CN214473051U - Pretreatment column for measuring acrylic acid sample in water by ion chromatography - Google Patents
Pretreatment column for measuring acrylic acid sample in water by ion chromatography Download PDFInfo
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- CN214473051U CN214473051U CN202022435697.9U CN202022435697U CN214473051U CN 214473051 U CN214473051 U CN 214473051U CN 202022435697 U CN202022435697 U CN 202022435697U CN 214473051 U CN214473051 U CN 214473051U
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Abstract
The utility model relates to an acrylic acid sample pretreatment column in ion chromatography survey water, be in including column tube and loading the filling layer of the inside of column tube, a serial communication port, column tube upper portion is equipped with one and goes up the import, the column tube bottom is equipped with down the export, the filling layer is including distributing three-layer ion exchange resin layer, one deck adsorbed layer and the four layers microporous filter membrane layer of co-altitude in the column tube, be one deck microporous filter membrane layer below every layer of ion exchange resin layer and the adsorbed layer of filling layer. The utility model discloses can once detach interfering substance such as suspended solid, hydrophobic organic matter, heavy metal ion, transition metal ion, chloride ion and sulfate ion in the different grade type water sample, experimental efficiency is high, and is with low costs, and the acrylic acid rate of recovery is high.
Description
Technical Field
The utility model relates to a water sample pretreatment technique, specifically a pretreatment device before acrylic acid in ion chromatography survey aquatic.
Background
Acrylic acid is an important chemical basic raw material, plays a significant role in the field of fine chemical engineering, is an important organic synthetic raw material and a synthetic resin monomer, is applied to polymer production in various fields, including the fields of resin, synthetic fiber, building materials, coatings, daily chemicals, textiles, adhesives, medical treatment, water treatment, electronics and the like.
However, the polymerization process may leave a small amount of residue of unpolymerized acrylic acid monomers, resulting in discharge of industrial wastewater containing acrylic acid monomers into rivers and offshore areas, causing water pollution. The acidity of the acrylic acid is strong, the polluted water body is acidified, acid-resistant algae and fungi are increased, rooted plants, bacteria and vertebrates are reduced, the decomposition rate of organic matters is reduced, and fishes in lakes and rivers are reduced or die seriously, so that the ecological system of the water body is damaged. In addition, acrylic acid solution or high concentration steam has irritation to human eyes and nasal mucosa, corrosion and irritation to skin when being applied on skin, and moderate toxicity. Therefore, monitoring of acrylic acid in water is essential.
The ion chromatography is used for measuring acrylic acid in water samples such as underground water, surface water, domestic sewage, industrial wastewater and the like, has high sensitivity, good selectivity and good repeatability, but suspended matters in water have larger particle size, easily causes the blockage of ion chromatography pipelines and damages instruments,therefore, a 0.45 mu m filter membrane is needed to filter a water sample before sample injection, and the interference of suspended matters is eliminated. Hydrophobic compounds, heavy metals and transition metals in higher concentrations in water can affect the chromatographic separation and shorten the useful life of the chromatographic column. C18The adsorption material can remove hydrophobic compounds in a water sample, and the Na-type sulfonate group ion exchange resin can remove heavy metals and transition metals in the water sample. Cl-And SO4 2-The concentration of common ions in the water is high, the content of acrylic acid is low, and the difference between the concentration of common ions in the water and the content of acrylic acid is generally 3-4 orders of magnitude. When the low-concentration acrylic acid is measured, the low-concentration acrylic acid is directly measured without diluting a water sample, and at the moment, if Cl is contained in the water sample-And SO4 2-Too high a concentration will have some effect on the lifetime of the column. The Ag type sulfonate group ion exchange resin and the Ba type sulfonate group ion exchange resin can respectively reduce Cl in water-And SO4 2-The concentration of (c).
At present, before measuring acrylic acid in water by using ion chromatography, suspended substances, hydrophobic organic matters, heavy metal ions, transition metal ions and Cl in water are removed if a sample is purified-And SO4 2-The interfering substances are preferably 0.45 μm filter membrane and C18A plurality of pretreatment columns such as columns, Na columns, Ag columns, Ba columns and the like not only waste time and labor and are expensive, but also have the problem of low recovery rate of acrylic acid.
