CN212214673U - Allochroic azo solid-phase extraction column - Google Patents
Allochroic azo solid-phase extraction column Download PDFInfo
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- CN212214673U CN212214673U CN202020635846.3U CN202020635846U CN212214673U CN 212214673 U CN212214673 U CN 212214673U CN 202020635846 U CN202020635846 U CN 202020635846U CN 212214673 U CN212214673 U CN 212214673U
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Abstract
The utility model relates to the technical field of chemical instruments and discloses a color-changing azo solid-phase extraction column, which comprises a column tube, an upper sieve plate and a lower sieve plate which are arranged in the column tube at intervals; the top of the column tube is provided with an open sample adding port, and the bottom of the column tube is provided with a conical discharge port; an extraction cavity is formed between the upper sieve plate and the lower sieve plate, a color changing layer and an extraction layer are sequentially arranged in the extraction cavity from top to bottom, the color changing layer and the extraction layer are both filled with purified and activated diatomite, and flavanthrone is adsorbed on the diatomite of the color changing layer; the aperture of the lower sieve plate is smaller than the particle size of the diatomite of the extraction layer. The utility model discloses an azo solid phase extraction post discolours simple structure, convenient to use easily makes, and has the instruction function of discolouing, and the extraction in-process velocity of flow is fast and stable, continuous layer, and the powder that does not leak, aromatic amine rate of recovery are stable and good reproducibility, are fit for popularizing and applying.
Description
Technical Field
The utility model relates to a chemical instrumentation technical field, more specifically relates to an azo solid phase extraction post discolours.
Background
After textiles, clothes, leather products and footwear products are dyed by azo dyes containing forbidden aromatic amine, if the products are used for a long time, azo fuel can enter a human body through skin, and the azo dyes can generate decomposition reduction reaction under the biochemical condition of normal metabolism of the human body to release carcinogenic aromatic amine. The carcinogenic aromatic amine can change the DNA structure of a human body through activation, and finally causes human body pathological changes and induces cancers.
For the detection of azo dyes in textiles, clothing, leather products and footwear products, the detection methods specified in the national standard GB/T17592 plus 2011 'determination of azo dyes forbidden for textiles' and GB/T19942 plus 2005 'determination of azo dyes forbidden for leather and fur chemical tests' are mainly adopted at present, and although the two standard determination methods refer to the treatment steps of 'extracting by using a kieselguhr extraction column and then concentrating the extraction liquid', the method only provides that the extraction column using kieselguhr as a filler is used for purifying and enriching decomposed aromatic amine, and has no detailed description about the structure of the extraction column.
At present, azo solid-phase extraction columns commonly used by detection mechanisms are mainly commercially available diatomite extraction columns of different manufacturers, and due to different structures and specifications, the recovery rate of forbidden aromatic amine by the extraction columns is unstable, the repeatability is poor, especially for aromatic amine with unstable properties such as 2, 4-diaminoanisole, the influence is great, the recovery rate fluctuates between 2% and 90%, and the recovery rate is seriously beyond the range specified by the standard; meanwhile, most of the existing extraction columns have the defects of low and unstable flow rate, low extraction efficiency, easy breaking of diatomite, easy powder leakage and the like in the extraction process, and the accuracy and the detection efficiency of detection results are seriously influenced.
In addition, although some existing azo solid-phase extraction columns have the function of color change of test paper and can detect whether the preparation of azo mixed detection liquid meets the standard requirements or not and develop color, the extraction columns have the disadvantages of complex manufacturing process, need to prepare and install test paper, complex structure and high cost.
Therefore, it is necessary to provide a color-changing azo solid phase extraction column which solves the above problems.
SUMMERY OF THE UTILITY MODEL
The utility model provides an azo solid phase extraction post discolours, mainly used solve the forbidden aromatic amine rate of recovery that the present azo diatomaceous earth extraction post that detects exists unstable, the repeatability is relatively poor, the velocity of flow is slow and unstable, the extraction inefficiency and the extraction in-process diatomaceous earth easily fault, easily leak the powder, seriously influence the problem of the accuracy of testing result.
