CN102495159A - Ion chromatography-valve switching analysis system for simultaneously detecting iodide ions and iodate ions - Google Patents
Ion chromatography-valve switching analysis system for simultaneously detecting iodide ions and iodate ions Download PDFInfo
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- CN102495159A CN102495159A CN2011103167008A CN201110316700A CN102495159A CN 102495159 A CN102495159 A CN 102495159A CN 2011103167008 A CN2011103167008 A CN 2011103167008A CN 201110316700 A CN201110316700 A CN 201110316700A CN 102495159 A CN102495159 A CN 102495159A
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- ion
- ions
- chromatographic column
- iodate
- exchange
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- 150000002500 ions Chemical class 0.000 title claims abstract description 49
- 238000004458 analytical method Methods 0.000 title claims abstract description 15
- -1 iodide ions Chemical class 0.000 title claims abstract 9
- 238000005349 anion exchange Methods 0.000 claims abstract description 5
- ICIWUVCWSCSTAQ-UHFFFAOYSA-M iodate Chemical compound [O-]I(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-M 0.000 claims description 32
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 claims description 28
- 229940006461 iodide ion Drugs 0.000 claims description 28
- 229940005633 iodate ion Drugs 0.000 claims description 24
- 238000005342 ion exchange Methods 0.000 claims description 20
- 238000004587 chromatography analysis Methods 0.000 claims description 19
- 238000001514 detection method Methods 0.000 claims description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 11
- 230000000694 effects Effects 0.000 claims description 3
- 150000001450 anions Chemical class 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 abstract 3
- HNSDLXPSAYFUHK-UHFFFAOYSA-N 1,4-bis(2-ethylhexyl) sulfosuccinate Chemical compound CCCCC(CC)COC(=O)CC(S(O)(=O)=O)C(=O)OCC(CC)CCCC HNSDLXPSAYFUHK-UHFFFAOYSA-N 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 3
- 230000000717 retained effect Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 125000000129 anionic group Chemical group 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 206010020880 Hypertrophy Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 230000004641 brain development Effects 0.000 description 1
- 230000018109 developmental process 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
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 208000003532 hypothyroidism Diseases 0.000 description 1
- 230000002989 hypothyroidism Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- ICIWUVCWSCSTAQ-UHFFFAOYSA-N iodic acid Chemical class OI(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-N 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 150000008040 ionic compounds Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000005477 standard model Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000001685 thyroid gland Anatomy 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a use system for instrumental analysis, in particular to an ion chromatography-valve switching analysis system for simultaneously detecting iodide ions and iodate ions. The ion chromatography-valve switching analysis system is provided with an anion exchange chromatographic column comprising a chromatographic column with low exchange capacity and a chromatographic column with high exchange capacity, wherein the chromatographic column with the low exchange capacity retains the iodide ions to a certain degree while hardly retaining some weak retention ions including the iodate ions, and the chromatographic column with the high exchange capacity is capable of effectively separating various weak retention ions. The iodide ions can be rapidly eluted only through the chromatographic column with the low exchange capacity, by means of simple valve switching, the weak retention ions including the iodate ions and the like can be effectively separated, analysis time is shortened, and analysis efficiency is improved.
Description
Technical field
The present invention relates to the using system that a kind of chemical apparatuses is analyzed, particularly a kind ofly relate to chromatography of ions-valve switching analytic system that iodide ion and iodate ion detect simultaneously.
Background technology
Chromatography of ions is widely used in the detection of various ionic compounds as the modern analysis means.Contain various ions in the complex sample, need consume long analysis time usually, but our object ion is wherein several kinds sometimes, there is no need all ions in the sample are detected.Adopt chromatography of ions-valve handoff technique to detect by the selected target ion, preferably resolve this problem.Iodine is the human body essential trace element of (comprising all animals); Mainly be present in occurring in nature with iodide ion and iodate ion form; The shortage of I will cause various diseases; Like thyroid gland hypertrophy, hypothyroidism, intelligence development obstacle etc., especially the infant is human brain development's important stage period.Chromatography of ions especially can separate element different valence state of the same race because of its effective separating power simultaneously, is widely used in the detection of I different shape.The detecting device that adopts mainly contains ampere detector, UV-detector, electric conductivity detector and inductively coupled plasma mass spectrometry detecting device (ICP-MS); But most methods can only detect to certain form of I, rather than detect two kinds of forms the time.Advantages such as ICP-MS has the detection sensitivity height, and antijamming capability is strong because of itself intrinsic element separating power, can detect iodate under the situation that other interfering ion exists.But because this instrument and equipment costs an arm and a leg, reason such as strongly professional can not be used to analyze industry widely.Up to now, do not see the report of measuring iodide ion and iodate with ion chromatographic conductance method simultaneously.
