In-situ cleaning method for ion transfer tube
Technical Field
The invention relates to an in-situ cleaning method for an ion transfer tube.
Background
The ion mobility spectrometry is widely applied to detection of chemical toxicants, explosives, drugs and the like due to the advantages of high analysis speed, high sensitivity, small volume, simple operation and the like. In addition, ion mobility spectrometry can separate isomers, and is often used in combination with mass spectrometry to detect biological samples. In recent years, the application of ion mobility spectrometry has been advanced to the field of medical diagnosis, such as the detection of small molecule metabolites in exhaled breath, anesthetics in blood, and the like. However, when the ion mobility spectrometry is used for detecting complex samples or is used for field detection, a signal saturation memory effect is easily generated. When the migration tube is not used for a long time, the migration tube is easy to be polluted, and when the migration tube is used again, a plurality of unknown peaks generally exist in a spectrogram, so that qualitative and quantitative detection is influenced. Because the mobility spectrometry works under the atmospheric pressure, the residual ions and the neutralized ions of the sample are easily adsorbed on the inner wall of the migration tube, and are difficult to directly purge through drift gas. In addition, the migration tube has a complex structure, generally adopts a stacked structure, has multiple and fine parts, and is troublesome to directly unpick and wash. Particularly, the teflon insulator commonly used in the transfer pipe is expanded and deformed after the transfer pipe is heated and used, and is often difficult to reassemble after being disassembled and washed, or the sealability is deteriorated after the reassembly.
The patent of dense jade army applied for "an ion migration tube convenient to dismantle and wash" authorizes in 2019, 1 month and 4 days, and its technical characteristics are that the inner tube and the outer tube of the ion migration tube used for ion migration number experiment are connected through integrated into one piece's inner plug and outer canning, seal, and the dismantlement of the inner tube of being convenient for is washd, but this kind of mode still need be unpacked the washing apart from the ion migration tube, then at the equipment reduction, still is not convenient enough. The patent of the first research institute of the ministry of public security "-a purification treatment method for sample strips by ion mobility spectrometry", the sample strips after sampling detection are treated by a dissolving solvent, a cleaning solvent and pure water in sequence, and then dried to recover the performance, but the cleaning in a migration tube is not involved.
In addition, when the migration tube works, a uniform electric field needs to be formed in the migration tube and a pulse control ion gate needs to be applied, so that the connection of a conducting wire on the migration tube is complex, and the migration tube generally needs to be matched with a heating sheet and a heat-insulating material for use together, so that the detachment of the migration tube from the whole migration spectrum machine is troublesome.
If the transfer pipe can be directly cleaned under the condition of keeping the transfer pipe intact on the whole machine, a large amount of labor and time can be saved.
Disclosure of Invention
The invention aims to provide a time-saving and labor-saving method for cleaning an ion transfer tube, which can be used for directly cleaning the ion transfer tube under the condition of keeping the ion transfer tube intact on the whole machine.
In order to achieve the above purpose, the invention adopts the technical scheme that:
1) cutting off the power supply of the ion migration tube;
2) a container with an opening at the upper end and filled with cleaning fluid is adopted, a sealing cover is arranged at the upper opening end of the container, and the sealing cover is hermetically connected with the upper opening end of the container; one end of a cleaning liquid outflow pipe penetrates through the side wall surface of the sealing cover or the container and extends below the liquid level of the cleaning liquid, the other end of the cleaning liquid outflow pipe is connected with a gas inlet or outlet at one end (close to one side of the receiving electrode or close to the ionization source) of the ion migration pipe, and a gas inlet or outlet facing upwards at the other end (close to one side of the ionization source or close to one side of the receiving electrode) of the ion migration pipe is connected with a cleaning liquid recovery bottle through a pipeline; one end of a pressurized gas pipe penetrates through the sealing cover or the side wall surface of the container and extends into the container, and the other end of the pressurized gas pipe is connected with an outlet of an air compressor or an outlet of a high-pressure gas cylinder through a valve; opening an outlet valve of an air compressor or a high-pressure gas cylinder to continuously introduce the cleaning liquid in the container into the ion migration tube, and discharging the cleaning liquid from the ion migration tube after the whole ion migration tube is filled with the cleaning liquid, so that the online cleaning of the ion migration tube is realized; the outlet air of the air compressor is purified by a molecular sieve and activated carbon and then is introduced into the container, and the flow rate is controlled by the flow controller and is between 1 and 500 mL/min.