For solving the technical problem, the utility model discloses the technical scheme who adopts as follows:
a color-changing azo solid-phase extraction column comprises a column tube, an upper sieve plate and a lower sieve plate which are arranged in the column tube at intervals, wherein the top of the column tube is provided with an open sample adding port, and the bottom of the column tube is provided with a conical discharge port;
an extraction cavity is formed between the upper sieve plate and the lower sieve plate, a color changing layer and an extraction layer are sequentially arranged in the extraction cavity from top to bottom, the color changing layer and the extraction layer are both filled with purified and activated diatomite, flavanthrone is adsorbed on the diatomite of the color changing layer after impregnation, and the color changing reaction can occur when the diatomite meets a sodium hydrosulfite solution;
the aperture of the lower sieve plate is smaller than the particle size of the diatomite of the extraction layer.
Solid phase extraction, also known as solid phase extraction, is a separation technique combining processes such as selective retention and selective elution, and has been increasingly regarded as an important means for sample pretreatment. The principle is as follows: when a complex sample solution passes through the adsorbent, the adsorbent can selectively retain a target compound and a small amount of interferent with similar properties to the target compound through polar interaction, hydrophobic interaction or ion exchange and other acting forces, other components flow out of the small column through the adsorbent, and then the target compound is selectively eluted by using another solvent system with stronger elution capacity, so that the separation, purification and enrichment of the complex sample are realized.
The utility model discloses an azo solid phase extraction post discolours uses diatomaceous earth as the adsorbent. The diatomite is siliceous biological sedimentary rock with opal as main mineral component and SiO as main chemical component2The diatomite has white, grey and other colors, and may be used as excellent extracting medium for purifying and activating soil before use and changing its granularity distribution state and surface property.
Furthermore, the inner diameter of the column tube is 26-28 mm, and the length of the column tube is not less than 150 mm.
Further, go up the sieve and all adopt the sintering of polyethylene powder to form with lower sieve, go up the sieve all with the diameter of sieve down with the internal diameter of column tube is the same, and go up the side of sieve and lower sieve respectively with column tube inner wall butt and relatively fixed. The polyethylene powder is adopted for sintering, so that the upper sieve plate and the lower sieve plate have uniform holes, the uniform distribution of the extraction liquid is facilitated, the stable flow velocity is ensured, and a smooth flow channel is provided for the extraction liquid; simultaneously, go up the sieve and can play the upper and lower effect that compresses tightly to the diatomaceous earth on discoloration layer and extraction layer with lower sieve, lower sieve can also play the supporting role to the diatomaceous earth on last sieve and discoloration layer and extraction layer, can prevent like this that the diatomaceous earth is loose, avoids extraction in-process diatomaceous earth to appear the fault and the slow, unstable phenomenon of velocity of flow, and then ensures azo solid phase extraction post normal use.
Furthermore, the thickness of the upper sieve plate is 2.4-2.6 mm, and the aperture of the upper sieve plate is not less than 80 μm.
Furthermore, the thickness of the lower sieve plate is 2.2-2.5 mm, and the aperture of the lower sieve plate is 20-40 μm.
Furthermore, the diatomite of the extraction layer has the particle size of 0.2-2.0 mm and the specific surface area of 25-40 m2The diatomite filling particle size distribution rule of the extraction layer is as follows: the particle size of the diatomite gradually becomes coarse from bottom to top along the column tube, and the particle size distribution is favorable for forming a hierarchical adsorption extraction effect, so that the flow speed of the extraction solution is high and stable, the elution time is shortened, and the extraction efficiency is improved.
Furthermore, the filling thickness of the diatomite in the extraction layer is 88-94 mm, and the filling amount of the diatomite is 15-20 g.
Furthermore, the diatomite filling thickness of the color changing layer is 2-3 mm.
Further, the column tube top is provided with the otic placode around the sample addition port level, like this, is convenient for place the extraction post on test-tube rack or other supports, can steadily carry out the extraction operation safely, moreover, also is convenient for take or remove the extraction post through the otic placode.
Furthermore, the pillar tube is of an integrally formed structure, and the pillar tube is made of plastic, so that the pillar tube is corrosion-resistant, good in strength, easy to machine and form and low in cost.
