CN103983736A - Method for analyzing and detecting fluorine ions in complex matrix through membrane distillation technology as sample pretreatment method combined with ion chromatography - Google Patents
Method for analyzing and detecting fluorine ions in complex matrix through membrane distillation technology as sample pretreatment method combined with ion chromatography Download PDFInfo
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Abstract
The invention discloses a method for analyzing and detecting fluorine ions in a complex matrix through a membrane distillation technology as a sample pretreatment method combined with ion chromatography. The method comprises the following steps: performing pretreatment enrichment on a complex sample by the membrane distillation technology for extracting fluorine ions from the sample, and detecting through an ion chromatography method; adding sulfuric acid into the sample for acidifying, vaporizing the fluorine ions on the membrane surface in an HF form under a heated distillation condition, allowing the fluorine ions to enter the other side through membrane pores to be absorbed by an alkaline absorption solution, and intercepting other interfering components in a distilling flask by a hydrophobic membrane, thereby obtaining a solution of fluorine ions without matrix interference, wherein the membrane used by membrane distillation is a special polytetrafluoroethylene hydrophobic membrane, and the separated and purified fluorine ions are analyzed and detected by an ion chromatography system. The method has an excellent fluorine ion extraction effect, and is convenient, sensitive, rapid and accurate, and the influence of organic acids and other interferents on the fluorine ion detection is eliminated.
Description
Technical field
The invention provides a kind of film distillation (MD) technology of utilizing the complex matrices of fluoride ion is carried out to pre-treatment, and coupling ion chromatography carries out the new method of the analyzing and testing of fluorine ion to the product after processing.
Background technology
Fluorine is element common in environmental chemistry and life science, and it is also one of necessary trace element of human body, and fluorine depends on dosage to the health benefit of human body, takes in fluorine too much or very fewly all can bring adverse influence to health.Therefore, more note the impact of fluorine content on health in nature, drinking-water and food.
At present, the detection method of fluorine ion has: Fluoride ion selective electrode method, volumetric analysis, emission spectrometry, fluorometry, colourimetry etc.Wherein, Fluoride ion selective electrode method is to measure the standard method of fluorine ion, but the method exists following some deficiency: (1) is measured the pH value of solution and must strictly be controlled, and solution meta-acid or alkali all can affect the measurement result of fluorine ion; (2) if contain Fe in test solution
3+, Al
3+the complex compound that meeting and fluorine ion form difficult ionization affects measurement result; (3) fluoride ion selective electrode is measured and is subject to influence of temperature change larger; (4) fluorine ion of high concentration can make fluoride ion selective electrode produce passivation phenomenon, causes blank progressively to raise, the reappearance variation of mensuration, and accuracy of measurement declines.
In recent years, along with the development of Modern Analytical Instrument, the application of ion chromatographic method was more and more extensive, chromatography of ions has quick, sensitive, good selective.Use film distillation technology to there is not yet report as the method for the content of fluoride ion in the method detection of complex matrix of sample-pretreating method coupling chromatography of ions.The advantage that the method is analyzed micro-fluorine ion is significant, can obtain accurate result, reappearance, and the recovery is also higher, and film distillation pre-treating method stability is higher.
Adopt film distillation technology to there is not yet report as the method detection content of fluoride ion of sample-pretreating method coupling chromatography of ions.
Summary of the invention
The object of this invention is to provide a kind of new sample pretreating method, the method is that the complex matrices of fluoride ion is extracted to fluorine ion wherein with the enrichment of film distillation preprocess method, then sends out fluorine ion is carried out to analyzing and testing with chromatography of ions.
