative detection device and detection method is disclosed in front case, per hourly detect 60 samples, compare with current methods, reduce testing cost, save detection time, result can be gone out in scene, highly promote.
But China's iodizedsalt is different according to the crude salt place of production, is divided into sea lake salt, well mine salt etc., usually the well mine salt that is produced from Sichuan is called " river salt ".There is reducing substances in the former halogen of river salt, make due to the physical and chemical condition change of weather, Potassiumiodate to be separated in the salt compounded of iodine processed, considerable part Potassiumiodate forms free-iodine.
These free-iodine can not reverse back Potassiumiodate, and are still present in salt compounded of iodine with iodide ion or at different compound form.These free-iodine do not affect edible, do not affect the I trophism of salt compounded of iodine and the control of IDD (Iodine deficiency disorders).
And the detection method recorded in front case, the total content of iodine in well mine salt can not be detected, testing result and reality can be caused to occur large deviation, make it apply and receive limitation.
For this reason, the application attempts to propose a kind of new detection method, solves the problem.
Summary of the invention
For the deficiencies in the prior art, the object of the invention is to: content of iodine fast quantitative measurement method for detecting in a kind of well mine salt is provided, make it be applicable to the mensuration of content of iodine in well mine salt.
For achieving the above object, the technical solution used in the present invention is:
Content of iodine fast quantitative measurement method for detecting in a kind of well mine salt, is characterized in that, comprise following operation steps:
(1) take appropriate salt compounded of iodine, be placed in bottle, be dissolved in water;
(2) in described bottle, the mixing of appropriate phosphoric acid solution is first added, to provide acid condition; Add appropriate liquor natrii hypochloritis mixing again, for iodide ion is oxidized to iodate ion; Then add appropriate oxalic acid solution, react rear remaining sodium hypochlorite to eliminate with iodide ion;
(3) in described bottle, add appropriate liquor kalii iodide, make described potassium iodide and iodate ion occur fully to react;
(4) by sodium thiosulfate solution titrated, to described bottle, solution is faint yellow, and faint yellow showing has iodine molecule to separate out;
(5) in described bottle, add starch indicator solution, after shaking up, continue to use described sodium thiosulfate solution titrated, to described bottle, solution colour disappears just;
(6) according to the concentration of hypo solution and the volume of consumption, the content of iodine in salt compounded of iodine is conversed.
In described well mine salt in content of iodine fast quantitative measurement method for detecting: in step (2), after adding oxalic acid solution, heating liquid in described bottle is taken off immediately to boiling, is then cooled to room temperature.
In described well mine salt in content of iodine fast quantitative measurement method for detecting: in step (3), after adding liquor kalii iodide, leave standstill a period of time.
In described well mine salt in content of iodine fast quantitative measurement method for detecting: the reagent concentration used in described detection method is:
0.005mol/L hypo solution;
2mol/L sulfuric acid solution;
Mass percent concentration 2.5% liquor natrii hypochloritis;
0.24mol/L oxalic acid solution;
1mol/L phosphoric acid solution;
Mass percent concentration 10% liquor kalii iodide; And,
Mass percent concentration 1% starch indicator solution.
In described well mine salt in content of iodine fast quantitative measurement method for detecting: concrete operation step comprises:
(1) take 10.0g salt compounded of iodine, be placed in 150ml conical flask, add the water-soluble solution of 50ml;
(2) in described conical flask, 1mol/L phosphoric acid solution mixing described in 2ml is first added, to provide acid condition; Add 2.5% liquor natrii hypochloritis's mixing described in 1ml again, iodide ion is oxidized to iodate ion; Then add 0.24mol/L oxalic acid solution described in 2ml, be heated to boiling and take off immediately, be cooled to room temperature, react remaining sodium hypochlorite to eliminate with iodide ion;
(3) in described conical flask, add 10% liquor kalii iodide described in 5ml, leave standstill a period of time, liquor kalii iodide and iodate ion are fully reacted;
(4) by described 0.005mol/L sodium thiosulfate solution titrated, to described conical flask, solution is faint yellow;
(5) in described conical flask, add 1% starch indicator solution described in 2ml, after shaking up, continue by described 0.005mol/L sodium thiosulfate solution titrated, to described conical flask, solution colour disappears just;
(6) write down sodium thiosulfate scale value in buret, according to the volume that hypo solution consumes, converse the content of iodine of surveyed salt compounded of iodine.