The utility model discloses a color-changing layer diatomaceous earth dipping dyeing method in the azo solid phase extraction post that discolours is as follows:
taking 5-10 g of flavanthrone, adding 60-100 mL of 20-60% NaOH solution, uniformly mixing, adding distilled water to dilute to 1000mL, and adding 10-30 g of sodium hydrosulfite to carry out reduction reaction for 30-60 min to prepare dye liquor;
and secondly, adding a proper amount of purified and activated white diatomite into the dye solution obtained in the step I, soaking and dyeing, standing for 5-10 min, taking out, oxidizing and airing in the air to obtain the diatomite which is uniform, bright and yellow, and further filling the diatomite into the column tube according to the amount to form a color-changing layer.
Flavanthrone: also called vat yellow G, orange (or golden yellow) powder, is a vat dye type high-grade organic pigment variety, and has higher transparency, light resistance and weather fastness. The flavanthrone is dark orange in concentrated sulfuric acid and generates yellow precipitate after being diluted; blue in alkaline sodium hydrosulfite solution (sodium hydrosulfite dye liquor); green in acid reducing solution.
The reaction color change principle of the color change layer in the color change azo solid phase extraction column is as follows: the diatomite of the color-changing layer is impregnated and adsorbed with flavanthrone, so that a sodium hydrosulfite solution (sodium hydrosulfite dye solution) meeting alkalinity can generate a color-changing reaction, the color is changed from bright yellow to blue, and a color-developing indicating effect is achieved, so that whether the preparation step of the azo mixed standard solution to be extracted is correct or not can be judged, and if the color is not changed, the preparation step of the azo mixed standard solution is wrong, and the final azo detection result can be influenced.
Compared with the prior art, the utility model discloses technical scheme's beneficial effect is:
1. the color-changing azo solid-phase extraction column has simple structure, few internal accessories, material saving, easy manufacture, low cost and convenient use, and is suitable for popularization and application;
2. the utility model discloses an azo solid phase extraction post discolours is provided with upper screen plate and lower sieve in, can play relative compaction and supporting role from top to bottom to the diatomaceous earth on discolour layer and extraction layer, prevents that the diatomaceous earth is loose, can avoid extraction liquid velocity of flow slow, unstable phenomenon in the extraction process, and aromatic amine recovery rate is stable and good repeatability, and diatomaceous earth is difficult for the fault in the extraction process, and extraction liquid velocity of flow is fast and stable, and elution consuming time is short, can improve the accuracy of testing result and promote extraction detection efficiency;
3. the aperture of the lower sieve plate of the color-changing azo solid-phase extraction column is smaller than the diatomite particle diameter of the extraction layer, so that the powder leakage phenomenon in the extraction process can be prevented, the accuracy of the final detection result is ensured, and the service life of the extraction column is prolonged;
4. the utility model discloses a set up the discoloration layer in the azo solid phase extraction post that discolours, because the diatomaceous earth adsorption of discoloration layer has flavanthrone, meets alkaline sodium hydrosulfite solution (sodium hydrosulfite dye liquor) and can take place the discoloration reaction, and the directive property is strong, consequently can be used for judging whether the preparation step of the azo mixing standard solution that needs the extraction detection accords with the standard requirement, ensures final azo testing result's accuracy.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a diagram showing the installation relationship between a column tube and an upper and a lower sieve plate;
FIG. 2 is a perspective view of the azo solid phase extraction column of the present invention;
fig. 3 is a sectional view taken along line a-a of fig. 2.
In the figure: 1-column tube, 11-sample adding port, 12-discharge port, 13-ear plate, 2-upper sieve plate, 3-lower sieve plate, 4-extraction cavity, 41-color changing layer and 42-extraction layer.
Detailed Description
The drawings are for illustrative purposes only and are not to be construed as limiting the patent; for better illustration of the present embodiment, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
The terms "upper", "lower", "inner", "outer", and the like in the embodiments of the present invention refer to the orientation or positional relationship shown in the drawings only for convenience of description and simplification of description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted", "connected" and "abutted" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, so to speak, as communicating between the two elements. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.
For the purpose of clearly understanding the technical features, objects, and effects of the present invention, the detailed description of the embodiments of the present invention will be given with reference to the accompanying drawings, but the embodiments of the present invention are not limited thereto.
