CN103969365A - Method for pretreating and measuring trivalent chromium ions and hexavalent chromium ions on line by ion chromatographic column switching method - Google Patents
Method for pretreating and measuring trivalent chromium ions and hexavalent chromium ions on line by ion chromatographic column switching method Download PDFInfo
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Abstract
The invention discloses a novel method for pretreating and measuring trivalent chromium ions and hexavalent chromium ions on line by an ion chromatographic column switching method. A system comprises a sample injector, a six-way valve, a reversed-phase column, a six-way valve and column switcher, a receiving pipe, a negative ion separation column, a four-source gradient pump, a liquid conveying pump, a three-way joint, a derivative reaction pipe, an ultraviolet visible spectrophotometer, a waste liquid bottle and the like. The problems that two ions are separated through a special separation column and are respectively detected through a double-wavelength ultraviolet visible detector at present are solved, and the dependency of detection on instrument equipment is reduced; meanwhile, due to the application of an on-line pretreatment system, water-soluble organic matters are removed from a sample, labor consumption is reduced, the time for sample pretreatment is saved, and the complicated operation process is avoided.
Description
Technical field
The present invention relates to a kind of ion chromatography circulating column switched system, specifically, is a kind of new method of utilizing ion chromatographic column to switch the online pre-treatment mensuration trivalent chromium of method and hexavalent chromium.
Background technology
Chromium element is extensively present in occurring in nature, often exists with Cr (III) and two kinds of forms of Cr (VI).The two has diverse character, and wherein Cr (III) is the trace element of needed by human, and Cr (VI) has certain toxic and side effect to human body, even can cause death [1] when concentration is large.Just because of this, development just seems particularly important for the method for different valence state chromium.
The current chromium for different valence state in sample, there is oxidation-reduction method, spectrophotometric method, the detection methods such as atomic absorption spectrography (AAS), relatively several method, oxidation-reduction method principle is simple and cost is low, but the reaction time is long, need the strict solution acidity of controlling, prevent Cr (VI) and Cr (III) phase co-conversion, easily make testing result inaccurate; Spectrophotometric method and atomic absorption spectrography (AAS) development are very fast, apply also more and more extensive, easily there is matrix interference in spectrophotometric method wherein in the time measuring, cause erroneous results [2-3], and atomic absorption spectrum itself cannot be differentiated Cr (III) and Cr (VI), need be by media such as silica gel, after absorption, wash-out detects respectively, complicated operation and cost higher [4-5].In recent years, the method for utilizing the efficient separating property of chromatogram to combine to measure different valence state chromium with several detecting devices had had larger development, and what be wherein most widely used is chromatography of ions [6] and reverse-phase paired ion chromatography [7].
List of references
1ChenChun-tian,Leatherchemicals,2003,20(4):24-27；
2AbdollahiH.,Anal.Chim.Acta.,2001,442(2):327–336；
3AndradeF.J.,TudinoM.B.,TroccoliO.E.,Analyst,1996,121(5):613-616；
4MaltezH.F.,CarasekE.,Talanta,2005,65(2):537–542；
5MartendalE.,MaltezH.F.,CarasekE.,J.Hazard.Mater.,2009,161(1):450–456；
6ThreepromJ.,MeelapsomR.,Som-AumW.,LinJ.M.,Talanta,2007,71(1):103-108；
7.WolfR.E.,MorrisonJ.M.,GoldhaberM.B.,J.Anal.At.Spectrom.,2007,22(9):1051-1060。
Summary of the invention
The object of the invention is to further improve on existing detection method basis, can remove online the organism matrix in sample, utilize common anion exchange column to complete the detection under same visible wavelength to trivalent chromic ion and hexavalent chromium, method has the collectivity of height simultaneously.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:
A kind of ion chromatographic column switches the method for the online pre-treatment mensuration trivalent chromium of method and hexavalent chromium, described system comprises injector, six-way valve, reversed-phase column, six-way valve post switch, receiving tube, anion separation column, four source gradient pumps, infusion pump, threeway, derivatization reaction pipe, ultraviolet-visible pectrophotometer, waste liquid bottle, injector is connected with six-way valve, six-way valve is connected with four source gradient pumps and reversed-phase column respectively, on six-way valve post switch, connect receiving tube, six-way valve post switch respectively with infusion pump, anion separation column connects, infusion pump is connected with threeway, after described threeway, connect successively derivatization reaction pipe, ultraviolet-visible pectrophotometer and waste liquid bottle.
