CN117288548A - System and method for vaporizing a sample and a delivery needle assembly for use in the system - Google Patents

System and method for vaporizing a sample and a delivery needle assembly for use in the system Download PDF

Info

Publication number
CN117288548A
CN117288548A CN202210679191.3A CN202210679191A CN117288548A CN 117288548 A CN117288548 A CN 117288548A CN 202210679191 A CN202210679191 A CN 202210679191A CN 117288548 A CN117288548 A CN 117288548A
Authority
CN
China
Prior art keywords
channel
container
sample
gas
delivery needle
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202210679191.3A
Other languages
Chinese (zh)
Inventor
吴洪田
陆艮峰
陈晨
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Thermo Fisher Scientific Shanghai Instruments Co Ltd
Original Assignee
Thermo Fisher Scientific Shanghai Instruments Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Thermo Fisher Scientific Shanghai Instruments Co Ltd filed Critical Thermo Fisher Scientific Shanghai Instruments Co Ltd
Priority to CN202210679191.3A priority Critical patent/CN117288548A/en
Priority to PCT/CN2023/100369 priority patent/WO2023241645A1/en
Publication of CN117288548A publication Critical patent/CN117288548A/en
Pending legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/02Cleaning by the force of jets or sprays
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B5/00Cleaning by methods involving the use of air flow or gas flow
    • B08B5/02Cleaning by the force of jets, e.g. blowing-out cavities
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4022Concentrating samples by thermal techniques; Phase changes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4022Concentrating samples by thermal techniques; Phase changes
    • G01N2001/4027Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • G01N2001/4061Solvent extraction

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The present disclosure relates to systems and methods for vaporizing a sample and a delivery needle assembly for use in such systems. In the method and system disclosed at all, the delivery needle has a first channel and a second channel, the second channel being located outside said first channel, and the outer wall of the delivery needle forming the second channel having a plurality of holes through which the sample can enter the container, the second channel of the delivery needle being capable of providing a solvent and a gas such that the solvent located in the second channel is applied to the inner wall of the container through the holes, and further, during heating of the container to evaporate the sample in the container, the gas is provided to said container through said first channel. According to the system and the method, sample injection, acceleration in the evaporation process and residual sample collection of the container wall can be automatically performed, and the residual sample collection is performed on the inner wall of the container, so that sample defects in the sample preparation process are avoided, and the sample recovery rate obtained after final evaporation is improved.