The present invention is achieved by the following technical solution:
The invention discloses a kind of film distillation (MD) technology and as sample-pretreating method coupling ion chromatography, be used for the method for the analyzing and testing of complex matrices fluorine ion, the method is first carried out pre-service enrichment extraction fluorine ion wherein with film distillation technology to complex sample, then sends out and detect with chromatography of ions.What sample pretreatment adopted is that film distillation technology extracts the fluorine ion in complex sample, specific as follows, first in sample, add sulfuric acid acidation, adding in thermal distillation situation, making fluorine ion vaporize and see through fenestra at face with HF form enters opposite side and is absorbed by alkaline absorption solution, and other interfering components are trapped in cucurbit by hydrophobic membrane, thereby obtain removing the solution of the fluorine ion of matrix interference, it is special teflon hydrophobic membrane that film distills film used.Fluorine ion after separation and purification is used ion chromatography system analyzing and testing again.The extraction effect of the method fluorine ion is good, and eliminated the impact that the chaff interferences such as organic acid detect fluorine ion, facilitates sensitive, quick and precisely.
As improving further, film distillation time of the present invention is 15min.
As improving further, method of the present invention also can be generalized to the detection of the negative ion (as inferior sulfate radical, chlorion, sulphion, cyanate radical, nitrite anions etc.) of other available film way of distillations extractions, and the detection of the kation that extracts of the available film way of distillation (as ammonium radical ion etc.), with similar scheme analysis, can eliminate the interference of interfering ion.
The present invention has following beneficial effect:
When film distillation technology carries out pre-service to complex sample first by sample sulfuric acid acidation, adding in thermal distillation situation, volatile components HF vaporizes and sees through fenestra at face and enters opposite side and absorbed by alkaline absorption solution, and other interfering components are trapped in cucurbit by hydrophobic membrane, thereby obtain removing the fluorine ion of matrix interference.Fluorine ion after separation and purification is used ion chromatography system analyzing and testing again, and the method can be measured trace or the Trace Fluoride ion in complex matrices, also can be used for having the detection of fluorine ion in the sample that a large amount of interfering ions exist.
The method is distilled this pre-treating method by film, make has the organic matter that pollutes and disturb to be eliminated to ion chromatography system in chromatography of ions, thereby greatly widened the range of application of chromatography of ions detection fluorine ion, sensitivity and the accuracy measured have greatly been improved, the method is not only applicable to fluid sample simultaneously, also applicable to solid sample, hydrophobic membrane can be reused in addition, vapo(u)rizing temperature is relatively low, so the method can be widely used in the detection analysis of fluorine ion in water quality detection, food security, industrial standard, environmental monitoring etc.There is no this type of detection method report both at home and abroad.
In sum, the present invention may be summarized to be following feature:
1. sample pretreatment is convenient and swift, and film still-process only needs 15min;
2. eliminated the interference that the organic acids such as formate, acetate detect fluorine ion, made the method there is universality;
3. film distillation technology has the effect of enrichment simultaneously to the extraction of fluorine ion in complex matrices, can make the detection limit of fluorine ion in sample greatly reduce;
4. the method has a wide range of applications face to sample, and not only fluid sample can carry out pre-treatment with film distillation technology, and solid sample also can be distilled and be carried out ion chromatography again by film;
5. in film distillation, applicable hydrophobic poly tetrafluoroethylene can repeat to be suitable for, energy-conserving and environment-protective;
6. film distillation is compared with common distillation, and vapo(u)rizing temperature is low, can save energy consumption;
7. sulfate by ion chromatography has the feature sensitive and accurate, detection limit is low, can carry out the detection of Trace Fluoride ion, and detects quick and convenient pollution-free.
Accompanying drawing explanation
Fig. 1 is the molecular structure of teflon (PTFE) hydrophobic membrane that in the present invention, film distillation is used;
Fig. 2 is device and the work schematic diagram that in the present invention, film distills fluorine ion in complex pretreatment matrix;
In Fig. 2, be labeled as: 1-cucurbit, 2-enrichment absorption bottle, 3-teflon (PTFE) hydrophobic membrane;
In Fig. 2, be the distillation device of autonomous Design, left side is special cucurbit, and sample is acidifying in cucurbit, and is heated distillation, and volatile constituent is entered enrichment absorption bottle and is completely absorbed by elite teflon hydrophobic membrane.Before sample being carried out to film distillation pre-treatment, need to enrichment absorption bottle and pipe path, clean with deionized water.
