CN112915589B - Filler filling device of solid-phase extraction column and application thereof - Google Patents
Filler filling device of solid-phase extraction column and application thereof Download PDFInfo
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- CN112915589B CN112915589B CN201911237693.5A CN201911237693A CN112915589B CN 112915589 B CN112915589 B CN 112915589B CN 201911237693 A CN201911237693 A CN 201911237693A CN 112915589 B CN112915589 B CN 112915589B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
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Abstract
A filling device of solid phase extraction column filler and application thereof are used for filling the solid phase extraction column filler. The filling device mainly comprises two parts: a filler funnel and a filler plug which are matched with the size of the solid phase extraction column. The application of the filling material is as follows: the solid-phase extraction hollow column with the sieve plate arranged at the lower end is placed into a stepped cylinder at the bottom end of a filler funnel with the opening facing upwards, a certain amount of filler is placed into the solid-phase extraction hollow column from the upper end of the filler funnel, the filler is filled into the solid-phase extraction column through a funnel hole, and then the solid-phase extraction hollow column is slightly vibrated to enable the filler to be tightly and uniformly filled into the solid-phase extraction column. And after the filler is filled, taking down the filler funnel, installing the filler plug, and continuing to slightly vibrate. The filler plug is then removed and the screen plate is installed. The device has simple structure and filling method, reasonable structural design and low cost, and simultaneously, the device and the method also provide a scheme for automatically filling the solid-phase extraction column.
Description
Technical Field
The invention relates to the technical field of analytical instruments, in particular to a filler filling device of a solid-phase extraction column and application thereof, which are used for filling fillers of the solid-phase extraction column, ensure that the pressure resistance of the solid-phase extraction column meets the requirement, improve the filling qualification rate of the solid-phase extraction column and provide a scheme for automatically filling the solid-phase extraction column.
Background
Solid Phase Extraction (SPE) is mainly used for separation, purification and concentration of samples, and compared with the traditional liquid-liquid extraction method, the SPE can improve the recovery rate of analytes, more effectively separate the analytes from interfering components and reduce the pretreatment process of the samples. With the development of the technology, in order to improve the efficiency of sample analysis, it is necessary to realize full automation and high throughput processing of the SPE process and online combination with liquid chromatography. In recent years, a small SPE column which is resistant to high pressure (not less than 15MPa) leaching and elution is developed, and direct sample introduction is carried out on liquid chromatography, so that the processes of nitrogen blowing concentration and constant volume are omitted. The technology needs to place a plurality of high-pressure-resistant solid-phase extraction columns on a solid-phase extraction instrument, each solid-phase extraction column can be repeatedly sealed under high pressure, and the enrichment and separation effects are good. This requires that the packing be packed as densely as possible to avoid large voids and to ensure high enrichment and separation efficiency. In the prior art, a liquid-transfering gun is generally adopted to add a solvent dispersed with filler into a filler filling cavity for multiple times. Although the method can be used for filling the filler, the filler is easily extruded when the sieve plate is installed, so that the sieve plate is blocked, and the pressure of the solid-phase extraction column exceeds the standard, so that the solid-phase extraction column cannot be used. Meanwhile, the filling mode in the prior art is not beneficial to automation.
Disclosure of Invention
Aiming at the technical problem, the invention provides the filler filling device of the solid-phase extraction micro column, which can avoid excessive extrusion of a sieve plate to the filler in the installation process and ensure the filler to be filled, thereby improving the filling qualification rate of the solid-phase extraction micro column, improving the filling efficiency and saving the cost. Meanwhile, a scheme is provided for automatically filling the solid phase extraction column.
