CN112505336B - Ultrahigh vacuum sample transfer equipment and method - Google Patents
Ultrahigh vacuum sample transfer equipment and method Download PDFInfo
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- CN112505336B CN112505336B CN201910872736.0A CN201910872736A CN112505336B CN 112505336 B CN112505336 B CN 112505336B CN 201910872736 A CN201910872736 A CN 201910872736A CN 112505336 B CN112505336 B CN 112505336B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
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Abstract
The invention discloses ultrahigh vacuum sample transfer equipment and a transfer method, and belongs to the technical field of material testing. The transfer equipment comprises a transfer main body and an auxiliary device which are detachably connected, wherein the transfer main body comprises a sample chamber and a vacuum device, and a first valve and a second valve are respectively arranged at two ends of the sample chamber; the auxiliary device comprises a first cooling corrugated pipe, a second cooling corrugated pipe and a sample transfer device, one end of the first cooling corrugated pipe is communicated with the sample transfer device, the other end of the first cooling corrugated pipe is communicated or disconnected with the sample introduction chamber through a first valve, one end of the second cooling corrugated pipe is communicated or disconnected with the sample introduction chamber through a second valve, the other end of the second cooling corrugated pipe can be communicated with the target chamber through a third valve, the second cooling corrugated pipe is communicated with the sample transfer device and communicated with the mobile pump group, cooling parts are arranged on the peripheries of the first cooling corrugated pipe and the second cooling corrugated pipe, and the sample transfer device can grab a sample in the sample introduction chamber and send the sample to the target chamber. The invention ensures an ultra-vacuum environment and avoids the sample from being polluted in the transferring process.
Description
Technical Field
The invention relates to the technical field of material testing, in particular to ultrahigh vacuum sample transfer equipment and a method for transferring a sample by using the same.
Background
An ultrahigh vacuum equipment system is an indispensable important hardware basis in performing ultrahigh vacuum experiments, and is generally formed by combining a vacuum pump, a vacuum gauge, a vacuum cavity and other elements according to certain requirements by means of a vacuum pipeline. The method ensures that a specific ultrahigh vacuum environment (the typical vacuum degree is better than 10E-10 mbar) is obtained and maintained in a certain space, ensures that a certain process or physical process is implemented in a vacuum system, and has wide application in various research fields of semiconductors, machining, physics, chemistry, materials, bioscience and the like.
After the sample is prepared in the ultra-high vacuum system, it is usually tested and analyzed in an environment without destroying the ultra-high vacuum in order to ensure the stable properties of the sample. Currently, it is possible to integrate sample preparation and testing equipment into an ultra-high vacuum system, which generally includes a robot arm that can be used to transfer a sample at a specific location within a chamber, so that both sample preparation and testing can be performed in the same ultra-high vacuum environment. However, the testing equipment required in one set of equipment is limited, and to analyze the properties of the sample more comprehensively, the sample has to be taken out from a certain vacuum system and transferred to other ultrahigh vacuum systems for testing and analysis, and the process inevitably contacts air and dust to cause the pollution of the sample.
At present, several methods can protect a sample, for example, inert gas is introduced into a vacuum cavity to be used as protective gas, and then the sample is taken out and is rapidly placed into a clean sample box or a vacuum box; or plating a protective film on the sample and taking out the sample. However, most of them are complicated to operate, and each method cannot avoid the operation of "open cavity sampling" in which the sample is exposed to a non-vacuum gas atmosphere. Once the vacuum environment around the sample is broken, the gas is adsorbed to the surface of the sample, and the sample is polluted to some extent.
In view of the above problems, related ultra-high vacuum sample transfer devices have appeared in the industry, but besides the problem of high manufacturing cost of the device, there still exist many problems in the using process, such as: the vacuum degree of the whole equipment is difficult to ensure. Long-distance transportation is inconvenient, and the ultrahigh vacuum degree cannot be maintained for a long time. Need toast the intermediate junction at the in-process that carries out sample from transferring chamber to vacuum cavity, the heat can transmit to transfer apparatus among the toasting process, can make the vacuum degree variation more than two orders of magnitude, can not guarantee that the sample is in the environment of ultrahigh vacuum all the time, can not satisfy the requirement of ultrahigh vacuum (1E-10 mbar).
