CN103048318A - Rapid quantitative detection method for determining iodine content in well and rock salt - Google Patents
Rapid quantitative detection method for determining iodine content in well and rock salt Download PDFInfo
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- CN103048318A CN103048318A CN2012105587662A CN201210558766A CN103048318A CN 103048318 A CN103048318 A CN 103048318A CN 2012105587662 A CN2012105587662 A CN 2012105587662A CN 201210558766 A CN201210558766 A CN 201210558766A CN 103048318 A CN103048318 A CN 103048318A
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- iodine
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- iodide
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Links
- 229910052740 iodine Inorganic materials 0.000 title claims abstract description 48
- 239000011630 iodine Substances 0.000 title claims abstract description 48
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000001514 detection method Methods 0.000 title claims abstract description 11
- 235000002639 sodium chloride Nutrition 0.000 title abstract description 38
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 title abstract description 11
- 239000011780 sodium chloride Substances 0.000 title abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 42
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 39
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229920002472 Starch Polymers 0.000 claims abstract description 18
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 18
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims abstract description 18
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 18
- 235000019698 starch Nutrition 0.000 claims abstract description 18
- 239000008107 starch Substances 0.000 claims abstract description 18
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 10
- 239000005708 Sodium hypochlorite Substances 0.000 claims abstract description 9
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229940006461 iodide ion Drugs 0.000 claims description 15
- 238000000691 measurement method Methods 0.000 claims description 14
- ICIWUVCWSCSTAQ-UHFFFAOYSA-M iodate Chemical compound [O-]I(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-M 0.000 claims description 12
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 claims description 12
- 229940005633 iodate ion Drugs 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 5
- 239000001230 potassium iodate Substances 0.000 abstract description 4
- 235000006666 potassium iodate Nutrition 0.000 abstract description 4
- 229940093930 potassium iodate Drugs 0.000 abstract description 4
- -1 iodine ions Chemical class 0.000 abstract 3
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 235000000396 iron Nutrition 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 42
- 239000012153 distilled water Substances 0.000 description 3
- 150000002496 iodine Chemical class 0.000 description 3
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010067997 Iodine deficiency Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 150000001875 compounds Chemical group 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 235000006479 iodine deficiency Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 230000009469 supplementation Effects 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 rapid quantitative detection method for determining iodine content in well salt. The method comprises the following steps: (1), an appropriate amount of iodized salt is weighted, placed in a bottle and dissolved in water; (2), an appropriate amount of phosphoric acid is added in the bottle first to provide an acidic condition, then an appropriate amount of sodium hypochlorite solution is added and mixed evenly to oxidize iodine ions into iodate ions, and then an appropriate amount of oxalic acid solution is added to remove the residual sodium hypochlorite after the reaction with iodide irons; (3), an appropriate amount of potassium iodide solution is added in the bottle to allow full reaction between potassium iodide and iodate ions; (4), the solution in the bottle is titrated with sodium thiosulfate solution until the color of the solution in the bottle turns to be faint yellow; (5), starch indicator solution is added in to the bottle and shook evenly and then the solution in the bottle is titrated with the sodium thiosulfate solution until the color of the solution in the bottle disappear; and (6), the iodine content of the iodized salt is worked out according to the consumption amount of the sodium thiosulfate solution. Therefore, the method provided by the invention can be used to quickly and accurately determine the total iodine content in the well and rock salt.
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 the well mine salt.
Background technology
Supplementation of iodine salt is the effective way of prevention and control of iodine deficient disease, and Iodine Salt Surveillance is the main work in the preventing and controlling.Daily frequent, a large amount of Iodine Salt Surveillances requirement detection method should be accurate simply again.Yet existing salt compounded of iodine quantitative detecting method is more loaded down with trivial details, detects sample length consuming time, and speed is slow, can not adapt to large sample amount and Site Detection requirements of one's work.
For this situation, the application's applicant had once 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 are disclosed in the front case, per hour can detect 60 samples, compare with current methods, reduced testing cost, saved detection time, can go out the result in the scene, be worthy to be popularized very much.
