CN103983710A - Method for determining silicate and phosphate ions with ion chromatography post-column derivatization method - Google Patents
Method for determining silicate and phosphate ions with ion chromatography post-column derivatization method Download PDFInfo
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- CN103983710A CN103983710A CN201410212541.0A CN201410212541A CN103983710A CN 103983710 A CN103983710 A CN 103983710A CN 201410212541 A CN201410212541 A CN 201410212541A CN 103983710 A CN103983710 A CN 103983710A
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Abstract
The invention discloses a method for determining silicate and phosphate ions with an ion chromatography post-column derivatization method. The method comprises the steps that a water solution of a sample to be determined is diluted to a certain multiple times firstly and then the solution is sampled; after the solution is separated and eluted by an anion exchange chromatography column, the separated and diluted solution is derived by an acidified sodium molybdate solution and reduced by ascorbic acid, a product is strongly absorbed in a near infrared region, so that the silicate and phosphate ions are subjected to separated detection; the concentration and the acidity of a post-column derivatization reagent and a reductant are adjusted before determination, so that a derivative compound has the concentration with maximum absorption value, and further high limit of detection and accuracy can be obtained. According to the method, a conventional anion exchange analytical column is used for separating two ions; compared with other reported separation methods, an ion exchange chromatography has higher separation capability and is usually applied to separating ions with similar properties, and therefore, the ion exchange chromatography can be applied to separating the silicate and phosphate ions in complex matrix systems; the method has high application prospects and values.
Description
Technical field
The present invention relates to a kind of ion chromatography post-column derivatization system, specifically, is a kind of new method of utilizing ion chromatography post-column derivatization method to measure silicate and phosphate radical.
Background technology
As everyone knows, two kinds of elements of silicon phosphorus have the effect can not be substituted in biosome, and silicon is the second largest element that on the earth, content is only second to oxygen, and phosphorus is the basic composition element of inhereditary material nucleic acid.The two content in water body has a significant impact the growth of phycophyta, and in monitoring water body, the content of two kinds of elements of silicon phosphorus has very large effect [1-2] for the eutrophication pollution of controlling water body.
At present for two kinds of elements, utilize the two to react with molybdate more and generate molybdenum yellow and the yellow heteropoly acid of phosphorus molybdenum [3], or further use reductive agent to reduce [4] after generation molybdenum blue, carry out respectively the mensuration of absorbance with ultraviolet-visible pectrophotometer.Because the two is to form when heteropoly acid character comparatively similar, so measuring for two kinds of ions time, development there is very large challenge.At present existing Using Flow Injection Analysis [5], the multiple separation methods such as capillary electrophoresis [6] are developed application.
Chromatography of ions is a kind of efficient separation method conventional while detecting different kinds of ions.In recent years, existing post-column derivation ion exclusion chromatography [7] and column front derivation ion pair chromatogram [8] were applied to the separation of silicic acid phosphoric acid.Compared with these two kinds of separation means, ion-exchange chromatography has higher selectivity and separating power, can be applied to better the separation of two kinds of ions in complex matrices sample, and be aided with post-column derivation system, there is high sensitivity, low detection limit, method is simple to operation.
List of references
1M.D.Krom,E.M.S.Woodward,B.Herut,N.Kress,P.Carbo,R.F.C.Mantoura,G.Spyres,T.F.Thingstad,P.Wassmann,C.Wexels-Riser,V.Kitidis,C.S.Law,G.Zodiatis,Deep-SeaRes.II,52(2005)2879；
2C.Neal,M.Neal,H.Wickham,Sci.TotalEnviron.,251/252(2000)511；
3M.F.Osmond,Bull.Soc.Chim.Fr.47(1887)745；
4J.Murphy,J.P.Riley,Anal.Chim.Acta,27(1962)31；
5Y.S.Li,Y.Muo,H.M.Xie,Anal.Chim.Acta,455(2002)315；
6M.C.BarcielaAlonso,R.Prego,Anal.Chim.Acta,416(2000)21；
7M.Ikedo,M.Mori,K.Kurachi,W.Hu,K.Tanaka,Anal.Sci.,22(2006)117；
7Y.Yokoyama,T.Danno,M.Haginoya,Y.Yaso,H.Sato,Talanta,79(2009)308。
Summary of the invention
The object of the invention is to further improve on existing detection method basis, can utilize chromatography of ions to separate with phosphate radical the silicate in sample, after post-column derivation, detect with ultraviolet-visible pectrophotometer, method has the collectivity of height.Institute's use instrument and equipment is simple, and highly sensitive, can be widely used in each fields such as environmental monitoring, food security, health and epidemic prevention.