3) And introducing air or nitrogen into a gas inlet or outlet at one end (close to the side of the receiving electrode or close to the ionization source) of the ion migration tube, and emptying the gas inlet or outlet at the other end (close to the side of the ionization source or close to the side of the receiving electrode) of the ion migration tube to remove the cleaning liquid in the ion migration tube.
4) After cleaning, the container is removed, a gas inlet or an outlet at one end (close to one side of an ionization source or close to one side of a receiving electrode) of the ion migration tube faces downwards, purified air is introduced into the ion migration tube from the gas inlet or the outlet at the other end (close to one side of the receiving electrode or close to one side of the ionization source) of the ion migration tube, after all residual cleaning liquid is removed, the high-voltage power supply of the ion migration tube is opened after the ion migration tube is dried, the gas circuit is recovered to be normal, and the instrument is recovered to be used.
The invention has the advantages that:
the method is simple and rapid, and the ion migration tube can be cleaned on line.
The ion migration tube does not need to be disassembled and assembled in the cleaning process.
Drawings
FIG. 1 is a schematic view of a cleaning apparatus of the present invention. Wherein, (1) the container, (2) the gland bonnet, (3) the silicone tube of seal, (4) carry the gas pipeline, (5) the ion migration tube, (6) the cleaning fluid, (7) float the gas pipeline, (8) float the gas entry, (9) the tail gas outlet, (10) the pressurized gas tube
Fig. 2 is a background spectrum of an ion mobility tube after long-term use and a background spectrum of the ion mobility tube after being washed with purified water and methanol in sequence by adopting the washing mode of the invention.
Detailed Description
Please refer to fig. 1, which is a schematic diagram of the present invention.
And closing the main power supply of the ion migration tube, and blocking other air outlets on the ion migration tube except the floating air inlet on one side of the receiving electrode and the tail gas outlet on one side of the ionization source. A container (1) with an opening at the upper end and filled with pure water cleaning solution (6) is adopted, a sealing cover (2) is arranged at the upper opening end of the container, and the sealing cover is hermetically connected with the upper opening end of the container; two round holes are punched on the sealing cover, and two small sections of silicone tubes (3) are respectively inserted into the two round holes. One end of an outflow pipe (4) of the cleaning liquid penetrates through one section of the silicone tube and extends into the bottom of the container, the other end of the outflow pipe is connected with a floating gas inlet (8) of the ion migration pipe (5), and a tail gas outlet (9) positioned on one side of an ionization source of the ion migration pipe is connected with a cleaning liquid recovery bottle through a pipeline (7); one end of a pressurized gas pipe (10) penetrates through the other section of silicone tube and extends into the container, and the other end of the pressurized gas pipe is connected with an outlet of the air compressor; opening an outlet valve of an air compressor to continuously introduce pure water cleaning liquid in the container into the ion migration tube, and discharging the pure water cleaning liquid from the ion migration tube after the ion migration tube is filled with the pure water cleaning liquid, so that the ion migration tube is cleaned on line; the outlet air of the air compressor is purified by a molecular sieve and activated carbon and then is introduced into the container, and the flow rate is controlled to be 50mL/min by using a flow controller. After the pure water in the container is used up, ethanol is added as a cleaning solution, and the migration tube is further cleaned. After the cleaning is finished, the container is removed, the air floating inlet of the ion migration tube is downward, purified air is introduced into the ion migration tube from the air floating inlet of the ion migration tube, all residual cleaning liquid is removed, the cleaning liquid in the ion migration tube is purged completely, then the high-voltage power supply of the ion migration tube is opened, the gas circuit is recovered to be normal, and the instrument is recovered to be used.
Example 1: by using the cleaning method, the cleaning solution is selected to be water and ethanol to clean the ion transfer tube after long-term use. The background spectrogram of the migration tube before and after cleaning is shown in fig. 2, and it can be seen that after the ion migration tube is cleaned by using the rigid method, the impurity peak basically disappears completely, the intensity of the reagent ion peak is greatly enhanced, and the detection sensitivity is favorably improved.