CN217112200U - Rapid purification column for trace analysis of halogenated organic pollutants - Google Patents

Abstract

The utility model discloses a rapid purification column for trace analysis of halogenated organic pollutants, which comprises a purification column body with a containing cavity, a sample liquid storage tank arranged at the top end of the purification column body, a filtering component arranged above the inside of the containing cavity of the purification column body, and a purification liquid outlet pipe arranged at the bottom end of the purification column body; the filter assembly is used for filtering solid matters in organic pollutants, a filler reaction area is arranged in the containing cavity of the purification column body, and the filler reaction area is used for purifying and degreasing a sample. The utility model discloses organic pollutant's sample extract is not through the concentration, directly filters solid-state particle through filter assembly, and the mixture reaction in with the purification column post is purified fast, effectively simplifies the pretreatment process of halogenated organic pollutant in the environmental sample, can avoid purifying the column post and be blockked up.

Description

Rapid purification column for trace analysis of halogenated organic pollutants

Technical Field

The utility model relates to an organic pollutant purifies technical field, mainly relates to a purify post fast for halogenated organic pollutant trace analysis.

Background

In recent years, Persistent Organic Pollutants (POPs) in the environment have attracted much attention, and the ministry of ecological environment of China indicates that persistent organic pollutants are monitored and incorporated into the national environmental monitoring system in' 2019 communique of ecological environmental conditions of China. The level of POPs in environmental samples is relatively low, typically at the ppb level, and therefore, analysis of POPs in environmental samples is typically trace analysis. Because POPs generally exist in a laboratory environment, the biggest difficulty of trace analysis is to avoid pollution of the background value of a laboratory; generally, the more complex the pretreatment process, the higher the background value of the target compound; therefore, the pretreatment process is simplified, the experimental efficiency can be improved, and the background pollution can be reduced.

At present, more than 50% of POPs are halogenated organic pollutants, because the halogenated organic pollutants are weak polar compounds, fat in a sample can be extracted simultaneously in the extraction process, and the interference of the fat on a target compound is large in the analysis of an instrument, so that the purification of the halogenated organic pollutants needs a degreasing purification step. The degreasing method comprises gel permeation chromatography, concentrated sulfuric acid extraction method and acidic silica gel column method. Gel permeation chromatography is to remove most of fat according to the difference of molecular size of the fat and a target compound, and then an acid silica gel column method is still adopted for further fat removal and purification. The halogenated organic pollutants have acid resistance, and can be purified and degreased by adopting a concentrated sulfuric acid extraction method or an acidic silica gel column method. The principle is that concentrated sulfuric acid is used for carbonizing fat, so that the purposes of degreasing and purifying are achieved.

The simplest pretreatment method for halogenated organic pollutants in an environmental sample at present is as follows: extracting the sample with solvent to obtain extractive solution, concentrating, purifying with acidic silica gel column or concentrated sulfuric acid to remove lipid, concentrating the purified eluate, diluting to desired volume, and performing analysis. The pretreatment process needs two times of concentration and is complicated. The concentrated sulfuric acid liquid-liquid extraction method is relatively less in use because the emulsification phenomenon is easy to generate.

The acidic silica gel column method is a common purification method, however, after the extract is concentrated, fat is also concentrated, and the fat content in the concentrated solution of the extract is high, which can cause the blockage of the acidic silica gel column, especially for biological samples rich in fat. For a sample with high fat content, gel permeation chromatography is usually adopted to remove most of fat, and then an acid silica gel method is adopted to further remove fat and purify, so that the operation is complicated.

SUMMERY OF THE UTILITY MODEL

The utility model aims to solve the technical problem that a quick purification column for halogenated organic pollutant trace analysis is provided, which is simple and convenient in sample pretreatment and effectively avoids blockage of an acidic silica gel column.