Summary of the invention
The present invention to the weak point of prior art, provides a kind of chromatography of ions-valve handoff technique just, is used for iodide ion and iodate ion ground detects simultaneously, has shortened analysis time, has improved detection efficiency.
Concrete technical scheme of the present invention is following:
The present invention is that chromatography of ions-valve that a kind of iodide ion and iodate ion are measured simultaneously switches analytical system; Be used for iodide ion and iodate ion ground detects simultaneously; Adopt anion-exchange column; Comprise a low ion exchange capacity post and a high-exchange-capacity post; The low ion exchange capacity chromatographic column has certain reservation to iodide ion, and to comprising that keeping ion a little less than some of iodate keeps hardly; And the high-exchange-capacity chromatographic column can well be separated the various weak ions that keep; Only need to switch by simple valve; Can make iodide ion only pass through the low ion exchange capacity chromatographic column and quick wash-out; The separating effect that weak reservation anion such as while iodate can obtain; Shorten analysis time, improved analysis efficiency.
The detection of iodate ion of the present invention does not receive the weak interference that keep ion such as fluorine ion; And whole analytic system is formed simple; Adopt the self-control chromatographic column with low cost, go for the problem that a series of strong reservation ions and weak reservation ion are analyzed simultaneously, have very high practical value.
Chromatography of ions provided by the invention-valve handoff technique can be used for iodide ion and iodate ion ground detects simultaneously.When all ions in the sample get into the low ion exchange capacity chromatographic column through six-way valve; Iodide ion is kept and other ion inflow high-exchange-capacity chromatographic column subsequently by chromatographic column; At this moment, make the low ion exchange capacity chromatographic column be in the downstream of high-exchange-capacity chromatographic column, reach iodide ion and get into conductance cell purpose to be detected prior to weak ions that keeps such as iodates through the valve switching; Simultaneously, the various negative ion of inflow high-exchange-capacity chromatographic column also can access good separation.
The present invention has following advantage:
1. the present invention adopts homemade anion-exchange column and chromatography of ions-valve handoff technique, can detect two kinds of different shapes---the iodide ion and the iodate ion of I simultaneously, and the detection of iodate ion does not receive the weak interference that keep ion such as fluorine ion.Whole analytic system is formed simple; Adopt the self-control chromatographic column with low cost, can make iodide ion only pass through the low ion exchange capacity chromatographic column and quick wash-out, keep the separating effect that negative ion can obtain a little less than the while iodate etc.; Shorten analysis time, improved analysis efficiency.
2. the present invention can also be applicable to the problem that other a series of strong reservations and weak reservation ion are analyzed simultaneously, has very high practical value.