Description

System and method for vaporizing a sample and a delivery needle assembly for use in the system
Technical Field
The present disclosure relates generally to the technical field of chemical analysis instruments, and more particularly to a system and method for vaporizing a sample, and also to a delivery needle assembly for use in the system and method.
Background
Evaporation equipment is often used in the food detection, environmental detection, pharmaceutical, biological, etc. industries to evaporate samples to obtain concentrated samples. There are currently on the market instruments capable of concentrating multiple samples simultaneously, and such evaporators can be used in combination with other instruments, such as solvent extraction systems. Solvent extraction systems extract analytes from solid or semi-solid materials using solvents at high temperature and pressure to obtain liquid samples, and then a plurality of test tubes or sample containers containing the liquid samples are placed into an evaporator to be heated, so that the samples are concentrated or dried. In the prior art, samples containing analytes extracted by solvent extraction systems need to be manually placed on a vaporizer for concentration, and thus, sample preparation process time is long and samples may be contaminated during operation.
US10124270B2 discloses a delivery needle for a blow evaporation and drying system, which comprises a solution introduction tube, a gas introduction tube and a cleaning liquid introduction tube sleeved together, wherein the solution introduction tube, the gas introduction tube and the cleaning liquid introduction tube are sequentially arranged from inside to outside. Which are used to deliver solutions, gases and cleaning solutions, respectively, into the container.
Although existing evaporation equipment has been improved on some of the problems existing in the use process, how to improve the recovery rate of analytes, the concentration efficiency of analytes, and the degree of automation between the evaporation equipment and the previous sample extraction device remain problems to be solved.
Disclosure of Invention
To overcome the deficiencies in the prior art, the present disclosure provides a method of vaporizing a sample in a container, the method comprising: providing a sample to be vaporized to the container through a delivery needle, wherein the delivery needle comprises a first channel and a second channel, the second channel is positioned outside the first channel, the outer wall of the delivery needle forming the second channel is provided with a plurality of holes, and the sample enters the container through the first channel; providing a solvent and a gas to the second channel such that the solvent located in the second channel is applied to the inner wall of the container through the aperture; and heating the container to evaporate the sample in the container, optionally providing a gas to the container through the first channel during the heating.
The method can realize multiple functions of sample introduction, residual sample collection on the inner wall of the container and accelerated sample evaporation. The collection of residual samples of the inner wall of the container can be achieved by providing solvents and gases applied to the inner wall of the container, which residues may be caused by sample splatter when the delivery needle provides the container with the sample to be evaporated. And the collection of the residual sample on the inner wall of the container avoids the sample loss in the preparation process, thereby improving the final sample recovery rate.
In the method of the present disclosure, preferably, the step of providing a solvent and a gas further comprises, in order: providing a solvent to the second channel; a gas is provided to the second channel before the solvent leaves the pores of the second channel, and the gas is combined with the solvent to form a gas-liquid mixture and passed out of the pores. The step of providing a solvent and a gas improves the collection efficiency of collecting the residual sample from the inner wall by providing a gas-liquid mixture for residual sample collection from the inner wall of the container.
In the method of the present disclosure, preferably, the step of providing a solvent and a gas further comprises: applying a compressed gas to the solvent, causing the gas-liquid mixture to pass out of the aperture to form droplets, at least a portion of the droplets being applied to the inner wall of the container. Under the action of the compressed gas, the gas and the solvent can form tiny liquid drops, the liquid drops can be uniformly attached to the inner wall of the container, the tiny liquid drops flow downwards along the inner wall of the container, and the residual sample on the inner wall of the container is brought back into the liquid sample in the container, so that the residual sample on the inner wall of the container can be collected as completely as possible, the defect of the sample in the preparation process is avoided, and the recovery rate of the sample obtained after final evaporation is improved.
In the method of the present disclosure, preferably, the step of providing the solvent and gas further comprises moving the delivery needle downward to a first position that is lower than the position of the delivery needle when the step of providing the solvent and gas is performed. The step of moving the delivery needle downwardly further comprises providing a gas to the container through the first passageway. The delivery needle is moved to a first position for subsequent execution of the step of delivering compressed gas to accelerate vaporization. It will be appreciated that the position of the delivery needle when the needle is providing solvent and gas is higher than the first position for blowing compressed gas, and therefore, the delivery needle has a higher position for collecting residual sample by applying fluid into the container, which helps to cover the inner wall of the container relatively fully, so that the first position for blowing the more complete delivery needle for collecting residual sample on the inner wall of the container is relatively lower, and thus the delivery needle is able to deliver gas to a position closer to the liquid sample to be evaporated in the container, which is advantageous to accelerate evaporation of the sample.
Preferably, the step of heating the container to evaporate the sample in the container is performed simultaneously with the step of supplying the sample to be evaporated to the container through the first channel, thereby enabling a saving of total sample preparation time.
In another aspect of the disclosure, the step of heating the container to evaporate the sample within the container further comprises: the second channel is closed when gas is supplied to the container through the first channel. Closing the second passage can prevent the back flow of gas in the container through the second passage.
The present disclosure also provides a system for vaporizing a sample, comprising: a sample providing device that provides the sample to a container; a gas supply device that supplies gas to the container; a solvent supply device that supplies a solvent to the container; a heating device configured to heat the sample in the container; and a delivery needle device including a delivery needle including a first channel and a second channel, the second channel being located outside of the first channel, an outer wall forming the second channel having a plurality of holes. The delivery needle device is configured to fluidly connect the first channel with the sample providing device, and the first channel is optionally fluidly connected with the gas providing device, and the delivery needle device is configured to fluidly connect the second channel with the solvent providing device or the gas providing device.
According to the system disclosed by the invention, multiple functions of sample introduction, residual sample collection on the inner wall of the container and sample evaporation can be realized, the conveying needle can be used for conveying samples and collecting the residual samples on the inner wall of the container, and the conveying needle can also be used for providing gas to realize the function of accelerating the evaporation of the gas. The system according to the present disclosure is highly automated and sample recovery is also significantly improved.
In the system of the present disclosure, the delivery needle device includes a movement mechanism that moves the delivery needle up and down relative to the container. Preferably, the movement mechanism is configured to move the delivery needle to a first position with the first channel in fluid communication with the gas supply, the first position being lower than the position of the delivery needle when the second channel is optionally in fluid communication with the solvent supply or the gas supply. It will be appreciated that the delivery needle is positioned higher when it is in fluid communication with the solvent or gas supply means, and therefore that solvent and/or gas applied to the container through the outer wall aperture of the second passage of the delivery needle will also have a higher position when it exits the delivery needle, thereby providing a more complete coverage of the inner wall of the container and a more complete collection of the residual sample from the inner wall of the container. When the conveying needle is positioned at the lower first position, the conveying needle can convey gas to a position which is closer to the liquid sample to be evaporated in the container, so that the evaporation of the sample is accelerated.
The system according to the present disclosure is due to the moving mechanism for delivering the needle. The design can enable the system to be suitable for containers of different specifications, and can also enable different functions of sample injection, collection of residual samples on the inner wall of the container, acceleration of evaporation through air blowing and the like to be achieved by allowing the conveying needle to be located at different heights, so that the whole system is high in adaptability, compact in structure and capable of saving limited operation space in a laboratory.
In the system of the present disclosure, preferably, the delivery needle device comprises a cap through which the first channel and the second channel pass sealingly, the cap being configured to sealingly mate to a container mouth of a container, and the delivery needle being movable relative to the cap.
In the system of the present disclosure, preferably, the system further comprises a negative pressure application device and/or an exhaust gas recovery device. The cover is provided with ports connected to said negative pressure applying means and/or said exhaust gas recovery means.
In the system of the present disclosure, preferably, the system includes a switching mechanism, the first channel is fluidly connected to the gas supply device via the sample supply device and the switching mechanism, the second channel is fluidly connected to the gas supply device and the solvent supply device via the switching mechanism, respectively, the switching mechanism has a first switching position, a second switching position, and a third switching position. In a first switching position, the first channel is in fluid connection with the gas supply via the sample supply; in a second switching position, the second channel bypasses the sample providing device and is directly in fluid connection with the gas providing device; in a third switching position, the second channel bypasses the sample providing device and is directly in fluid connection with the solvent providing device. Providing a switching mechanism in the system to enable fluid communication of the first and second channels of the delivery needle with the respective providing means simplifies the fluid supply line arrangement of the system.
In the system of the present disclosure, preferably, the system comprises a shut-off device for the second channel, the shut-off device being configured to close the second channel when the first channel is in fluid connection with the sample providing device. By means of the shut-off device, the second channel can be closed when gas is supplied to the first channel of the delivery needle, so that a backflow of gas in the container through the second channel is avoided.