The present invention is achieved by the following technical solutions:
The invention discloses a kind of ion chromatography post-column derivatization method and measure the method for silicate and phosphate radical, first by testing sample aqueous solution dilution certain multiple, then by solution sample introduction, separate wash-out through an anion-exchange column, sodium molybdate solution through acidifying is derivative, after ascorbic acid reduction, product has absorption more by force in near-infrared region, accomplish thus the detection that separates with phosphate radical to silicate, before mensuration first by post-column derivation reagent, reductant concentration and acidity regulate, to determine that derivative compound has the concentration of obtained the maximum absorption, thereby obtain higher detectability and accuracy.
As improving further, the present invention utilizes silicate and the phosphate anion in anion-exchange column sample separation, has higher selectivity and separating power.
As improving further, the silicate of the present invention after anion-exchange column separates reacts with the acid sodium molybdate solution of derivative liquid and reductive agent ascorbic acid after post with phosphate anion, product has more by force and absorbs at 710nm-810nm, improve method sensitivity, reduced the detection limit of method.
As improving further, product of the present invention has the strongest absorption at 805nm.
Method of the present invention is also applied to measures the inorganic ions in complex mechanism system with UV, visible light absorption.
Beneficial effect of the present invention is as follows:
1. the present invention uses conventional anion exchange analytical column to realize the separation to two kinds of ions, ion-exchange chromatography is compared other separation methods of having reported, there is higher separating power, often be applied to the similar ion of separating property, therefore can be applicable to, for the separating of complex matrices system mesosilicic acid root and phosphate radical, to there is very high application prospect and value;
2. utilize the inhibition conductance detection of conventional anion-exchange chromatography to be difficult to the detection to silicate, this method is by anion-exchange chromatography and the coupling of post-column derivation ultraviolet-visible spectrophotometry, make chromatography of ions can be applied to the detection to silicate, and there is higher detection limit and sensitivity.
Brief description of the drawings
Fig. 1 be ion chromatography post-column derivatization method of the present invention measure silicate and phosphate anion structure and the schematic diagram of working;
In Fig. 1,1-injector; 2-six-way valve; 3-anion separation column; 4-infusion pump A; 5-infusion pump B; 6-infusion pump C; 7-derivatization reaction pipe; 8-ultraviolet-visible pectrophotometer; 9-waste liquid bottle.
Fig. 2 is the separate colors spectrogram of silicate ion and phosphate anion;
In Fig. 2,1-silicate ion; 2-phosphate anion.
Embodiment
The invention provides a kind of ion chromatography post-column derivatization method and measure the method for silicate and phosphate anion, described system comprises injector 1, six-way valve 2, anion separation column 3, infusion pump A4, infusion pump B5, infusion pump C5, threeway, derivatization reaction pipe 7, ultraviolet-visible pectrophotometer 8, waste liquid bottle 9, injector 1 is connected with six-way valve 2, six-way valve 2 is connected with infusion pump A4 and anion separation column 3 respectively, anion separation column 3 after being connected with threeway successively with liquid pump B5, infusion pump C5 connects, after described threeway, connect successively derivatization reaction pipe 7, ultraviolet-visible pectrophotometer 8 and waste liquid bottle 9.
This ion chromatography post-column derivatization method is measured the method for silicate and phosphate anion, first by after testing sample aqueous solution dilution certain multiple, through membrane filtration sample introduction, separate wash-out through an anion-exchange column 3, two constant current infusion pumps pump into the sodium molybdate solution of acidifying and reductive agent ascorbic acid in stream by two threeways, three kinds of solution react in braiding reaction tube, reaction product has absorption more by force in near-infrared region, accomplish thus the detection that separates with phosphate radical to silicate, before mensuration first by post-column derivation reagent, reductant concentration and acidity regulate, to determine that derivative compound has the concentration of obtained the maximum absorption, thereby obtain higher detectability and accuracy.
Be applied to and measure an inorganic ions after certain method is derivative in complex mechanism system with UV, visible light absorption by described method, can improve sensitivity and improve detectability with similar scheme analysis.