SUMMERY OF THE UTILITY MODEL
The utility model aims at solving the shortcoming that exists among the prior art, and provide an acrylic acid sample pretreatment column in ion chromatography survey water, this pretreatment column can once detach interfering substance such as suspended solid, hydrophobic organic matter, heavy metal ion, transition metal ion, chloride ion and sulfate radical ion in the different grade type water sample, and the experimental efficiency is high, and is with low costs, and the acrylic acid rate of recovery is high. The utility model aims at being realized by the following technical scheme:
the utility model provides an acrylic acid sample pretreatment column in ion chromatography survey water, includes column tube 1 and loads the filling layer of the inside of column tube, its characterized in that, column tube upper portion is equipped with one and goes up import 3, the column tube bottom is equipped with down export 8, the filling layer is including distributing three-layer ion exchange resin layer, one deck adsorbed layer 7 and four layers microporous membrane layer 2 of different heights in the column tube, be one deck microporous membrane layer below every layer of ion exchange resin layer and the adsorbed layer of filling layer.
Further, three ion exchange resin layers of the filling layer are a Na type sulfonate group cation exchange resin layer 4, an Ag type sulfonate group cation exchange resin layer 5 and a Ba type sulfonate group cation exchange resin layer 6 respectively.
Further, the adsorption layer 7 of the filling layer is C18And an adsorption layer.
Further, the column tube 1 has a volume of 4 ml.
Further, the column tube 1 is cylindrical.
Further, the upper inlet 3 can be adapted to the plastic outlet of the syringe.
Further, the thin tubular lower outlet 8 can be directly inserted into the sample inlet of the ion chromatograph.
Furthermore, the shape of the microporous filter membrane layer 2 of the filling layer is circular, and the size of the microporous filter membrane layer is matched with that of the inner wall of the column tube.
Furthermore, the size of the microporous filter membrane layer of the filling layer is matched with the inner wall of the column tube.
Furthermore, the microporous filter membrane layer 2 of the filling layer is an acetate fiber filter membrane, and the diameter of the micropores is 0.45 μm.
Compared with the prior art, the utility model, beneficial effect does:
1. a plurality of pretreatment steps for measuring the acrylic acid by the ion chromatography can be simplified into one step, so that the recovery rate of the acrylic acid is improved, and the labor is saved;
2. the function of a plurality of pretreatment columns can be realized by one pretreatment column, so that the cost of consumables is reduced;
3. the method can remove interfering substances such as suspended matters, hydrophobic organic matters, heavy metal ions, transition metal ions, chloride ions, sulfate ions and the like in a water sample at one time, protect an ion chromatography system from being polluted by impurities, and improve the experimental efficiency;
4. the method is suitable for pretreatment of different types of water samples such as underground water, surface water, domestic sewage, industrial wastewater and the like;
5. the outlet of the pretreatment column can be inserted into the sample inlet of the ion chromatograph, so that the effluent can be directly injected, and the operation is convenient.
Therefore, compared with the prior art, the utility model, have advantages such as simple operation, acrylic acid rate of recovery are high, the experimental efficiency is high, use manpower sparingly, with low costs, be suitable for different grade type water sample pretreatment such as groundwater, surface water, domestic sewage and industrial waste water.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
In the figure:
1-column tube
2-microporous filter membrane layer
3-thin tubular upper inlet
4-Na type sulfonate group cation exchange resin layer
5-Ag type sulfonate group cation exchange resin layer
6-Ba type sulfonate group cation exchange resin layer
7-adsorption layer
8-thin tubular lower outlet.
Detailed Description
The invention will be further described with reference to the accompanying drawings:
with excess saturated Na+、Ag+And Ba2+The solution is respectively acted with a macroporous sulfonic acid resin column to obtain Na type sulfonate group ion exchange resin, Ag type sulfonate group ion exchange resin and Ba type sulfonate group ion exchange resin, and ion chromatography pretreatment small columns with different functions such as a Na column, an Ag column, a Ba column and the like are respectively prepared. Wherein, the Na column can remove heavy metals and transition metals in the water sample, and the Ag column can remove Cl-Ba column can remove SO4 2-。C18The adsorbing material can be used for preparing C18A column for removing hydrophobic compounds from a water sample.