In the system of the present disclosure, preferably, the gas supply means is arranged to supply gas to the container at a pressure of 350-500 Psi.
In the system of the present disclosure, preferably, the delivery needle further comprises a third channel interposed between the first channel and the second channel. The third channel is optionally in fluid connection with the solvent supply or the gas supply.
In addition, the present disclosure also provides a delivery needle assembly for an evaporation system, comprising: a first channel having a first end and a second end; a second channel having a third end and a fourth end, the second channel being located outside of the first channel; and a closure through which the first and second channels sealingly pass, the closure configured to sealingly mate to a container mouth of a container; wherein the first channel has an opening disposed at the first end; the third end of the second channel is closed, and the outer wall forming the second channel is provided with a plurality of holes.
The disclosed delivery needle assembly is compact in design and can be used to support the system to perform various operations, which may include sample/solvent introduction, gas delivery for accelerated evaporation, solvent application to the interior wall of the container, gas application, which support the automatic continuous delivery of fluid during evaporation.
The outer wall of the second channel of the delivery needle assembly according to the present disclosure is provided with holes, so that the container wall is spray cleaned before evaporation heating is performed or according to a setting, and sample residues on the inner wall of the container are collected, avoiding defects of the sample during the preparation process. The looped holes in the outer wall ensure that the sample remaining on the inner wall of the container is collected more adequately.
In the delivery needle assembly of the present disclosure, preferably, the second channel surrounds the first channel, the second channel being separated from the first channel by at least one inner wall, wherein the outer wall and the inner wall are fixed as one piece. The conveying needle has the first channel and the second channel surrounding the first channel, so that multiple functions of sample injection, collection of residual sample on the inner wall of the container, accelerated evaporation of conveying pressure gas and the like can be realized by only one conveying needle, the pipeline structure is simplified, and the system is convenient to manufacture and install. In the delivery needle assembly of the present disclosure, preferably, the plurality of holes are disposed proximate the third end of the second channel.
In the delivery needle assembly of the present disclosure, preferably, the hole includes a plurality of hole groups arranged in a circle on the outer wall around the second passage, the hole groups being spaced apart from each other by a predetermined distance in a longitudinal direction of the outer wall, and/or the holes are arranged in the outer wall perpendicularly to the longitudinal direction of the second passage or so that a radially outer side of the holes is arranged obliquely closer to the third end than a radially inner side of the holes. The arrangement modes of the holes are beneficial to efficiently collecting the residual sample on the inner wall of the container, avoiding the residual dead angle of the sample and reducing the defect of the sample in the preparation process as much as possible.
Preferably, the pore diameter is between 0.2 and 0.3 mm. The pore size facilitates droplet formation.
In the delivery needle assembly of the present disclosure, preferably, at the third end of the second channel, the outer wall is fixed to the inner wall by a weld, the weld closing the third end of the second channel. The weld enables a reliable connection and sealing of the two channels.
Drawings
For a more complete understanding of the present disclosure, reference is made to the following description of exemplary embodiments taken in conjunction with the accompanying drawings, in which:
fig. 1 shows a schematic block diagram of a system for evaporating a sample according to a preferred embodiment of the present disclosure.
Fig. 2 shows a schematic view of a delivery needle device cooperatively mounted to a container according to a preferred embodiment of the present disclosure.
Fig. 3A shows a perspective view of a delivery needle according to a preferred embodiment of the present disclosure.
Fig. 3B shows an enlarged perspective view of both ends of the delivery needle shown in fig. 3A.
Fig. 4 shows a cross-sectional view of a longitudinal section of a portion of a delivery needle according to a preferred embodiment of the present disclosure.
Figure 5 shows a cross-section taken in the direction A-A in figure 4.
Fig. 6 shows a cross-sectional view taken in the direction B-B in fig. 4.
Fig. 7A shows a schematic view of the delivery of a sample to be vaporized to a container by a delivery needle as shown in fig. 3A.
Fig. 7B shows a schematic view of the supply of gas to the container through the delivery needle as shown in fig. 3A while the sample is vaporized.
Fig. 7C shows a schematic diagram of residual sample collection for the inner wall of the container by transport as shown in fig. 3A.
Fig. 8A shows an enlarged perspective view of the end of a delivery needle according to a preferred embodiment.
Fig. 8B shows an enlarged perspective view of the end of a delivery needle according to another preferred embodiment.
Fig. 9 shows a flow chart of the steps of a method of evaporating a sample according to a preferred embodiment.
List of reference numerals
System for evaporating a sample
10. Solvent supply device
20. Gas supply device
30. Sample providing device
31. Control valve
40. Switching mechanism
50. Negative pressure applying device
60. Needle delivery device
61. Movable retainer
62 O-shaped ring
63. Gasket for a vehicle
64. Fixed retainer
65. 66 retainer channel
67 O-shaped ring
70. Delivery needle
71. A first channel
72. Second channel
75. First pipe fitting
76. Second pipe fitting
77. Hole(s)
78. Retainer
80. Sealing cover
90. Container
91. Container mouth
110. Solvent supply pipeline
120. Gas supply pipeline
150. Bypass pipeline
Detailed Description
Further details are set forth in the following description and drawings in order to provide a thorough understanding of the present disclosure, it will be apparent that the present disclosure can be embodied in many other forms than described herein, and that those skilled in the art may make a similar generalization or deduction from the actual practice without departing from the spirit of the present disclosure, and therefore should not be taken to limit the scope of the present disclosure in its context.
Fig. 1 shows a schematic block diagram of a system for evaporating a sample according to a preferred embodiment of the present disclosure. The sample to be evaporated is placed in the system by means of a container, and the system is used for heating the container, so that the temperature of the liquid sample in the container is raised, and the vaporizable component in the sample can escape, thereby achieving the purpose of concentrating or drying the sample. At the same time, the system is also capable of applying a pressurized gas to the vaporized sample to accelerate the concentration or drying process.
Those skilled in the art understand that in many cases the chemical of interest (i.e., the analyte) to be analyzed must be extracted from the substance so that it can be detected by a corresponding detection technique, e.g., qualitative or quantitative analysis. For example, such extraction may be performed by solid-liquid extraction, with the analyte being dissolved from a solid or semi-solid substance. The solid or semi-solid substance may be any material or matrix containing the analyte, such as a pharmaceutical, soil, or food product, etc. The subsequent separation of "analytes" from solid or semi-solid materials in the present invention may be used in analytical techniques to detect (e.g., qualitatively or quantitatively) chemicals, such as active ingredients in pharmaceuticals, pesticides in soil, or lipids in food. The term "sample" as used herein refers to a liquid solvent containing an analyte that can be fed to an evaporation device for concentration. Taking the example of a sample from solid-liquid extraction, it should contain analytes dissolved from solid or semi-solid materials.
As shown in fig. 1, the system for vaporizing a sample mainly includes a sample providing device 30, a gas providing device 20, a solvent providing device 10, a switching mechanism 40, and a transporting needle device 60. Each of the providing devices 10, 20, 30 is connected in fluid communication to a delivery needle device 60, through which the liquid sample, gas and solvent are delivered into a container 90 placed in the system.
Fig. 1 shows schematically four containers 90, each configured with one delivery needle device 60.
The sample providing device 30 in the system is configured to provide a sample to be vaporized to a container 90 disposed within the system. It should be appreciated that the sample providing device 30 in the system may comprise any type of device capable of providing a sample to a container. Typically, the sample providing device 30 includes a reservoir containing the sample to be vaporized and a transport mechanism. The sample provided in the sample providing device 30 may be prepared directly in the device 30 and provided to the container 90 by the device 30, or may be prepared by other independent sample preparation devices and provided to the container 90 by the sample providing device.
In a preferred embodiment, the sample providing device 30 may be configured as a solvent extraction accelerating device that primarily includes one or more heated extraction units. In the sample providing device 30, a solid or semi-solid substance containing an analyte is placed in a heated extraction cell, and a solvent from the solvent providing device 10 is fed into the heated extraction cell, and as the temperature and pressure of the cell increase, the analyte precipitates into the solvent, thereby extracting to obtain a liquid sample for subsequent evaporation.
The sample providing device 30 shown in fig. 1 comprises four heated extraction units, each connected to one delivery needle device 60 by means of a control valve 31. It should be appreciated that the number of heated extraction units may be greater or lesser and the number of heated extraction units may be provided to correspond to the number of delivery needle devices 60.
The gas supply 20 in the system is configured to supply gas to the sample supply 30 to accelerate extraction of the sample supply 30. The gas supply device 20 is also capable of directly supplying gas to the container 90 through the delivery needle device 60 without passing through the sample supply device 30. Along the gas delivery path, the sample providing device 30 is disposed between the gas providing device 20 and the container 90, and gas may be delivered to the container 90 through the gas providing device 20 via the sample providing device 30.
The gas provided by the gas providing device 20 is typically an inert gas, such as nitrogen. During the sample evaporation process, the gas supply device 20 can blow nitrogen into the container 90, that is, realize the nitrogen blowing function, so that the sample evaporation speed is increased, and the evaporation time is reduced. On the other hand, during collection of residual samples on the inner wall of the container, the gas supply device 20 supplies gas that can be used to accelerate and disperse the liquid, forming a spray fluid or mist of liquid, to be applied to the inner wall of the container 90 to effect collection of residual samples on the inner wall. The gas supply 20 is preferably configured to supply a gas in the pressure range of 350 to 500Psi, which would be suitable for the accelerated evaporation and container residual sample collection process of the system.
In addition, the solvent supply apparatus 10 included in the system is configured to supply solvent to a container 90 disposed within the system, and also to supply solvent to the sample supply apparatus 30 for solvent extraction operations on various types of analytes.