Example 1:
as shown in fig. 1 to 3, a color-changing azo solid-phase extraction column comprises a column tube 1, and an upper sieve plate 2 and a lower sieve plate 3 which are arranged in the column tube 1 at intervals; the top of the column tube 1 is provided with an open sample adding port 11, and the bottom of the column tube 1 is provided with a conical discharge port 12; an extraction cavity 4 is formed between the upper sieve plate 2 and the lower sieve plate 3, a color changing layer 41 and an extraction layer 42 are sequentially arranged in the extraction cavity 4 from top to bottom, the color changing layer 41 and the extraction layer 42 are both formed by filling purified and activated diatomite, and flavanthrone is adsorbed in the diatomite of the color changing layer 41; the pore diameter of the lower sieve plate 3 is smaller than the particle diameter of the diatomite of the extraction layer 42.
The pillar tube 1 is integrally formed by plastic materials, and the inner diameter of the pillar tube 1 is 26.4mm, and the length of the pillar tube is 154 mm.
The upper sieve plate 2 and the lower sieve plate 3 are both formed by sintering polyethylene powder, the aperture of the upper sieve plate 2 is 100 microns, and the aperture of the lower sieve plate 3 is 30 microns.
The diameter of going up sieve 2 and sieve 3 down all is the same with the internal diameter of column casing 1, and the thickness of going up sieve 2 is 2.5mm, and the thickness of sieve 3 down is 2.4mm, goes up sieve 2 and the side of sieve 3 down and the butt of 1 inner wall of column casing respectively and relatively fixed.
The diatomite of the extraction layer 42 has a filling thickness of 92mm, a filling amount of 18.5g, a diatomite particle size of 0.5-1.8 mm and a specific surface area of 30-40 m2The diatomite filling particle size distribution rule of the extraction layer 42 is as follows: the particle size of the diatomite gradually becomes thicker along the column tube 1 from bottom to top, and the particle size distribution is favorable for forming a hierarchical adsorption extraction effect, so that the flow speed of the extraction solution is ensured to be fast and stable, the elution time is shortened, and the extraction efficiency is improved.
The diatomite filling thickness of the color changing layer 41 is 2mm, the particle size of the diatomite is 1.8mm, and the diatomite of the color changing layer 41 is bright yellow after being soaked and dyed.
The kieselguhr in the color-changing azo solid-phase extraction column is uniformly and compactly filled, and the loosening and the fault of the kieselguhr do not occur after beating and vibration.
To verify the effectiveness of the azo color-changing solid phase extraction column of example 1, the following procedure was used to perform an azo mixed standard solution extraction experiment:
firstly, preparing an azo mixed standard solution with the concentration of 30 mu g/ml according to GB/T17592-;
pouring 20ml of the azo mixed standard solution prepared in the step I into the color-changing azo solid-phase extraction column in the embodiment 1, wherein the azo mixed standard solution rapidly penetrates through the upper sieve plate 2 and enters the diatomite of the color-changing layer 41, and because a sodium dithionite solution needs to be added in the preparation process of the azo mixed standard solution, after the azo mixed standard solution is contacted with the diatomite of the color-changing layer 41, the bright yellow diatomite and the sodium dithionite solution react to become blue, which indicates that the preparation step of the azo mixed standard solution is correct, and if the color of the diatomite of the color-changing layer 41 is not changed, indicates that the preparation step of the azo mixed standard solution is wrong, and the final azo detection result is influenced;
③ after the azo mixed standard solution passes through the diatomite of the discoloring layer 41 and fully absorbs and reacts with the diatomite of the extraction layer 42 for 15min, then 20mL of ether is added from the sample adding port 11 at the top of the column tube 1, the diatomite is eluted and the eluent is collected, the elution step is repeated for 4 times, 80mL of ether is used, the whole elution process takes 4min, and the eluent is merged;
and fourthly, carrying out rotary evaporation on the collected eluent (after the rotary evaporation, diatomite powder should not be arranged at the bottom of the rotary evaporation bottle), then fixing the volume, and measuring the recovery rate of the aromatic amine by using a gas chromatograph-mass spectrometer, wherein the finally measured recovery rates of the 24 aromatic amines are shown in table 1.