At present, ion chromatography is used to determine acrylic acid in waterPurifying the sample to remove suspended substances, hydrophobic organic substances, heavy metal ions, transition metal ions, and Cl-And SO4 2-The interfering substances are preferably 0.45 μm filter membrane and C18A plurality of pretreatment columns such as a column, a Na column, an Ag column, and a Ba column. The embodiment improves the prior art, integrates all pretreatment columns, and designs a single pretreatment column comprising a plurality of filling layers.
As shown in figure 1, the utility model discloses an acrylic acid sample pretreatment column in ion chromatography survey water, be in including column tube 1 and loading the filling layer of the inside of column tube, its characterized in that, column tube upper portion is equipped with one and goes up import 3, the column tube bottom is equipped with down export 8, the filling layer is including distributing three-layer ion exchange resin layer, one deck adsorbed layer 7 and four layers microporous filter membrane layer 2 at the column tube co-altitude not, be one deck microporous filter membrane layer below every layer of ion exchange resin layer and the adsorbed layer of filling layer. The three ion exchange resin layers are three types of sulfonate group cation exchange resin layers respectively. The adsorption layer 7 is C18The adsorption layer 7 and the microporous filter membrane layer 2 are acetate fiber microporous filter membrane layers 2.
Example (b):
the pretreatment column for measuring the acrylic acid sample in water by the ion chromatography comprises a column tube 1 and a filling layer, wherein the column tube is cylindrical and is made of transparent plastic, the diameter of the column tube is 1.0cm, and the volume of the column tube is 4 ml. The middle of the upper part of the column tube is provided with a thin tubular upper inlet 3 with the diameter of 0.3cm, which can be connected with a plastic outlet of a universal injector, and the middle of the bottom of the column tube is provided with a thin tubular lower outlet 8 with the diameter of 0.3cm, which can be directly inserted into a sample inlet of an ion chromatograph.
The packing layer is filled in the column tube, and comprises 2g of Na type sulfonate group cation exchange resin layer 4, 2g of Ag type sulfonate group cation exchange resin layer 5, 2g of Ba type sulfonate group cation exchange resin layer 6 and 2g C18An adsorption layer 7 and four acetate fiber microporous filter membrane layers 2 with the diameter of 0.45 mu m.
In this embodiment, each ion exchange resin layer is a sulfonate group cation exchange resin layerNa type sulfonate group cation exchange resin layer 4, Ag type sulfonate group cation exchange resin layer 5, Ba type sulfonate group cation exchange resin layer 6. Na type sulfonate group cation exchange resin layer 4, Ag type sulfonate group cation exchange resin layer 5, Ba type sulfonate group cation exchange resin layer 6 and C18The adsorption layers are sequentially arranged from top to bottom. A microporous filter membrane layer 2 is arranged under each ion exchange resin layer and each adsorption layer.
The section of each microporous filter membrane layer 2 is circular, and the size of the microporous filter membrane layer is matched with the inner wall of the cylindrical column tube. The microporous filter membrane layer is made by using a high molecular chemical material and coating a pore-forming additive on the supporting layer after special treatment, and plays a role in isolating and buffering other layers of filling layers, so that a sample needing to be treated can be prevented from directly flowing to the bottom from the upper part of the column tube. The microporous filter membrane layer 2 has the advantages of uniform pore diameter, high porosity, no medium falling, thin texture, small resistance, high filtration speed and extremely small adsorption.
The working principle is as follows:
the utility model discloses an acrylic acid sample pretreatment column in ion chromatography survey water needs the activation before the use. 5ml of methanol is sucked by a disposable syringe, a plastic outlet of the syringe is inserted into a thin tubular upper inlet 3 of the pretreatment column, the column tube 1 is kept vertical to the ground direction, and the column tube is pushed into the pretreatment column at a speed of less than 2 ml/min. And then a disposable syringe is used for absorbing 10ml of deionized water, a plastic outlet of the syringe is inserted into the upper inlet 3 of the pretreatment thin tube, the column tube 1 is kept vertical to the ground direction, the column tube is pushed into the pretreatment column at the speed of less than 2ml/min, and the column tube is kept still and laid for 30min for activation.