The switching mechanism 40 in the system is configured to effect flow path selection in different modes, such that solvent and gas are delivered to corresponding channels of the delivery needle (as will be described in more detail below) as required by the operational steps performed by the system.
As shown in fig. 1, the solvent supply apparatus 10 includes a solvent supply line 110, and the gas supply apparatus 20 includes a gas supply line 120, the solvent supply line 110 and the gas supply line 120 being respectively in fluid communication with the switching mechanism 40. Preferably, the switching mechanism 40 comprises an electronic rotary valve (ERV valve). Preferably, the electronic rotary valve includes at least one inlet port, at least two outlet ports, and a rotary switching valve selectively communicating the inlet port with one of the outlet ports. The inlet port is in operative communication with the gas supply means 20 and the solvent supply means 10, while one outlet port is connected to the sample supply means 30 and thus to a first channel of a delivery needle in the delivery needle means and the other outlet port is connected to a second channel of a delivery needle in the delivery needle means. By controlling the rotary switching valve, the inlet port can be selectively communicated with the selected outlet port, thereby realizing the flow path selection under different modes.
For the four sample providing device 30 and four delivery needle device 60 system shown in FIG. 1, the electronic rotary valve may have one inlet port and eight outlet ports, with four outlet ports each connected to one sample providing device 30 for selectively delivering gas or solvent to a first channel of a corresponding delivery needle 70 and the other four outlet ports each connected to a second channel of a corresponding delivery needle 70 for selectively delivering gas or solvent to the delivery needle device.
Providing the switching mechanism 40 in the present system simplifies the solvent and gas delivery line arrangement. It should be appreciated that in other alternative embodiments, switching mechanism 40 may include a one-way valve and a control valve, solvent supply 10 and gas supply 20 being controlled to deliver solvent and gas to sample supply 30 and container 90, respectively, via a one-way valve and a control valve on separate, respectively, connected lines.
The sample providing device 30 is disposed downstream of the switching mechanism 40, and the delivery needle device 60 and the container 90 are further disposed downstream of the sample providing device 30, so that the solvent from the solvent providing device 10 and the gas from the gas providing device 20 can be delivered to the sample providing device 30 through the switching mechanism 40. When it is desired to deliver gas into the container 90 in operation, gas from the gas supply device 20 can flow through the sample supply device 30 and the delivery needle device 60 into the container 90 via the switching mechanism 40.
It will be appreciated by those skilled in the art that in certain steps, depending on the requirements, gas from the gas supply device 20 may also enter the sample supply device 30 directly without passing through the switching mechanism 40 and flow through the delivery needle device 60 into the container 90.
On the other hand, as shown in FIG. 1, a bypass line 150 is connected between the switching mechanism 40 and the needle unit 60, and the bypass line 150 does not pass through the sample providing device 30. Under control of the switching mechanism 40, solvent from the solvent supply apparatus 10 will bypass the sample supply apparatus 30 and be delivered directly to the delivery needle apparatus 60 via the bypass line 150 into the container 90.
The delivery needle device 60 in the system is configured for use with a plurality of gauges of containers 90, the device 60 being capable of holding and moving a delivery needle for delivering a gas, liquid or gas-liquid mixture to the container.
The container 90 may be configured to have a variety of different capacities, such as 60ml, 100ml, 250ml, etc. The container 90 may be configured to have a variety of different shapes, such as a flat bottom bottle shape with a container mouth 91 only at the top as shown in fig. 2, a shape with two small middle ends and two openings up and down as shown in fig. 7B, with the opening at the lower end adapted to mate with a vial (e.g., a 2ml capacity vial) to receive a small volume of evaporated sample. Alternatively, the container and vial may be coupled by an adapter.
Fig. 2 shows a preferred embodiment of a delivery needle device 60 and a container 90 for use with the delivery needle device 60. The delivery needle device 60 mainly includes a delivery needle 70, a moving holder 61, a moving mechanism for moving the delivery needle 70 up and down, a fixed holder 64, and a cover 80. As shown in fig. 2, the moving holder 61 is fixed
The upper part of the transfer needle 70 is fixedly held, and the fixed holder 64 slidably holds the middle lower part of the transfer needle 70, both of the holders 61 and 64 functioning to hold the transfer needle 70. Wherein the moving holder 61 is a movable member and the fixed holder 64 is a stationary member, and the delivery needle 70 is moved up and down by the relative movement of the two members.
The movement holder 61 and the driver of the delivery needle device 60 are used as a movement mechanism of the delivery needle 70, wherein the movement holder 61 is configured to hold the delivery needle 70. The actuator is then attached to the movable holder 61 to move the movable holder 61 up and down relative to the underlying fixed holder 64, thereby allowing the delivery needle 70 to move up and down relative to the container through the fixed holder 64 and the closure 80. In a preferred embodiment, the drive is preferably an electric motor.
It should be appreciated that in other alternative embodiments, the delivery needle device 60 may also move the delivery needle in other ways, such as by a driver directly attached to the delivery needle.
The setting of moving mechanism can make the system can adapt to the container of different specifications and use, also can make through allowing the delivery needle to be located different co-altitude and realize different functions such as injecting sample, collection of container inner wall residual sample and evaporation through the air blast acceleration to make the whole suitability of system strong, and compact structure saves limited operating space in the laboratory.
Preferably, one or more seals, such as O-rings 67, are provided between the fixed retainer 64 and the delivery needle 70 to provide a sliding seal.
In a preferred embodiment, the movement mechanism may be configured such that the delivery needle 70 is movable to some or all of the following positions relative to the same size container: a home position where no operation is performed, a position where the delivery needle 70 supplies a sample to the container, a position where the delivery needle 70 applies a gas-liquid mixture to the container, and a position where the delivery needle 70 delivers a gas when the container is heated (hereinafter referred to as a first position). Typically, the first position is below the position where the delivery needle 70 begins to apply gas and solvent to the container. The position of the delivery needle when providing solvent and gas is thus higher than the first position at which the gas is blown, and therefore, the delivery needle has a higher position when applying fluid into the container for residual sample collection, which helps to cover the inner wall of the container relatively comprehensively, so that the first position at which the more complete delivery needle is blown for residual sample collection from the inner wall of the container is relatively lower, and thus, the delivery needle can deliver gas to a position closer to the liquid sample to be evaporated in the container, which is beneficial to accelerating evaporation of the sample. In addition, the position of the delivery needle 70 at which the gas-liquid mixture is applied to the container is preferably set higher than the position at which the delivery needle 70 supplies the sample to the container. Such positioning helps to allow the delivery needle 70 to apply the gas-liquid mixture to more fully cover the sample that remains splattered to the interior walls of the container when the delivery needle is providing the sample.
When the container 90 is placed within the system, the delivery needle device 60 may be attached to the container mouth 91 of the container 90 by at least a portion of the cap 80, with the lower projection of the cap 80 insertedly attached into the container mouth 91 as shown in fig. 2, one end of the delivery needle 70 extending through the container mouth 91 of the container 90 and being inserted into the interior of the container 90 through a through hole in the cap 80, and a plurality of seals such as O-rings 62 being provided between the cap 80 and the delivery needle 70 to effect a seal, the delivery needle 70 being movable relative to the cap 80. The closure 8 should form a sealing engagement with respect to the container mouth 91 to prevent fluid escape. To achieve a sealing fit, in a preferred embodiment, a gasket 63, such as made of an elastomeric material, may be added between the lid 80 and the container mouth 91, the lid 80 pressing the gasket 63 against the container mouth 91, which will help to achieve a sealing fit between the lid 80 and the container mouth 91.
In order to perform sample introduction, collection of residual sample on the inner wall of the container, and evaporation blowing in the system, the transfer needle 70 includes at least a first channel 71 and a second channel 72, the second channel 72 being located outside the first channel 71, and the two channels 71 and 72 being spaced apart from each other, so that fluids can be transferred independently.
Fig. 4 shows in particular a double-layered delivery needle 70. The delivery needle 70 includes a first tube 75 and a second tube 76, the second tube 76 surrounding the first tube 75, the two tubes 75 and 76 preferably being disposed substantially concentrically. Thus, in the preferred embodiment, the first passage 71 is formed by the hollow space of the inner first tube 75 and the second passage 72 is formed by the tubular space between the second tube 76 and the first tube 75. Thus, the second channel 72 surrounds the first channel 71, and the two channels 71, 72 are separated by at least one wall.
Along the longitudinal direction of the delivery needle 70, the first channel 71 has a first end that can extend into the container 90 and a second end that is in communication with the sample providing device 30, and the second channel 72 has a third end that can extend into the container 90 and a fourth end that is switchably in communication with the solvent providing device 10 of the gas providing device 20. The first channel 71 has an opening provided at a first end, in other words, the first end of the first tube 75 is open.
In a preferred embodiment, the end face of the open end of the first tube 75 may be provided as an inclined face, as shown in fig. 8A. In another alternative preferred embodiment, the end of the first tube 75 may be notched in the longitudinal direction of the tube, as shown in FIG. 8B.
In particular, the third end of the second channel 72 of the delivery needle 70 is closed, in other words the second tube 76 has a closed end at the third end.
In the preferred embodiment, as shown in fig. 4, the first tube member 75 and the second tube member 76 are joined by welding assembly to form an integrated delivery needle. Preferably, the end of the second tube 76 corresponding to the third end of the second channel 72 is fixed to the outer surface of the first tube 75 by a weld, which closes the third end of the second channel 72.
At the other end of the delivery needle 70, as shown in fig. 3B, the delivery needle 70 may also include a retainer 78. The holder 78 is fixedly attached to the first tube 75 and the second tube 76, respectively, such that the relative position between the two tubes is maintained. Preferably, the retainer 78 includes a ring fixedly attached to the end of the second tube 76 and a plurality of connecting ribs extending from the inside of the ring fixedly attached to the outer surface of the first tube 75. The holder 78 is preferably also secured by welding to the first tube 75 and the second tube 76.
