CN103969369A - Method for measuring trace ammonium ions in high salt matrix through ion chromatography single pump column switching - Google Patents
Method for measuring trace ammonium ions in high salt matrix through ion chromatography single pump column switching Download PDFInfo
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Abstract
The invention discloses a method for measuring trace ammonium ions in high salt matrix through ion chromatography single pump column switching. The trace ammonium ions in a complex sample can be detected. The system comprises a liquid feeding pump, a six-way valve A, an injector, a quantitative loop, a six-way valve B, a receiving pipe, a protective column, an analytical column and a suppressor, wherein the liquid feeding pump, the receiving pipe, a conductivity detector, a waste liquid bottle and the six-way valve B are connected to the six-way valve A; the six-way valve B is respectively connected with the six-way valve A, the quantitative loop, the injector, the waste liquid bottle and the protective column; the protective column is sequentially connected with the analytical column, the suppressor and the conductivity detector. The trace ions in the high salt matrix can be detected by using single pump circulating column switching ion chromatography, the problem that ions which are similar in retention effect and large in concentration difference cannot be separated by a conventional common ion chromatographic column is solved, the requirements of detection substances on the chromatographic column are lowered, a single leacheate pump is used, and the equipment is simple and convenient to use.
Description
Technical field
The present invention relates to a kind of ion chromatography single-pump column switching system, specifically, is the method for the ammonium ion of trace in the online detection of complex matrix sample of a kind of chromatography of ions, can realize the detection to trace ammonium radical ion in complex sample.
Technical background
NH
4 +be the important composition composition of the circulation-nitrogen cycle of occurring in nature maximum, be extensively present in each field of nature.As nutriment, compare NO
3 -, NH
4 +more easily be absorbed and used by plants, still, excessive NH in aqueous solution
4 +existence by promoting the eutrophication process of water body, impel phytoplankton bloom, to such an extent as to dissolved oxygen DO in water consumed in a large number, cause the mass mortality of the animals such as fishes and shrimps.At present, NH
4 +be listed in the significant ion of body eutrophication.Therefore, NH
4 +quantitative detection received increasing concern.Because NH
4 +itself does not have uv absorption, is not suitable for atomic spectrum method yet, and therefore traditional detection method is to adopt derivative reagent to NH
4 +carry out derivatization, then utilize the methods such as ultraviolet, fluorescence, chemiluminescence to detect.Although the method can meet NH to a certain extent
4 +the demand detecting, but operation steps complexity is time-consuming, and need extra derivative reagent, when sample substrate is comparatively complicated, be easily disturbed.
Chromatography of ions is present analysis ionic substance effective method the most, and the contribution of its maximum aspect cation detection is exactly to NH
4 +detection.But, as water-soluble sample substrate complexity and NH
4 +concentration when lower, the application of chromatography of ions is just limited by very large.The present invention utilizes the single pump plunger shaft of circulation to switch and collection tube has been set up a set of ion chromatographic column switched system, can be to the trace NH in complex sample
4 +detect online, without sample pre-treatments.
Summary of the invention
The present invention has set up trace ammonium radical ion chromatographic column switched system in a kind of Direct Analysis complex sample online, has avoided loaded down with trivial details time-consuming sample pre-treatments step.The present invention is achieved through the following technical solutions:
For detection of an ion chromatographic column switched system for trace ion in complicated substrate, described system comprises infusion pump, six-way valve A, syringe, quantitative ring, six-way valve B, receiving tube, guard column, analytical column, rejector, electric conductivity detector and waste liquid bottle.On six-way valve A, connect infusion pump, receiving tube, electric conductivity detector, waste liquid bottle, six-way valve B.Six-way valve B is respectively with six-way valve A, quantitatively ring, syringe, waste liquid bottle, guard column are connected, linking parsing post, rejector, electric conductivity detector successively after described guard column.
As improving further, infusion pump of the present invention only has one, and solution part in whole system recycles.
As improving further, receiving tube of the present invention, after post switches, is removed complicated substrate, by receiving tube, receives trace ion to be analyzed, reaches the object that detects trace ion detection.
