CN117912931A - Non-contact sample atomization sampling device and method - Google Patents
Non-contact sample atomization sampling device and method Download PDFInfo
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- CN117912931A CN117912931A CN202410314415.XA CN202410314415A CN117912931A CN 117912931 A CN117912931 A CN 117912931A CN 202410314415 A CN202410314415 A CN 202410314415A CN 117912931 A CN117912931 A CN 117912931A
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- 238000000889 atomisation Methods 0.000 title claims abstract description 30
- 238000005070 sampling Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 89
- 230000005540 biological transmission Effects 0.000 claims abstract description 23
- 238000001514 detection method Methods 0.000 claims abstract description 9
- 239000011229 interlayer Substances 0.000 claims description 13
- 230000005284 excitation Effects 0.000 claims description 10
- 230000005684 electric field Effects 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 239000000443 aerosol Substances 0.000 claims 2
- 238000002347 injection Methods 0.000 description 7
- 239000007924 injection Substances 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- Sampling And Sample Adjustment (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a non-contact sample atomization sampling device and a method, wherein the non-contact sample atomization sampling device comprises an ultrasonic unit and a sample container, wherein ultrasonic waves emitted by the ultrasonic unit act on a sample in the sample container, and liquid drops are generated on the liquid surface of the sample; the lower end of the first transmission pipe is opened and is arranged on the upper side of the liquid level of the sample in the sample container; the gas channel provides gas which surrounds the lower end opening, part of the gas flows upwards through the lower end opening, and part of the gas flows downwards and sweeps the liquid level; the distance detection unit obtains the distance between the first transmission pipe and the liquid level of the sample; the first driving unit is used for driving the sample container or the first transmission pipe, so that the distance between the first transmission pipe and the liquid surface of the sample is set value h. The invention has the advantages of simplicity, stability, good ionization effect and the like.
Description
Technical Field
The invention relates to ionization, in particular to a non-contact sample atomization sampling device and method.
Background
At present, the ultrasonic atomization technology is used for quantitative sample atomization, and has the characteristic of non-contact high flux. Ultrasonic atomization generates high-frequency ultrasonic waves by means of an ultrasonic generator, the ultrasonic waves are focused on the upper surface of a liquid sample through a concave lens, and droplets with specific volume size are excited and atomized. The atomized liquid drops can upwards enter the air under the action of ultrasonic energy and are subjected to sample transfer, and then enter a flow path system or are directly ionized to enter mass spectrum detection. The shortcomings of this approach are mainly:
1. When a general sample is placed in a porous plate, the sample amount is inconsistent, so that the liquid level height is inconsistent, ultrasonic atomization energy deviation is easy to cause, and thus, the sample detection amount is inconsistent, and the quantitative detection result is affected.
2. Atomized liquid drops are easy to cause loss in the transmission process, and the detection result is further influenced.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a non-contact sample atomization and injection device.
The invention aims at realizing the following technical scheme:
The non-contact sample atomization and sampling device comprises an ultrasonic unit and a sample container, wherein ultrasonic waves emitted by the ultrasonic unit act on a sample in the sample container, and liquid drops are generated on the liquid surface of the sample; the non-contact sample atomization sampling device further comprises:
the lower end of the first transmission pipe is open and is arranged on the upper side of the liquid level of the sample in the sample container;
a gas passage providing gas surrounding the lower end opening, a portion of the gas flowing upwardly through the lower end opening, a portion of the gas flowing downwardly through the lower end opening of the gas passage and purging the liquid surface;
a distance detection unit, which obtains the distance between the bottom end opening and the liquid level of the sample;
and the first driving unit is used for driving the sample container or the first transmission pipe, so that the distance between the bottom end opening and the sample liquid level is set as a set value h.
The invention further aims to provide a non-contact sample atomization and injection method, which is realized by the following technical scheme:
The non-contact sample atomization sampling method comprises the following steps:
Adjusting the distance between the bottom end opening of the gas channel and the liquid level of the sample in the sample container so that the distance is a set value;
Ultrasonic wave is applied to the sample in the sample container, the liquid level of the sample is atomized, and the generated liquid drops move upwards;
At the same time, gas enters the gas channel, part of the gas flows upwards, collides with the liquid drops, the liquid drops are atomized into smaller liquid drops, and part of the gas flows downwards through the bottom end opening as the gas passes upwards through the lower end opening of the first conveying pipe.
