CN113049716B - Pretreatment device and method for analyzing water-soluble cation content in filth based on ion chromatography - Google Patents
Pretreatment device and method for analyzing water-soluble cation content in filth based on ion chromatography Download PDFInfo
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- CN113049716B CN113049716B CN202110454731.3A CN202110454731A CN113049716B CN 113049716 B CN113049716 B CN 113049716B CN 202110454731 A CN202110454731 A CN 202110454731A CN 113049716 B CN113049716 B CN 113049716B
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
Abstract
The invention belongs to the field of maintenance of operation states of power transmission and transformation equipment, and provides a pretreatment device and a pretreatment method for analyzing the content of water-soluble cations in pollutants based on ion chromatography. The fixing frame is used for fixing the auxiliary column, the communicating pipe, the anion exchange column and the filtrate collector. The method overcomes the problem that the sample after being exchanged by the anion exchange resin and removing interfering ions can not be directly used for ion chromatographic analysis because the pH value of the solution is increased after the sample passes through the anion exchange resin to cause cation precipitation.
Description
Technical Field
The invention relates to the technical field of maintenance of operation states of power transmission and transformation equipment, in particular to a pretreatment device and a pretreatment method for analyzing the content of water-soluble cations in pollutants by using an ion chromatography method.
Background
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Solid, liquid and gas pollutants are inevitably adhered to the surface of the power transmission and transformation equipment serving in the atmosphere. The composition of the filth can be divided into soluble substances and insoluble substances. Under the humid environment, water-soluble substances in the filth are ionized to form water-soluble ions which can conduct electricity and mainly comprise Zn 2+ 、Al 3+ 、Fe 3+ 、NH 4 + 、K + 、Na + 、Mg 2+ 、Ca 2+ Isocation and F - 、Cl - 、SO 4 2- 、NO 3 - 、HCO 3 - And the anions can reduce the insulating property of the external insulating part, thereby causing the potential safety hazard of the operation of the power transmission and transformation equipment. Research shows that the dirt layer is conductiveThe electrical properties are not only affected by the degree of fouling, but also related to the fouling composition. The composition and solubility differences of soluble salts in the dirt affect the conductivity of the dirt layer and further affect the insulating properties of the external insulating part. Therefore, the research on the composition and the content of the soluble components in the pollutants has important significance for evaluating the insulation state of the external insulation part.
The method for analyzing the positive ions in the pollutant components mainly comprises a titration method, a flame atomic absorption method, an inductively coupled plasma emission spectrometer and the like. The titration method has low cost and small technical difficulty, but is not suitable for measuring the trace components; the flame atomic absorption method and the inductive coupling plasma method have low detection limit and high detection speed, but are only suitable for the direct detection of metal elements and cannot directly detect the important component NH of pollutants 4 + . The ion chromatography can simultaneously analyze Li in the filth + 、Na + 、NH 4 + 、K + 、Mg 2+ 、Ca 2+ And the main cations are detected quickly and have low detection limit. However, ion chromatography requires a high sample requirement, and cannot contain components which easily poison the chromatographic column, so for a sample to be tested with a complex composition, pretreatment is usually performed before sample introduction. The ion exchange method is a common pretreatment technology for ion chromatography, and has the advantages of low cost, easily obtained materials, renewable resin and the like. The problems faced by the prior art are: the pH value of the sample is increased after the sample passes through the anion exchange resin, and Fe contained in the filth 3+ 、Al 3+ 、Zn 2+ 、Mg 2+ When metal cations are used, hydroxide precipitates are easily formed after the sample is treated according to the prior art, so that the sample is turbid and cannot be directly analyzed by an ion chromatography instrument.
Disclosure of Invention
In order to solve the problems, the invention provides a pretreatment device and a pretreatment method for analyzing the content of water-soluble cations in pollutants based on ion chromatography, which solve the problem that an ion chromatograph cannot be used for direct analysis because a sample becomes turbid after being treated by strong-base anion exchange resin on the premise of keeping the concentration of ions to be detected in the sample unchanged.