The technical scheme of the invention is as follows:
a packing device of a solid phase extraction column comprises a packing funnel and a packing plug;
the solid phase extraction column is a cylinder, the upper end surface and the lower end surface of the solid phase extraction column are respectively provided with a corresponding circular groove A for placing the sieve plate, a circular through hole A is arranged between the two circular grooves, and the diameter of the circular groove A is larger than that of the circular through hole A;
the top of the filler funnel is provided with a funnel-shaped groove, the bottom of the filler funnel is provided with a circular groove B, and the diameter of the circular groove B is larger than the outer diameter of the solid-phase extraction column; a cylindrical protrusion is arranged at the bottom of the circular groove, the diameter of the cylindrical protrusion is smaller than that of the circular groove A and larger than that of the circular through hole A, and a through hole communicated with the funnel-shaped groove is formed in the end face of the cylindrical protrusion;
the bottom of the filler plug is provided with a circular groove C, and the diameter of the circular groove C is larger than the outer diameter of the solid-phase extraction column; the bottom of the circular groove is provided with a cylindrical protrusion, and the diameter of the cylindrical protrusion is smaller than the diameter of the circular groove A and larger than the diameter of the circular through hole A.
The filler funnel and the filler plug are cylindrical blocks, the upper end of the filler funnel is an inverted cone frustum-shaped hole, the lower end of the filler funnel is a cylindrical groove hole with an inner coaxial cylinder, and the diameter D of the groove hole meets the requirement D0<D≤D0+0.2mm，D0The diameter of the outer circle of the solid phase extraction column; the depth h of the slot hole satisfies L multiplied by 1/3<h<L and L are the height of the solid phase extraction column; a cylindrical through hole is arranged between the inverted truncated cone-shaped hole and the inner cylindrical end surface of the slotted hole, and the diameter d' of the through hole satisfies 0.5mm<d’≤D2，D2The inner diameter of the circular through hole A; the diameter d of the cylinder satisfies d'<d≤D1-0.2mm, height h1Satisfy h1≥L1，D1Is the diameter of the circular groove A, L1The depth of the circular groove A;
the bottom of the filler plug is provided with a circular groove C, and the diameter D of the circular groove C3Satisfies D0<D3≤D0+0.2mm, depth L of circular groove C2Is L × 1/3<L2<L, a cylindrical protrusion with diameter D is arranged at the bottom of the circular groove C4D 'is satisfied'<D4≤D10.2mm, height h of the protrusions2≥L1。
The cone angle of the inverted cone frustum-shaped hole of the filler funnel is 30-120 degrees.
The filler funnel and the filler plug are made of metal materials, preferably brass, stainless steel or titanium alloy.
The application of a filling device of a solid phase extraction column is characterized in that an opening of the solid phase extraction column to be filled, the lower end of which is provided with a sieve plate, is upwards arranged in a cylindrical slot hole of a filling funnel, and a cylinder is ensured to be arranged in a circular groove A of a solid phase extraction column placing sieve plate; filling the prepared filler into the solid-phase extraction column through the inverted cone frustum-shaped hole and the cylindrical through hole of the filler funnel; then slightly vibrating to enable the filler to be tightly filled into the solid phase extraction column; after filling the filler, taking down the filler funnel, sleeving the circular groove C of the filler plug on the extraction micro-column, ensuring that the protrusion is positioned in the circular groove A of the sieve plate for placing the extraction micro-column, and slightly vibrating again to tightly fill the filler into the solid-phase extraction column; and then taking down the filler plug, and installing an upper sieve plate at the upper end of the solid-phase extraction column.
The slight vibration mode is knocking the filler plug or knocking the extraction micro-column on a table top or vibrating by ultrasonic waves.
The filling device and the method for the solid phase extraction column filler have the following advantages:
1. the device can avoid packing on the platform that solid-phase extraction post placed the sieve in the filling process leaves over, uses through the cooperation of packing funnel and filler stopper, can ensure to pack not excessively when the installation sieve to the packing failure that the sieve jam leads to has been avoided.
2. The application method of the filling device can not only avoid the blockage of the sieve plate, but also ensure the filling of the filler, thereby filling the solid phase extraction column with high enrichment and separation efficiency.
3. The device has simple structure and filling method, reasonable structural design and low cost, and the device and the method also provide a scheme for automatically filling the solid-phase extraction column.