Fig. 3 is device and the work schematic diagram of intermediate ion stratographic analysis fluorine ion of the present invention;
In Fig. 3, be labeled as: 4-leacheate, 5-pump, 6-six-way valve, 7-guard column, 8-anion separation column, 9-anion suppressor, 10-detecting device;
Fig. 4 is the chromatography of ions spectrogram of the complex matrices sample Tie Guanyin tea fluorine ion that enrichment extracts after film distillation pre-service;
In Fig. 4, be labeled as: the peak of fluorine ion after the distillation of 11-Tie Guanyin tea film;
Fig. 5 is the chromatography of ions spectrogram of the strong white toothpaste of tooth of the complex matrices sample China fluorine ion that enrichment extracts after film distillation pre-service;
In Fig. 5, be labeled as: the peak of fluorine ion after the strong tooth tunica albuginea distillation of 12-China.
Embodiment
The invention discloses a kind of film distillation (MD) technology and as sample-pretreating method coupling ion chromatography, be used for the method for the analyzing and testing of complex matrices fluorine ion, first to the acidifying of complex matrices sample and carry out film distillation and process, film distillation technology can make volatile components HF in the sample after acidifying vaporize at face, thereby HF gas permeation fenestra enters opposite side and is absorbed, and other complexity or noisy not volatile components are trapped in cucurbit by hydrophobic membrane, thereby realize the separating-purifying of fluorine ion to be measured and enrichment, use again the content of fluoride ion in ion-chromatographic determination product.Film distillation preconditioning technique is as follows: utilize the distillation device designing, in complex matrices, add excess sulfuric acid with souring soln, make the fluorine ion in sample be converted into hydrogen fluoride, this distilling apparatus is heated to 80 ℃ simultaneously, hydrogen fluoride is distilled out from cucurbit with gas form, and see through hydrophobic membrane and enter in the alkaline absorbent solution of opposite side, thereby obtain the fluorine ion solution of separating-purifying, this solution can direct injected to analyzing and testing in ion chromatography system.The method is for there being a large amount of interfering ions to exist the fluorine ion in situation to detect especially effective in the analyzing and testing of the fluorine ion of trace in complex matrices or trace or sample, and pre-treating method is all suitable for fluid sample and solid sample, film distillation technology also has fast and convenient efficient, the advantage such as film can reuse, vapo(u)rizing temperature is relatively low in addition, can be widely used in the detection analysis of fluorine ion in water quality detection, food security, industrial standard, environmental monitoring etc.
Fig. 1 is the molecular structure of teflon (PTFE) hydrophobic membrane that in the present invention, film distillation is used: teflon molecule has unique helical structure.This unique helical structure has been protected teflon carbochain skeleton just, and fluorine atom has high chemical inertness simultaneously, and this makes teflon become the polymkeric substance that surface energy is minimum, resistance to chemical attack is optimum.What the present invention simultaneously selected is hydrophobicity poly tetrafluoroethylene, and its hydrophobic property makes water can not penetrate film, only has gas phase can pass through film.
Fig. 2 is device and the work schematic diagram that in the present invention, film distills fluorine ion in complex pretreatment matrix:
Complex matrices (as tealeaves) is put into the cucurbit 1 of Fig. 2, and add slightly excess sulfuric acid acidifying, open heating arrangement simultaneously cucurbit 1 is carried out to laser heating, heating-up temperature general control is 80 ℃ of left and right, in this process, volatile constituent in complex matrices is constantly distilled out, volatile component arrives teflon hydrophobic membrane 3 assemblies through pipeline, hydrophobic property due to film, moisture can not penetrate film, only have escaping gas can pass through membrane module, fluorine ion can be absorbed by membrane module and in enrichment absorption bottle 2 after being reacidified to hydrogen fluoride gas.In absorption bottle, fill sodium hydroxide solution, not only accelerated other absorption of hydrogen fluoride, and can make hydrogen fluoride thoroughly be absorbed with fluorine ion form.The result of film distillation pre-treatment be by the not volatile rejection to organics of Various Complex in sample in stoste, fluorine ion enrichment is extracted in the absorption bottle 2 in Fig. 2 distillation device simultaneously.When sample being carried out to film distillation pre-treatment, first with deionized water, whole device is cleaned, meanwhile, before each use, need teflon hydrophobic membrane 3 to carry out the ultrasonic processing of deionized water 20 minutes, to prevent the pollution of fluorine to film, poly tetrafluoroethylene is reusable.As further improvement, the teflon hydrophobic membrane 3 in film distillation pretreating device is for to be embedded in the bottle cap of cucurbit 1, and whole distillation device will guarantee good impermeability simultaneously.