In order to achieve the purpose, the invention relates to the following technical scheme:
in a first aspect of the present invention, there is provided a pretreatment apparatus for analyzing a content of water-soluble cations in a filth based on ion chromatography, comprising: auxiliary column, anion exchange column, communicating pipe, filtrate collector; the bottoms of the auxiliary column and the anion exchange column are connected through a communicating pipe, the middle part of the communicating pipe is also provided with a liquid outlet, and a filtrate collector is arranged below the liquid outlet; the auxiliary column is internally provided with strong acid cation exchange resin, and the anion exchange column is internally provided with strong base anion exchange resin.
In a second aspect of the present invention, there is provided an ion chromatography system comprising: any of the above pretreatment devices.
In a third aspect of the present invention, there is provided a pretreatment method for analyzing the content of water-soluble cations in a foulant based on ion chromatography, comprising:
dissolving a sample to be detected in a solvent, and filtering insoluble substances to obtain a sample A;
taking two solutions with equal volumes from the sample A, and respectively recording the two solutions as a solution B, C;
and (3) treating the solution B by using a strong-acid cation exchange resin, treating the solution C by using a strong-base anion exchange resin, mixing the treatment solutions, diluting and fixing the volume to obtain a solution D, namely the pretreated sample solution to be detected.
In a fourth aspect of the invention, there is provided a use of any one of the above pretreatment apparatuses for operating condition maintenance of power transmission and transformation equipment.
The invention has the beneficial effects that:
(1) The invention overcomes the problem that the sample after being exchanged by anion exchange resin and removing interfering ions can not be directly used for ion chromatographic analysis because the pH value of the solution is increased after the sample passes through the anion exchange resin to cause cation precipitation.
(2) The pretreatment device has the advantages of easily available raw materials, low price, repeated regeneration and use and good economic benefit.
(3) The established sample pretreatment method can keep the ion concentration before and after sample treatment unchanged on the premise of not introducing impurity ions.
Drawings
FIG. 1 is a diagram of a pretreatment apparatus according to the present invention.
1. An auxiliary column; 2. an anion exchange column; 3. a strong acid cation exchange resin; 4. a strongly basic anion exchange resin; 5. an auxiliary column flow rate control valve; 6. an anion exchange column flow rate control valve; 7. a filtrate collector; 8. a fixed mount 9 and a communicating pipe.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
A pretreatment device for analyzing the content of water-soluble cations in pollutants based on ion chromatography comprises an auxiliary column, an anion exchange column, strong-acid cation exchange resin, strong-base anion exchange resin, an auxiliary column flow rate control valve, an anion exchange column flow rate control valve, a filtrate collector, a fixing frame and a communicating pipe. The fixing frame is used for fixing the auxiliary column, the communicating pipe, the anion exchange column and the filtrate collector.
In some embodiments, the auxiliary column and the anion exchange column are glassware with a rotary piston, the auxiliary column is internally filled with a strong acid cation exchange resin, and the anion exchange column is internally filled with a strong base anion exchange resin.
In some embodiments, the resin volume ratio of the auxiliary column to the anion exchange column is 1; the volume ratio of the filtrate collector to the anion exchange column is 3:1-5:1.
The invention also provides a pretreatment method for analyzing the content of water-soluble cations in the filth based on ion chromatography, which comprises the following steps:
s1, dissolving and filtering a sample to be detected by using deionized water, and filtering insoluble substances to obtain a sample A.
S2, taking 2 parts of solution B, C with a certain and equal volume from the solution A, passing the solution B through an auxiliary column filled with strong-acid cation exchange resin, and passing the solution C through an exchange column filled with strong-base anion exchange resin.
And S3, replacing ions in the exchange column with deionized water, mixing the strong-acid effluent flowing out of the auxiliary column and the strong-base turbid liquid flowing out of the anion exchange column in a communicating pipe, and then feeding the mixed liquid into a filtrate collector.
And S3, transferring the liquid in the filtrate collector to a volumetric flask, and using deionized water to fix the volume to a scale to obtain a solution D.
And S4, analyzing the composition and concentration of the cations in the solution D by using an ion chromatograph.
In some embodiments, the dissolving in step S1 comprises using a 0.45 μm filter membrane in the filtration operation; the filtration operation adopts reduced pressure filtration.
In some embodiments, the volume ratio of solution D to solution B or solution C is 10.
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The test methods in the following examples, which are not specified under specific conditions, are generally carried out under conventional conditions.
