The present invention relates to an autosampler that supplies a sample to be analyzed to an analysis device.
There is an autosampler that is used by an analysis device such as a liquid chromatograph. A needle included in the autosampler collects a sample from a vial storing the sample to be analyzed and injects the collected sample into an analysis flow path of the liquid chromatograph. The autosampler can supply samples stored in a plurality of vials successively to the analysis flow path of the liquid chromatograph.
After a sample is supplied to the analysis flow path by the autosampler, part of the sample may remain in a needle of the autosampler. For example, a sample adsorbs on the needle, thereby remaining in the needle. The remaining sample adsorbed on the needle may be mixed with a sample supplied to the analysis flow path in a step of supplying a next sample. The mixed remaining sample influences a result of analysis in the liquid chromatograph. For example, a component of the mixed remaining sample appears as a subtle peak in a result of analysis of the next sample. This phenomenon is referred to as carryover. It is required that carryover is minimum as performance of the autosampler.
As measures against carryover, the needle is cleaned before and after a step of sucking a sample. The needle is cleaned by insertion of the needle into a rinse port filled with a cleaning liquid. Alternatively, the needle is cleaned by suction and discharge of the cleaning liquid filling the rinse port by the needle (see Patent Document 1, for example).
Various liquids are selected in accordance with an analysis condition or a sample type as a cleaning liquid to be used in the rinse port. Further, a highly corrosive liquid such as chlorine may be used as a cleaning liquid. When a highly corrosive cleaning liquid stored in the rinse port is evaporated, an evaporated gas fills the autosampler. Thus, a metallic member in a casing of the autosampler may rust due to an evaporated highly corrosive gas.
As such, it is necessary to have a mechanism for preventing rusting by regularly ventilating the casing of the autosampler. There is a conventional autosampler including a gas exhaust fan at a side surface of a casing as the mechanism. Thus, air in the autosampler is ventilated regularly by the gas exhaust fan.
[Patent Document 1] JP 2017-207391 A
A method of ventilating the autosampler with use of a fan provided at the side surface of the casing of the autosampler requires a long period of time for ventilation. With an autosampler having a large casing, it requires a particularly long period of time for ventilation.
Further, there is an autosampler that includes a cooling system for cooling air in the autosampler for the purpose of preventing condensation or the purpose of realizing a uniform cooling temperature. The method of ventilating the autosampler with use of a gas exhaust fan exhausts the air cooled by the cooling system outwardly of the casing and lowers cooling performance.
An object of the present invention is to exhaust gas evaporated from a rinse port outwardly of an autosampler without requiring a long period of time for ventilating a casing of the autosampler and lowering cooling performance in the casing of the autosampler.
(1) An autosampler according to one aspect of the present invention supplies a sample to an analysis device, and includes an injection port for supplying the sample to be analyzed to the analysis device, a needle that collects the sample to be analyzed stored in a vial and injects the sample to be analyzed into the injection port, a cleaning unit that cleans the needle, and a gas exhaust fan. The cleaning unit includes a cleaning container which stores a cleaning liquid and into which the needle that needs to be cleaned is inserted in the stored cleaning liquid, and a unit main body that has a space for storing the cleaning container and receiving the cleaning liquid overflowing from the cleaning container, and a unit gas exhaust passage for exhausting gas in the space outwardly of the cleaning unit. The unit main body has a unit opening through which the needle passes when accessing the cleaning container. The autosampler further includes a boundary portion that separates a first region in which the injection port, the needle and the unit opening are arranged from a second region in which the gas exhaust fan is arranged, and a gas exhaust region which is connected to the unit gas exhaust passage via a gas exhaust opening provided at the boundary portion and into which gas exhausted from the space flows due to a negative pressure generated by the gas exhaust fan.
In this autosampler, the first region in which the injection port, the needle and the unit opening are arranged is separated from the second region in which the exhaust fan is arranged by the boundary portion. The space in the cleaning unit is connected to the gas exhaust region in the second region through the unit gas exhaust passage in the cleaning unit. The gas in the space of the cleaning unit is exhausted to the gas exhaust region in the second region through the unit gas exhaust passage and the gas exhaust opening provided at the boundary portion due to a negative pressure generated by the gas exhaust fan.