Therefore, there is a need for an ultra-high vacuum sample transferring apparatus and transferring method, which can solve the problem of the vacuum degree of the transferring apparatus becoming poor during the baking process.
Disclosure of Invention
The invention aims to provide an ultrahigh vacuum sample transfer device and a transfer method, which are used for ensuring that a sample is always in an ultrahigh vacuum environment in the processes of storage, transportation and transfer and the sample is not polluted.
In order to realize the purpose, the following technical scheme is provided:
the invention provides an ultrahigh vacuum sample transfer device, which comprises a transfer main body and an auxiliary device which are detachably connected,
the transfer main body comprises a sample chamber for placing a sample and a vacuum device for vacuumizing the sample chamber, wherein a first valve and a second valve are respectively arranged at two ends of the sample chamber;
the auxiliary device comprises a first cooling corrugated pipe, a second cooling corrugated pipe and a sample transfer device, one end of the first cooling corrugated pipe is communicated with the sample transfer device, the other end of the first cooling corrugated pipe can be communicated with the sample introduction chamber through the first valve or disconnected, one end of the second cooling corrugated pipe is communicated with the sample introduction chamber through the second valve or disconnected, the other end of the second cooling corrugated pipe can be communicated with the target chamber, the sample transfer device is communicated with the mobile pump set through the third valve, the first cooling corrugated pipe and the periphery of the second cooling corrugated pipe are provided with cooling parts for the cooling of the sample introduction chamber, and the sample transfer device can grab samples in the sample introduction chamber and send the samples to the target chamber.
Further, the sampling chamber includes the main cavity room and stretches into advance the appearance platform in the main cavity room, advance the appearance platform and be used for depositing the sample, it can to advance the appearance platform reciprocate in the main cavity room.
Further, the first cooling bellows and the second cooling bellows are provided with three adjusting screws along the axial direction thereof, and the three adjusting screws can selectively adjust the axial direction of the corresponding cooling bellows.
Furthermore, the auxiliary device further comprises a connecting pipeline, a tee joint and a cross joint, wherein the tee joint is respectively connected with the sample transfer device, the first cooling corrugated pipe and one end of the connecting pipeline, and the cross joint is respectively connected with the second cooling corrugated pipe, the other end of the connecting pipeline, the mobile pump group and the target chamber.
Further, the first valve, the second valve and the third valve are hand valves.
Further, the vacuum device comprises an adsorption pump and an ion pump, the adsorption pump is communicated with the sampling chamber, and the ion pump is communicated with the adsorption pump.
Furthermore, the sample transfer device comprises a magnetic rod extending into the sample chamber from the outside of the sample chamber, and the magnetic rod can clamp the sample in the sample chamber and control the movement and rotation of the sample.
Further, the cooling member is a water pipe wound around the outer peripheries of the first cooling bellows and the second cooling bellows.
Furthermore, two sides of the sampling chamber are respectively provided with an observation window.
The invention also provides a method for transferring a sample by using the ultrahigh vacuum sample transfer device, which comprises the following steps:
s1, closing the first valve and the second valve, and vacuumizing a sample chamber by using a vacuum device;
s2, connecting a first cooling corrugated pipe and a second cooling corrugated pipe of the auxiliary device to a first valve and a second valve of the sampling chamber respectively;
s3, opening a third valve, vacuumizing the auxiliary device by using a movable pump group, starting cooling parts on the peripheries of the two cooling corrugated pipes, and baking the parts, except the two cooling corrugated pipes, of the auxiliary device at the baking temperature of 100-130 ℃ for more than two days;
s4, stopping baking, naturally cooling the auxiliary device to room temperature, closing the third valve, communicating the second cooling corrugated pipe with the target chamber, and opening the first valve and the second valve;
s5, adjusting the first cooling corrugated pipe, enabling the sample transfer device to enter the sample introduction chamber for sampling, adjusting the second cooling corrugated pipe, and pushing the sample to the target chamber by the sample transfer device;
s6, after the process is finished, taking out the sample, placing the sample into a sample introduction chamber, firstly cutting off the communication between the second cooling corrugated pipe and the target chamber, then closing the first valve and the second valve, and taking down the auxiliary device.