Yet China's iodizedsalt is different according to the crude salt place of production, is divided into sea lake salt, well mine salt etc., and the well mine salt that is usually produced from Sichuan is called " river salt ".Have reducing substances in the former halogen of river salt, so that the physical and chemical condition variation owing to weather separates Potassiumiodate in the salt compounded of iodine of processing, the considerable part Potassiumiodate consists of free-iodine.
These free-iodine can not reverse back Potassiumiodate, and still are present in the salt compounded of iodine with iodide ion or at different compound forms.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 of putting down in writing in the front case can not detect the total content of iodine in the well mine salt, can cause testing result and reality large deviation to occur, it is applied be subject to limitation.
For this reason, the application attempts to propose a kind of new detection method, addresses the above 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, makes it be applicable to the mensuration of content of iodine in the well mine salt.
For achieving the above object, the technical solution used in the present invention is:
The content of iodine fast quantitative measurement method for detecting is characterized in that in a kind of well mine salt, comprises following operation steps:
(1) takes by weighing an amount of salt compounded of iodine, place bottle, be dissolved in water;
(2) in described bottle, add first an amount of phosphoric acid solution mixing, so that acid condition to be provided; Add again an amount of liquor natrii hypochloritis's mixing, be used for iodide ion is oxidized to iodate ion; Then add an amount of oxalic acid solution, to eliminate and the rear remaining sodium hypochlorite of iodide ion reaction;
(3) in described bottle, add an amount of liquor kalii iodide, make described potassium iodide and iodate ion that fully reaction occur;
(4) use sodium thiosulfate solution titrated, solution is faint yellow in the extremely described bottle, and faint yellow showing has iodine molecule to separate out;
(5) add the starch indicator solution in described bottle, after shaking up, continue to use described sodium thiosulfate solution titrated, solution colour disappears just in the extremely described bottle;
(6) according to the concentration of hypo solution and the volume of consumption, converse the content of iodine in the salt compounded of iodine.
In the described well mine salt in the content of iodine fast quantitative measurement method for detecting: in the step (2), after adding oxalic acid solution, heating liquid to boiling in the described bottle is taken off immediately, then be cooled to room temperature.
In the described well mine salt in the content of iodine fast quantitative measurement method for detecting: in the step (3), after adding liquor kalii iodide, leave standstill a period of time.
In the described well mine salt in the content of iodine fast quantitative measurement method for detecting: employed reagent concentration is in the described detection method:
0.005mol/L hypo solution;
The 2mol/L sulfuric acid solution;
Mass percent concentration 2.5% liquor natrii hypochloritis;
0.24mol/L oxalic acid solution;
The 1mol/L phosphoric acid solution;
Mass percent concentration 10% liquor kalii iodide; And,
Mass percent concentration 1% starch indicator solution.
In the described well mine salt in the content of iodine fast quantitative measurement method for detecting: concrete operation step comprises:
(1) takes by weighing the 10.0g salt compounded of iodine, place the 150ml conical flask, add the water-soluble solution of 50ml;
(2) in described conical flask, add first the described 1mol/L phosphoric acid solution of 2ml mixing, so that acid condition to be provided; Add again the described 2.5% liquor natrii hypochloritis's mixing of 1ml, iodide ion is oxidized to iodate ion; Then add the described 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 described 10% liquor kalii iodide of 5ml, leave standstill a period of time, liquor kalii iodide and iodate ion are fully reacted;
(4) with described 0.005mol/L sodium thiosulfate solution titrated, extremely solution is faint yellow in the described conical flask;
(5) add the described 1% starch indicator solution of 2ml in described conical flask, after shaking up, continue with described 0.005mol/L sodium thiosulfate solution titrated, extremely solution colour disappears just in the described conical flask;
(6) write down sodium thiosulfate scale value in the buret, according to the volume that hypo solution consumes, converse the content of iodine of the salt compounded of iodine of surveying.
Compared with prior art, the beneficial effect that has of the present invention is: can measure the total content of iodine in the well mine salt quickly and accurately.
