CN101571530A - Compound for ultraviolet-detecting anions containing sulfur by ion chromatography post-column derivatization - Google Patents
Compound for ultraviolet-detecting anions containing sulfur by ion chromatography post-column derivatization Download PDFInfo
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- CN101571530A CN101571530A CNA2009100971955A CN200910097195A CN101571530A CN 101571530 A CN101571530 A CN 101571530A CN A2009100971955 A CNA2009100971955 A CN A2009100971955A CN 200910097195 A CN200910097195 A CN 200910097195A CN 101571530 A CN101571530 A CN 101571530A
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- iodine
- containing sulfur
- anions containing
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Abstract
The invention relates to a compound for ultraviolet-detecting anions containing sulfur by ion chromatography post-column derivatization and provides a new method for detecting anions containing sulfur. The method comprises the following steps: anions reacts with acidized iodine solution after being separated by ion chromatography; the acidized iodine solution enters a knotted reaction tube after passing through a post-column derivative device and generates oxidation-reduction reaction with the anions which contains sulfur and also enters the knotted reaction tube after flowing out of chromatography; and finally three-valent iodide ions are generated and leading the three-valent iodide ions generated finally to have the strongest ultraviolet absorption peaks by adjusting the concentration and acidity of different iodine solutions, thus greatly improving the sensitivity of detection. The invention can be applied to aminated compounds for environmental monitoring, food safety, biological medicine, health and epidemic prevention and the like.
Description
Technical field
The invention provides a kind of new method of utilizing ion chromatograph-post-column derivation uv detection method to measure the anions containing sulfur compound, during mensuration the anions containing sulfur compound is passed through ion chromatographic separation, enter the woollen yarn knitting reaction tube by a three-way connection again, the liquid of deriving simultaneously also enters the woollen yarn knitting reaction tube by the post-column derivation device through three-way connection, anionic compound after the separation is instead given birth to reaction with the liquid of deriving, reactant detects with ultraviolet luminosity, and this method can be measured the negative ion with reductibility sulfur-bearing.
Background technology
At present, the detection method of anions containing sulfur compound has kapillary electricity pulpating method, pulse ampere method, high performance liquid chromatography, spectrophotometric method and the chromatography of ions etc.Have the anionic compound of reported in literature ion-chromatographic determination sulfur-bearing to have: chromatography of ions suppresses electricity and leads detection thiocyanate [1], ion exclusion chromatography Amperometric Detection Coupled sulphite [2], ion pair chromatogram ultraviolet detection thiosulfate, thiocyanate, polythionate plasma [3], on-line preconcentration chromatography of ions spectrophotometric method detects thiocyanate [4], chromatography of ions Indirect UV Detection sulphite [5] and the indirect iodine liquid of chromatography of ions ultraviolet detection sulfide, sulphite, thiosulfate and thiocyanate.But derive behind employing direct ion chromatogram-iodine fluid column ultraviolet detection sulfide, formaldehyde sulfoxylate hydrogen salt, sulphite, thiosulfate and five kinds of compounds of thiocyanate are tasted and are not appeared in the newspapers.
Summary of the invention
The purpose of this invention is to provide a kind of new detection method, this method is that the anions containing sulfur compound separates back and the anti-living reaction of the iodine derivative reagent of acidifying by separating column, the final iodonium negative ion that generates, this ion has maximum absorption peak at 288 nano wave lengths, by detecting the absorption value at 288 nano wave length places, can finally detect the content of anions containing sulfur.The reaction of sulfocompound and acidifying iodine solution following (is example with sulphite):
This method can be by adjusting the derive concentration and the acidity of iodine in the liquid, and the sensitivity that can improve mensuration greatly can be widely used in classes of compounds such as environmental monitoring, food security, biological medicine, health and epidemic prevention.
Still there is not this type of detection method both at home and abroad.
Description of drawings
Fig. 1 is ultraviolet-detecting anions containing sulfur by ion chromatography post-column derivatization compound structure of the present invention and work synoptic diagram.
Be labeled as among Fig. 1:
The 1-leacheate; The 2-pump; The 3-six-way valve; The 4-guard column; The 5-anion separation column; The 6-three-way connection; 7-ultraviolet deriving device; The 8-liquid reservoir of deriving; 9-weaves reaction tube; The 10-UV-detector.
The separate colors spectrogram of five kinds of anions containing sulfurs of Fig. 2
Be labeled as among Fig. 2:
The chromatogram of 1-sulphion; 2-formaldehyde sulfoxylate hydrogen radical ion chromatogram; The chromatogram of 3-sulfite ion; The chromatogram of 4-thiocyanate ion; The chromatogram of 5-thiosulfate ion.
Fig. 3 is the chromatography of ions figure of bean curd stick sample
Be labeled as among Fig. 3:
The chromatogram of 1-sulfite ion; The chromatogram of 2-thiosulfate ion
Embodiment
Embodiment
The separation of sodium sulphide, sodium sulphite, sodium thiosulfate, formaldehyde hydration sodium sulphite, sodium thiocyanate is as follows with the detection concrete steps:
1, the preparation of sodium sulphide, sodium sulphite, sodium thiosulfate, formaldehyde hydration sodium sulphite, sodium thiocyanate standard solution: take by weighing a certain amount of analytical reagent preparation 1000mg.L earlier
-1The standard stock solution, the time spent per sample content the standard stock solution be diluted to standard use solution, this standard stock solution and use liquid newly to prepare every day.