This ion chromatographic column switches the method for the online pre-treatment mensuration trivalent chromium of method and hexavalent chromium, first testing sample aqueous solution is mixed to fully reaction with certain density EDTA solution, make trivalent chromic ion and EDTA complexing wherein generate negative ion product, this negative ion product has absorption more by force in visible-range, then by solution sample introduction, first remove online water soluble organic substance through reversed-phase column, the solution of wash-out separates wash-out with leacheate through an anion chromatographic column, enter braiding reaction tube by a threeway again, the diphenylcarbazide solution of acidifying also enters braiding reaction tube by this threeway by a post-column derivation device, react in braiding reaction tube with hexavalent chromium, reaction product has absorption more by force at Same Wavelength place, when accomplishing thus trivalent chromic ion and hexavalent chromium, detect, before mensuration first by before post, post-column derivation reagent 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, before post of the present invention, trivalent chromic ion in sample is derived, make it generate anionic group, in visible wavelength range, have more by force and absorb simultaneously, meanwhile, hexavalent chromium has more by force and absorbs with diphenylcarbazide solution post-column derivation product under identical wavelength, thereby detects when accomplishing two kinds of ions, compared with the method for having reported with other, reduce the requirement to instrument and chromatographic column.
As improving further, the present invention connects high performance liquid chromatography reversed-phase column with anion-exchange column, utilize reversed-phase column organic retention characteristic to be removed to the water soluble organic substance existing in sample, the rear different reserve capability of anion-exchange column to different ions of utilizing, treat measured ion wash-out respectively by two kinds, detect with ultraviolet-visible spectrophotometer, realized organic online removal in sample, saved the time of sample pre-treatments and complicated operating process.
Be applied to measure by described method and in complex mechanism system, there is the inorganic ions that UV, visible light absorbs, can improve sensitivity and improve detectability with similar scheme analysis.
Beneficial effect of the present invention is as follows:
When the present invention uses conventional anion analysis post and single channel UV-vis detector can realize two kinds of ions, Same Wavelength detects, solve and manyly at present separated the present situation that two kinds of ions and dual wavelength ultraviolet visible detection device detect respectively two kinds of ions with special separating column, reduced the dependence of detection to instrument and equipment; The application of simultaneously online preprocessing system, remove the water soluble organic substance in sample, needn't use as existing pre-treatment organic matter removal the state of disposable C18 post, reduce manpower consumption, the time of sample pre-treatments and complicated operating process are saved, the activating and regenerating processing of NG1, compared with the disposable operating characteristic of C18 pillar also more environmental protection, there is no this type of detection method both at home and abroad in addition.
Brief description of the drawings
Fig. 1 is that ion chromatographic column of the present invention switches structure and the work schematic diagram that trivalent chromium and hexavalent chromium are measured in the online pre-treatment of method;
In Fig. 1,1-injector; 2-six-way valve; 3-reversed-phase column; 4-six-way valve post switch; 5-receiving tube; 6-anion separation column; 7-four source gradient pumps; 8-NaOH leacheate; 9-infusion pump; 10-infusion pump; 11-derivative liquid; 12-reaction tube; 13-ultraviolet-visible pectrophotometer; 14-NaOH leacheate; 15-acetonitrile; 16-waste liquid bottle.
Fig. 2 is the separate colors spectrogram of trivalent chromic ion and hexavalent chromium;
In Fig. 2,1-trivalent chromic ion; 2-hexavalent chromium.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail:
Below in conjunction with Figure of description, technical scheme of the present invention is described further:
The invention provides a kind of new analytical approach of simultaneously measuring trivalent chromic ion and hexavalent chromium, utilize a SHCIC ion chromatograph to comprise a six-way valve 2, two infusion pumps 9,10, past column reaction pipe 12, ultraviolet-visible pectrophotometer 13, ZQH-100 six-way valve post switch 4 and P680 high performance liquid chromatography four source gradient pumps 7 can be realized online pre-treatment and measure trivalent chromic ion and hexavalent chromium, have greatly improved analysis efficiency.
The present invention utilizes reversed-phase column 3 to remove online the water-soluble base in sample, anion-exchange column separates trivalent chromic ion and hexavalent chromium, ultraviolet-visible pectrophotometer 13 detects, installation drawing as shown in Figure 1, system comprises injector 1, six-way valve 2, reversed-phase column 3, six-way valve post switch 4, receiving tube 5, anion separation column 6, four source gradient pumps 7, infusion pump 9, threeway, derivatization reaction pipe 12, ultraviolet-visible pectrophotometer 13, waste liquid bottle 16, injector 1 is connected with six-way valve 2, six-way valve 2 is connected with four source gradient pumps 7 and reversed-phase column 3 respectively, on six-way valve post switch 4, connect receiving tube 5, six-way valve post switch 4 respectively with infusion pump 9, anion separation column 6 connects, infusion pump 9 is connected with threeway, after described threeway, connect successively derivatization reaction pipe 12, ultraviolet-visible pectrophotometer 13 and waste liquid bottle 16.