Compared with the prior art, the ultrahigh vacuum sample transfer equipment has the advantages that the transfer main body is detachably connected with the auxiliary device, the sample can be separately transported during transportation, the space is saved, the transfer main body is always kept in a vacuum state, the sample can be kept in an ultrahigh vacuum environment of 1E-10mbar in the sample introduction chamber, the auxiliary device can be exposed in the atmosphere, the requirements on storage and transportation conditions are low, and the ultrahigh vacuum sample transfer equipment is convenient to store and transport. When the auxiliary device is used and connected, two ends of the sample inlet chamber are respectively communicated with one end of a first cooling corrugated pipe and one end of a second cooling corrugated pipe of the auxiliary device through a first valve and a second valve, and cooling parts on the peripheries of the first cooling corrugated pipe and the second cooling corrugated pipe are used for cooling the sample inlet chamber, so that when parts except the two cooling corrugated pipes on the auxiliary device are baked, the baking process can be ensured, when heat is transferred to the two cooling corrugated pipes, redundant heat is taken away, the sample inlet chamber is not influenced by baking, the normal temperature is kept, the vacuum of 1E-10mbar is kept in the sample inlet chamber, the sample inlet chamber can keep an ultrahigh vacuum environment in the transportation process and the sample transfer process, and samples are not polluted.
The invention provides an ultrahigh vacuum sample transfer method, wherein a transfer main body and an auxiliary device are detachable, and when in use, two corrugated pipes of the auxiliary device are firstly connected to a first valve and a second valve of the transfer main body. The auxiliary device is vacuumized again, the parts of the auxiliary device except the cooling corrugated pipes are baked to remove gas and moisture, the cooling parts on the periphery of the cooling corrugated pipes can ensure the baking process, when heat is transferred to the two cooling corrugated pipes, redundant heat is taken away, the sample inlet chamber is not affected by baking and is kept at normal temperature, so that the vacuum of 1E-10mbar is kept in the sample inlet chamber, the sample inlet chamber can be kept in an ultrahigh vacuum environment in the transportation process and the sample transfer process, and a sample is not polluted.
Drawings
FIG. 1 is a schematic diagram of an ultra-high vacuum sample transfer apparatus in an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a transfer body in an embodiment of the present invention;
fig. 3 is a schematic structural diagram of a first cooling bellows in an embodiment of the present invention.
Reference numerals are as follows: 1-a main chamber; 2-an adsorption pump; 3-an ion pump; 4-a first valve; 5-a second valve; 6-a sample introduction table; 7-a first cooling bellows; 701-adjusting a screw rod; 702-a cooling member; 8-a second cooling bellows; 9-magnetic pole; 10-a tee joint; 11-four-way; 12-connecting a pipe; 13-third valve.
Detailed Description
In order to make the technical problems solved, technical solutions adopted and technical effects achieved by the present invention clearer, the technical solutions of the embodiments of the present invention will be described in further detail below with reference to the accompanying drawings. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
As shown in fig. 1, the present embodiment provides an ultrahigh vacuum sample transfer apparatus, which includes a transfer main body and an auxiliary device detachably connected, wherein the transfer main body includes a sample chamber for placing a sample and a vacuum device for vacuumizing the sample chamber, and a first valve 4 and a second valve 5 are respectively installed at two ends of the sample chamber; the auxiliary device comprises a first cooling corrugated pipe 7, a second cooling corrugated pipe 8 and a sample transfer device, one end of the first cooling corrugated pipe 7 is communicated with the sample transfer device, the other end of the first cooling corrugated pipe can be communicated or disconnected with the sample introduction chamber through a first valve 4, one end of the second cooling corrugated pipe 8 is communicated or disconnected with the sample introduction chamber through a second valve 5, the other end of the second cooling corrugated pipe can be communicated with the target chamber, the second cooling corrugated pipe is communicated with the sample transfer device, the third valve 13 is communicated with the mobile pump group, cooling parts 702 are arranged on the peripheries of the first cooling corrugated pipe 7 and the second cooling corrugated pipe 8 and used for cooling the sample introduction chamber, and the sample transfer device can grab a sample in the sample introduction chamber and send the sample to the target chamber.