With this autosampler, the gas in the cleaning unit is exhausted to the second region through the unit gas exhaust passage in the cleaning unit. Thus, the gas in the cleaning unit is prevented from flowing out via the unit opening and filling the first region. Even in a case where a highly corrosive liquid such as chlorine is used as the cleaning liquid, an evaporated gas is prevented from filling the first region. Thus, rusting of a metallic member in the first region due to a highly corrosive gas is prevented.
With this autosampler, the gas flowing out from the cleaning unit does not fill the first region. Therefore, it is not necessary to provide a gas exhaust fan at a side surface of the casing of the autosampler and ventilate the first region as conventionally done, and a period of time required to ventilate the first region is shortened. Further, because this autosampler does not ventilate the first region with a gas exhaust fan, cooling performance in the first region is not lowered.
(2) The unit main body may have a partition wall that separate the space from the unit gas exhaust passage, and gas in the space is exhausted to the unit gas exhaust passage via a partition wall opening provided at the partition wall. The partition wall separates the space for receiving the cleaning liquid overflowing from the cleaning container from the space to which gas is exhausted.
(3) The unit gas exhaust passage may extend in an up-and-down direction. The gas exhausted from the partition wall opening flows in the up-and-down direction and is exhausted.
(4) The partial wall opening may be provided at an upper end of the partition wall. A large space that receives the cleaning liquid overflowing from the cleaning container can be ensured.
(5) The cleaning unit may include a cleaning unit cover that covers the unit opening while enabling the needle to access the cleaning container.
This autosampler includes the cleaning unit cover that covers the unit opening of the cleaning unit, so that the gas in the cleaning unit is further prevented from filling the first region. Thus, rusting of a metallic member in the first region due to a highly corrosive gas is effectively prevented.
(6) The cleaning unit cover may be provided on a path through which the needle passes when accessing the cleaning container, and may have a cap provided to enable the needle to access the cleaning container.
Because the cleaning unit cover has the cap on the path through which the needle passes, the gas in the cleaning unit is further prevented from filling the first region. Further, while a portion through which the needle passes in the cleaning unit cover may be contaminated by a sample or the like, it is possible to remove a contaminated portion by replacing the cap.
(7) The cap may have a hole through which the needle passes. Except for a portion including a hole through which the needle passes, the space in the cleaning unit is separated from the first region.
(8) The cap may have a hole region in which a hole through which the needle passes is to be formed when the cap is pierced by the needle.
The hole though which the needle passes is not present until the needle passes. The space in the cleaning unit is effectively separated from the first region. The gas in the cleaning unit is further effectively prevented from flowing into the first region.
(9) The autosampler may further include an external gas exhaust passage through which gas that has flowed into the gas exhaust region from the space due to a negative pressure generated by the gas exhaust fan is sent outwardly of the autosampler.
The gas that has flowed into the gas exhaust region in the second region is further sent outwardly of the autosampler. A member in the second region is also prevented from being contaminated by the gas.
With the present invention, it is possible to exhaust gas evaporated form a rinse port outwardly of an autosampler without requiring a long period of time to ventilate a casing of the autosampler and lowering cooing performance in the casing of the autosampler.
An autosampler 7 according to embodiments of the present invention will be described below in detail with reference to the drawings.
A sample plate 71 is arranged at a predetermined location in the autosampler 7. A plurality of sample vials 72 are arranged in the sample plate 71. A sample is stored in a sample vial 72. The needle 73 is movable among the sample vials 72, the rinse port 1 and the injection port 74. The needle 73 collects a sample from a sample vial 72. The needle 73 supplies the sample to the column 81 by injecting the sample into the injection port 74. After the sample is injected into the injection port 74 or the sample is collected from the sample vial 72, the needle 73 is cleaned in the rinse port 1.
