CN211652297U - Purifying column for dioxin analysis experiment - Google Patents
Purifying column for dioxin analysis experiment Download PDFInfo
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- CN211652297U CN211652297U CN202020159794.7U CN202020159794U CN211652297U CN 211652297 U CN211652297 U CN 211652297U CN 202020159794 U CN202020159794 U CN 202020159794U CN 211652297 U CN211652297 U CN 211652297U
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Abstract
The utility model relates to a purifying column for dioxin analysis experiments belongs to the laboratory and uses the device field, including activated carbon column, polytetrafluoroethylene coupling head and multilayer silica gel column triplex. The utility model discloses can realize one step and accomplish multilayer silica gel column and activated carbon column enrichment purification, avoid carrying out multilayer silica gel column purification and activated carbon column purification operation respectively to reduced experiment step and organic solvent quantity, shortened when the analysis, raise the efficiency.
Description
Technical Field
The utility model relates to a purifying column for dioxin type analysis experiments especially relates to a purifying column for dioxin type analysis experiments through series connection multilayer silica gel and active carbon purifying column purification dioxin type extraction solution.
Background
The multi-layer silica gel column purification refers to a method of using a chromatographic column, sequentially filling neutral silica gel, alkaline silica gel, neutral silica gel, sulfuric acid silica gel, neutral silica gel and silver nitrate silica gel (the dosage can be adjusted according to experimental conditions), concentrating a sample, transferring the sample to the chromatographic column, and leaching the sample by using a normal hexane solvent. Purifying the extraction solution for analyzing dioxin samples to remove various interferents such as fat, pigment and the like, thereby achieving an excellent purification result. Besides being suitable for analysis of dioxins, the method can also be used for analysis of polychlorinated biphenyl, polychlorinated naphthalene and brominated dioxins with dioxin-like characteristics.
The purification with activated carbon column is a method of using chromatographic column, filling activated carbon dispersed silica gel or buried silica gel, utilizing the special adsorbability of the activated carbon substance to coplanar organic pollutants, and separating coplanar (mainly referring to some dioxin and pollutants with dioxin-like characteristics) substances from interferents. The method is a purification technology widely used in trace analysis of dioxin and the like, and can achieve an excellent purification result.
The multi-layer silica gel column purification and the activated carbon column purification are sequentially carried out in dioxin analysis, and after the first-step multi-layer silica gel column purification is generally finished, leacheate is collected and concentrated and then transferred to carry out activated carbon column purification. Concentration and sample transfer are required, and efficiency is slow and cumbersome. Therefore, the utility model aims at solving the above problem, invent a purifying column device for dioxin class analysis experiments, have and develop multilayer silica gel column and active carbon column purification performance in step, under the condition that satisfies the experimental accuracy, accomplish two steps of purifications through one operation.
Disclosure of Invention
The utility model discloses can provide a purification post for dioxin class analysis experiments has and develops multilayer silica gel column and active carbon column purification performance simultaneously. Two-step purification is completed through one-time operation, the efficiency is high, the operation is simple, the sample concentration and transfer time is reduced, the use of organic solvents is reduced, and meanwhile, the method has good internal standard recovery rate and is simple and reliable.
In order to realize the above function, the utility model relates to a purifying column for dioxin analysis experiments, its characterized in that: comprises three parts of an active carbon column (1), a polytetrafluoroethylene coupling head (2) and a multi-layer silica gel column (3).
The upper opening and the lower opening of the polytetrafluoroethylene coupling head (2) are quick-connection slots, the lower end of the multilayer silica gel column (3) is in sealed plug-in connection with the inner side of the upper opening, and the upper end of the activated carbon column (1) is in sealed plug-in connection with the outer side of the lower opening.
The activated carbon column (1) is a straight-through glass tube with the inner diameter of 8mm, and the middle part of the activated carbon column is sequentially packaged with 1g of anhydrous sodium sulfate, 1g of activated carbon dispersed silica gel and 1g of anhydrous sodium sulfate and is plugged and compacted by two ends of glass wool.
The upper opening of the multilayer silica gel column (3) is 24 openings or any standard-specification interface, the inner diameter of the main glass tube is 1-2 cm, 1g of neutral silica gel, 4g of alkaline silica gel, 1g of neutral silica gel, 8g of acidic silica gel, 1g of neutral silica gel, 3g of silver nitrate silica gel and 5g of anhydrous sodium sulfate are sequentially filled from bottom to top, and a polytetrafluoroethylene throttle (4) is arranged at the lower end of the multilayer silica gel column.
Has the advantages that: the utility model relates to a dioxin class analysis purification column for experiment has purification and separation function, and the solution after purifying through multilayer silica gel column is adsorbed the entrapment by the activated carbon column, recycles the solvent and elutes. Through the operation, the purification and separation of the multi-layer silica gel column and the activated carbon column can be more efficient than the purification and separation of the multi-layer silica gel column and the activated carbon column, the time for sample concentration and transfer is reduced, the use of organic solvents is reduced, and meanwhile, the method has good internal standard recovery rate, and is simple and reliable.
Drawings
FIG. 1 is a schematic view of a purification column for analysis experiments of dioxins.
Wherein: 1. an activated carbon column; 2. a polytetrafluoroethylene coupling head; 3. multilayer silica gel column; 4. a polytetrafluoroethylene throttle;
Detailed Description
To explain the technical content, the objects and the effects of the present invention in detail, the following description is made with reference to the accompanying drawings 1 in conjunction with the embodiments
Example 1
The test is a dioxin analysis test, 1g of activated carbon dispersed silica gel is packaged in an activated carbon column (1), two ends of the activated carbon dispersed silica gel are plugged and compacted by glass wool, and 1g of neutral silica gel, 4g of alkaline silica gel, 1g of neutral silica gel, 8g of acidic silica gel, 1g of neutral silica gel, 3g of silver nitrate silica gel and 5g of anhydrous sodium sulfate are sequentially filled in a multilayer silica gel column from bottom to top.
The apparatus was connected according to FIG. 1 and the column was pre-rinsed with 100mL of n-hexane. And transferring the sample to be purified to a multi-layer silica gel column by using n-hexane, then leaching by using 150mL of n-hexane, taking down the activated carbon column after leaching is finished, and enriching dioxin and coplanar polychlorinated biphenyl substances on the activated carbon column. And then eluting the activated carbon column by using a mixed solvent of n-hexane and dichloromethane to remove impurities.
And then inverting the activated carbon column, and eluting and collecting the dioxin-like substances by using 40mL of toluene solvent.
The experimental effect shows that the device can be used for purifying samples for analyzing dioxins, has good purifying effect and recovery rate, and is simple and reliable.
The above embodiments are provided only for illustrating the present invention, and are not intended to limit the present invention; it should be noted that, for a person skilled in the art, various changes and modifications can be made without departing from the scope of the invention, which is within the protection scope of the invention; therefore, all equivalent changes and modifications made within the scope of the claims of the present invention should fall within the scope of the claims of the present invention.
Claims (1)
1. A purifying column for dioxin analysis experiments is characterized in that: comprises three parts of an active carbon column (1), a polytetrafluoroethylene coupling head (2) and a multi-layer silica gel column (3); the upper opening and the lower opening of the polytetrafluoroethylene coupling head (2) are quick-connection slots, the lower end of the multilayer silica gel column (3) is hermetically inserted inside the upper opening, and the upper end of the activated carbon column (1) is hermetically inserted outside the lower opening; the activated carbon column (1) is a straight-through glass tube with the inner diameter of 8mm, the middle part of the activated carbon column is sequentially packaged with 1g of anhydrous sodium sulfate, 1g of activated carbon dispersed silica gel and 1g of anhydrous sodium sulfate, and two ends of the activated carbon column are plugged and compacted by glass wool; the upper opening of the multilayer silica gel column (3) is 24 openings or any standard-specification interface, the inner diameter of the main glass tube is 1-2 cm, 1g of neutral silica gel, 4g of alkaline silica gel, 1g of neutral silica gel, 8g of acidic silica gel, 1g of neutral silica gel, 3g of silver nitrate silica gel and 5g of anhydrous sodium sulfate are sequentially filled from bottom to top, and a polytetrafluoroethylene throttle (4) is arranged at the lower end of the multilayer silica gel column.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020159794.7U CN211652297U (en) | 2020-01-19 | 2020-01-19 | Purifying column for dioxin analysis experiment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020159794.7U CN211652297U (en) | 2020-01-19 | 2020-01-19 | Purifying column for dioxin analysis experiment |
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| CN211652297U true CN211652297U (en) | 2020-10-09 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112494992A (en) * | 2020-11-02 | 2021-03-16 | 河北伊莱莎生物技术有限公司 | Dioxin pretreatment purification combined column and preparation method and application thereof |
| CN112834669A (en) * | 2020-12-31 | 2021-05-25 | 中国农业科学院农业质量标准与检测技术研究所 | High-efficient sample purification and separation column of dioxin suitable for mass spectrometry |
-
2020
- 2020-01-19 CN CN202020159794.7U patent/CN211652297U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112494992A (en) * | 2020-11-02 | 2021-03-16 | 河北伊莱莎生物技术有限公司 | Dioxin pretreatment purification combined column and preparation method and application thereof |
| CN112834669A (en) * | 2020-12-31 | 2021-05-25 | 中国农业科学院农业质量标准与检测技术研究所 | High-efficient sample purification and separation column of dioxin suitable for mass spectrometry |
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