Fig. 3 is device and the work schematic diagram of intermediate ion stratographic analysis fluorine ion of the present invention:
The fluorine ion solution being extracted by the film distillation pretreating device of Fig. 2 through injector to inject sample introduction in chromatography of ions system.In chromatography of ions system, leacheate 4 is 30mmolL-1KOH solution; leacheate 4 pumps in chromatography of ions stream by pump 5; by the valve of six-way valve 6, cut and can make leacheate 4 by fluorine ion eluant solution; enter successively afterwards guard column 7, anion analysis post 8, anion suppressor 9, finally by 10 pairs of fluorine ions of detecting device, detect.
Fig. 4 is the chromatography of ions spectrogram of the complex matrices sample Tie Guanyin tea fluorine ion that enrichment extracts after film distillation pre-service:
Fig. 4 utilizes the film distillation pre-treating method designing in Fig. 2 to carry out enrichment extraction to Tea Samples, and coupling chromatography of ions detects test quantity of fluoride in tea ion, thus the chromatography of ions image obtaining, and 11 in Fig. 4 is the chromatographic peak of fluorine ion.Than not carrying out the pre-treatment of the film way of distillation just directly with the content of fluoride ion in sulfate by ion chromatography tealeaves, this method has obvious advantage: as shown in Figure 4, the interference that this method does not exist complicated organic substrate to detect fluorine ion, can contaminated ion chromatogram system, especially can not damage chromatographic column, in addition, this method pre-treatment has inrichment to fluorine ion, even content of fluoride ion seldom also can be detected in sample.
Fig. 5 is that the chromatography of ions spectrogram of the strong white toothpaste of tooth of the complex matrices sample China fluorine ion that enrichment extracts after film distillation pre-service: Fig. 5 utilizes the film distillation pre-treating method designing in Fig. 2 to carry out enrichment extraction to toothpaste sample, and coupling chromatography of ions detects Fluoride in Toothpaste ion, thereby the chromatography of ions image obtaining, 12 in Fig. 5 is the chromatographic peak of fluorine ion.Than not carrying out the pre-treatment of the film way of distillation just directly with the content of fluoride ion in sulfate by ion chromatography toothpaste, this method has obvious advantage: as shown in Figure 5, the interference that this method does not exist complicated organic substrates to detect fluorine ion, can contaminated ion chromatogram system, especially can not damage chromatographic column, in addition, this method pre-treatment has inrichment to fluorine ion, even content of fluoride ion seldom also can be detected in sample.
Below by specific embodiment, technical scheme of the present invention is further described:
Embodiment 1
In complex matrices Tie Guanyin tea, the separated coupling ion chromatography analysis detection of the film distillation technology of fluorine ion concrete steps are as follows:
1, preparation simulation Tea Samples: according to each Contents of Main Components in tealeaves, take the tea water extract of corresponding a certain amount of reagent (caffeine, vitamin C, zinc fluoride, flavonols, manganese, selenium etc.) preparation simulation.
2, sample pretreatment: simulation Tea Samples is carried out to film distillation pre-service with film way of distillation pretreatment unit.By condition optimizing, test, show that optimum film distillation time is 15min.
3, the selection of leacheate: test different eluent concentrations, be finally defined as 30mmolL-1KOH solution as leacheate, can make fluorine ion go out fast peak in 3 minutes.
4, the separation and detection of fluorine ion in actual Tea Samples: actual Tea Samples is carried out to film distillation pre-service according to the optimal conditions obtaining, and coupling chromatography of ions detects content of fluoride ion wherein, reach a conclusion for content of fluoride ion in Tie Guanyin tea sample be 199.50mg/L.