The present invention also provides a kind of detection method of the ion chromatographic column switched system for detection of trace ion in complicated substrate solution, described method comprises the reception of the collection of baseline, the removal of complicated substrate and object ion, three steps of the stratographic analysis of object ion, and concrete steps are as follows:
(1), the drafting of baseline: infusion pump is continuously delivered to above-mentioned ion chromatographic column switched system by leacheate, makes system reach equilibrium state, and conductance signal is detected by electric conductivity detector and got off to draw out corresponding figure line by computer record;
(2), the removal of complicated substrate and the reception of object ion: high salt matrix sample enters analytic system, by post changing method, high salt matrix in complex sample is removed, and receiving tube optionally receives from electric conductivity detector object ion out, to be analyzed;
(3), the stratographic analysis of object ion: post switches again, and infusion pump carries leacheate that the ion in receiving tube is delivered to guard column, separating column, rejector, electric conductivity detector analysis.
Beneficial effect of the present invention is:
The present invention uses single pump circulating column to switch the detection that chromatography of ions can be realized trace ion in high base status, solved current with the separation of conventional ion chromatographic column not similar the but concentration of retention differ the difficult problem of larger ion, the use of the method, prepare special chromatographic column and come separated retention ion feasibility similar but that concentration differs larger stronger, lowered the requirement of detection material to chromatographic column; Simultaneously single pump circulating column switches with conventional ion chromatogram and more only increases a six-way valve, uses single drip washing liquid pump, and equipment is simple, easy to use.
Accompanying drawing explanation
Fig. 1 is the single-pump column switching system that the present invention sets up;
In Fig. 1,1-receiving tube, 2-infusion pump, 3-quantitatively encircles, 4-syringe, 5-guard column, 6-analytical column, 7-rejector, 8-electric conductivity detector, 9-waste liquid bottle, 10-six-way valve A, 11-six-way valve B;
Fig. 2 is 2.0mg/LNH in 700mg/LNa+ matrix
4 +standard solution post switching chromatograph figure;
Fig. 3 is ammonium radical ion post switching chromatograph figure in 5 times of seawater samples of dilution.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail:
The invention provides a kind of ion chromatography single-pump column and switch the new analytical approach of measuring the ammonium ion of trace in high base status, utilize one to wear peace IC-90 ion chromatograph and comprise a six-way valve A, infusion pump 2, receiving tube 1, electric conductivity detector 8, external six-way valve B11 can realize single pump plunger shaft switching and remove the high base status in complex sample, reaches the object of analyzing trace ammonium radical ion.
In seawater, the detection concrete steps of ammonium root are as follows:
The configuration of standard solution: take a certain amount of ammonium chloride analytical reagent, the standard reserving solution of configuration 1000mg/L is preserved at 4 ℃, and the used time is diluted to desired concn by standard reserving solution.
The collection of the removal of complicated substrate and ammonium root: get 5 times of sample introductions of seawater sample 2g dilution to quantitatively encircling in 3, switch six-way valve B11, infusion pump 2 pumps into 10mmol/L pyrovinic acid, and (flow velocity is 1mL.min
-1) through receiving tube 1, the seawater sample quantitatively encircling in 3 is brought into guard column 5, analytical column 6 separation; treat that complicated substrate (sodion) is removed substantially and before ammonium radical ion to be analyzed is about to out peak; switch six-way valve A10, receiving tube 1 receives ammonium radical ion to be analyzed.
The trace ammonium root receiving enters chromatogram column analysis for the second time: switch six-way valve A10, infusion pump 2 is carried 10mmol/L pyrovinic acid, and (flow velocity is 1mL.min
-1) trace ammonium radical ion in receiving tube 1 enters guard column 5, analytical column 6 separation; the too low existing ammonium root for the second time of 10mmol/L pyrovinic acid eluent concentration elutes peak; use afterwards 16mmol/L pyrovinic acid leacheate instead separated for the first time strong reservation ion (magnesium ion, calcium ion) is eluted to peak, electric conductivity detector 8 detects.
Fig. 2 is the chromatogram that ion chromatography single-pump column switching method is measured 2.0mg/L ammonium root standard solution in 700mg/L sodion matrix.In figure, show that No. 1 peak is the peak that post switches front sodion, concentration is 700mg/L, and No. 2 peak is after post switches, the peak of the ammonium radical ion that receiving tube 1 receives, and concentration is 2.0mg/L.