Example 1
Selecting Dionex TM An ICS-600 analytical ion chromatograph analyzes the cation component in a sample. The instrument parameters were as follows: dionex TM ICS-600 analytical ion chromatograph, chromeleon 7.2.10 chromatography workstation (Thermo Fisher Co.); ICS-600 scoreChromatography column of chromatography ion system: protective column IonPac CG12A (50 mm. Times.4 mm), analytical column IonPac CS12A (250 mm. Times.4 mm); suppressor CERS 500-mm; a CONDUCTIVITY DETECTOR DIONEX DS5 CONDUCTIVITY DETECTOR; leacheate: methanesulfonic acid (echiei (shanghai) chemical industry development limited); flow rate 1.0 ml/min -1 (ii) a The injection volume was 25. Mu.l. Li + 、Na + 、NH 4 + 、K + 、Mg 2+ 、Ca 2+ The cation mixed standard solution is purchased from the national analysis and test center for nonferrous metals and electronic materials, and is diluted into standard working solution by ultrapure water step by step. Resistivity of experimental water>18.2 M.OMEGA.cm of ultrapure water.
And (4) mixing the cation with the standard stock solution to prepare standard solutions with different mass concentrations. Measuring each concentration for 3 times, taking peak area as ordinate and standard solution mass concentration as abscissa, establishing standard working curve, and obtaining linear equation and correlation coefficient shown in Table 1, wherein y is peak area (μ S. Min), and x is mass concentration (mg. L) of component -1 )。
Table 1 element work curve correlation coefficient
Example 1
Referring to fig. 1, the present invention provides a pretreatment device for analyzing the content of cations in contaminants based on ion chromatography, which includes an auxiliary column 1, an anion exchange column 2, a strong acid cation exchange resin 3, a strong base anion exchange resin 4, an auxiliary column flow rate control valve 5, an anion exchange column flow rate control valve 6, a filtrate collector 7, a fixing frame 8 and a communicating tube 9. The fixing frame is used for fixing the auxiliary column 1, the communicating pipe 9, the anion exchange column 2 and the filtrate collector 7.
The soil sample a to be treated was transferred to a 100mL beaker and dissolved using 50mL of deionized water. Transferring the solution and insoluble substances in the beaker together to a suction filtration funnel, rinsing the beaker with deionized water for three times, wherein the deionized water is about 30mL in total, transferring the rinsing solution to the suction filtration funnel, performing suction filtration, and using 0.4Filtering with 5 μm filter membrane to obtain filtrate A 1 Filtering the filtrate A 1 Transferring to a 100mL volumetric flask for constant volume to obtain a solution A 2 。
Pipette 5.00mL of solution A with pipette 2 Transferring into auxiliary column 1 containing strong acid cation exchange resin 3, and transferring 5.00mL of solution A with liquid transfer gun 2 Transferring into an anion exchange column 2 filled with strongly basic anion exchange resin 4. Opening the auxiliary column flow rate control valve 5 and the anion exchange column flow rate control valve 6 to control the flow rates of the solution flowing out of the auxiliary column 1 and the anion exchange column 2 to be 5 mL/min -1 Within.
When the liquid level flows to be nearly level with the height of the strong acid cation exchange resin 3 or the strong base anion exchange resin 4, deionized water is added into the auxiliary column 1 or the anion exchange column 2, the liquid level of water in the ion exchange column is kept higher than the liquid level of the resin all the time, and air bubbles are prevented from entering the resin. Each column was used to replace the ions in the column with deionized water 4 to 5 times, each time with about 8mL of water. The strong acid liquid exchanged by the auxiliary column 1 and the strong alkaline turbid liquid containing the cations to be detected exchanged by the anion exchange column are mixed in the communicating pipe 9 and then subjected to acid-base neutralization, and the mixture enters the filtrate collector 7.
Transferring the clear transparent liquid in the filtrate collector 7 to a 100mL volumetric flask for constant volume to obtain clear transparent solution A to be detected 3 . And A 2 Solution comparison, test solution A 3 The composition of the cation in (1) is unchanged, and the concentration is diluted by 20 times.