The utility model discloses the technical problem that will solve can adopt following technical scheme to realize:

a rapid purification column for trace analysis of halogenated organic pollutants is characterized by comprising a purification column body with a containing cavity, a sample liquid storage tank arranged at the top end of the purification column body, a filtering component arranged above the inside of the containing cavity of the purification column body, and a purification liquid outlet pipe arranged at the bottom end of the purification column body;

the inner diameter of the purification column cylinder is smaller than that of the sample liquid storage tank, and the inner diameter of the purification liquid outlet pipe is smaller than that of the purification column cylinder; the filtering component is used for filtering solid matters in organic pollutants, a packing reaction area is arranged in the containing cavity of the purifying column body, and the packing reaction area is used for purifying and degreasing a sample.

In a preferred embodiment of the present invention, the filler reaction zone is filled with a mixture of acidic silica gel and anhydrous sodium sulfate.

In a preferred embodiment of the present invention, a packing baffle is further disposed in the accommodating cavity of the purifying column body, and the packing baffle is disposed below the inside of the accommodating cavity; the region between the filler baffle and the filtering component is the filler reaction region, and the filler baffle is used for preventing solid mixture in the filler reaction region from leaking out and flowing to the purification liquid outlet pipe.

The utility model has the advantages that: a quick purification column for trace analysis of halogenated organic pollutants, wherein a sample extracting solution of organic pollutants is not concentrated, solid particles are directly filtered out through a filtering component, and the solid particles react with a mixture in a purification column body to be quickly purified, so that the pretreatment process of the halogenated organic pollutants in an environmental sample is effectively simplified, and the blockage of the purification column body can be avoided.

Drawings

Fig. 1 is a schematic structural diagram of a rapid purification column for trace analysis of halogenated organic pollutants according to the present invention.

Fig. 2 is a schematic structural diagram of a second embodiment of the present invention.

Fig. 3 is a schematic structural diagram of the filter assembly of the present invention.

Detailed Description

In order to make the technical means, creation features, achievement purposes and functions of the present invention easy to understand and understand, the present invention is further explained by combining with the specific drawings.

Referring to fig. 1 to 2, there is shown a rapid purification column for trace analysis of halogenated organic pollutants, comprising a purification column body 100 having a receiving chamber, a sample reservoir disposed at the top end of the purification column body 100, a filter assembly 400 disposed above the inside of the receiving chamber 110 of the purification column body 100, and a purification effluent pipe 300 disposed at the bottom end of the purification column body 100. The sample liquid storage tank, the purification column body 100 and the purification liquid outlet pipe 300 are made of glass materials, and the purification and degreasing processes of the sample are not influenced.

The height of the sample liquid storage tank is 50 mm; the sample reservoir may be a hollow cylindrical canister 210 (FIG. 1), the hollow cylindrical canister 210 having an inner diameter of 30 mm. Referring to fig. 2, the sample reservoir may also be a hollow cylindrical table 220, and the inner diameter of the hollow cylindrical table 220 is 50 mm. The sample liquid storage tank is provided with a scraping component, and the scraping component comprises a scraping plate arranged on the inner wall of the sample liquid storage tank, a motor for providing power for the scraping plate, and a transmission shaft for connecting an output shaft of the motor and the scraping plate; the motor is arranged above the outer side of the sample liquid storage tank, and the transmission shaft is vertically arranged on the symmetry axis of the sample liquid storage tank. And starting a motor, wherein an output shaft of the motor rotates to drive a transmission shaft to rotate around the shaft center, and the transmission shaft rotates to drive a scraper plate to horizontally scrape the halogenated organic pollutant sample extracting solution on the inner wall of the sample liquid storage tank.

The inner diameter of the purification column cylinder 100 is smaller than that of the sample reservoir, and the inner diameter of the purification effluent pipe 300 is smaller than that of the purification column cylinder 100. The inner diameter of the column body 100 of the purifying column is 10-20mm, and the height is 50 mm; preferably, the inner diameter of the purification column 100 is 15 mm. The inner diameter of the purified liquid outlet pipe 300 is 5-7mm, and the height is 10 mm; preferably, the inner diameter of the effluent purification tubes 300 is 6 mm.