TABLE 1 recovery of 24 aromatic amines from azo mixed standard solution
Therefore, the allochroic azo solid-phase extraction column in the embodiment 1 is used for extraction and collection, the recovery rates of 24 aromatic amines in the azo mixed standard solution are all over 74%, the recovery rates are stable, the standard requirements are met, the operation is simple, the extraction time is short, the extraction efficiency is high, repeated tests are easy to perform, the repeatability is good, and the method is suitable for popularization and application.
Example 2:
as shown in fig. 1 to 3, a color-changing azo solid-phase extraction column comprises a column tube 1, and an upper sieve plate 2 and a lower sieve plate 3 which are arranged in the column tube 1 at intervals; the top of the column tube 1 is provided with an open sample adding port 11, and the bottom of the column tube 1 is provided with a conical discharge port 12; an extraction cavity 4 is formed between the upper sieve plate 2 and the lower sieve plate 3, a color changing layer 41 and an extraction layer 42 are sequentially arranged in the extraction cavity 4 from top to bottom, the color changing layer 41 and the extraction layer 42 are both formed by filling purified and activated diatomite, and flavanthrone is adsorbed in the diatomite of the color changing layer 41; the pore diameter of the lower sieve plate 3 is smaller than the particle diameter of the diatomite of the extraction layer 42.
The pillar tube 1 is integrally formed by plastic materials, and the inner diameter and the length of the pillar tube 1 are 26mm and 150mm respectively.
The upper sieve plate 2 and the lower sieve plate 3 are both formed by sintering polyethylene powder, the aperture of the upper sieve plate 2 is 80 microns, and the aperture of the lower sieve plate 3 is 20 microns.
The diameter of going up sieve 2 and sieve 3 down all is the same with the internal diameter of column casing 1, and the thickness of going up sieve 2 is 2.4mm, and the thickness of sieve 3 down is 2.2mm, and the side of going up sieve 2 and sieve 3 down is respectively with 1 inner wall butt of column casing and relatively fixed.
The diatomite filling thickness of the extraction layer 42 is 88mm, the filling amount is 15.0g, the particle size of the diatomite is 0.2-1.6 mm, and the specific surface area is 35-40 m2The diatomite filling particle size distribution rule of the extraction layer 42 is as follows: the particle size of the diatomite gradually becomes thicker along the column tube 1 from bottom to top, and the particle size distribution is favorable for forming a hierarchical adsorption extraction effect, so that the flow speed of the extraction solution is ensured to be fast and stable, the elution time is shortened, and the extraction efficiency is improved.
The diatomite filling thickness of the color changing layer 41 is 3mm, the particle size of the diatomite is 1.6mm, and the diatomite of the color changing layer 41 is bright yellow after being soaked and dyed.
The kieselguhr in the color-changing azo solid-phase extraction column is uniformly and compactly filled, and the loosening and the fault of the kieselguhr do not occur after beating and vibration.
To verify the use effect of the color-changing azo solid-phase extraction column in example 2, the following steps were used to perform an azo mixed standard solution extraction experiment:
firstly, preparing an azo mixed standard solution with the concentration of 30 mu g/ml according to GB/T17592-;
taking 20ml of the azo mixed standard solution prepared in the step I, pouring the azo mixed standard solution into the color-changing azo solid-phase extraction column in the embodiment 2, enabling the azo mixed standard solution to rapidly penetrate through the upper sieve plate 2 and enter the diatomite of the color-changing layer 41, and because a sodium dithionite solution needs to be added in the preparation process of the azo mixed standard solution, after the azo mixed standard solution is contacted with the diatomite of the color-changing layer 41, the bright yellow diatomite and the sodium dithionite solution react to become blue, so that the preparation step of the azo mixed standard solution is correct, and if the color of the diatomite of the color-changing layer 41 is not changed, the preparation step of the azo mixed standard solution is wrong, so that the final azo detection result is influenced;
③ after the azo mixed standard solution passes through the diatomite of the discoloring layer 41 and fully absorbs and reacts with the diatomite of the extraction layer 42 for 15min, then 20mL of ether is added from the sample adding port 11 at the top of the column tube 1, the diatomite is eluted and the eluent is collected, the elution step is repeated for 4 times, 80mL of ether is used, the whole elution process takes 6min, and the eluent is merged;
and fourthly, carrying out rotary evaporation on the collected eluent (after the rotary evaporation, diatomite powder should not be arranged at the bottom of the rotary evaporation bottle), then fixing the volume, and measuring the recovery rate of the aromatic amine by using a gas chromatograph-mass spectrometer, wherein the finally measured recovery rates of the 24 aromatic amines are shown in table 2.