For sample A under the above conditions 3 The cation component in (1) was analyzed to obtain Na + 、NH 4 + 、K + 、Mg 2+ 、Ca 2+ Respectively, the ion concentration of (A) is 6.65 mg.L -1 、3.55mg·L -1 、0.86mg·L -1 、1.22mg·L -1 、7.29mg·L -1 。
Example 2
Because of mixing the standard solution B 1 The filter is clear and transparent, does not need to be filtered, and only needs to be processed by a sample pretreatment device. Mixing of Standard solution B 1 Middle Li + 、Na + 、NH 4 + 、K + 、Mg 2+ 、Ca 2+ The ion concentration is 25 mg.L respectively -1 、100mg·L -1 、200mg·L -1 、100mg·L -1 、100mg·L -1 、500mg·L -1 Using a pipette to pipette 5.00mL of solution B 1 Transferring into auxiliary column 1 containing strong acid cation exchange resin 3, and transferring 5.00mL of solution B with liquid transfer gun 1 Transferring into an anion exchange column 2 filled with strongly basic anion exchange resin 4. Opening the auxiliary column flow rate control valve 5 and the anion exchange column flow rate control valve 6 to control the flow rates of the solution flowing out of the auxiliary column 1 and the anion exchange column 2 to be 5 mL/min -1 Within.
When the liquid level flows to be nearly level with the height of the strong acid cation exchange resin 3 or the strong base anion exchange resin 4, deionized water is added into the auxiliary column 1 or the anion exchange column 2, the liquid level of water in the ion exchange column is kept higher than the liquid level of the resin all the time, and air bubbles are prevented from entering the resin. Each column was used to replace the ions in the column with deionized water 4 to 5 times, each time with about 8mL of water. The strong acid liquid exchanged by the auxiliary column 1 and the strong alkaline turbid liquid containing the cations to be detected and exchanged by the anion exchange column are mixed in a communicating pipe 9, and then subjected to acid-base neutralization, and enter a filtrate collector 7.
Transferring the clear transparent liquid in the filtrate collector 7 to a 100mL volumetric flask for constant volume to obtain clear transparent solution B to be detected 2 . With solution B 1 In contrast, solution B 2 The composition of the cation in (1) is unchanged, and the concentration is diluted by 20 times.
Analysis of the cationic component under the above conditions gave B 2 Sample Li + 、Na + 、NH 4 + 、K + 、Mg 2+ 、Ca 2+ The ion concentration is 1.25 mg.L -1 、4.99mg·L -1 、9.99mg·L -1 、5.00mg·L -1 、4.98mg·L -1 、24.98mg·L -1 。
Comparative example 1
The soil sample a to be treated was transferred to a 100mL beaker and dissolved using 50mL of deionized water. Mixing the solution in the beaker with insoluble substancesTransferring into a suction filter funnel, rinsing the beaker with about 30mL of deionized water for three times, transferring the rinsing solution into the suction filter funnel, suction-filtering, and suction-filtering with a 0.45 μm filter membrane to obtain filtrate A 1 . 5mL of filtrate A was taken 1 The volume is determined to be 100mL volumetric flask to obtain filtrate A 2 。
Sample A was selected by using iCAP6300 full-spectrum direct-reading spectrometer of America thermal Power company 2 The cationic component in (1) was analyzed. The instrument parameters were as follows: power 1150W, atomizer pressure 30psi, assist flow 0.5L min -1 Pump speed 50 r.min -1 。
According to the basic principle of analysis spectral line selection, the selection sensitivity is high, the matrix has no interference or less interference on the selected spectral line, and the wavelengths of the spectral lines selected by the elements to be tested are determined through a spectral line selection experiment and are shown in the table 2.
TABLE 2 elemental spectral line wavelength (nm)
Since the iCAP6300 can simultaneously measure multiple elements, the elements to be measured are prepared in the same standard solution. The metal element is easily oxidized, and the standard solution needs 1% of HNO 3 The solution is fixed to a 100mL volumetric flask, and a mixed type standard solution calibration curve is prepared, wherein the concentration and the related coefficient are shown in Table 3.
TABLE 3 element concentration and calibration curve correlation coefficient
Sample A 2 After dilution by 20 times, sample A was obtained 3 ', measurement of sample A under the above-mentioned experimental conditions 3 ' in each element to be tested Na + 、K + 、Mg 2+ 、Ca 2+ The ion concentrations of (A) are: 6.53 mg. L -1 、0.84mg·L -1 、1.30mg·L -1 、7.31mg·L -1 . Comparative example and example 1 each element Na to be measured + 、K + 、Mg 2+ 、Ca 2+ Ion concentration of (2) 6.65 mg. Multidot.L -1 、0.86mg·L -1 、1.22mg·L -1 、7.29mg·L -1 The data consistency is good, which shows that the concentration of the ions to be detected in the sample is not changed after the pretreatment device and the pretreatment method are adopted.