Below by specific embodiment and in conjunction with Figure of description, technical scheme of the present invention is described in further detail:
The invention provides a kind of new analytical approach of simultaneously measuring silicate ion and phosphate anion, utilize an ICS-2000 ion chromatograph to comprise a six-way valve 2, an infusion pump A4, two constant current infusion pump B5, infusion pump C6, post-column derivation reaction tube 7, ultraviolet-visible pectrophotometer 8, can realize post-column derivation and measure silicate ion and phosphate anion, greatly improve analysis efficiency.
The present invention utilizes silicate ion and the phosphate anion in anion exchange analytical column 3 sample separation, ultraviolet-visible pectrophotometer 8 detects, installation drawing as shown in Figure 1, system comprises injector 1, six-way valve 2, anion exchange analytical column 3, constant current infusion pump A4, infusion pump B5, infusion pump C6, derivatization reaction pipe 7, ultraviolet-visible pectrophotometer 8, waste liquid bottle 9, injector 1 is connected with six-way valve 2, six-way valve 2 is connected with constant current infusion pump 4 and anion exchange analytical column 3 respectively, two constant current infusion pump B5, infusion pump C6 is connected in stream by two threeways, after described threeway, connect successively derivatization reaction pipe 7, ultraviolet-visible pectrophotometer 8 and waste liquid bottle 9.
Fig. 1 is structure and the work schematic diagram that ion chromatography post-column derivatization method is measured silicate and phosphate anion.Concrete implementation step is: by constant current infusion pump A4, by being full of on six-way valve 2 quantitatively the testing sample through certain dilution of ring (25 μ L), at NaOH leacheate, (flow velocity is 1mL.min
-1) under conveying, deliver in anion-exchange column 3 and separate wash-out.The post-column derivation reagent adopting is 67mmolL
-1sodium molybdate and 0.2molL
-1the mixed liquor of sulfuric acid, by infusion pump, B5 carries, and flow velocity is 0.35mLmin
-1, reductive agent is 36mmolL
-1ascorbic acid, by infusion pump, C6 carries, and flow velocity is 0.35mLmin
-1.Silicate fully reacts with derivative liquid in reaction tube 7 with phosphate anion, and last ultraviolet-visible pectrophotometer 9 carries out absorbance detection to derivative products under 805nm wavelength.
Fig. 2 is the chromatogram that ion chromatography post-column derivatization method is measured silicate and phosphate anion standard solution.In figure, show that No. 1 peak and No. 2 peaks are respectively silicate ion and phosphate radical responds after anion chromatographic column separates on ultraviolet-visible pectrophotometer, two kinds of ion concentrations are 2.5mg/L.
Utilize ion chromatography post-column derivatization method to measure different water sample mesosilicic acid roots and phosphate anion, in actual sample lake water, recording silicate is 16.16mg/L, and phosphate anion does not record, and in snow-broth, recording silicate is 0.79mg/L, and phosphate anion does not record.4 times of deionization dilutions for lake water sample, snow-broth is undiluted, and after 0.22 μ m nylon leaching film filters, collection filtrate is stand-by.
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 many distortion.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 (5)
1. an ion chromatography post-column derivatization method is measured the method for silicate and phosphate radical, it is characterized in that, first by testing sample aqueous solution dilution certain multiple, then by solution sample introduction, separate wash-out through an anion-exchange column, sodium molybdate solution through acidifying is derivative, after ascorbic acid reduction, product has absorption more by force in near-infrared region, accomplish thus the detection that separates with phosphate radical to silicate, before mensuration first by post-column derivation reagent, reductant concentration and acidity regulate, to determine that derivative compound has the concentration of obtained the maximum absorption, thereby obtain higher detectability and accuracy.
2. ion chromatography post-column derivatization method according to claim 1 is measured the method for silicate and phosphate radical, it is characterized in that, utilizes silicate and phosphate anion in anion-exchange column sample separation.
3. ion chromatography post-column derivatization method according to claim 1 is measured the method for silicate and phosphate radical, it is characterized in that, silicate after anion-exchange column separates reacts with the acid sodium molybdate solution of derivative liquid and reductive agent ascorbic acid after post with phosphate anion, and product has more by force and absorbs at 710nm-810nm.
4. ion chromatography post-column derivatization method according to claim 3 is measured the method for silicate and phosphate radical, it is characterized in that, described product has the strongest absorption at 805nm.
5. one kind is applied to and is measured the inorganic ions in complex mechanism system with UV, visible light absorption by the method described in claim 1 or 2 or 3 or 4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| 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 |
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