Compared with the prior art, the invention has the following beneficial effects:
1. The structure is simple;
The device integrates the functions of liquid level detection, air flow auxiliary ion transmission, ultrasonic generation of liquid drops, liquid drop movement and the like, and has a compact and simple structure;
2. The stability is good;
The distance between the first transmission pipe and the liquid level is set as a set value through relative movement, and ultrasonic waves are focused on the liquid level of the sample, so that non-contact ultrasonic atomization is ensured to occur at a gas-liquid interface, the size and the size of ultrasonic atomized liquid drops are ensured to be consistent, and quantitative deviation caused by inconsistent sample amounts is avoided;
3. the ionization efficiency is high;
And carrying out air flow auxiliary transmission and plasma ionization (in the first transmission pipe) on the liquid drops, further reducing the volume of single liquid drops, reducing the liquid drop transmission loss and improving the ionization efficiency.
Drawings
The present disclosure will become more readily understood with reference to the accompanying drawings. As will be readily appreciated by those skilled in the art: the drawings are only for illustrating the technical scheme of the present invention and are not intended to limit the scope of the present invention. In the figure:
fig. 1 is a schematic structural diagram of a non-contact sample atomization and injection device according to an embodiment of the invention.
Detailed Description
Fig. 1 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. In order to teach the technical solution of the present invention, some conventional aspects have been simplified or omitted. Those skilled in the art will appreciate variations or alternatives derived from these specific embodiments that fall within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the invention is not limited to the following alternative embodiments, but only by the claims and their equivalents.
Example 1
In the non-contact sample atomization and injection device of the embodiment 1 of the present invention, as shown in fig. 1, the non-contact sample atomization and injection device includes:
An ultrasonic unit 51 and a sample container 31, wherein ultrasonic waves emitted by the ultrasonic unit 51 are applied to a sample in the sample container 31, and a liquid drop is generated on a sample liquid level 71;
a first transfer tube 11, wherein the lower end of the first transfer tube 11 is provided with an opening 12 and is arranged above the sample liquid level 71 in the sample container 31;
A gas channel 81, the gas channel 81 providing gas around the lower end opening 12, part of the gas flowing upward through the lower end opening 12, part of the gas flowing downward through the bottom end opening 22 of the gas channel 81, and purging the sample liquid surface 71;
A distance detecting unit 61, said distance detecting unit 61 obtaining a distance between said bottom end opening 22 and a sample liquid level 71;
A first driving unit for driving the sample container 31 or the first transfer tube 11 such that the distance between the bottom end opening 22 and the sample liquid surface 71 is set at a set value h.
In order to ensure that the sample liquid drop can accurately enter the sampling channel and improve the sampling efficiency, the set valueB is a first correction coefficient, the value is 0.4-0.6, E is the excitation energy of the liquid drop, f is the ultrasonic frequency, sigma is the surface tension, c is the propagation speed of ultrasonic waves in a sample, and ρ is the sample density.
In order to improve the atomization efficiency of the sample liquid drops and the transmission efficiency of the sample liquid drops in the sampling channel, the gas flow rateA is a second correction coefficient, the value is 0.01-0.04, E is the excitation energy of the liquid drop, f is the ultrasonic frequency, c is the propagation speed of ultrasonic waves in a sample, and ρ is the density of the sample.
In order to atomize the sample at the sample level 71, the non-contact sample atomization sampling device further comprises:
and a second driving unit for driving the sample container 31 or the ultrasonic unit 51 so that ultrasonic waves emitted from the ultrasonic unit 51 are focused on the sample liquid surface 71.
In order to drive the liquid drop at the sample liquid surface 71 to move upwards, the non-contact sample atomization sampling device further comprises:
a first electrode 41, the first electrode 41 being disposed above the sample liquid surface 71;
And a second electrode 42, the second electrode 42 is disposed in the interlayer at the bottom of the sample container 31, and the ultrasonic waves emitted by the ultrasonic unit 51 sequentially pass through the second electrode 42 and the sample in the interlayer.
In order to provide a controlled gas, further, a second transfer tube 21 is provided outside the first transfer tube 11, the gas passage 81 is formed in the interlayer between the first transfer tube 11 and the second transfer tube 21, the second transfer tube 21 has a bottom end opening 22 (same as the bottom end opening 22 of the gas passage 81), and liquid droplets sequentially pass through the bottom end opening 22 and the lower end opening 12 from bottom to top.
The non-contact sample atomization sampling method provided by the embodiment of the invention comprises the following steps of:
the distance between the bottom end opening 22 of the gas channel 81 and the sample liquid surface 71 in the sample container 31 is adjusted so that the distance is set to a set value h;
The ultrasonic wave is applied to the sample in the sample container 31, and the sample is atomized at the sample liquid surface 71, so that the generated liquid drops move upwards;
At the same time, gas enters the gas channel 81, part of the gas flows upwards, collides with the droplets, the droplets are atomized into smaller droplets, and as the gas passes upwards through the lower end opening 12 of the first transfer pipe 11, part of the gas flows downwards through said lower end opening 22.