In the outer wall of the second tube 76 forming the second passage 72, a plurality of holes 77 are provided at a position near the third end of the second passage 72, and these holes 77 allow the second passage 72 to communicate with the outside to allow the solvent or gas to enter and exit through these holes 77. The purpose of these holes 77 in the outer wall of the second channel 72 is to allow fluid to be ejected for residual sample collection on the inner wall of the container 90, avoiding sample defects during preparation. Typically, the fluid is a gas-liquid mixture formed by combining compressed gas and solvent, a part of the gas-liquid mixture is directly sprayed to the inner wall of the container under the action of gas pressure, and then the liquid flows down along the inner wall to carry away residues possibly existing on the inner wall; the other part of solvent can be atomized under the action of high-pressure gas, micro liquid drops are formed in the inner space of the container, the micro liquid drops can adhere to the inner wall and flow down along the inner wall, and the part of the inner wall surface which is not covered by spraying application can be supplemented by the solvent of the atomized part, so that the residual sample on the inner wall of the container is more fully collected. The pressure of the compressed gas can be controlled generally in the range of 350-500Psi, which is advantageous for adequate removal of residues on the inner wall of the container.
A plurality of holes 77 are arranged in a circle around the second channel 72 forming a plurality of circle hole sets in the outer wall. The plurality of sets of holes are spaced apart a predetermined distance in the longitudinal direction of the outer wall of the second passage 72. In the embodiment shown in fig. 4, preferably, a plurality of holes 77 are arranged to form two ring sets of holes. Each ring of hole sets has 12 holes, and the plurality of holes 77 in each ring of hole sets are equally spaced from each other in the circumferential direction of the outer wall.
In the embodiment shown in fig. 4, the direction of extension of the bore 77 in the tube wall is at 90 degrees with respect to the longitudinal axis of the delivery needle 70. It should be understood that it is also contemplated to arrange these holes 77 in the direction of extension of the walls of the tube member, relative to the longitudinal axis of the delivery needle 70 (i.e., the longitudinal direction of the delivery needle), toward the lower end of the delivery needle 7 as shown in fig. 2, such that the radially outer side of the holes 77 is closer to the third, lower end than the radially inner side of the holes 77, such that the fluid ejected will have a component toward the bottom of the container 90, which component, when applied to the inner wall of the container 90, will accelerate the fluid downward along the inner wall of the container 90, enhancing the residual sample collection effect.
It can be seen from fig. 5 and 6 that the positions of the holes 77 in the two ring hole sets are not necessarily aligned along the longitudinal direction of the conveying needle, as shown in fig. 6, an angle α, for example, 15 degrees, is offset in the circumferential direction between the radial center lines of one hole 77 in the ring hole set close to the third end and the closest hole 77 in the ring hole set far away from the third end, so that when the liquid is sprayed through the holes 77 to collect the residual sample on the inner wall of the container, the collection coverage of the residual sample on the inner wall can be more complete, and dead angles of the residual sample are avoided.
It should be appreciated that the number of apertures 77 of the delivery needle 70 may be greater or lesser, preferably between 8 and 16 apertures per ring of aperture sets. Preferably, the aperture d1 of the hole 77 in the second channel 72 of the delivery needle 70 may be set between 0.2 and 0.3mm, preferably 0.25mm. The apertures 77 of this range of apertures facilitate the formation of atomized droplets upon conformal ejection, thereby enabling the application of solvent to the interior walls of the container in both jet and atomized droplets, thereby allowing for more complete coverage of the interior walls. The aperture d2 of the opening of the third end of the delivery needle may be set between 0.8 and 1.2mm, preferably 1mm. The distance between the outer wall surface of the first tube member 75 and the inner wall surface of the second tube member 76 may be between 0.3-0.5 mm.
In a preferred embodiment according to the present disclosure, the delivery needle 70 of the delivery needle device 60 includes a first channel 71 and a second channel 72 located outside the first channel 71. As shown in fig. 2, at least two holder passages 65, 66 are provided in the moving holder 61. One end of one of the holder passages 65 communicates with the first passage 71 of the delivery needle 70, and the other end of the holder passage 65 communicates with the sample providing device 30 and with the gas providing device 20 and the solvent providing device 10 via the sample providing device 30 and the switching mechanism 40. One end of the other holder passage 66 communicates with a second passage 72 of the delivery needle 70, and the other end of the passage 66 is connected by tubing to an outlet end of the switching mechanism 40 to operatively communicate the gas supply 20 and the solvent supply 10, respectively. Thus, by delivering the needle device 60, the first channel 71 may be fluidly connected to the sample providing device 30, and the first channel 71 may optionally be fluidly connected to the gas providing device 20, and the second channel 72 may optionally be fluidly connected to the solvent providing device 10 or the gas providing device 20.
To control the flow of sample and solution through the first channel 71 and the second channel 72, in a preferred embodiment, the switching mechanism 40 is configured to have at least a first switching position, a second switching position, and a third switching position. In the first switching position, the first channel 71 is in fluid connection with the gas supply device 20 via the sample supply device 30; in the second switching position, second channel 72 bypasses sample providing device 30 and is directly fluidly connected to gas providing device 20 via bypass line 150; in the third switching position, the second channel 72 is directly in fluid communication with the solvent supply via the bypass line 150 bypassing the sample supply 30.
In addition, the system may further comprise a shut-off device for the second channel 72, which is configured to close the second channel 72 when the first channel 71 is in fluid connection with the sample providing device 30, to avoid a backflow of the gas flow in the container out of the system through the second channel 72. For example, the shut-off device may be a shut-off valve mounted in the holder passage 66 in communication with the second passage 72.
Specifically, as shown in fig. 1, the sample providing device 30 is disposed upstream of the conveying needle device 60 with a conveying line provided therebetween, and therefore, the obtained sample in the sample providing device 30 can flow into the first passage 71 via the holder passage 65 in the conveying needle device. Alternatively, the gas in the gas supply device 20 flows into the first channel 71 through the gas supply line 120, the switching mechanism 40, the sample supply device 30, and the holder channel 65. It will be appreciated by those skilled in the art that in certain steps, depending on the requirements, gas from the gas supply device 20 may also enter the sample supply device 30 directly without passing through the switching mechanism 40 and flow through the holder channel 65 into the first channel 71. On the other hand, the gas from the gas supply device 20 or the solvent from the solvent supply device 10 flows through the bypass line 150 through the switching mechanism 40, is fed into the second passage 72 of the delivery needle through the holder passage 66 in the delivery needle device 60, to perform the corresponding operational steps.
As further shown in fig. 1, the system for sample evaporation further comprises a negative pressure application device 50. The negative pressure applying device 50 communicates with the container 90 to provide a negative pressure, e.g., a vacuum, to the container 90. Preferably, a negative pressure port through which the negative pressure applying device 50 can be connected may be provided on the cover 80 attached to the container 90.
In addition, preferably, during evaporation, gas escaping from the container 90 may also be vented through the negative pressure port. The system may also include an exhaust gas recovery device to which the negative pressure port on the cover 80 may be connected to allow the exhaust gas to be recovered, avoiding environmental pollution and injury to the human body from escaping gases. It will be appreciated by those skilled in the art that a separate exhaust port may also be provided on the closure 80 of the container 90 for venting of the escaping gas.
Next, specific steps performed on the sample in the container according to the preferred embodiment will be described with reference to fig. 7A, 7B and 7C, and 9. FIG. 9 is a flow chart showing the steps of a method for vaporizing a sample in accordance with a preferred embodiment of the present disclosure
Specifically, the preferred method flow shown in FIG. 9 includes: a step S100 of moving the transporting needle to a position where the sample is supplied to the container, a step S102 of supplying the sample to be vaporized to the container through the transporting needle, a step S104 of moving the transporting needle to a position where the solvent and the gas are applied to the inner wall of the container, a step S106 of applying the solvent and the gas to the inner wall of the container, a step S108 of moving the transporting needle to a first position where the gas is applied, a step S110 of vaporizing the sample in the container, and a step S112 of supplying the gas from the gas supply device to the container through the transporting needle. As shown after step S112 in fig. 9, the sample is in a prepared completed state at S114. The step S110 of evaporating the sample in the container refers to a step of evaporating the sample by performing at least one means, for example, heating. It should be understood that the flow shown in fig. 9 is merely exemplary, and that not every step in the flow is necessary, nor is it necessary to perform the steps in the order that they are shown in fig. 9. The step S102 of supplying the sample to be evaporated to the container through the delivery needle and the step S110 of evaporating the sample in the container may be simultaneously started to be performed. However, in alternative embodiments, step S110 may also be performed after step S102 is completed, or after step S102 is completed. For example, the delivery needle may not be moved but directly perform step S102 of supplying the sample to be vaporized to the container through the delivery needle. For another example, the step S112 of supplying the gas from the gas supply device to the container through the delivery needle may be omitted, and the sample evaporation concentration may be achieved by performing only the step S110 of evaporating the sample in the container.
In performing step S102 of supplying the sample to be evaporated to the container 901 through the transporting needle 70, as shown in fig. 7A, the system supplies the sample to be evaporated from the sample supplying device 30 to the container 901 through the first passage 71 where the transporting needle 70 is located inside. The sample entering the container 901 may be obtained on-the-fly by solvent extraction of the analyte. When the sample is transported, a part of the gas supplied from the gas supply device 20 to the sample supply device 30 is also supplied to the container 901 together with the sample. As fluid is fed from the first passageway 71 into the vessel, excess gas in the vessel 901 escapes through the waste port of the cover 80, preferably to be collected in a waste recovery device, and the pressure within the vessel 901 is relieved.