Utilize ion chromatography single-pump column switching method to measure the ammonium radical ion of extra large underwater trace, the ammonium radical ion of surveying in actual sample is 0.2666mg/L.Fig. 3 is 5 times of seawater posts switching chromatography of ions figure of dilution, in figure, show that No. 1 peak is sodion cutting edge of a knife or a sword before post switches, No. 2 peaks are potassium ion cutting edge of a knife or a sword after post switches, switch the sodion obtain and the chromatogram of ammonium root for post No. 3, detail view is in the upper right side of Fig. 3, No. 4 peaks are magnesium ion cutting edge of a knife or a sword, and No. 5 peaks are calcium ion cutting edge of a knife or a sword.
Utilize ion chromatography single-pump column switching method to measure the ammonium radical ion in sodium chloride (analyzing pure).Get and analyze pure sodium chloride sample 0.25g 100ML deionized water dissolving, sodium chloride solution after dissolved dilution is crossed to 0.22 μ m filter membrane to be analyzed, in actual sample, do not record ammonium radical ion, add respectively 0.05mg/L, 0.1mg/L, 0.2mg/L ammonium radical ion standard solution, recovery of standard addition is at 91.7%-107.2%, and result method of proof is effectively reliable.
Finally, it is also to be noted that, what more than enumerate is only specific embodiments of the invention.Obviously, the invention is not restricted to above embodiment, can also have the application that in many high base status, trace materials is measured.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (4)
1. the ion chromatography single-pump column switching system for detection of trace ion in complicated substrate sample, it is characterized in that, described system comprises infusion pump (2), six-way valve A (10), syringe (4), quantitative ring (3), six-way valve B (11), receiving tube (1), guard column (5), analytical column (6), rejector (7), electric conductivity detector (8) and waste liquid bottle (9); On described six-way valve A (10), connect infusion pump (2), receiving tube (1), electric conductivity detector (8), waste liquid bottle (9), six-way valve B (11); Described six-way valve B (11) is respectively with six-way valve A (10), quantitatively ring (3), syringe (4), waste liquid bottle (9), guard column (5) are connected, linking parsing post (6), rejector (7), electric conductivity detector (8) successively after described guard column (5).
2. the ion chromatography single-pump column switching system for detection of trace ion in complicated substrate sample according to claim 1, is characterized in that, described infusion pump (2) only has one, and solution part in whole system recycles.
3. the ion chromatography single-pump column switching system for detection of trace ion in complicated substrate sample according to claim 1, it is characterized in that, described receiving tube (1) is after post switches, remove complicated substrate, by receiving tube (1), receive trace ion to be analyzed, reach the object that detects trace ion detection.
4. according to the detection method for detection of the ion chromatography single-pump column switching system of trace ion in complicated substrate sample described in claim 1 or 2 or 3, it is characterized in that, described method comprises the reception of the collection of baseline, the removal of complicated substrate and object ion, three steps of the stratographic analysis of object ion, and concrete steps are as follows:
(1), the drafting of baseline: infusion pump (2) is continuously delivered to above-mentioned ion chromatographic column switched system by leacheate, make system reach equilibrium state, conductance signal is detected and is got off to draw out corresponding figure line by computer record by electric conductivity detector (8);
(2), the removal of complicated substrate and the reception of object ion: high salt matrix sample enters analytic system, by post changing method, high salt matrix in complex sample is removed, and receiving tube (1) optionally receives from electric conductivity detector (8) object ion out, to be analyzed;
(3), the stratographic analysis of object ion: post switches again, and infusion pump (2) carries leacheate that the ion in receiving tube (1) is delivered to guard column (5), analytical column (6), rejector (7), electric conductivity detector (8) analysis.