NH 4 + Is an important component of the filth, and the iCAP6300 full-spectrum direct-reading spectrometer cannot measure NH 4 + Content of (2), measuring sample A by ion chromatography 3 Middle NH 4 + The content is 3.55 mg.L -1 Showing that the ion chromatograph measures NH in the filth 4 + The advantages of the content of the components.
Comparative example 2
As described in comparative example 1, except that B 1 Is a mixed standard solution without passing through a sample pretreatment device, li + 、Na + 、NH 4 + 、K + 、Mg 2+ 、Ca 2+ Respectively at a concentration of 25 mg. L -1 、100mg·L -1 、200mg·L -1 、100mg·L -1 、100mg·L -1 、500mg·L -1 Sample B 2 Is a mixed standard solution B 1 The concentration of the sample obtained after passing through the pretreatment device is diluted by 20 times. Sample B of example 2 2 Multiplying the concentration by 20 times to obtain Li + 、Na + 、NH 4 + 、K + 、Mg 2+ 、Ca 2+ The ion concentration is 25 mg.L respectively -1 、99.8mg·L -1 、199.8mg·L -1 、100mg·L -1 、99.6mg·L -1 、498.0mg·L -1 After the standard solution is processed by the device of the patent, li + 、Na + 、NH 4 + 、K + 、Mg 2+ 、Ca 2+ The recovery rates of (A) are respectively as follows: 100%, 99.8%, 99.9%, 100%, 99.6% and 99.6%, which shows that the recovery rate of the sample pretreatment device meets the requirement of ionic colorAnd (4) spectrum analysis requirements.
It should be noted that the above examples are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to the examples given, those skilled in the art can modify the technical solution of the present invention as needed or equivalent substitutions without departing from the spirit and scope of the technical solution of the present invention.
Claims (4)
1. A pretreatment method for analyzing the content of water-soluble cations in a filth based on ion chromatography is characterized by comprising the following steps:
dissolving a sample to be detected in a solvent, and filtering insoluble substances to obtain a sample A;
taking two solutions with equal volumes from the sample A, and respectively recording the two solutions as a solution B, C;
and (3) treating the solution B by using a strong-acid cation exchange resin, treating the solution C by using a strong-base anion exchange resin, mixing the treatment solutions, diluting and fixing the volume to obtain a solution D, namely the pretreated sample solution to be detected.
2. The pretreatment method for analyzing the content of water-soluble cations in a foulant based on ion chromatography according to claim 1, wherein a 0.22 μm or 0.45 μm filter is used in the solubilization and filtration operation.
3. The pretreatment method for analyzing the content of water-soluble cations in a foulant based on ion chromatography as set forth in claim 1, wherein the filtration operation is filtration under reduced pressure.
4. The pretreatment method for analyzing the content of water-soluble cations in a filth based on ion chromatography according to claim 1, wherein the volume ratio of the solution D to the solution B or the solution C is 10 to 25.
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| US5633171A (en) * | 1995-03-03 | 1997-05-27 | Dionex Corporation | Intermittent electrolytic packed bed suppressor regeneration for ion chromatography |
| CN205506774U (en) * | 2016-03-01 | 2016-08-24 | 中国石油化工股份有限公司 | Duolite device of survey sulfonic acid group content |
| CN106770886A (en) * | 2016-12-13 | 2017-05-31 | 国网山东省电力公司电力科学研究院 | Insulator contamination water-soluble cationic composition detection analyzes the chromatography of ions |
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| US5633171A (en) * | 1995-03-03 | 1997-05-27 | Dionex Corporation | Intermittent electrolytic packed bed suppressor regeneration for ion chromatography |
| CN205506774U (en) * | 2016-03-01 | 2016-08-24 | 中国石油化工股份有限公司 | Duolite device of survey sulfonic acid group content |
| CN106770886A (en) * | 2016-12-13 | 2017-05-31 | 国网山东省电力公司电力科学研究院 | Insulator contamination water-soluble cationic composition detection analyzes the chromatography of ions |
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