The connection can be dismantled to the transfer main part and the auxiliary device of this embodiment, and the detachable transportation during the transportation practices thrift the space, and transfers the main part and remain the vacuum state all the time, and the sample can keep super high vacuum environment 1E-10mbar in the appearance chamber, and auxiliary device can expose in the atmosphere, deposits and transport condition and requires lowly, is convenient for deposit and transport. When baking the part outside two cooling bellows on the auxiliary device, cooling part 702 can ensure to bake the in-process, and when heat transfer was to two cooling bellows, unnecessary heat was taken away, and the sampling room is not toasted the influence, keeps the normal atmospheric temperature to make and keep 1E-10mbar vacuum in the sampling room, realize that the sampling room can both keep the ultrahigh vacuum environment in transportation process and sample transfer process, the sample does not receive the pollution.
Specifically, as shown in fig. 2, the sample introduction chamber comprises a main chamber 1 and a sample introduction table 6 extending into the main chamber 1, wherein the sample introduction table 6 is used for storing samples and can store 5 flag-type sample holders, and the sample introduction table 6 can move up and down in the main chamber 1, specifically, the up and down movement of the sample introduction table 6 can be realized by rotating an operating rod. As shown in fig. 1, the sample transfer device includes a magnetic rod 9 extending into the main chamber 1 from the outside of the main chamber 1, the magnetic rod 9 can clamp the sample in the main chamber 1 and control the sample to move and rotate, so as to realize the grabbing and parking of the sample on the sample introduction table 6, and transfer the sample to the target chamber.
Further, the first cooling bellows 7 and the second cooling bellows 8 have the same structure, and specifically, as shown in fig. 3, three adjusting screws 701 are respectively disposed outside the first cooling bellows 7 and the second cooling bellows 8 along the axial direction thereof, and the three adjusting screws 701 can selectively adjust the axial direction of the corresponding cooling bellows, so as to achieve fine adjustment of the axial direction of the magnetic rod 9. Specifically, by adjusting the adjusting screw 701 on the first cooling corrugated pipe 7, the sampling head at the end of the magnetic rod 9 can smoothly grab the sample in the main chamber 1; by adjusting the adjusting screw on the second cooling bellows 8, the magnetic rod 9 can smoothly transfer the grasped sample to the target chamber.
In this embodiment, the main chamber 1 adopts a spherical chamber structure, and two sides are respectively provided with an observation window, so that the sample can be conveniently transferred and observed.
Further, the auxiliary device further comprises a connecting pipeline 12, a tee joint 10 and a cross joint 11, wherein the tee joint 10 is respectively connected with the sample transfer device, the first cooling corrugated pipe 7 and one end of the connecting pipeline 12, the cross joint 11 is respectively connected with the second cooling corrugated pipe 8, the other end of the connecting pipeline 12, the mobile pump group and the target chamber, and the connecting pipeline 12 is used for communicating the cross joint 11 with the magnetic rod 9. The tee joint 10 mainly can realize vacuumizing the magnetic rod 9 when the magnetic rod 9 is partially atmospheric, and the tee joint 11 can be connected with the mobile pump group through the third valve 13. In this embodiment, the first valve 4, the second valve 5, and the third valve 13 are preferably hand valves. Wherein the first valve 4 and the second valve 5 are used for keeping the main chamber 1 closed, and the transfer main body and the auxiliary device are separated conveniently and are convenient to carry and transport by dismounting side parts of the first valve 4 and the second valve 5.
Optionally, the vacuum device comprises an adsorption pump 2 and an ion pump 3, the adsorption pump 2 is communicated with the main chamber 1, and the ion pump 3 is communicated with the adsorption pump 2. The sorption pump 2 maintains a vacuum, typically around 1E-10mbar, in the main chamber 1, mainly by rare metals, which react chemically in combination with air. The ion pump 3 can be vacuumized after being electrified, and the vacuum degree of the main chamber 1 can be displayed at the same time.