Before performing step S102 of supplying the sample to be evaporated to the container through the transfer needle 70, step S100 of moving the transfer needle 70 to a position of supplying the sample to the container is optionally performed according to the need of using the container. In this step S100, the moving mechanism of the delivery needle device 60 moves the delivery needle 70 from the home position to a specific position where the supply of the sample to the container is performed. The home position of the delivery needle 70 is typically a position where the lower end of the delivery needle 70 is adjacent to the cover 80. The position where the delivery needle performs supplying the sample to the container is lower than the original position of the delivery needle 70 as shown in fig. 7A, and thus the delivery needle 70 moves vertically downward. The location at which the needle provides the sample is preferably located at a suitable location under the necked shoulder of the container. Fig. 7A and 7B show two different sizes of containers 901 and 902, and for performing the step of delivering the sample to be vaporized to the containers by the delivering needle, it is understood that the distance of downward movement of the delivering needle 70 from the home position is different, and the specific distance of movement can be set according to the different heights of the containers 901 and 902.
Fig. 7C schematically shows a step S106 of applying a solvent and a gas to the inner wall of the container. The fluid is applied to the inner wall in order to collect as much sample as possible that remains on the inner wall of the container 901, avoiding final sample analysis errors due to sample residues on the inner wall. Such sample residues may be splashed onto the inner wall when the sample is fed into the container 901 or may adhere to the inner wall of the container 901 during the lowering of the sample level.
According to a preferred embodiment of the present disclosure, the step of applying fluid to the interior wall of container 901 is performed through second passageway 72 of delivery needle 70. In step S106 of applying the solvent and the gas, the solvent is first supplied from the solvent supply apparatus 10 to the second passage 72 of the delivery needle 70 through the bypass line 150. At this point, the solvent does not completely leave the second channel 72 from the holes in the outer wall of the second channel 72, but is at least partially trapped in the second channel 72 or in a line connecting the second channel 72. The gas supply means 20 then supplies compressed gas to the second channel 72 via the bypass line 150, the compressed gas acting on the solvent trapped in the line, causing the gas to combine with the solvent to form a gas-liquid mixture and pass out of the aperture 77 of the second channel 72 and onto the inner wall of the container 901.
In the step S106, the solvent is sprayed from the hole 77 of the second channel 72, and as the high-pressure gas is used, a part of the solvent is directly sprayed onto the inner wall of the container 901 under the action of the gas pressure, and the liquid flows down along the inner wall to take away the residues possibly existing on the inner wall; another portion of the solvent will atomize under the pressure of the gas, forming droplets within the vessel 901, which adhere to and flow down the inner wall. It is thus understood that with this step S106, only a small amount of solvent needs to be provided to the second channel 72 to enable effective collection of residual samples from the inner walls of the container. In this step S106, the pressure of the compressed gas may be controlled in the range of 350-500Psi, which is advantageous for sufficiently removing residues on the inner wall of the container.
It should be appreciated that in the operation S106 of applying the solvent and the gas to the inner wall of the container, the solvent is sent out toward the second passage 72 of the delivery needle 70 through the bypass line 150 between the switching mechanism 40 and the delivery needle device 60, and this portion of the solvent does not pass through the sample providing device 30. The solvent fed into the container 901 in this step is not required to be supplied by the sample supply device 30, and the flow distance through which the solvent passes before being applied to the inner wall of the container is shortened by such a design, so that the influence of the resistance in the flow path is reduced, so that the force exerted by the solvent when the solvent and the gas are applied to the inner wall of the container is more precisely controlled, and the effect of cleaning the inner wall is better. Furthermore, the shortening of the flow distance also allows the amount of solvent fed into the container 901 in this step to be relatively accurately metered.
In an alternative embodiment, the step S106 of applying the solvent and the gas to the inner wall of the container may be repeatedly performed a plurality of times, that is, the solvent supply device 10 supplies a small amount of the solvent to the second passage 72, then the gas supply device 20 supplies the compressed gas through the bypass line 150 to perform the primary injection to the inner wall surface of the container, and then, immediately or at intervals, the operations of the solvent supply device 10 supplying a small amount of the solvent to the second passage 72 and supplying the compressed gas to the gas supply device 20 are performed again to perform the secondary injection. The number of sprays can be determined according to the specifications of the container and the kind of sample.
Preferably, before performing the operation step S106 of applying the solvent and the gas to the inner wall of the container 901, the transfer needle is optionally moved to a position of applying the solvent and the gas to the inner wall of the container S104. In this step S104, the movement mechanism in the delivery needle device 60 moves the delivery needle 70 to a position where the solvent and gas are applied to the inner wall of the container, for example, as shown in fig. 7C, the position where the delivery needle 70 applies the solvent and gas to the inner wall of the container being preferably disposed under or near the necked shoulder of the container.
Preferably, for containers of the same gauge, the position of the delivery needle 70 shown in FIG. 7C where the solvent and gas are applied to the interior wall is slightly higher than the position of the delivery needle shown in FIG. 7A where the sample is provided. Likewise, the location of the delivery needle 70 for applying the solvent and gas to the interior wall may be programmed according to the specifications of the container selected.
In other alternative embodiments, the location where the delivery needle applies the solvent and gas to the inner wall of the container and the location where the sample to be vaporized is provided to the container by the delivery needle may be the same location for containers of the same specification, in which case step S104 may be omitted.
Preferably, as shown in fig. 9, the step S110 of vaporizing the sample in the container may be performed while the step S102 of supplying the sample to be vaporized to the container 901 is started, so that the total length of time for sample preparation may be reduced. In this case, step S106 of applying a solvent and a gas to the inner wall of the container is also performed while step S110 of evaporating the sample in the container is performed.
In an alternative embodiment, step S102 of vaporizing the sample in the container 901 may be provided and step S110 of vaporizing the sample in the container may be performed after step S106 of applying the solvent and the gas to the inner wall of the container is completed.
In other alternative embodiments, the two steps S102 and S106 described above may be omitted, and step S110 may be performed directly after, for example, the operator manually places the container with the sample to be evaporated into the system.
In order to accelerate the evaporation, step S112 of supplying the gas from the gas supply device to the container through the delivery needle is optionally performed. In this step S112, the gas from the gas supply device 20 is supplied to the container 901 through the first passage 71 of the delivery needle 70. The gas is preferably nitrogen, which is supplied at a pressure, typically in the range of 350-500 Psi.
In a preferred embodiment, the step S112 of supplying the gas from the gas supply means to the container through the delivery needle may be started after the step S102 of supplying the sample to be evaporated to the container 901 and the step S106 of applying the solvent and the gas to the inner wall of the container are completed, and at this time, the step S110 of evaporating the sample in the container is performed. Alternatively, in an alternative embodiment, step S112 may begin simultaneously with step S110 of vaporizing the sample within the container. Step S112 is preferably continuously performed until the sample evaporation is completed, but it is also possible to set an execution time to end step S112 before the sample evaporation is completed.
In order to concentrate the gas on the liquid sample of the container in step S112 of supplying the gas from the gas supply means to the container through the transporting needle, it is preferable that step S108 of moving the transporting needle to the first position of applying the gas may be performed before performing step S112 of supplying the gas from the gas supply means to the container through the transporting needle. In step S108, the moving mechanism may move the transfer needle 70 to a first position set for a container of a specific specification to apply gas through the first passage, which is lower than a position where the transfer needle applies solvent and gas and a position where a sample to be evaporated is supplied to the container. Typically, this step is performed when the container with the vial attached at its lower end is in use, with both ends open as shown in fig. 7B, and with the delivery needle 70 in the first position, the lower end of the delivery needle 70 is adjacent to the opening below the container. The first channel 71 of the delivery needle 70 is capable of applying nitrogen to the sample in the container, thereby achieving oxygen-free concentration of the sample, so that purity of the sample can be ensured and evaporation can be accelerated.
Finally, when the concentration of the sample in the container reaches the set requirement, the system stops heating the container, and after the interior of the system is fully cooled and the temperature is reduced to a safe value, the prepared sample can be taken out from the system, so that the target sample is obtained.
For the conventional sample feeding and sample evaporating operation, the system can automatically perform the step S102 of providing the sample to be evaporated to the container by the conveying needle, the step S106 of applying the solvent and the gas to the inner wall of the container and the step S110 of evaporating the sample in the container for multiple samples by setting corresponding time, temperature and other corresponding parameters.
It will be appreciated that the control means or control method of the system may also be arranged to be able to optionally perform any of the steps of providing the sample to be evaporated to the container by its delivery needle S102, applying the solvent and gas to the inner wall of the container S106 and heating the container to evaporate the sample in the container S110 to meet the specific requirements of sample preparation in some cases.
In other alternative embodiments, the delivery needle 70 may also include one or more third channels between the first channel 71 and the second channel 72. For example, the third channel is placed in fluid communication with one or more of the solvent providing device 10, the gas providing device 20, and the sample providing device 30 to perform additional operations.
Alternatively, the third passage may be in communication with an exhaust gas recovery device or a negative pressure application device, and application of negative pressure or recovery of exhaust gas may be performed through the third passage.
While the present disclosure has been described in terms of preferred embodiments, it is not intended to limit the disclosure, and variations and modifications may be made by those skilled in the art without departing from the spirit and scope of the disclosure. Therefore, any modification, equivalent variation and modification of the above embodiments according to the technical substance of the present disclosure fall within the protection scope defined by the claims of the present disclosure.