TABLE 2 recovery of 24 aromatic amines from azo mixed standard solution
Therefore, the allochroic azo solid-phase extraction column in the embodiment 2 is used for extraction and collection, the recovery rates of 24 aromatic amines in the azo mixed standard solution are all over 74%, the recovery rates are stable, the standard requirements are met, the operation is simple, the extraction time is short, the extraction efficiency is high, repeated tests are easy to perform, the repeatability is good, and the method is suitable for popularization and application.
Example 3:
as shown in fig. 1 to 3, a color-changing azo solid-phase extraction column comprises a column tube 1, and an upper sieve plate 2 and a lower sieve plate 3 which are arranged in the column tube 1 at intervals; the top of the column tube 1 is provided with an open sample adding port 11, and the bottom of the column tube 1 is provided with a conical discharge port 12; an extraction cavity 4 is formed between the upper sieve plate 2 and the lower sieve plate 3, a color changing layer 41 and an extraction layer 42 are sequentially arranged in the extraction cavity 4 from top to bottom, the color changing layer 41 and the extraction layer 42 are both formed by filling purified and activated diatomite, and flavanthrone is adsorbed in the diatomite of the color changing layer 41; the pore diameter of the lower sieve plate 3 is smaller than the particle diameter of the diatomite of the extraction layer 42.
The pillar tube 1 is integrally formed by plastic materials, and the inner diameter of the pillar tube 1 is 28mm and the length is 154 mm.
The upper sieve plate 2 and the lower sieve plate 3 are both formed by sintering polyethylene powder, the aperture of the upper sieve plate 2 is 120 mu m, and the aperture of the lower sieve plate 3 is 40 mu m.
The diameter of going up sieve 2 and sieve 3 down all is the same with the internal diameter of column casing 1, and the thickness of going up sieve 2 is 2.6mm, and the thickness of sieve 3 down is 2.5mm, and the side of going up sieve 2 and sieve 3 down is respectively with 1 inner wall butt of column casing and relatively fixed.
The diatomite of the extraction layer 42 has a filling thickness of 94mm, a filling amount of 20g, a diatomite particle size of 1.0-2.0 mm and a specific surface area of 25-30 m2The diatomite filling particle size distribution rule of the extraction layer 42 is as follows: the particle size of the diatomite gradually becomes thicker along the column tube 1 from bottom to top, and the particle size distribution is favorable for forming a hierarchical adsorption extraction effect, so that the flow speed of the extraction solution is ensured to be fast and stable, the elution time is shortened, and the extraction efficiency is improved.
The diatomite filling thickness of the color changing layer 41 is 2.5mm, the particle size of the diatomite is 2.0mm, and the diatomite of the color changing layer 41 is bright yellow after being soaked and dyed.
The kieselguhr in the color-changing azo solid-phase extraction column is uniformly and compactly filled, and the loosening and the fault of the kieselguhr do not occur after beating and vibration.