Embodiment
Principle of the present invention is under acid condition, use sodium hypochlorite that iodide ion is oxidized to iodate, use oxalic acid and remove superfluous sodium hypochlorite, with potassium iodide the iodate reduction is generated iodine again, 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 by weighing sodium thiosulfate (Na
2S
2O
35H
2O) 1.24g is dissolved in the 1L volumetric flask with deionized water, and is diluted to scale, places refrigerator to keep in Dark Place.
2mol/L sulfuric acid solution: lentamente the 5.56ml concentrated sulphuric acid is added approximately in the 90ml distilled water, be diluted to again 100ml.
Mass percent concentration 2.5% liquor natrii hypochloritis: with the 10%(Cl in (in the date of production) in the term
2) liquor natrii hypochloritis presses the 1:4(volume with deionized water) dilution gets final product.
0.24mol/L oxalic acid solution: take by weighing 15 gram 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 by weighing the pure potassium iodide 10g of top grade, use dissolved in distilled water in the 100ml volumetric flask, and be diluted to scale, put in the refrigerator and keep in Dark Place.
Mass percent concentration 1% starch indicator solution: take by weighing 1g sodium chloride, use dissolved in distilled water in the 100ml volumetric flask, and be diluted to scale, be prepared into sodium chloride solution.Take by weighing soluble starch lg and be placed in the l00ml beaker, adding distil water 10ml, fully dissolving is boiled in heating, and then adds the above-mentioned sodium chloride solution of 90ml, is prepared into the starch indicator solution.The described starch indicator solution time spent needs fresh preparation.
Content of iodine fast quantitative measurement method for detecting in the well mine salt provided by the invention comprises following operation steps:
1, takes by weighing the 10.0g salt compounded of iodine, place the 150ml conical flask, add the water-soluble solution of 50ml;
2, corresponding to above-mentioned formula (1) and (2), in described conical flask, add first the described 1mol/L phosphoric acid solution of 2ml mixing, so that acid condition to be provided; Add again the described 2.5% liquor natrii hypochloritis's mixing of 1ml, iodide ion is oxidized to iodate ion; Then add the described 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, corresponding to above-mentioned formula (3), in described conical flask, add described 10% liquor kalii iodide of 5ml, left standstill approximately 10 minutes, purpose is that liquor kalii iodide and iodate ion are fully reacted.
4, corresponding to above-mentioned formula (4), with described 0.005mol/L sodium thiosulfate solution titrated, extremely solution is faint yellow in the described conical flask.Faint yellow showing has iodine molecule to separate out, and at this moment just is fit to add 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), in described conical flask, add the described 1% starch indicator solution of 2ml, after shaking up, continue with described 0.005mol/L sodium thiosulfate solution titrated, extremely solution colour disappears just in the described conical flask.Because it is blue that iodine and starch reaction can become, starch is titration endpoint indicator.When blueness disappears, show the arrival titration end-point.
6, write down sodium thiosulfate scale value in the buret, the volume according to hypo solution consumes checks in content of iodine from the Iodine concentration in salt table of comparisons (lower attached).
As seen, use method provided by the present invention, can measure the true content of iodine in the well mine salt quickly and accurately.
The Iodine concentration in salt table of comparisons.
Claims (5)
1. content of iodine fast quantitative measurement method for detecting in the well mine salt is characterized in that, comprises following operation steps:
(1) takes by weighing an amount of salt compounded of iodine, place bottle, be dissolved in water;
(2) in described bottle, add first an amount of phosphoric acid solution mixing, so that acid condition to be provided; Add again an amount of liquor natrii hypochloritis's mixing, be used for iodide ion is oxidized to iodate ion; Then add an amount of oxalic acid solution, to eliminate and the rear remaining sodium hypochlorite of iodide ion reaction;
(3) in described bottle, add an amount of liquor kalii iodide, make described potassium iodide and iodate ion that fully reaction occur;
(4) use sodium thiosulfate solution titrated, solution is faint yellow in the extremely described bottle, and faint yellow showing has iodine molecule to separate out;
(5) add the starch indicator solution in described bottle, after shaking up, continue to use described sodium thiosulfate solution titrated, solution colour disappears just in the extremely described bottle;
(6) according to the concentration of hypo solution and the volume of consumption, converse the content of iodine in the salt compounded of iodine.