Claims (21)

1. A method for evaporating a sample in a container,
the method comprises the following steps:
-providing the container with a sample to be evaporated by means of a delivery needle comprising a first channel and a second channel, the second channel being located outside the first channel, and the outer wall of the delivery needle forming the second channel having a plurality of holes, the sample entering the container through the first channel;
-providing a solvent and a gas to the second channel such that the solvent located in the second channel is applied to the inner wall of the container through the aperture; and
-heating the container, causing the sample within the container to evaporate, optionally providing a gas to the container through the first channel during the heating.
2. The method of claim 1, wherein the step of providing a solvent and a gas further comprises, in order:
-providing a solvent to the second channel;
-providing a gas to the second channel before the solvent leaves the pores of the second channel, combining the gas with the solvent to form a gas-liquid mixture and passing out of the pores.
3. The method of claim 2, wherein the step of providing a solvent and a gas further comprises:
-applying compressed gas to the solvent, causing the gas-liquid mixture to pass out of the aperture forming droplets, at least a portion of the droplets being applied to the inner wall of the container.
4. The method of claim 1, wherein the step of providing a solvent and a gas further comprises, after:
-moving the delivery needle downwards to a first position lower than the position where the delivery needle is in when performing the step of providing solvent and gas;
and the step of moving the delivery needle downward further comprises:
-providing a gas to the container through the first channel.
5. The method of claim 4, wherein the step of heating the container to evaporate the sample in the container is performed simultaneously with the step of providing the container with the sample to be evaporated through the first channel.
6. The method of claim 1, wherein the step of heating the container to evaporate the sample in the container further comprises:
-closing the second channel when gas is supplied to the container through the first channel.
7. A system for vaporizing a sample, comprising:
a sample providing device that provides the sample to a container;
a gas supply device that supplies gas to the container;
a solvent supply device that supplies a solvent to the container;
a heating device configured to heat the sample in the container; and
a delivery needle device comprising a delivery needle comprising a first channel and a second channel, the second channel being located outside the first channel, the outer wall forming the second channel having a plurality of holes,
Wherein the delivery needle device is configured to fluidly connect the first channel with the sample providing device, and the first channel is optionally fluidly connected with the gas providing device, and the delivery needle device is configured to fluidly connect the second channel with the solvent providing device or the gas providing device.
8. The system of claim 7, wherein the delivery needle device includes a movement mechanism that moves the delivery needle up and down relative to the container.
9. The system of claim 8, wherein,
the movement mechanism is configured to move the delivery needle to a first position with the first channel in fluid communication with the gas supply, the first position being lower than the position of the delivery needle when the second channel is optionally in fluid communication with the solvent supply or the gas supply.
10. The system of claim 7, wherein the delivery needle device comprises a cap through which the first channel and the second channel sealingly pass, the cap configured to sealingly mate to a container mouth of a container, and the delivery needle is movable relative to the cap.
11. The system according to claim 10, wherein the system further comprises negative pressure application means and/or exhaust gas recovery means,
the cover is provided with ports connected to the negative pressure applying means and/or the exhaust gas recovery means.
12. The system of claim 7, wherein the system comprises a plurality of sensors,
the system includes a switching mechanism that is configured to switch between,
the first channel is fluidly connected to the gas supply via the sample supply and the switching mechanism,
the second channel is in fluid connection with the gas supply means and the solvent supply means respectively via the switching mechanism,
the switching mechanism has a first switching position, a second switching position and a third switching position,
in the first switching position, the first channel is in fluid connection with the gas supply via the sample supply;
in the second switching position, the second channel bypasses the sample providing device and is directly in fluid connection with the gas providing device;
in the third switching position, the second channel bypasses the sample providing device and is directly in fluid connection with the solvent providing device.
13. The system of claim 12, comprising a shut-off device for the second channel, the shut-off device configured to close the second channel when the first channel is in fluid communication with the sample providing device.
14. The system of claim 7, wherein the gas supply means is arranged to supply gas to the container at a pressure of 350-500 Psi.
15. The system of claim 7, wherein the delivery needle further comprises a third channel interposed between the first channel and the second channel
The third channel is optionally in fluid connection with the solvent supply or the gas supply.
16. A delivery needle assembly for an evaporation system, comprising:
a first channel having a first end and a second end;
a second channel having a third end and a fourth end, the second channel being located outside of the first channel; and
a closure through which the first and second channels sealingly pass, the closure configured to sealingly mate to a container mouth of a container;
it is characterized in that the method comprises the steps of,
the first channel has an opening disposed at the first end;
the third end of the second channel is closed, and the outer wall forming the second channel is provided with a plurality of holes.
17. The delivery needle assembly of claim 16, wherein the second channel surrounds the first channel, the second channel being separated from the first channel by at least one inner wall,
Wherein the outer wall and the inner wall are fixed as one body.
18. The delivery needle assembly of claim 16, wherein the needle is,
the plurality of holes are disposed proximate the third end of the second channel.
19. The delivery needle assembly of claim 16, wherein the needle is,
the holes include a plurality of hole groups arranged in a circle on the outer wall around the second passage, the hole groups being spaced apart from each other by a predetermined distance in a longitudinal direction of the outer wall, and/or the holes are arranged in the outer wall perpendicularly with respect to the longitudinal direction of the second passage or so that a radially outer side of the holes is inclined closer to the third end than a radially inner side of the holes.
20. The delivery needle assembly of claim 16, wherein the needle is,
the pore diameter of the pore is between 0.2 and 0.3 mm.
21. The delivery needle assembly of claim 17, wherein at the third end of the second channel, the outer wall is secured to the inner wall by a weld that closes the third end of the second channel.
CN202210679191.3A 2022-06-16 2022-06-16 System and method for vaporizing a sample and a delivery needle assembly for use in the system Pending CN117288548A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN202210679191.3A CN117288548A (en) 2022-06-16 2022-06-16 System and method for vaporizing a sample and a delivery needle assembly for use in the system
PCT/CN2023/100369 WO2023241645A1 (en) 2022-06-16 2023-06-15 System and method for evaporating sample, and delivery needle assembly for system