To verify the effectiveness of the azo color-changing solid phase extraction column of example 3, the following procedure was used to perform an azo mixed standard solution extraction experiment:
firstly, preparing an azo mixed standard solution with the concentration of 30 mu g/ml according to GB/T17592-;
pouring 20ml of the azo mixed standard solution prepared in the step I into the color-changing azo solid-phase extraction column in the embodiment 3, wherein the azo mixed standard solution rapidly penetrates through the upper sieve plate 2 and enters the diatomite of the color-changing layer 41, and because a sodium dithionite solution needs to be added in the preparation process of the azo mixed standard solution, after the azo mixed standard solution is contacted with the diatomite of the color-changing layer 41, the bright yellow diatomite and the sodium dithionite solution react to become blue, which indicates that the preparation step of the azo mixed standard solution is correct, and if the color of the diatomite of the color-changing layer 41 is not changed, indicates that the preparation step of the azo mixed standard solution is wrong, and the final azo detection result is influenced;
③ after the azo mixed standard solution passes through the diatomite of the discoloring layer 41 and fully absorbs and reacts with the diatomite of the extraction layer 42 for 15min, then 20mL of ether is added from the sample adding port 11 at the top of the column tube 1, the diatomite is eluted and the eluent is collected, the elution step is repeated for 4 times, 80mL of ether is used, the whole elution process takes 5min, and the eluent is merged;
and fourthly, carrying out rotary evaporation on the collected eluent (after the rotary evaporation, diatomite powder should not be arranged at the bottom of the rotary evaporation bottle), then fixing the volume, and measuring the recovery rate of the aromatic amine by using a gas chromatograph-mass spectrometer, wherein the finally measured recovery rates of the 24 aromatic amines are shown in table 3.
TABLE 3 recovery of 24 aromatic amines from azo mixed standard solution
Therefore, the color-changing azo solid-phase extraction column in the embodiment 3 is used for extraction and collection, the recovery rates of 24 aromatic amines in the azo mixed standard solution are all over 74%, the recovery rates are stable, the standard requirements are met, the operation is simple, the extraction time is short, the extraction efficiency is high, repeated tests are easy to perform, the repeatability is good, and the method is suitable for popularization and application.
In the drawings, the positional relationship is described for illustrative purposes only and is not to be construed as limiting the present patent; it is to be understood that the above-described embodiments of the present invention are merely examples provided for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The color-changing azo solid-phase extraction column is characterized by comprising a column tube, an upper sieve plate and a lower sieve plate which are arranged in the column tube at intervals, wherein the top of the column tube is provided with an open sample adding port, and the bottom of the column tube is provided with a conical discharge port;
an extraction cavity is formed between the upper sieve plate and the lower sieve plate, a color changing layer and an extraction layer are sequentially arranged in the extraction cavity from top to bottom, the color changing layer and the extraction layer are both filled with diatomite, and flavanthrone is adsorbed on the diatomite of the color changing layer;
the aperture of the lower sieve plate is smaller than the particle size of the diatomite of the extraction layer.
2. The color-changing azo solid-phase extraction column according to claim 1, wherein the upper sieve plate and the lower sieve plate are both sintered from polyethylene powder;
the diameters of the upper sieve plate and the lower sieve plate are the same as the inner diameter of the column tube, and the side edges of the upper sieve plate and the lower sieve plate are respectively fixed with the inner wall of the column tube in an abutting mode.
3. The color-changing azo solid-phase extraction column according to claim 2, wherein the upper sieve plate has a thickness of 2.4-2.6 mm, and the pore diameter of the upper sieve plate is not less than 80 μm.
4. The color-changing azo solid-phase extraction column according to claim 3, wherein the lower sieve plate has a thickness of 2.2 to 2.5mm, and the pore diameter of the lower sieve plate is 20 to 40 μm.
5. The color-changing azo solid-phase extraction column according to claim 4, wherein the column tube has an inner diameter of 26-28 mm and a length of not less than 150 mm.
6. The azoic discoloration solid phase extraction column according to any one of claims 1 to 5, wherein the diatomaceous earth in said extraction layer has a particle size of 0.2 to 2.0mm and a specific surface area of 25 to 40m2/g；
The diatomite of the extraction layer gradually becomes coarse from bottom to top in particle size.
7. The color-changing azo solid-phase extraction column according to claim 6, wherein the diatomite packing thickness of the extraction layer is 88-94 mm, and the diatomite packing amount is 15-20 g.
8. The color-changing azo solid-phase extraction column according to claim 7, wherein the diatomite packing thickness of the color-changing layer is 2-3 mm.
9. The color-changing azo solid phase extraction column according to claim 8, wherein the top of the column tube is provided with an ear plate around the sample addition port.
10. The solid phase extraction column of azo-compound according to claim 9, wherein the column tube is an integrally formed structure and is made of plastic.
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| CN202020635846.3U CN212214673U (en) | 2020-04-24 | 2020-04-24 | Allochroic azo solid-phase extraction column |
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