Description of drawings
Fig. 1 switches preceding device synoptic diagram for six-way valve;
Fig. 2 is the device synoptic diagram of six-way valve after switching;
Fig. 3 is the standard model (I that chromatography of ions-valve switches analytic system
-, F
-, IO
3 -) chromatogram;
Fig. 4 is actual sample (Betagen Solution) chromatogram that chromatography of ions-valve switches analytic system;
Be labeled as among Fig. 1:
The 1-waste liquid, 2-electric conductivity detector, 3-rejector, 4-low ion exchange capacity chromatographic column, 5-high-exchange-capacity chromatographic column, 6-injection port, 7-six-way valve, 8-leacheate generator, 9-syringe pump, 10-six-way valve;
Be labeled as among Fig. 2:
The 1-waste liquid, 2-electric conductivity detector, 3-rejector, 4-low ion exchange capacity chromatographic column, 5-high-exchange-capacity chromatographic column, 6-injection port, 7-six-way valve, 8-leacheate generator, 9-syringe pump, 10-six-way valve;
Be labeled as among Fig. 3:
1-I
-，2-F
-，3-IO
3 -；
Be labeled as among Fig. 4:
1-I
-；2-F
-；3-IO
3 -。
Embodiment
The present invention detects when utilizing Dionex ICS-2000 ion chromatograph, Dionex ICS-900 ion chromatograph and self-control anion-exchange column to realize iodide ion and iodate ion, and wherein Dionex ICS-900 ion chromatograph has only used its sampling valve.Low ion exchange capacity chromatographic column and high-exchange-capacity chromatographic column are linked in sequence on the six-way valve of Dionex ICS-2000 ion chromatograph.Before valve switched, the stream of system was followed successively by leacheate generator 8, quantifying ring, low ion exchange capacity chromatographic column 4, high-exchange-capacity chromatographic column 5, rejector 3 and electric conductivity detector 2; After valve switches; The stream of system is followed successively by leacheate generator 8, quantifying ring, high-exchange-capacity chromatographic column 5, low ion exchange capacity chromatographic column 4, rejector 3 and electric conductivity detector 2, and the low ion exchange capacity chromatographic column 4 and the ordinal position of high-exchange-capacity chromatographic column 5 are changed.In addition, this method adopts the online leacheate of simple KOH, single pump single current road system, and inhibition type electricity is led detection.
The operation steps that the chromatography of ions that iodide ion and iodate ion detect simultaneously-valve switches analytic system is following:
1. sample loads, and for guaranteeing that enough representative samples are housed in the quantifying ring, the sample size volume must be greater than four times of quantifying ring volumes;
2. weak reservation negative ion separates with strong reservation is anionic; Fig. 1 switches preceding device synoptic diagram for six-way valve; The switching of six-way valve 7 gets in the low ion exchange capacity chromatographic column 4 sample in the quantifying ring, and this moment, iodide ion was retained; Fluorine ion and iodate ion then keep on chromatographic column hardly, flow out chromatographic column 4 simultaneously with the water negative peak and the high-exchange-capacity chromatographic column 5 that gets into subsequently is separated.
3. the cleaning of the detection of object ion and system, Fig. 2 is the device synoptic diagram of six-way valve after switching; When iodide ion still is retained on the low ion exchange capacity chromatographic column 4 and fluorine ion and iodate ion when flowing into high-exchange-capacity chromatographic column 5 subsequently fully; Switch six-way valve 10; The purpose that valve switches is to make iodide ion only pass through low ion exchange capacity chromatographic column 4; And fluorine ion and iodate ion need pass through low ion exchange capacity chromatographic column 4 and high-exchange-capacity chromatographic column 5 simultaneously, and it is to be detected only to get into electric conductivity detector at first through the iodide ion of low ion exchange capacity chromatographic column 4, and fluorine ion and iodate ion are then separated afterwards to be detected in high-exchange-capacity chromatographic column 5; After object ion is all analyzed completion; Improve the eluent concentration of leacheate generator 8, make the ion that still is retained in the chromatographic column flow out chromatographic system fast, reach the purpose of cleaning overall flow paths.
The detection of standard sample and actual sample:
Instrument: Dionex ICS2000 and Dionex ICS900 ion chromatograph, Dionex electric conductivity detector, DionexASRS-ULTRA (4mm) self-reproduction suppresser;
Sample: the mixing standard specimen of iodide ion, fluorine ion and iodate ion, Betagen Solution;
Leacheate: KOH solution;
Separating column: the stainless steel column of homemade 4.6 * 150mm;
Flow velocity: 1ml/min;
Referring to accompanying drawing 3 and accompanying drawing 4, be three kinds of anionic chromatograms of target;
Among Fig. 3: 1-I
-(25mg L
-1); 2-F
-(0.25mg L
-1); 3-IO
3 -(25mg L
-1);
Among Fig. 4: 1-I
-(16.73mg L
-1); 2-F
-(0.0361mg L
-1); 3-IO
3 -(12.73mg L
-1).