After activation, a 10ml disposable injector is used for sucking a water sample to be detected, a plastic outlet of the injector is inserted into a pre-treatment thin tubular upper inlet 3, the direction of the column tube 1 perpendicular to the ground is kept, the water sample is injected at a speed of less than 2ml/min, the water sample flows out from a lower outlet 8 of the column tube, the initial 3ml effluent liquid is discarded, the subsequent effluent liquid is transferred into a sample cup, and an ion chromatograph automatic sample injector is used for sample injection analysis, or the thin tubular lower outlet 8 is inserted into a sample inlet of the ion chromatograph for direct sample injection.
The utility model is suitable for an ion chromatography detects acrylic acid's in aqueous survey pretreatment, can detach suspended solid, hydrophobic nature organic matter, heavy metal ion, transition metal ion, chloride ion and sulfate ion, and protection ion chromatographic system does not receive impurity contamination, simplifies complicated pretreatment step into one step, and the experimental efficiency is high, and the acrylic acid rate of recovery is high, and the simple operation uses manpower sparingly, and the consumptive material is with low costs.
Claims (10)
1. The utility model provides an acrylic acid sample pretreatment column in ion chromatography survey water, includes column tube (1) and loads the filling layer of the inside of column tube, its characterized in that, column tube upper portion is equipped with one and goes up import (3), the column tube bottom is equipped with down export (8), the filling layer is including distributing three-layer ion exchange resin layer, one deck adsorbed layer (7) and four layers micropore rete (2) of different heights in the column tube, be one deck micropore rete below every layer of ion exchange resin layer and the adsorbed layer of filling layer.
2. The pretreatment column for measuring acrylic acid in water by ion chromatography according to claim 1, wherein the three ion exchange resin layers of the packed layer are a Na sulfonate group cation exchange resin layer (4), an Ag sulfonate group cation exchange resin layer (5) and a Ba sulfonate group cation exchange resin layer (6).
3. The pretreatment column for measuring acrylic acid in water by ion chromatography as claimed in claim 1, wherein the adsorption layer (7) of the packing layer is C18And an adsorption layer.
4. The pretreatment column for measuring acrylic acid in water by ion chromatography as claimed in claim 1, wherein said column tube (1) has a volume of 4 ml.
5. The pretreatment column for measuring acrylic acid in water by ion chromatography as claimed in claim 1, wherein said column tube (1) has a cylindrical shape.
6. The pretreatment column for measuring acrylic acid in water by ion chromatography as claimed in claim 1, wherein said upper inlet (3) is adapted to be connected to a plastic outlet of a syringe.
7. The pretreatment column for measuring acrylic acid in water by ion chromatography as claimed in claim 1, wherein said lower outlet (8) can be directly inserted into the inlet of ion chromatograph.
8. The pretreatment column for measuring acrylic acid in water by ion chromatography as claimed in claim 1, wherein the microporous membrane layer (2) of the packing layer is circular in shape and has a size fitting the inner wall of the column tube.
9. The pretreatment column for measuring acrylic acid in water by ion chromatography as claimed in claim 1, wherein the size of the microporous filter membrane layer of the packing layer is matched with the inner wall of the column tube.
10. The pretreatment column for measuring acrylic acid in water by ion chromatography as claimed in claim 1, wherein the microporous membrane layer (2) of the packing layer is an acetate fiber membrane, and the diameter of the micropores is 0.45 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022435697.9U CN214473051U (en) | 2020-10-28 | 2020-10-28 | Pretreatment column for measuring acrylic acid sample in water by ion chromatography |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022435697.9U CN214473051U (en) | 2020-10-28 | 2020-10-28 | Pretreatment column for measuring acrylic acid sample in water by ion chromatography |
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| CN214473051U true CN214473051U (en) | 2021-10-22 |
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| CN202022435697.9U Active CN214473051U (en) | 2020-10-28 | 2020-10-28 | Pretreatment column for measuring acrylic acid sample in water by ion chromatography |
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