2. content of iodine fast quantitative measurement method for detecting in the well mine salt according to claim 1 is characterized in that: in the step (2), after adding oxalic acid solution, heating liquid to boiling in the described bottle is taken off immediately, then be cooled to room temperature.
3. content of iodine fast quantitative measurement method for detecting in the well mine salt according to claim 1 is characterized in that: in the step (3), after adding liquor kalii iodide, leave standstill a period of time.
4. content of iodine fast quantitative measurement method for detecting in the well mine salt according to claim 1, it is characterized in that: employed reagent concentration is in the described detection method:
0.005mol/L hypo solution;
The 2mol/L sulfuric acid solution;
Mass percent concentration 2.5% liquor natrii hypochloritis;
0.24mol/L oxalic acid solution;
The 1mol/L phosphoric acid solution;
Mass percent concentration 10% liquor kalii iodide; And,
Mass percent concentration 1% starch indicator solution.
5. content of iodine fast quantitative measurement method for detecting in the well mine salt according to claim 4, it is characterized in that: concrete operation step comprises:
(1) takes by weighing the 10.0g salt compounded of iodine, place the 150ml conical flask, add the water-soluble solution of 50ml;
(2) in described conical flask, add first the described 1mol/L phosphoric acid solution of 2ml mixing, so that acid condition to be provided; Add again the described 2.5% liquor natrii hypochloritis's mixing of 1ml, iodide ion is oxidized to iodate ion; Then add the described 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 described 10% liquor kalii iodide of 5ml, leave standstill a period of time, liquor kalii iodide and iodate ion are fully reacted;
(4) with described 0.005mol/L sodium thiosulfate solution titrated, extremely solution is faint yellow in the described conical flask;
(5) add the described 1% starch indicator solution of 2ml in described conical flask, after shaking up, continue with described 0.005mol/L sodium thiosulfate solution titrated, extremely solution colour disappears just in the described conical flask;
(6) write down sodium thiosulfate scale value in the buret, according to the volume that hypo solution consumes, converse the content of iodine of described salt compounded of iodine.
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|---|---|---|---|
| CN201210558766.2A CN103048318B (en) | 2012-12-20 | 2012-12-20 | Content of iodine fast quantitative measurement method for detecting in well mine salt |
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Cited By (9)
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|---|---|---|---|---|
| CN103472057A (en) * | 2013-09-25 | 2013-12-25 | 哈尔滨医科大学 | Rapid iodized salt detection liquid |
| 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 |
| CN108645961A (en) * | 2018-08-09 | 2018-10-12 | 漳州傲农牧业科技有限公司 | A kind of method of content of iodine in measurement feedstuff |
| CN110044891A (en) * | 2019-05-13 | 2019-07-23 | 山东省食品药品检验研究院 | A kind of detection method of amino acid iodine content of iodine |
| CN110567948A (en) * | 2019-09-10 | 2019-12-13 | 张鹏 | Iodide ion detection kit |
| CN111175241A (en) * | 2020-03-09 | 2020-05-19 | 薛原 | 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 |
| CN115078628A (en) * | 2022-07-25 | 2022-09-20 | 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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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103472057A (en) * | 2013-09-25 | 2013-12-25 | 哈尔滨医科大学 | Rapid iodized salt detection liquid |
| 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 |
| CN108645961A (en) * | 2018-08-09 | 2018-10-12 | 漳州傲农牧业科技有限公司 | A kind of method of content of iodine in measurement feedstuff |
| CN110044891A (en) * | 2019-05-13 | 2019-07-23 | 山东省食品药品检验研究院 | A kind of detection method of amino acid iodine content of iodine |
| 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 |
| CN111175241A (en) * | 2020-03-09 | 2020-05-19 | 薛原 | High-precision urine iodine detection method |
| 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 |
| CN115078628A (en) * | 2022-07-25 | 2022-09-20 | 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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| CN103048318B (en) | 2015-08-26 |
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