Embodiment 2
It is as follows that the separated coupling ion chromatography analysis of film distillation technology of the strong white Fluoride in Toothpaste ion of tooth of complex matrices China detects concrete steps:
1, preparation simulation toothpaste sample: according to each Contents of Main Components in toothpaste, take the toothpaste leachate of corresponding a certain amount of reagent (calcium carbonate, calcium monohydrogen phosphate, calcium pyrophosphate, silicon dioxide, aluminium hydroxide, glycerine, sorbierite, xylitol, fluoride etc.) preparation simulation.
2, sample pretreatment: simulation toothpaste sample is carried out to film distillation pre-service with film way of distillation pretreatment unit.By condition optimizing, test, show that optimum film distillation time is 15min.
3, the selection of leacheate: test different eluent concentrations, be finally defined as 30mmolL-1KOH solution as leacheate, can make fluorine ion go out fast peak in 3 minutes.
4, the separation and detection of fluorine ion in actual toothpaste sample: actual toothpaste sample is carried out to film distillation pre-service according to the optimal conditions obtaining, and coupling chromatography of ions detection content of fluoride ion wherein, reaching a conclusion as China is good for content of fluoride ion in the white toothpaste sample of tooth is 121.30mg/L.
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 (6)
1. a film distillation technology is used for the method for the analyzing and testing of complex matrices fluorine ion as sample-pretreating method coupling ion chromatography, it is characterized in that, described method is first with film distillation technology, complex sample to be carried out to pre-service enrichment extraction fluorine ion wherein, then sends out and detect with chromatography of ions.
2. film distillation technology according to claim 1 is used for the method for the analyzing and testing of complex matrices fluorine ion as sample-pretreating method coupling ion chromatography, it is characterized in that, what described sample pretreatment adopted is that film distillation technology extracts the fluorine ion in complex sample.
3. film distillation technology according to claim 1 and 2 is used for the method for the analyzing and testing of complex matrices fluorine ion as sample-pretreating method coupling ion chromatography, it is characterized in that, described concrete steps are, first in sample, add sulfuric acid acidation, adding in thermal distillation situation, making fluorine ion vaporize and see through fenestra at face with HF form enters opposite side and is absorbed by alkaline absorption solution, and other interfering components are trapped in cucurbit by hydrophobic membrane, thereby obtain removing the solution of the fluorine ion of matrix interference, fluorine ion after separation and purification is used ion chromatography system analyzing and testing again.
4. film distillation technology according to claim 3 is used for the method for the analyzing and testing of complex matrices fluorine ion as sample-pretreating method coupling ion chromatography, it is characterized in that, described film distillation time is 15min.
5. film distillation technology according to claim 3 application for the analyzing detecting method of complex matrices fluorine ion as sample-pretreating method coupling ion chromatography, it is characterized in that, the detection of the negative ion that described method is extracted for the film way of distillation, and the cationic detection of extracting for the film way of distillation, with similar scheme analysis, can eliminate the interference of interfering ion.
6. film distillation technology according to claim 5 application for the analyzing detecting method of complex matrices fluorine ion as sample-pretreating method coupling ion chromatography, it is characterized in that, the detection of the inferior sulfate radical that described method is extracted for the film way of distillation, chlorion, sulphion, cyanate radical, nitrite anions, and the detection of the ammonium radical ion extracting for the film way of distillation.
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| CN105301149A (en) * | 2015-12-06 | 2016-02-03 | 杭州飞山浩科技有限公司 | Analysis device and method for determining trace fluorine ions in blood sample online |
| 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 |
| CN106198846A (en) * | 2016-08-31 | 2016-12-07 | 大连博融新材料股份有限公司 | A kind of distillation absorbs chromatography of ions detection electrolyte sulfite radical content method |
| CN114486873A (en) * | 2022-02-28 | 2022-05-13 | 云南水富云天化有限公司 | Method for measuring content of chloride ions in polyglutamic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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