The filter assembly 400 is used for filtering solid substances in organic pollutants, that is, the filter assembly 400 is used for filtering particulate substances in an organic pollutant sample, and the filtered organic pollutant sample is a first processing sample. Filter assembly 400 is made of a polyethylene material and is not susceptible to corrosion by the mixture in packing reaction zone 110. The thickness of the filter assembly 400 is 0.9-1.2mm, and the inner diameter is 10-20 mm; preferably, the filter assembly 400 has a thickness of 1mm and an inner diameter of 15 mm.

Referring to fig. 3, the filter assembly 400 includes a shrink disk 410 with a reduced outer diameter, a filter screen 420 disposed inside the shrink disk 410, and a shrink rod 430 extending from the inside of the shrink disk 410 to the outside, wherein the filter screen 420 has a pore size of 30-50 μm, which can prevent the filler in the filler reaction zone 110 from spilling during transportation; an adsorption part is arranged above the filter screen 420 and is used for washing solid particles in the sample extracting solution.

The overall shape of the collapsible rod 430 when expanded is x-shaped, and the overall shape of the collapsible rod 430 when closed is 1-shaped. The filter screen 420 is divided into two parts by the contraction rod 430, namely the contraction rod 430 is multiplied by the shape of the Chinese character 'ji' and the included angle is 0-150 degrees; preferably, the contraction rod 430 divides the filter screen 420 into two uniform halves through a point on the circumference of the contraction disk 410, and the contraction rod 430 x forms an included angle of 90 °. The x-shaped driven part of the contraction rod 430 is disposed inside the contraction disk 410, the x-shaped driving part of the contraction rod 430 is disposed outside the contraction disk 410, and a protection cover 431 is disposed on the outer circumference of the x-shaped driving part.

A sliding groove 411 is arranged on the periphery of one side of the X-shaped driven part on the outer annular surface of the shrink disk 410, a sliding block 412 is arranged in the opening area of the X-shaped driven part on the outer annular surface of the shrink disk 410, and the sliding groove 411 and the sliding block 412 are both in a convex shape; the distance between the central axis of the sliding groove 411 and the intersection point of the X shape is smaller than the diameter of the contraction disk 410, the sliding directions of the sliding groove 411 and the sliding block 412 are opposite, namely the sliding block 412 is in positive sliding fit with the sliding groove 411; the slider 412 of the shrink disk 410 is made of silica gel and has slight elasticity, and the other parts have no elasticity; the slider 412 can swing in the direction of the x-shaped intersection, and when the left and right portions of the shrink disk 410 cross each other to reduce the circumferential area, the slider 412 can be finely adjusted by itself to slide into the sliding groove 411 more favorably. The length of the sliding slot 411 and the sliding block 412 is less than half of the circumference of the shrink disk 410, and preferably, the length of the sliding slot 411 and the sliding block 412 is equal to a quarter of the circumference of the shrink disk 410, i.e. the shrink disk 410 has a quarter of the circumference contracted and the total width shortened by a quarter of the chord length.

An extraction opening is formed in the upper end of the outer annular surface of the purification column body 100, the overall dimension of the extraction opening is slightly larger than the width of the contraction disk 410 after contraction, and a silica gel pad is arranged on the contact surface of the contraction disk 410 and the extraction opening, so that leakage in the sample purification and degreasing process is effectively prevented. After grease removal is carried out by using the purifying column body 100, the X-shaped driving part and the X-shaped driven part of the shrinkage rod 430 are pressed by two hands, the sliding block 412 of the shrinkage disc 410 slides along the inner wall of the sliding groove 411, the radius of the sliding block 412 is gradually reduced inwards in the sliding process, and one fourth of the shrinkage disc 410 is overlapped; then the x-shaped driving part of the contraction rod 430 is pulled outwards, and the contraction rod 430 drives the contraction disk 410, the filter screen 420 and the adsorption part to be pulled out of the purification column cylinder 100; and finally, the residual substances on the contraction disk 410, the filter screen 420 and the adsorption piece are washed away by using clean water, the filter assembly 400 is simple in extraction mode and high in cleaning efficiency, and the blockage of the column body of the purification column caused by accumulation of the residual substances is prevented.