Compared with prior art, the beneficial effect that the present invention has is: can measure the total content of iodine in well mine salt quickly and accurately.
Embodiment
Principle of the present invention is in acid condition, use sodium hypochlorite that iodide ion is oxidized to iodate, the sodium hypochlorite that the removing of application oxalic acid is superfluous, then with potassium iodide, iodate reduction is generated iodine, make indicator with starch, use sodium thiosulfate titration determination content of iodine.Reaction equation is as follows:
3CIO
-+I
-→IO
- 3+3CI
-……（1）
H
2C
2O
4+CIO
-→CI
-+2CO
2+H
2O ……（2）
IO
- 3+5I
-+6H
+→3I
2+3H
2O ……（3）
2S
2O
3 2-+I
2→2I
-+S
4O
62
-……（4）
Reagent:
0.005mol/L hypo solution: accurately take sodium thiosulfate (Na
2s
2o
35H
2o) 1.24g, is dissolved in 1L volumetric flask with deionized water, and is diluted to scale, is placed in refrigerator and keeps in Dark Place.
2mol/L sulfuric acid solution: lentamente the 5.56ml concentrated sulphuric acid is added in about 90ml distilled water, then be diluted to 100ml.
Mass percent concentration 2.5% liquor natrii hypochloritis: by the 10%(Cl in (in the date of production) in the term
2) liquor natrii hypochloritis with deionized water by 1:4(volume) dilute.
0.24mol/L oxalic acid solution: take 15 grams of oxalic acid and add water and be settled to 500ml.
1mol/L phosphoric acid solution: measure 85% phosphoric acid 34ml, add water and be settled to 500ml.
Mass percent concentration 10% liquor kalii iodide: take the pure potassium iodide 10g of top grade, be dissolved in 100ml volumetric flask with distilled water, and be diluted to scale, put in refrigerator and keep in Dark Place.
Mass percent concentration 1% starch indicator solution: take 1g sodium chloride, be dissolved in 100ml volumetric flask with distilled water, and be diluted to scale, be prepared into sodium chloride solution.Taking soluble starch lg is placed in l00ml beaker, adding distil water 10ml, and heating is boiled and dissolved completely, and then adds the above-mentioned sodium chloride solution of 90ml, is prepared into starch indicator solution.The described starch indicator solution used time needs Fresh.
Content of iodine fast quantitative measurement method for detecting in well mine salt provided by the invention, comprises following operation steps:
1, take 10.0g salt compounded of iodine, be placed in 150ml conical flask, add the water-soluble solution of 50ml;
2, corresponding to above-mentioned formula (1) and (2), in described conical flask, 1mol/L phosphoric acid solution mixing described in 2ml is first added, to provide acid condition; Add 2.5% liquor natrii hypochloritis's mixing described in 1ml again, iodide ion is oxidized to iodate ion; Then add 0.24mol/L oxalic acid solution described in 2ml, be heated to boiling and take off immediately, be cooled to room temperature, react remaining sodium hypochlorite to eliminate with iodide ion;
3, corresponding to above-mentioned formula (3), add 10% liquor kalii iodide described in 5ml in described conical flask, leave standstill about 10 minutes, object is that liquor kalii iodide and iodate ion are fully reacted.
4, corresponding to above-mentioned formula (4), by described 0.005mol/L sodium thiosulfate solution titrated, to described conical flask, solution is faint yellow.Faint yellow showing has iodine molecule to separate out, and is at this moment just applicable to adding end point indicator starch; If not, if end point indicator starch adds too early, iodine can generate chelate with starch,
Affect endpoint, cause measurement result higher.