Fig. 1 is that ion chromatographic column switches structure and the work schematic diagram that trivalent chromium and hexavalent chromium are measured in the online pre-treatment of method.Concrete implementation step is: by four source gradient pumps 7, to be full of the testing sample through pre-treatment that quantitatively encircles (100 μ L) on six-way valve 2 under the NaOH leacheate (flow velocity is 1mL.min-1) of 20mmolL-1 is carried, the online water soluble organic substance of removing wherein in reversed-phase column 3, in the solution of wash-out is retained in the receiving tube 5 being connected on six-way valve post switch 4 (receiving tube volume is 2mL), after 2min, utilize six-way valve post switch 4 automatic switchover six-way valve patterns, treating that NaOH leacheate 8 that measured ion is carried by infusion pump 9 is delivered in anion-exchange column 6 and separate wash-out in receiving tube 5.The post-column derivation reagent adopting is the mixed liquor of 0.4gL-1 diphenylcarbazide and 0.15molL-1 sulfuric acid, is carried by infusion pump 10, and flow velocity is 0.5mLmin-1.Hexavalent chromium fully reacts with derivative liquid in reaction tube 12, last ultraviolet-visible pectrophotometer 13 (UV-3292, You Lian photoelectricity technology corporation, Ltd. of BeiJing, China) carries out absorbance detection to the derivative products of trivalent chromium and hexavalent chromium under 545nm wavelength.
Fig. 2 is the chromatogram that ion chromatographic column switches the online pre-treatment mensuration trivalent chromium of method and hexavalent chromium standard solution.In figure, show that No. 1 peak is that trivalent chromic ion responds after ion chromatographic column separates with EDTA complexing product on ultraviolet-visible pectrophotometer, trivalent chromic ion concentration is 3mg/L, No. 2 peaks are that hexavalent chromium responds on ultraviolet-visible pectrophotometer with diphenylcarbazide complexing product after ion chromatographic column separates, and hexavalent chromium concentration is 0.3mg/L.
Utilize ion chromatographic column to switch the online pre-treatment of method and measure trivalent chromium and hexavalent chromium in leather, in actual sample, record trivalent chromium and hexavalent chromium content is respectively 24.19mg/kg and 4.89mg/kg.Leather sample pre-treating method is to take the about 0.30g of the leather shredding, add 10mL phosphate buffer solution, the about 3h of ultrasonic extraction in ultrasonic cell disrupte instrument, get 5mL solution, add the 100mmolL-1EDTA of 1mL and the 0.5molL-1NaOH of 0.2mL, be settled to 10mL with deionized water, react about 1h, filter through 0.22 μ m nylon leaching film, collection filtrate is stand-by.
Utilize ion chromatographic column to switch the online pre-treatment of method and measure trivalent chromium and hexavalent chromium in milk, in actual sample, do not record two kinds of ions, add respectively the mixed standard solution of 1mg/L trivalent chromium and 0.1mg/L hexavalent chromium, recovery of standard addition is 105.7% and 97.2%, and result method of proof is effectively reliable.Milk sample pre-treating method is for pipetting milk sample 1mL to be measured, add the nitric acid of 0.1mL33%, deionized water is settled to 10mL, and 2min, the centrifugal 10min of 8000r/min are boiled in heating, get 5mL supernatant, add the 100mmolL-1EDTA of 1mL and the 0.5molL-1NaOH of 0.2mL, be settled to 10mL with deionized water, react about 1h, filter through 0.22 μ m nylon leaching film, 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 (4)
1. the method for trivalent chromium and hexavalent chromium is measured in the online pre-treatment of an ion chromatographic column switching method, it is characterized in that, first testing sample aqueous solution is mixed to fully reaction with certain density EDTA solution, make trivalent chromic ion and EDTA complexing wherein generate negative ion product, this negative ion product has absorption more by force in visible-range, then by solution sample introduction, first remove online water soluble organic substance through reversed-phase column, the solution of wash-out separates wash-out with leacheate through an anion chromatographic column, enter braiding reaction tube by a threeway again, the diphenylcarbazide solution of acidifying also enters braiding reaction tube by this threeway by a post-column derivation device, react in braiding reaction tube with hexavalent chromium, reaction product has absorption more by force at Same Wavelength place, when accomplishing thus trivalent chromic ion and hexavalent chromium, detect, before mensuration first by before post, post-column derivation reagent 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 chromatographic column according to claim 1 switches the method for the online pre-treatment mensuration trivalent chromium of method and hexavalent chromium, it is characterized in that, before post, the trivalent chromic ion in sample is derived, make it generate anionic group, in visible wavelength range, have more by force and absorb simultaneously, meanwhile, hexavalent chromium has more by force and absorbs with diphenylcarbazide solution post-column derivation product under identical wavelength, thereby detects when accomplishing two kinds of ions.