4. The device and the method improve the filling qualification rate of the solid phase extraction column, save the filler cost and simultaneously can obtain excellent batch repeatability.
Drawings
FIG. 1-schematic view of a filling funnel used in a filling process, in which: 1-solid phase extraction column, 2-filler funnel, 4-sieve plate and 5-filler.
FIG. 2-schematic view of a packing plug used in a packing process, in which: 1-solid phase extraction column, 3-filler plug, 4-sieve plate and 5-filler.
FIG. 3-schematic view of the filler funnel. In the figure: 21-inverted cone frustum shaped hole, 22-slotted hole, 23-cylinder and 24-cylinder through hole.
Fig. 4-schematic view of a filler plug. In the figure: 31-circular recesses C, 32-cylindrical protrusions.
Detailed Description
The present invention will be described with reference to examples.
Example 1
A packing device for solid phase extraction micro-column is shown in figures 1 to 4, and comprises a packing funnel 2 and a packing plug 3;
the solid phase extraction column is a cylinder, the upper end surface and the lower end surface of the solid phase extraction column are respectively provided with a corresponding circular groove A for placing the sieve plate, a circular through hole A is arranged between the two circular grooves, and the diameter of the circular groove A is larger than that of the circular through hole A;
the top of the filler funnel 2 is provided with a funnel-shaped groove, the bottom of the filler funnel is provided with a circular groove B, and the diameter of the circular groove B is larger than the outer diameter of the solid-phase extraction column; a cylindrical protrusion is arranged at the bottom of the circular groove, the diameter of the cylindrical protrusion is smaller than that of the circular groove A and larger than that of the circular through hole A, and a through hole communicated with the funnel-shaped groove is formed in the end face of the cylindrical protrusion;
the bottom of the filler plug 3 is provided with a circular groove C, and the diameter of the circular groove C is larger than the outer diameter of the solid-phase extraction column; the bottom of the circular groove is provided with a cylindrical protrusion, and the diameter of the cylindrical protrusion is smaller than the diameter of the circular groove A and larger than the diameter of the circular through hole A.
The filler funnel 2 and the filler plug 3 are cylindrical blocks, the upper end of the filler funnel 2 is an inverted cone frustum-shaped hole 21, and the cone angle is 90 degrees; the lower end is a cylindrical slotted hole 22 with a coaxial cylinder 23 inside, the diameter of the slotted hole 22 is 9.05mm, and the height is 8 mm; a cylindrical through hole 24 is arranged between the inner cylindrical end surfaces of the inverted cone frustum-shaped hole 21 and the slotted hole 22, and the diameter of the through hole 24 is 1.9 mm; the cylinder 23 has a diameter of 2.7mm and a height of 1.3 mm. The bottom of the filler plug 3 is provided with a circular groove C31 with the diameter of 9.05mm and the depth of 8mm, and the bottom end of the circular groove C31 is provided with a cylindrical protrusion 32 with the diameter of 2.7mm and the height of 1.3 mm; the diameter of the excircle of the solid phase extraction column 1 is 9mm, the height is 12mm, the diameter of the circular groove A is 3mm, the depth is 1.2mm, and the diameter of the circular through hole A is 2 mm.
Filler funnel 2 and filler stopper 3 material are brass.
Example 2
Application of filling device of solid-phase extraction micro column
A packing method for solid phase extraction micro column, which is the device of embodiment 1, the solid phase extraction column 1 with a sieve plate at the lower end and to be packed is installed in the cylindrical slot 22 of the packing funnel 2 with the opening facing upwards, and the cylinder 23 is ensured to be installed in the circular groove A of the sieve plate for placing the solid phase extraction column 1; filling a proper amount of C18 filler into the solid-phase extraction column 1 through the inverted cone frustum-shaped hole 21 and the cylindrical through hole 24 of the filler funnel 22, and slightly knocking the solid-phase extraction column on a table top to tightly fill the filler into the solid-phase extraction column; after filling up the filler, take off filler funnel 2, overlap the circular recess C31 of filler stopper 3 on solid-phase extraction post 1, and guarantee that protruding 32 is located solid-phase extraction post 1 and place the circular recess A of sieve, through slightly knocking filler stopper 3 for in the filler closely filled the solid-phase extraction post, later take off filler stopper 3, install the sieve with the upper end of solid-phase extraction post 1.