In this embodiment, the cooling member 702 is preferably a water pipe wound around the periphery of the cooling bellows, and specifically, the water pipe is a copper water pipe wound around the periphery of the cooling bellows, and the copper water pipe has good thermal conductivity, and water flows through the water pipe during the baking and heating process, so that heat on the magnetic rod 9 is taken away by the water pipe when being transferred to the cooling bellows, thereby ensuring that the main chamber 1 is at room temperature and ensuring good vacuum degree.
The invention also provides a method for transferring a sample by using the ultrahigh vacuum sample transfer equipment, which comprises the following steps:
s1, closing a first valve 4 and a second valve 5, and vacuumizing a main chamber 1 by using an adsorption pump 2 and an ion pump 3;
s2, connecting a first cooling corrugated pipe 7 and a second cooling corrugated pipe 8 of the auxiliary device to a first valve 4 and a second valve 5 of the main chamber 1 respectively;
and S3, connecting a mobile pump group to a third valve 13, and vacuumizing the auxiliary device by using the mobile pump group, wherein the vacuumizing is usually carried out to 10E-7mbar, and preferably 10E-8mbar.
S4, opening the water pipe, and baking the magnetic rod 9, the tee joint 10, the connecting pipeline 12 and the cross joint 11 at the baking temperature of 100-130 ℃ for more than two days;
s5, stopping baking, naturally cooling the magnetic rod 9, the tee joint 10, the connecting pipeline 12 and the cross joint 11 to room temperature, closing the third valve 13, communicating the cross joint 11 with a target chamber, and opening the first valve 4 and the second valve 5;
s6, adjusting the first cooling corrugated pipe 7, enabling the magnetic rod 9 to enter the main cavity 1 for sampling, adjusting the second cooling corrugated pipe 8, and pushing the sample to a target cavity through the magnetic rod 9;
s7, after the process is finished, taking out the sample, placing the sample on a sample injection platform 6, firstly cutting off the communication between the four-way 11 and the target chamber, then closing the first valve 4 and the second valve 5, keeping the transfer main body in vacuum, breaking the atmosphere of the auxiliary device, and taking down the auxiliary device.
The baking temperature can be 100 ℃, 120 ℃ or 130 ℃, the baking time is preferably 120 ℃ in the embodiment, the baking time is preferably two days, the baking condition can meet the requirement of the vacuum degree of the sample, the temperature is proper, and the baking time is not long or short.
The present embodiment provides an ultra-high vacuum sample transfer method, wherein the transfer main body and the auxiliary device are detachable, and when in use, the two bellows of the auxiliary device are firstly connected to the first valve 4 and the second valve 5 of the transfer main body. Carry out the evacuation to auxiliary device again, toast the part outside two cooling bellows of auxiliary device simultaneously and remove gas and moisture, the water pipe of two cooling bellows periphery leads to water this moment, can ensure to toast the in-process, when heat transfer to two cooling bellows, unnecessary heat is taken away, main cavity 1 does not receive and toasts the influence, keep the normal atmospheric temperature, thereby make and keep 1E-10mbar vacuum in main cavity 1, the realization can both keep the super high vacuum environment in transportation and sample transfer process main cavity 1, the sample does not receive the pollution.
It is to be noted that the foregoing is only illustrative of the preferred embodiments of the present invention and the technical principles employed. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, but is capable of various obvious changes, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, although the present invention has been described in greater detail by the above embodiments, the present invention is not limited to the above embodiments, and may include other equivalent embodiments without departing from the spirit of the present invention, and the scope of the present invention is determined by the scope of the appended claims.