Fig. 3 is the mixing standard specimen chromatography of ions figure of iodide ion, fluorine ion and iodate ion; Chromatography of ions-valve through proposing switches analytic system; Each ion can access good separation and detection; The detection of iodate ion does not receive the interference of fluorine ion, and iodide ion goes out the peak earlier than iodate ion simultaneously.
Fig. 4 is the Betagen Solution chromatography of ions figure of 100 times of dilutions; Chromatography of ions-valve through proposing switches analytic system; Each ion in the actual sample can access good separation and detection; The detection of iodate ion does not receive the interference of fluorine ion, and iodide ion goes out the peak earlier than iodate ion simultaneously, and this technology satisfies the requirement that actual sample detects.
Claims (3)
1. chromatography of ions-valve of measuring simultaneously of iodide ion and iodate ion switches analytical system; Be used for iodide ion and iodate ion ground detects simultaneously; It is characterized in that: adopt anion-exchange column; Comprise a low ion exchange capacity post and a high-exchange-capacity post; The low ion exchange capacity chromatographic column has certain reservation to iodide ion, and to comprising that keeping ion a little less than some of iodate keeps hardly; And the high-exchange-capacity chromatographic column can well be separated the various weak ions that keep; Only need to switch by simple valve; Can make iodide ion only pass through the low ion exchange capacity chromatographic column and quick wash-out; The separating effect that weak reservation anion such as while iodate can obtain; Shorten analysis time, improved analysis efficiency.
2. chromatography of ions according to claim 1-valve switches analytic system, it is characterized in that: the detection of iodate ion does not receive the weak interference that keep ion such as fluorine ion, and whole analytic system composition is simple, adopts the self-control chromatographic column with low cost.
3. chromatography of ions according to claim 1-valve switches analytic system, it is characterized in that: go for the problem that a series of strong reservation ions and weak reservation ion are analyzed simultaneously, have very high practical value.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103167008A CN102495159A (en) | 2011-10-18 | 2011-10-18 | Ion chromatography-valve switching analysis system for simultaneously detecting iodide ions and iodate ions |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103167008A CN102495159A (en) | 2011-10-18 | 2011-10-18 | Ion chromatography-valve switching analysis system for simultaneously detecting iodide ions and iodate ions |
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| Publication Number | Publication Date |
|---|---|
| CN102495159A true CN102495159A (en) | 2012-06-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011103167008A Pending CN102495159A (en) | 2011-10-18 | 2011-10-18 | Ion chromatography-valve switching analysis system for simultaneously detecting iodide ions and iodate ions |
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| Country | Link |
|---|---|
| CN (1) | CN102495159A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103760262A (en) * | 2014-01-07 | 2014-04-30 | 安徽皖仪科技股份有限公司 | Ion chromatography method for measuring nitrite in food by using single pump valve switching technology |
| CN106324113A (en) * | 2015-06-30 | 2017-01-11 | 深圳翰宇药业股份有限公司 | Reagent, kit, application and detection method |
| CN109655548A (en) * | 2019-01-22 | 2019-04-19 | 南开大学 | A kind of high efficiency extraction and rapid assay methods of soil inorganic iodine form |
-
2011
- 2011-10-18 CN CN2011103167008A patent/CN102495159A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103760262A (en) * | 2014-01-07 | 2014-04-30 | 安徽皖仪科技股份有限公司 | Ion chromatography method for measuring nitrite in food by using single pump valve switching technology |
| CN103760262B (en) * | 2014-01-07 | 2015-09-30 | 安徽皖仪科技股份有限公司 | Single pump valve handoff technique is utilized to measure the ion chromatographic method of food nitrite nitrate radical |
| CN106324113A (en) * | 2015-06-30 | 2017-01-11 | 深圳翰宇药业股份有限公司 | Reagent, kit, application and detection method |
| CN109655548A (en) * | 2019-01-22 | 2019-04-19 | 南开大学 | A kind of high efficiency extraction and rapid assay methods of soil inorganic iodine form |
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Application publication date: 20120613 |