3. ion chromatographic column according to claim 1 switches the method for the online pre-treatment mensuration trivalent chromium of method and hexavalent chromium, it is characterized in that, high performance liquid chromatography reversed-phase column is connected with anion-exchange column, utilize reversed-phase column organic retention characteristic to be removed to the water soluble organic substance existing in sample, the rear different reserve capability of anion-exchange column to different ions of utilizing, treat measured ion wash-out respectively by two kinds, detect with ultraviolet-visible spectrophotometer, realized organic online removal in sample.
4. 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.
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Cited By (9)
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| CN104634912A (en) * | 2015-01-20 | 2015-05-20 | 大连依利特分析仪器有限公司 | Liquid phase chromatographic sample manager |
| CN105628796A (en) * | 2014-10-25 | 2016-06-01 | 上海梅山钢铁股份有限公司 | Ion chromatography detection method for trace anions in chromate passivation solution |
| CN105699530A (en) * | 2016-02-26 | 2016-06-22 | 杭州飞山浩科技有限公司 | Valve switching device and method for online pretreatment of sample for determining hexavalent chromium |
| CN105806989A (en) * | 2016-05-26 | 2016-07-27 | 四川大学 | Method for simultaneously measuring trivalent chromium and hexavalent chromium in water samples by aid of low-pressure ion chromatograms and inductively coupled plasma mass spectra in combination manner |
| CN106018596A (en) * | 2016-05-17 | 2016-10-12 | 华南理工大学 | Online microwave-assisted chiral derivatization-LC/MS (liquid chromatography/mass spectrometry) analysis system and method |
| CN106226439A (en) * | 2016-09-23 | 2016-12-14 | 深圳天祥质量技术服务有限公司 | Chromic method of testing and ion chromatograph in a kind of leatherware |
| CN107576742A (en) * | 2017-09-22 | 2018-01-12 | 广东中测食品化妆品安全评价中心有限公司 | The detection method of trivalent chromium in a kind of health food |
| WO2018188184A1 (en) * | 2017-04-12 | 2018-10-18 | 岛津企业管理（中国）有限公司 | Multifunctional on-line combination device for temperature and pressue increase-assisted extraction, trapping, and chromatographic separation |
| CN109406699A (en) * | 2018-08-28 | 2019-03-01 | 浙江省海洋水产研究所 | The determination method of trivalent chromium and Cr VI in a kind of marine product |
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| CN105628796A (en) * | 2014-10-25 | 2016-06-01 | 上海梅山钢铁股份有限公司 | Ion chromatography detection method for trace anions in chromate passivation solution |
| CN104634912A (en) * | 2015-01-20 | 2015-05-20 | 大连依利特分析仪器有限公司 | Liquid phase chromatographic sample manager |
| CN105699530A (en) * | 2016-02-26 | 2016-06-22 | 杭州飞山浩科技有限公司 | Valve switching device and method for online pretreatment of sample for determining hexavalent chromium |
| CN106018596A (en) * | 2016-05-17 | 2016-10-12 | 华南理工大学 | Online microwave-assisted chiral derivatization-LC/MS (liquid chromatography/mass spectrometry) analysis system and method |
| CN106018596B (en) * | 2016-05-17 | 2018-09-14 | 华南理工大学 | A kind of online microwave radiation technology chiral derivatization-LC-MS analysis system and method |
| CN105806989A (en) * | 2016-05-26 | 2016-07-27 | 四川大学 | Method for simultaneously measuring trivalent chromium and hexavalent chromium in water samples by aid of low-pressure ion chromatograms and inductively coupled plasma mass spectra in combination manner |
| CN106226439A (en) * | 2016-09-23 | 2016-12-14 | 深圳天祥质量技术服务有限公司 | Chromic method of testing and ion chromatograph in a kind of leatherware |
| WO2018188184A1 (en) * | 2017-04-12 | 2018-10-18 | 岛津企业管理（中国）有限公司 | Multifunctional on-line combination device for temperature and pressue increase-assisted extraction, trapping, and chromatographic separation |
| CN107576742A (en) * | 2017-09-22 | 2018-01-12 | 广东中测食品化妆品安全评价中心有限公司 | The detection method of trivalent chromium in a kind of health food |
| CN109406699A (en) * | 2018-08-28 | 2019-03-01 | 浙江省海洋水产研究所 | The determination method of trivalent chromium and Cr VI in a kind of marine product |
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Application publication date: 20140806 |