Claims (8)
1. An ultrahigh vacuum sample transfer device is characterized by comprising a transfer main body and an auxiliary device which are detachably connected,
the transfer main body comprises a sample chamber for placing a sample and a vacuum device for vacuumizing the sample chamber, wherein a first valve (4) and a second valve (5) are respectively arranged at two ends of the sample chamber;
the auxiliary device comprises a first cooling corrugated pipe (7), a second cooling corrugated pipe (8) and a sample transfer device, one end of the first cooling corrugated pipe (7) is communicated with the sample transfer device, the other end of the first cooling corrugated pipe is communicated or disconnected with the sample chamber through the first valve (4), one end of the second cooling corrugated pipe (8) is communicated or disconnected with the sample chamber through the second valve (5), the other end of the second cooling corrugated pipe can be communicated with a target chamber and is communicated with the sample transfer device, the second cooling corrugated pipe is communicated with a mobile pump group through a third valve (13), cooling parts (702) are arranged on the peripheries of the first cooling corrugated pipe (7) and the second cooling corrugated pipe (8) and used for cooling the sample chamber, and the sample transfer device can grab a sample in the sample chamber and send the sample to the target chamber;
the auxiliary device further comprises a connecting pipeline (12), a tee joint (10) and a cross joint (11), the tee joint (10) is respectively connected with the sample transfer device, the first cooling corrugated pipe (7) and one end of the connecting pipeline (12), and the cross joint (11) is respectively connected with the second cooling corrugated pipe (8), the other end of the connecting pipeline (12), the mobile pump group and the target chamber;
the cooling part (702) is a water pipe wound around the outer peripheries of the first cooling corrugated pipe (7) and the second cooling corrugated pipe (8).
2. Ultra-high vacuum sample transfer device according to claim 1, wherein the sample chamber comprises a main chamber (1) and a sample table (6) extending into the main chamber (1), the sample table (6) being used for storing samples, the sample table (6) being movable up and down within the main chamber (1).
3. The ultra-high vacuum sample transfer apparatus according to claim 1, wherein the first cooling bellows (7) and the second cooling bellows (8) are each externally provided with three adjusting screws (701) along the axial direction thereof, and the three adjusting screws (701) are capable of selectively adjusting the axial direction of the respective cooling bellows.
4. The ultra-high vacuum sample transfer device according to claim 1, wherein the first valve (4), the second valve (5) and the third valve (13) are hand valves.
5. The ultra-high vacuum sample transfer device according to claim 1, wherein the vacuum means comprises an adsorption pump (2) and an ion pump (3), the adsorption pump (2) being in communication with the sample entry chamber, the ion pump (3) being in communication with the adsorption pump (2).
6. The ultra-high vacuum sample transfer device according to claim 1, wherein the sample transfer means comprises a magnetic rod (9) extending into the sample chamber from outside the sample chamber, the magnetic rod (9) being capable of clamping the sample in the sample chamber and controlling the movement and rotation of the sample.
7. The ultra-high vacuum sample transfer device of claim 1, wherein the sample chamber is provided with viewing windows on both sides.
8. A method of sample transfer using the ultra-high vacuum sample transfer device of any of claims 1-7, the method comprising the steps of:
s1, closing a first valve (4) and a second valve (5), and vacuumizing a sampling chamber by using a vacuum device;
s2, connecting a first cooling corrugated pipe (7) and a second cooling corrugated pipe (8) of the auxiliary device to a first valve (4) and a second valve (5) of the sample chamber respectively;
s3, opening a third valve (13), vacuumizing the auxiliary device by using a movable pump group, starting cooling parts (702) on the peripheries of the two cooling corrugated pipes, and baking the parts, except the two cooling corrugated pipes, of the auxiliary device at the baking temperature of 100-130 ℃ for more than two days;
s4, stopping baking, naturally cooling the auxiliary device to room temperature, closing a third valve (13), communicating a second cooling corrugated pipe (8) with the target chamber, and opening a first valve (4) and a second valve (5);
s5, adjusting a first cooling corrugated pipe (7), enabling a sample transfer device to enter a sample introduction chamber for sampling, adjusting a second cooling corrugated pipe (8), and pushing a sample to a target chamber by the sample transfer device;
s6, after the process is finished, taking out the sample, placing the sample into a sample introduction chamber, firstly cutting off the communication between the second cooling corrugated pipe (8) and the target chamber, then closing the first valve (4) and the second valve (5), and taking down the auxiliary device.
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| CN114660315B (en) * | 2022-05-24 | 2022-10-14 | 季华实验室 | Sample transfer device, batch sample introduction system, analysis equipment and batch sample introduction method |
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