5, corresponding to above-mentioned formula (4), add 1% starch indicator solution described in 2ml in described conical flask, after shaking up, continue by described 0.005mol/L sodium thiosulfate solution titrated, to described conical flask, solution colour disappears just.Because iodine and starch reaction can become blue, starch is titration endpoint indicator.When blueness disappears, show to arrive titration end-point.
6, write down sodium thiosulfate scale value in buret, according to the volume that hypo solution consumes, from the Iodine concentration in salt table of comparisons (lower attached), check in content of iodine.
Visible, use method provided by the present invention, can measure the true content of iodine in well mine salt quickly and accurately.
The Iodine concentration in salt table of comparisons.
Claims (1)
1. a content of iodine fast quantitative measurement method for detecting in well mine salt, is characterized in that, comprises following operation steps:
(1) take 10.0g salt compounded of iodine, be placed in 150ml conical flask, add the water-soluble solution of 50ml;
(2) in described conical flask, the 1mol/L phosphoric acid solution mixing of 2ml is first added, to provide acid condition; Add 2.5% liquor natrii hypochloritis's mixing of 1ml again, iodide ion is oxidized to iodate ion; Then add the 0.24mol/L oxalic acid solution of 2ml, be heated to boiling and take off immediately, be cooled to room temperature, react remaining sodium hypochlorite to eliminate with iodide ion;
(3) in described conical flask, add 10% liquor kalii iodide of 5ml, leave standstill a period of time, liquor kalii iodide and iodate ion are fully reacted;
(4) use 0.005mol/L sodium thiosulfate solution titrated, to described conical flask, solution is faint yellow;
(5) in described conical flask, add the 1% starch indicator solution of 2ml, after shaking up, continue by described 0.005mol/L sodium thiosulfate solution titrated, to described conical flask, solution colour disappears just;
(6) write down sodium thiosulfate scale value in buret, according to the volume that hypo solution consumes, from the Iodine concentration in salt table of comparisons, check in the content of iodine of described salt compounded of iodine;
The described Iodine concentration in salt table of comparisons is as follows:
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103472057B (en) * | 2013-09-25 | 2015-11-25 | 哈尔滨医科大学 | A kind of salt compounded of iodine detects liquid fast |
| CN103592249A (en) * | 2013-11-11 | 2014-02-19 | 中国科学院青海盐湖研究所 | Method for determining iodate in salt |
| CN105301177A (en) * | 2015-11-19 | 2016-02-03 | 大连雅特盐业有限公司 | Alga delicious taste liquid iodine content examination method |
| CN108645961B (en) * | 2018-08-09 | 2021-05-11 | 漳州傲农牧业科技有限公司 | Method for measuring iodine content in feed raw materials |
| CN110044891B (en) * | 2019-05-13 | 2022-02-08 | 山东省食品药品检验研究院 | Method for detecting iodine content in amino acid iodized salt |
| CN110567948A (en) * | 2019-09-10 | 2019-12-13 | 张鹏 | Iodide ion detection kit |
| CN111175241B (en) * | 2020-03-09 | 2020-09-18 | 刘宇娜 | High-precision urine iodine detection method |
| CN113804820A (en) * | 2020-06-12 | 2021-12-17 | 天津科技大学 | Vision-based automatic measuring device and method for iodine content of salt |
| CN115078628B (en) * | 2022-07-25 | 2022-11-11 | 北京安图生物工程有限公司 | Method for detecting iodine content in amino acid iodized salt |
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Inventor after: Liu Ying Inventor after: Sun Dianjun Inventor after: Shen Hongmei Inventor after: Liu Shoujun Inventor after: Su Xiaohui Inventor after: Wei Honglian Inventor after: Sun Wei Inventor after: Meng Fangang Inventor after: Wang Dandan Inventor before: Liu Ying |
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