In order to drive the drop to move upwards, further, the way to drive the drop to move upwards is as follows:
The liquid drop is in an electric field between a first electrode 41 and a second electrode 42, and the first electrode 41 is arranged above the sample liquid level 71; the second electrode 42 is disposed in the interlayer at the bottom of the sample container 31, and the ultrasonic waves emitted by the ultrasonic unit 51 sequentially pass through the second electrode 42 and the sample in the interlayer.
In order to ensure that the sample liquid drop can accurately enter the sampling channel and improve the sampling efficiency, the set valueB is the first correction factor, E is the drop excitation energy, f is the ultrasonic frequency, σ is the surface tension, c is the propagation velocity of the ultrasonic wave in the sample, ρ is the sample density.
In order to ensure that sample liquid drops can accurately enter a sampling channel, the sampling efficiency is improved, and the gas flow rate is increasedA is the second correction coefficient, E is the drop excitation energy, f is the ultrasonic frequency, c is the propagation velocity of the ultrasonic wave in the sample, ρ is the sample density.
Example 2
Application of the non-contact sample atomization and injection device and method according to embodiment 1 of the present invention in mass spectrometry.
In this application example, as shown in fig. 1, the first transmission tube 11 and the second transmission tube 21 are made of glass, the second transmission tube 21 is fixedly sleeved outside the first transmission tube 11, and an interlayer between the two transmission tubes is a gas channel 81. The lower end opening 12 of the first transfer tube 11 and the bottom end opening 22 of the second transfer tube 21 are coaxial. The laser type distance detecting unit 61 is provided outside the second transfer tube 21, and the distance between the distance detecting unit 61 and the sample liquid surface 71 is obtained, thereby obtaining the distance between the bottom end opening 22 and the sample liquid surface 71 (the distance between the distance detecting unit 61 and the bottom end opening 22 is fixed).
The first driving unit adopts a combination of a vertical guide rail and a driving module, the second transmission pipe 21 is arranged on the vertical guide rail and is driven by the driving module to move up and down along the vertical guide rail, so that the distance between the bottom end opening 22 and the sample liquid level 71 is ensured to be at a set valueB is the first correction factor, E is the drop excitation energy, f is the ultrasonic frequency, σ is the surface tension, c is the propagation velocity of the ultrasonic wave in the sample, ρ is the sample density.
The gas provided by the gas source enters the gas channel 81 and the flow rateA is the second correction coefficient, E is the drop excitation energy, f is the ultrasonic frequency, c is the propagation velocity of the ultrasonic wave in the sample, ρ is the sample density. The gas flows downwards to the lowest part, part of the gas carries liquid drops upwards through the lower end opening 12 of the first conveying pipe 11 and enters the first conveying pipe 11, and part of the gas downwards passes through the bottom end opening 22 of the second conveying pipe 21, so that external gas is prevented from entering the first conveying pipe 11.
A ground electrode (first electrode 41) surrounds the bottom end opening 22 and is outside the second transfer tube 21. The discharge electrode 43 is provided outside the second transfer tube 21 and above the ground electrode (first electrode 41).
The sample container 31 has a cylindrical structure, and has a bottom portion having an interlayer isolated from the liquid sample, and a second electrode 42 is provided in the interlayer. When the second electrode 42 is energized, the liquid droplets at the sample liquid level 71 due to the ultrasound are driven upward.
The ultrasonic unit 51 is provided at the lower side of the sample container 31. The second driving unit adopts a combination of a vertical guide rail and a driving module, and the ultrasonic unit 51 is arranged on the vertical guide rail and is driven by the driving module to move up and down along the vertical guide rail, so that ultrasonic waves emitted by the ultrasonic unit 51 are ensured to be converged at the sample liquid level 71.
The non-contact sample atomization sampling method of the embodiment of the invention, namely the working method of the sampling device of the embodiment, is as follows:
The distance between the bottom end opening 22 and the sample liquid surface 71 is obtained according to the output distance of the distance detection unit 61, and the position of the second transmission pipe 21 on the vertical guide rail is adjusted by the first driving unit according to the deviation between the distance and the set value h, so that the distance between the bottom end opening 22 of the second transmission pipe 21 and the sample liquid surface 71 in the sample container 31 is set to the set value h;
The power supply supplies power to the discharge electrode 43 and the second electrode 42;
adjusting the position of the ultrasonic unit 51 on the vertical guide rail so that ultrasonic waves are converged at the sample liquid level 71 in the sample container 31, atomizing the sample liquid level 71, and moving the generated liquid drops upwards in the electric field between the first electrode 41 and the second electrode 42;
At the same time, a portion of the gas surrounding the lower end opening 12 flows upward, collides with the droplets, atomizes the droplets into smaller droplets, and as the gas passes upward through the lower end opening 12 of the first transfer tube 11, a portion of the gas passes through the bottom end opening 22 of the second transfer tube 21, flows downward, sweeps the sample liquid surface 71, and prevents the outside gas from entering the first transfer tube 11.