2, the selection of leacheate: test different leacheate proportionings, be defined as 4.5mmolL at last
-1Na
2CO
3+ 0.08mmolL
-1Na
2HCO
3, five kinds of negative ion of separation that can be successful.
3, the derive selection of liquid: the iodine solution and the acidity of test variable concentrations, to reach the optimal absorption value, this example is 0.25%I
2With 0.02% (V: V) H
3PO
4
List of references
[1]I.Demkowska，Z..Polkowska，J.Namies′nik，J.Chromatogr?B?875(2008)419.
[2]I.G.Casella，R.Marchese，Anal.Chim.Acta?311(1995)199-210
[3]Y.Miura，A.Kawaoi，J.Chromatogr?A?884(2000)81
[4]R.A.Niemann，D.L.Anderson，J.Chromatogr?A?1200(2008)193
[5]Y.Michigami，M.Morooka，K.Ueda，J.Chromatogr?A?732(1996)403
[6]Y.Miura，K.Fukasawa，T.Koh，J.Chromatogr?A?804(1998)143-150
Claims (3)
1. chromatography of ions-post-column derivation uv detection method is measured anions containing sulfur compound method, and its method is earlier the anions containing sulfur compound to be separated through anion-exchange column earlier, enters the braiding reaction tube by a threeway again.The iodine reagent of acidifying also enters the braiding reaction tube by this threeway by a post-column derivation device, the moon of sulfur-bearing from the iodine reagent of compound and acidifying redox reaction takes place in the braiding reaction tube, reaction product iodonium ion has stronger ultraviolet absorption peak, can increase the absorption signal value greatly.Earlier derivative reagent iodine solution and acidity are regulated before measuring, to determine that sulfocompound has the iodine concentration and the acidity of obtained the maximum absorption, to obtain higher detection limit and accuracy.
2. chromatography of ions according to claim 1-post-column derivation ultraviolet method detects anions containing sulfur compound method, it is characterized in that, anions containing sulfur with reductibility can instead be given birth to redox reaction with iodine under acid condition, iodine ion that generates and excessive iodine further react and generate the iodonium ion, the iodonium ion has stronger uv absorption signal, improves the detectability of measured object.
3. this method also can be applied to have reducing property by the compound of iodine oxidation, can improve sensitivity and improve detectability with similar scheme analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100971955A CN101571530A (en) | 2009-03-27 | 2009-03-27 | Compound for ultraviolet-detecting anions containing sulfur by ion chromatography post-column derivatization |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100971955A CN101571530A (en) | 2009-03-27 | 2009-03-27 | Compound for ultraviolet-detecting anions containing sulfur by ion chromatography post-column derivatization |
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| CN101571530A true CN101571530A (en) | 2009-11-04 |
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| CNA2009100971955A Pending CN101571530A (en) | 2009-03-27 | 2009-03-27 | Compound for ultraviolet-detecting anions containing sulfur by ion chromatography post-column derivatization |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103983710A (en) * | 2014-05-19 | 2014-08-13 | 浙江大学 | Method for determining silicate and phosphate ions with ion chromatography post-column derivatization method |
| CN105758982A (en) * | 2016-02-25 | 2016-07-13 | 杭州飞山浩科技有限公司 | Device and method for measuring nitrite ions in milk powder |
| CN106908547A (en) * | 2017-03-18 | 2017-06-30 | 天津市星河科技有限公司 | The chromatography of ions detection method of thiocyanate radical in oil field stratum water |
| WO2017202029A1 (en) * | 2016-05-26 | 2017-11-30 | 哈尔滨工业大学深圳研究生院 | Method and system for measuring content of dissolved organic halogens in water |
| CN112730722A (en) * | 2020-12-29 | 2021-04-30 | 中国地质大学（武汉） | Quantitative test method for thiotungstate in natural water |
-
2009
- 2009-03-27 CN CNA2009100971955A patent/CN101571530A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103983710A (en) * | 2014-05-19 | 2014-08-13 | 浙江大学 | Method for determining silicate and phosphate ions with ion chromatography post-column derivatization method |
| CN105758982A (en) * | 2016-02-25 | 2016-07-13 | 杭州飞山浩科技有限公司 | Device and method for measuring nitrite ions in milk powder |
| WO2017202029A1 (en) * | 2016-05-26 | 2017-11-30 | 哈尔滨工业大学深圳研究生院 | Method and system for measuring content of dissolved organic halogens in water |
| CN106908547A (en) * | 2017-03-18 | 2017-06-30 | 天津市星河科技有限公司 | The chromatography of ions detection method of thiocyanate radical in oil field stratum water |
| CN106908547B (en) * | 2017-03-18 | 2019-07-09 | 天津市星河科技有限公司 | The ion chromatography detection method of thiocyanate radical in oil field stratum water |
| CN112730722A (en) * | 2020-12-29 | 2021-04-30 | 中国地质大学（武汉） | Quantitative test method for thiotungstate in natural water |
| CN112730722B (en) * | 2020-12-29 | 2022-03-08 | 中国地质大学（武汉） | Quantitative test method for thiotungstate in natural water |
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Open date: 20091104 |