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| CN201410206848.XA CN103969369B (en) | 2014-05-15 | Ion chromatography single-pump column switching measures the method for the ammonium ion of trace in high base status |
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| CN201410206848.XA CN103969369B (en) | 2014-05-15 | Ion chromatography single-pump column switching measures the method for the ammonium ion of trace in high base status |
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| CN103969369B CN103969369B (en) | 2016-11-30 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104237426A (en) * | 2014-08-28 | 2014-12-24 | 浙江大学 | On-line pretreatment ion chromatogram column switching system and method used for detecting conventional anions and organic acids in biodiesel samples |
| CN104237433A (en) * | 2014-08-28 | 2014-12-24 | 浙江大学 | On-line pretreatment ion chromatogram column switching system for detecting conventional cations in biodiesel samples and detection method of on-line pretreatment ion chromatogram column switching system |
| CN104267131A (en) * | 2014-09-30 | 2015-01-07 | 浙江工业大学 | Ion chromatography single pump-column switching system for detecting trace inorganic anions in weak-acid salt |
| CN105954445A (en) * | 2016-05-10 | 2016-09-21 | 浙江大学 | Column switching device and method for synchronously measuring sucralose and other weak-retention saccharides in sample |
| CN104267131B (en) * | 2014-09-30 | 2017-01-04 | 浙江工业大学 | A kind of ion chromatography single pump-post switched system detecting trace inorganic anion in salt of weak acid |
| CN107850581A (en) * | 2015-12-29 | 2018-03-27 | 株式会社爱思迪科学 | The analysis preprocess method of sample containing the dramatically different Multiple components of concentration |
| CN108490107A (en) * | 2018-03-09 | 2018-09-04 | 山东省分析测试中心 | A kind of liquid chromatograph and working method for complex sample multi-cycle separation |
| CN109270192A (en) * | 2018-12-02 | 2019-01-25 | 太湖流域水文水资源监测中心（太湖流域水环境监测中心） | Pretreating device, method and purposes for the detection of aquatic products sulfa antibiotics |
| CN114994223A (en) * | 2022-04-29 | 2022-09-02 | 天津博纳艾杰尔科技有限公司 | Automatic sample injection liquid path system and automatic sample injection method |
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Cited By (11)
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| CN104237426A (en) * | 2014-08-28 | 2014-12-24 | 浙江大学 | On-line pretreatment ion chromatogram column switching system and method used for detecting conventional anions and organic acids in biodiesel samples |
| CN104237433A (en) * | 2014-08-28 | 2014-12-24 | 浙江大学 | On-line pretreatment ion chromatogram column switching system for detecting conventional cations in biodiesel samples and detection method of on-line pretreatment ion chromatogram column switching system |
| CN104267131A (en) * | 2014-09-30 | 2015-01-07 | 浙江工业大学 | Ion chromatography single pump-column switching system for detecting trace inorganic anions in weak-acid salt |
| CN104267131B (en) * | 2014-09-30 | 2017-01-04 | 浙江工业大学 | A kind of ion chromatography single pump-post switched system detecting trace inorganic anion in salt of weak acid |
| CN107850581A (en) * | 2015-12-29 | 2018-03-27 | 株式会社爱思迪科学 | The analysis preprocess method of sample containing the dramatically different Multiple components of concentration |
| CN107850581B (en) * | 2015-12-29 | 2021-01-05 | 株式会社爱思迪科学 | Method for the analytical pretreatment of samples containing a plurality of components in significantly different concentrations |
| CN105954445A (en) * | 2016-05-10 | 2016-09-21 | 浙江大学 | Column switching device and method for synchronously measuring sucralose and other weak-retention saccharides in sample |
| CN108490107A (en) * | 2018-03-09 | 2018-09-04 | 山东省分析测试中心 | A kind of liquid chromatograph and working method for complex sample multi-cycle separation |
| CN109270192A (en) * | 2018-12-02 | 2019-01-25 | 太湖流域水文水资源监测中心（太湖流域水环境监测中心） | Pretreating device, method and purposes for the detection of aquatic products sulfa antibiotics |
| CN109270192B (en) * | 2018-12-02 | 2024-02-02 | 太湖流域水文水资源监测中心（太湖流域水环境监测中心） | Pretreatment device, method and application for detecting aquatic product sulfonamide antibiotics |
| CN114994223A (en) * | 2022-04-29 | 2022-09-02 | 天津博纳艾杰尔科技有限公司 | Automatic sample injection liquid path system and automatic sample injection method |
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