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210679191.3A CN117288548A (en) 2022-06-16 2022-06-16 System and method for vaporizing a sample and a delivery needle assembly for use in the system

Publications (1)

Publication Number Publication Date
CN117288548A true CN117288548A (en) 2023-12-26

Family

ID=89192320

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210679191.3A Pending CN117288548A (en) 2022-06-16 2022-06-16 System and method for vaporizing a sample and a delivery needle assembly for use in the system

Country Status (2)

Country Link
CN (1) CN117288548A (en)
WO (1) WO2023241645A1 (en)

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5432098A (en) * 1994-10-31 1995-07-11 Dynatech Precision Sampling Corporation Apparatus, and process, for automatically sampling solids and semi-solids materials for analysis
US6706245B2 (en) * 2000-03-10 2004-03-16 Teledyne Tekmar Company Three stage needle for use with an autosampler
CN101639469A (en) * 2009-08-25 2010-02-03 成都科林分析技术有限公司 Gas displacement and dynamic compensation sampling method in headspace analysis
US9658144B1 (en) * 2010-06-01 2017-05-23 Brooks Rand Inc Systems and methods for chemically testing a sample and sampling probes therefor
CH703522B1 (en) * 2010-07-19 2014-07-31 Hpl Consult Gmbh Blow-off system for solvent.
CN103212212B (en) * 2012-10-18 2017-12-26 中华人民共和国绥芬河出入境检验检疫局 Multichannel acceleration evaporator
CN105606409B (en) * 2015-12-28 2018-06-05 成都科林分析技术有限公司 Multichannel head space extracts pin

Also Published As

Publication number Publication date
WO2023241645A1 (en) 2023-12-21

Similar Documents

Publication Publication Date Title
US11761971B2 (en) Arrangement for preparing a plurality of samples for an analytical method
US5585068A (en) Apparatus for automatically separating a compound from a plurality of discrete liquid specimens
JP7128810B2 (en) System and method for chemical analysis
CN103517764B (en) Capillary fluid flow controls
EP1888739B1 (en) Automated apparatus and method for treating biological specimens on slides
JP6332456B2 (en) Pretreatment kit, pretreatment apparatus for pretreatment of sample using the pretreatment kit, and analysis system including the pretreatment apparatus
JPH03183947A (en) Doser for analyzer
US20140053988A1 (en) Gas-blowing vaporizing and drying device
JP4304202B2 (en) Sample preparation method for analyzer and sample preparation station therefor
JP2007163492A (en) Method of preparing sample for analyzer, and sampling station for preparing sample for analyzer
KR102404442B1 (en) Spray process for coating substrates
WO2010113241A1 (en) Batching-off and refining device
CN117288548A (en) System and method for vaporizing a sample and a delivery needle assembly for use in the system
US20060108285A1 (en) Nozzle for collecting extracted material
EP1171762B1 (en) Evaporation of liquids and recirculation of purified gas
CN109564200B (en) Gas-liquid separator for collecting chromatographic fractions
JP3967331B2 (en) Liquid mixing method, liquid mixing apparatus and microchip
US11953408B2 (en) Methods and devices for sample capture using gas-pulse nanoparticle displacement
JP6260379B2 (en) Gas spray type liquid injection device and injection container used therefor
JP4653286B2 (en) Assemblies for detaching sampling vials, adapters and sampling vials explicitly intended for said assemblies, and parts kit for forming said assemblies
US11680929B2 (en) Dead volume-free fraction collection apparatus
CN117178191A (en) Systems and methods for humidity and/or temperature control in a sample analysis system
US20070110629A1 (en) Sampling device for a microreaction system
CN211652675U (en) Spray needle cleaning mechanism, CE-MS combined equipment and biochemical analysis system
JP6149770B2 (en) Gas spray type liquid sample injection device and injection container used therefor

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication