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An array type dynamic dispersion solid phase extraction device and extraction method

A technology for dispersing solid-phase and extraction devices, which is applied in measurement devices, material separation, and analysis of materials, etc., can solve the problems of filling uniformity affecting the efficiency of solid-phase extraction, unsatisfactory repeatability between samples, and non-compliance with sustainable development. Achieve the effect of reducing extraction time, saving maintenance costs, and high repeatability

Active Publication Date: 2019-10-25
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the traditional solid-phase extraction technology has the following problems: (1) The adsorbent particles in the solid-phase extraction column are fixed and tightly packed, and the particle size and distribution of the adsorbent as well as the uniformity of packing will significantly affect the efficiency of solid-phase extraction
(2) In order to improve the extraction efficiency, it is necessary to make the liquid sample slowly pass through the stationary phase packing layer, so that the two can fully contact and interact, so it takes a long time (1-2h) and the work efficiency is low
(3) Usually, under the action of a vacuum pump, the sample or solvent passes through the stationary phase packing layer at a rate of 2-3 drops, and the flow rate is difficult to control, resulting in unsatisfactory repeatability between samples
[0005] At present, bamboo charcoal and expanded graphite are commonly used as adsorbents for adsorbing polycyclic aromatic hydrocarbons or petroleum in water; bamboo charcoal is made of bamboo, which has high porosity and specific surface area, and strong adsorption performance, but because of its complicated preparation process , high energy consumption, and use bamboo as raw material, which does not meet the requirements of sustainable development; graphite exists in a large amount in nature, and expanded graphite is a kind of loose and porous graphite obtained by intercalation, washing, drying and high temperature expansion of natural graphite flakes The worm-like substance has adsorption properties, but its surface contains fewer functional groups, and its adsorption to substances is not strong. For the modification of expanded graphite, its adsorption performance can be improved by increasing its surface functional groups

Method used

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  • An array type dynamic dispersion solid phase extraction device and extraction method
  • An array type dynamic dispersion solid phase extraction device and extraction method
  • An array type dynamic dispersion solid phase extraction device and extraction method

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Such as figure 1 Shown, a kind of array type dynamic dispersive solid-phase extraction device comprises a base housing 1, a controller 2, a gantry 3, a tray 4, a longitudinal housing 5 and a loading plate 6 for carrying a liquid aspirator; the tray 4 is detachably connected with a disc changer 9; the gantry 3 is fixedly connected to the base shell 1, and the longitudinal shell 5 is longitudinally arranged and fixedly connected to the gantry 3;

[0045] Such as figure 2 and image 3 As shown, several rows of carrying holes 9-1 are set on the disc changer 9, and each row of carrying holes 9-1 has several; several electric liquid aspirators 7 are set on the carrying plate 6, and each row of carrying holes 9-1 The quantity of -1 is the same as that of the electric pipette 7; the electric pipette 7 is equipped with an extraction tip 8;

[0046] The inside of the carrying hole 9-1 is used to place EP tubes or sample bottles filled with liquid, and the liquid contained in ...

Embodiment 2

[0058] A kind of adsorbent is polyvinyl alcohol modified expanded graphite, and the specific preparation method is as follows:

[0059] (1) Weigh natural flake graphite, add it into 1mol / L NaOH solution, react at 25°C, 60rpm for 2.5h, after the reaction is completed, filter out graphite, rinse with deionized water, and dry at 100°C;

[0060] (2) After adding potassium permanganate to the dried graphite and mixing, slowly add concentrated sulfuric acid and concentrated nitric acid, stir and mix, and react for 40 minutes at 25°C; the graphite, concentrated sulfuric acid, concentrated nitric acid and permanganic acid The mass ratio of potassium is: 1:2:0.5:0.1;

[0061] (3) Slowly add concentrated sulfuric acid and concentrated nitric acid to the above reaction system in a mass ratio of 1:1, stir and mix, and react for 40 minutes at 25°C;

[0062] (4) After the reaction was completed, the graphite was filtered out, washed 3 times with dehydrated alcohol, each 5min, to obtain exp...

Embodiment 3

[0076] The polyvinyl alcohol prepared in Example 2 is based on the number of electric pipettes 7 being 6×1, the carrying holes 9-1 on the disc changer 9 having 6 rows, 6 holes in each row, and the adsorbent in the extraction tip 8 Modified expanded graphite was used as an example to perform solid-phase extraction on polycyclic aromatic hydrocarbon samples in seawater. The electric pipette 7 is a 5mL electric pipette; the extraction tip is 5mL.

[0077]The 6 rows of carrying holes are placed in order: EP tubes for activation solution, EP tubes for samples to be tested, EP tubes for cleaning solution, EP tubes for eluent, EP tubes for waste solution, and sample bottles.

[0078] The concentrations of 16 PAHs in the spiked seawater are all 0.5ppm

[0079] Set up Controller 2 to implement the following process:

[0080] (1) Driven by the first motor 11, the EP tube of the adorned activating liquid on the disc changer 9 moves to the electric liquid aspirator 7, and the electric l...

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Abstract

The invention relates to an array type dynamic dispersion solid phase extraction device, comprising a base casing, a controller, a portal frame, a tray, a longitudinal casing and a loading plate for loading liquid-sucking devices, wherein a tray changer is detachably connected to the tray and is provided with a plurality of rows of loading holes; a plurality of electric liquid-sucking devices are arranged on the loading plate, and the number of the loading holes in each row is the same as that of the electric liquid-sucking devices; an extraction sucking head is arranged on each electric liquid-sucking device. The array type dynamic dispersion solid phase extraction device provided by the invention adopts a form of bubble-assisted dynamic dispersion, so that the extraction time can be greatly reduced; an adsorbent namely polyvinyl alcohol modified expanded graphite special for dynamic dispersion solid phase extraction is adopted, so that a bigger surface area brings a higher extraction efficiency. By adopting multi-bit array full-automatic liquid-sucking devices, a plurality of samples can be treated at the same time, and while the working efficiency is improved, the array type dynamic dispersion solid phase extraction device ensures the high parallelism of the whole dynamic dispersion extraction and desorption processes, and the repeatability of test results is high.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry equipment and methods, and in particular relates to an array type dynamic dispersion solid-phase extraction device and an extraction method. Background technique [0002] Solid Phase Extraction (Solid Phase Extraction, SPE) is a sample pretreatment technology based on chromatographic separation, which is mainly used for the separation, purification and enrichment of samples, with the purpose of reducing sample matrix interference and improving detection sensitivity. The principle of solid phase extraction is to use a solid adsorbent to adsorb the target compound in the liquid sample, separate it from the sample matrix and interfering compounds, and then use the eluent to desorb the analyte, so as to achieve the purification and enrichment of the target compound. [0003] The traditional solid-phase extraction device is a small solid-phase extraction column. Its structure is: a certain...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/08G01N30/14C01B32/21
CPCG01N30/06G01N30/08G01N30/14G01N2030/062G01N2030/065
Inventor 观文娜高峻白罚利王聪
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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