Example 3
The filling device as described in example 1, with the difference that: the diameter of the cylindrical slot 22 of the filler funnel 2 is 9.10mm, the diameter of the cylinder 23 is 2.4mm, and the height is 1.2 mm; the diameter of the circular groove C31 of the filler plug 3 is 9.10mm, and the diameter of the protrusion 32 is 2.4 mm; the filler funnel 2 and the filler plug 3 are made of stainless steel.
Example 4
The filling device as described in example 1, with the difference that: the filler funnel 2 and the filler plug 3 are made of titanium alloy materials; the cone angle of the inverted cone frustum-shaped hole 21 of the filler funnel 2 is 120 degrees.
Claims (5)
1. The utility model provides a filler filling device of solid phase extraction post which characterized in that: comprises a filler funnel (2) and a filler plug (3);
the solid phase extraction column is a cylinder, the upper end surface and the lower end surface of the solid phase extraction column are respectively provided with a corresponding circular groove A for placing the sieve plate, a circular through hole A is arranged between the two circular grooves, and the diameter of the circular groove A is larger than that of the circular through hole A;
the top of the filler funnel (2) is provided with a funnel-shaped groove, the bottom of the filler funnel is provided with a circular groove B, and the diameter of the circular groove B is larger than the outer diameter of the solid-phase extraction column; a cylindrical protrusion is arranged at the bottom of the circular groove, the diameter of the cylindrical protrusion is smaller than that of the circular groove A and larger than that of the circular through hole A, and a through hole communicated with the funnel-shaped groove is formed in the end face of the cylindrical protrusion;
the bottom of the filler plug (3) is provided with a circular groove C, and the diameter of the circular groove C is larger than the outer diameter of the solid-phase extraction column; a cylindrical protrusion is arranged at the bottom of the circular groove, and the diameter of the cylindrical protrusion is smaller than that of the circular groove A and larger than that of the circular through hole A;
filler funnel (2) and filler stopper (3) are cylindrical blocks, filler funnel (2) upper end is a frustum of a cone hole (21), the lower extreme is cylindrical slotted hole (22) of inside area coaxial cylinder (23), slotted hole (22) diameter D satisfies D0 < D ≤ D0+0.2 mm，D0The diameter of the outer circle of the solid phase extraction column; the depth h of the slot hole (22) satisfies L x 1/3< h <L and L are the height of the solid phase extraction column; a cylindrical through hole (24) is arranged between the inner cylindrical end surfaces of the inverted cone frustum-shaped hole (21) and the slotted hole (22), and the diameter d' of the through hole (24) meets 0.5mm< d’≤D2，D2The inner diameter of the circular through hole A; the diameter d of the cylinder (23) satisfies d'< d ≤D1-0.2mm, height h1Satisfy h1 ≥ L1，D1Is the diameter of the circular groove A, L1The depth of the circular groove A;
the bottom of the filler plug (3) is provided with a circular groove C (31), and the diameter D of the circular groove C (31)3Satisfies D0 < D3≤D0+0.2mm, depth L of circular groove C (31)2Is L × 1/3< L2 <L, a cylindrical protrusion (32) is arranged at the bottom of the circular groove C (31), and the diameter D of the protrusion (32)4D 'is satisfied'< D4 ≤D1-0.2mm, height h of the protrusions (32)2 ≥ L1。
2. The packing device of the solid phase extraction column according to claim 1, wherein: the cone angle of the inverted cone frustum-shaped hole (21) of the filler funnel (2) is 30-120 degrees.
3. The packing device of a solid phase extraction column according to claim 1, wherein: the filler funnel (2) and the filler plug (3) are made of brass, stainless steel or titanium alloy materials.