The holding cavity of the purifying column 100 is provided with a filler reaction area 110, and the filler reaction area 110 is used for purifying and degreasing the sample and is a main body part for purification. Filling a mixture of acidic silica gel and anhydrous sodium sulfate in the filler reaction zone 110, uniformly mixing the acidic silica gel and the anhydrous sodium sulfate, and adding the mixed filler mixture into the purification column body 100; the first treated sample flows into the purifying column 100, and the first treated sample reacts with the mixture in the packing reaction region 110, i.e. the purifying and degreasing reaction, and the reacted first treated sample is the second treated sample. The composition ratio of the acid silica gel to the anhydrous sodium sulfate is 1 to 10, and preferably, the composition ratio of the acid silica gel to the anhydrous sodium sulfate is 2.

A filler baffle 500 is also arranged in the accommodating cavity of the purifying column body 100, and the filler baffle 500 is arranged below the inner part of the accommodating cavity; the area between the packing baffle 500 and the filter assembly 400 is the packing reaction zone 110, and the packing baffle 500 is used to prevent the solid mixture in the packing reaction zone 110 from leaking out and flowing to the purge effluent tube 300. Packing baffles 500 are made of a polyethylene material and are not susceptible to corrosion by the mixture in packing reaction zone 110. The thickness of the filler baffle 500 is 0.9-1.2mm, the inner diameter is 10-20mm, and the aperture range is 30-50 μm; preferably, the packing baffle 500 has a thickness of 1mm, an inner diameter of 15mm, and a pore size in the range of 40 μm.

The utility model discloses halogenated organic pollutant's sample treatment experimental method does:

the extract of sample after ultrasonic extraction need not the concentration, directly purifies the degrease through purifying column cylinder 100, and specifically, the extract of sample gets into the sample liquid storage pot from the top and stores.

When the purifying column body 100 is used, a liquid outlet valve of the sample liquid storage tank is opened, the sample extracting solution flows into the purifying column body 100, solid particles are filtered out of the sample extracting solution through the filtering component 400, and the filtered sample is a first processing sample; then the first processed sample contacts and reacts with the mixture of the filler reaction area 110, concentrated sulfuric acid in the filler reaction area 110 removes fat in the first processed sample, and the first processed sample after being purified and removed of fat is a second processed sample; finally, the second processing sample solution flows through the filler baffle 500 and the purification liquid outlet pipe 300 in sequence and is collected by a collection container below; blowing nitrogen to dry, fixing the volume of the organic solvent, and waiting for loading.

The extracting solution is not concentrated and is directly and rapidly purified by a purifying column 100, so that the aim of simplifying the pretreatment process of halogenated organic pollutants in an environmental sample is fulfilled; the extracting solution is not concentrated, so the fat concentration is low, and the blockage of the acidic silica gel purifying column body can be effectively prevented.

The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the above embodiments, and that the foregoing embodiments and descriptions are provided only to illustrate the principles of the present invention without departing from the spirit and scope of the present invention. The scope of the invention is defined by the appended claims and equivalents.

Claims (2)

1. A rapid purification column for trace analysis of halogenated organic pollutants is characterized by comprising a purification column body with a containing cavity, a sample liquid storage tank arranged at the top end of the purification column body, a filtering component arranged above the inside of the containing cavity of the purification column body, and a purification liquid outlet pipe arranged at the bottom end of the purification column body;

the inner diameter of the purification column cylinder is smaller than that of the sample liquid storage tank, and the inner diameter of the purification liquid outlet pipe is smaller than that of the purification column cylinder; the filter assembly is used for filtering solid matters in organic pollutants, a filler reaction area is arranged in the containing cavity of the purification column body, and the filler reaction area is used for purifying and degreasing a sample.

2. The rapid purification column for trace analysis of halogenated organic pollutants as claimed in claim 1, wherein a filler baffle is further arranged in the containing cavity of the purification column body, and the filler baffle is arranged below the inside of the containing cavity; the region between the filler baffle and the filtering component is the filler reaction region, and the filler baffle is used for preventing solid mixture in the filler reaction region from leaking out and flowing to the purification liquid outlet pipe.

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