The droplets entering the first transfer tube 11 are ionized by the discharge electrode 43 to form ions;
ions exit the first transfer tube 11 and enter the mass spectrometer 91.
The parameters in this embodiment are as follows: ethanol was used as solvent, f=4.5 mhz, a 0.023, b 0.51, e=50 μj, σ=22 mN/m, c=1207 m/s, ρ=789 kg/m 3, giving h=9.7mm, q=0.36L/min.
Example 3
The application example of the non-contact sample atomization and injection device and method according to embodiment 1 of the present invention in mass spectrometry is different from embodiment 2 in that:
The distance detecting unit 61 obtains the distance between the unit and the sample liquid surface 71, and the set value is the set distance (between the bottom end opening 22 and the sample liquid surface 71) plus the distance (between the distance detecting unit 61 and the bottom end opening 22).
Claims (10)
1. The non-contact sample atomization and sampling device comprises an ultrasonic unit and a sample container, wherein ultrasonic waves emitted by the ultrasonic unit act on a sample in the sample container, and liquid drops are generated on the liquid surface of the sample; the non-contact sample atomization sampling device is characterized by further comprising:
the lower end of the first transmission pipe is open and is arranged on the upper side of the liquid level of the sample in the sample container;
a gas passage providing gas surrounding the lower end opening, a portion of the gas flowing upwardly through the lower end opening, a portion of the gas flowing downwardly through the lower end opening of the gas passage and purging the liquid surface;
a distance detection unit, which obtains the distance between the bottom end opening and the liquid level of the sample;
and the first driving unit is used for driving the sample container or the first transmission pipe, so that the distance between the bottom end opening and the sample liquid level is set as a set value h.
2. The non-contact sample atomization and introduction device according to claim 1, wherein the set valueB is the first correction factor, E is the drop excitation energy, f is the ultrasonic frequency, σ is the surface tension, c is the propagation velocity of the ultrasonic wave in the sample, ρ is the sample density.
3. The non-contact sample atomization and introduction device according to claim 1, wherein the gas flow rate isA is the second correction coefficient, E is the drop excitation energy, f is the ultrasonic frequency, c is the propagation velocity of the ultrasonic wave in the sample, ρ is the sample density.
4. The non-contact sample aerosol delivery device of claim 1, further comprising:
And the second driving unit is used for driving the sample container or the ultrasonic unit so that ultrasonic waves emitted by the ultrasonic unit are focused on the liquid surface of the sample.
5. The non-contact sample aerosol delivery device of claim 1, further comprising:
a first electrode disposed above the sample liquid surface;
The second electrode is arranged in the interlayer at the bottom of the sample container, and the ultrasonic waves emitted by the ultrasonic unit sequentially pass through the second electrode and the sample in the interlayer.
6. The non-contact sample atomizing and feeding device according to claim 1, wherein a second conveying pipe is arranged outside the first conveying pipe, the gas channel is arranged in an interlayer between the first conveying pipe and the second conveying pipe, the second conveying pipe is provided with a bottom end opening, and liquid drops sequentially pass through the bottom end opening and the lower end opening from bottom to top.
7. The non-contact sample atomization sampling method comprises the following steps:
Adjusting the distance between the bottom end opening of the gas channel and the liquid level of the sample in the sample container to make the distance be a set value h;
Ultrasonic wave is applied to the sample in the sample container, the liquid level of the sample is atomized, and the generated liquid drops move upwards;
At the same time, gas enters the gas channel, part of the gas flows upwards, collides with the liquid drops, the liquid drops are atomized into smaller liquid drops, and part of the gas flows downwards through the bottom end opening as the gas passes upwards through the lower end opening of the first conveying pipe.
8. The method for atomizing and feeding a non-contact sample according to claim 7, wherein the method for driving the liquid drop to move upwards is as follows:
The liquid drop is positioned in an electric field between a first electrode and a second electrode, and the first electrode is arranged on the upper side of the liquid level of the sample; the second electrode is arranged in the interlayer at the bottom of the sample container, and the ultrasonic waves emitted by the ultrasonic unit sequentially pass through the second electrode and the sample in the interlayer.
9. The method for atomizing and feeding a non-contact sample according to claim 7, wherein the set valueB is the first correction factor, E is the drop excitation energy, f is the ultrasonic frequency, σ is the surface tension, c is the propagation velocity of the ultrasonic wave in the sample, ρ is the sample density.
10. The method for atomizing and feeding a non-contact sample according to claim 7, wherein the flow rate of the gas isA is the second correction coefficient, E is the drop excitation energy, f is the ultrasonic frequency, c is the propagation velocity of the ultrasonic wave in the sample, ρ is the sample density.
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