4. Use of a packing device for a solid phase extraction column according to any one of claims 1 to 3, wherein: installing a solid phase extraction column (1) with a sieve plate at the lower end to be filled into a cylindrical slotted hole (22) of a filler funnel (2) with an upward opening and ensuring that a cylinder (23) is installed into a circular groove A of the sieve plate for placing the solid phase extraction column (1); filling the prepared filler into the solid phase extraction column (1) through the inverted cone frustum-shaped hole (21) and the cylindrical through hole (24) of the filler funnel (2); then slightly vibrating to enable the filler to be tightly filled into the solid phase extraction column; the filling funnel (2) is taken down after the filling material is filled, the round groove C (31) of the filling material plug (3) is sleeved on the solid phase extraction column (1), the protrusion (32) is ensured to be positioned in the round groove A of the sieve plate for placing the solid phase extraction column (1), and the filling material is tightly filled in the solid phase extraction column by slightly vibrating again; then the filler plug (3) is taken down, and an upper sieve plate is arranged at the upper end of the solid phase extraction column (1).
5. Use of a packing unit for a solid phase extraction column according to claim 4, wherein: the slight vibration mode is knocking the filler plug (3) or knocking the extraction micro-column on a table top or vibrating by ultrasonic waves.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911237693.5A CN112915589B (en) | 2019-12-06 | 2019-12-06 | Filler filling device of solid-phase extraction column and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911237693.5A CN112915589B (en) | 2019-12-06 | 2019-12-06 | Filler filling device of solid-phase extraction column and application thereof |
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| CN112915589B true CN112915589B (en) | 2022-06-14 |
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Citations (2)
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| JP2009250862A (en) * | 2008-04-09 | 2009-10-29 | Fujibo Holdings Inc | Manufacturing method of cartridge filling column for solid phase extraction |
| CN209478774U (en) * | 2018-09-20 | 2019-10-11 | 嘉兴固特塑料制品有限公司 | A kind of polytetrafluoroethylene (PTFE) automatic extruding device filler assembly |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09184830A (en) * | 1995-12-28 | 1997-07-15 | Daicel Chem Ind Ltd | Apparatus and method for filling of filler as well as filler filling column assembly |
| US9116150B2 (en) * | 2007-11-19 | 2015-08-25 | Emd Millipore Corporation | Method of and device for packing a chromatography column |
| CN202351223U (en) * | 2011-12-12 | 2012-07-25 | 云南烟草科学研究院 | Solid-phase extraction column used for measuring benzo[alpha]pyrene in cigarette smoke |
| CN202631493U (en) * | 2012-06-29 | 2012-12-26 | 孙惠青 | Solid-phase extraction column special for residue analysis of pesticide in tobacco |
| JP2015114293A (en) * | 2013-12-16 | 2015-06-22 | 株式会社日立ハイテクノロジーズ | Column for liquid chromatograph and liquid chromatograph apparatus |
| JP2016090336A (en) * | 2014-10-31 | 2016-05-23 | アークレイ株式会社 | Column for chromatography, chromatography apparatus, and method for producing column for chromatography |
| CN204841030U (en) * | 2015-08-10 | 2015-12-09 | 山西省交通科学研究院 | Packing chromatography post preparation facilities |
| GB2570082A (en) * | 2016-10-24 | 2019-07-10 | Jnc Corp | Chromatography column |
| CN108152429A (en) * | 2016-12-04 | 2018-06-12 | 中国科学院大连化学物理研究所 | A kind of Solid Phase Extraction microtrabeculae and application |
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- 2019-12-06 CN CN201911237693.5A patent/CN112915589B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009250862A (en) * | 2008-04-09 | 2009-10-29 | Fujibo Holdings Inc | Manufacturing method of cartridge filling column for solid phase extraction |
| CN209478774U (en) * | 2018-09-20 | 2019-10-11 | 嘉兴固特塑料制品有限公司 | A kind of polytetrafluoroethylene (PTFE) automatic extruding device filler assembly |
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