The rinse port 1 stores cleaning containers 3A, 3B. The liquid sending tube 52A is connected to the cleaning container 3A. The end of the liquid sending tube 52A is arranged in the cleaning liquid tank 76A. The pump 75A is connected to the liquid sending tube 52A between the cleaning container 3A and the cleaning liquid tank 76A. With this configuration, when the pump 75A is driven, the cleaning liquid in the cleaning liquid tank 76A is sent to the cleaning container 3A through the liquid sending tube 52A. In the present embodiment, the pump 75A serves as both of a cleaning liquid pump for sending the cleaning liquid stored in the cleaning liquid tank 76A to the cleaning container 3A and a metering pump for collecting and discharging a sample with the use of the needle 73. For example, a pump that can adjust a flow rate with high accuracy is used as the pump 75A. In
The liquid sending tube 52B is connected to the cleaning container 3B. The end of the liquid sending tube 52B is arranged in the cleaning liquid tank 76B. The pump 75B is connected to the liquid sending tube 52B between the cleaning container 3B and the cleaning liquid tank 76B. With this configuration, when the pump 75B is driven, the cleaning liquid in the cleaning liquid tank 76B is sent to the cleaning container 3B through the liquid sending tube 52B. In the present embodiment, the pump 75B is a dedicated pump for sending the cleaning liquid stored in the cleaning liquid tank 76B to the cleaning container 3B. As the pump 75B, a pump having a volume larger than that of the pump 75A is used, for example.
The autosampler 7 has a casing 701. Further, the autosampler 7 has a boundary portion 702. The space in the autosampler 7 is sectioned into a first region A1 and a second region A2 by the boundary portion 702. In the first region A1, the rinse port 1, the sample plate 71, the needle 73, the injection port 74 and the cooling system 78 are arranged. In the second region A2, the liquid sending tubes 52A, 52B, the liquid drainage tube 55 and the pumps 75A, 75B are arranged.
The first region A1 is covered by the casing 701 and the boundary portion 702 and closed from the outside of the autosampler 7. The first region A1 is cooled by the cooling system 78. The cooling system 78 includes a fan that circulates air in the first region A1, and the entire first region A1 is cooled.
The second region A2 is separated from the first region A1 by the boundary portion 702. While the second region A2 is partially separated from the outside of the autosampler 7 by the casing 701, the entire region is not separated from the outside. That is, differently from the first region A1, the second region A2 is not closed from the outside of the autosampler 7. While the first region A1 and the second region A2 are connected to each other via a portion through which the cleaning liquid or the like is sent, the first region A1 and the second region A2 are separated from each other in the rest. Air in the region cannot move between the first region A1 and the second region A2. Description will be provided below. Thus, although the second region A2 is not closed from the outside, the cooling effect in the first region A1 is maintained.
As described above, the liquid chromatograph 8 includes the column 81 and the detector 82. A sample that has been injected into the injection port 74 by the needle 73 is sent to the column 81. A sample continuously sent from the autosampler 7 is supplied to the column 81. A sample that is separated into components in the column 81 is detected by the detector 82.
The overall configuration of the rinse port 1 according to the present embodiment will be described below next.
As shown in
As shown in
As shown in
The upper end of the liquid sending tube 52B is inserted into the second supply port 24B. The liquid sending tube 52B is fixed to the main body lower portion 22 by the fastening members 51A and 53B. A screw thread is formed on the inner wall of the cylindrical member of the second supply port 24B, and a screw thread is formed on the outer periphery of the fastening member 51B. Further, in each of the fastening members 51B and 53B, a tube insertion hole penetrating in the up-and-down direction is formed in a rotation center axis portion, and the liquid sending tube 52B is inserted into this tube insertion hole. With this structure, the fastening members 51B and 53B hold the liquid sending tube 52B, and the fastening member 51B is fixed to the main body lower portion 22 by the screw structure.
The configuration of the rinse port main body 2 will be described next with reference to
As shown in
As shown in
As shown in
A gas exhaust port 201 is provided at the end of the inner space 20. A unit gas exhaust passage 200 is provided close to the gas exhaust port 201. The gas exhaust port 201 is connected to the unit gas exhaust passage 200. The function of the gas exhaust port 201 and the unit gas exhaust passage 200 will be described below in detail.
As shown in
Next, the configuration of the cleaning containers 3A, 3B will be described with reference to
As shown in
Further, as shown in
As shown in
Further, as described above with reference to
Further, as described above with reference to
Further, as described above with reference to
The rinse port 1 that is configured as described above is stored in the autosampler 7 as shown in
The needle 73 is cleaned in the cleaning container 3A or 3B, after the needle 73 collects a sample in a sample vial 72, for example. Before the needle 73 is cleaned in the cleaning container 3A or 3B, the cleaning container 3A or 3B that is to be utilized for cleaning is filled with a cleaning liquid. The needle 73 is cleaned by the cleaning liquid by accessing the cleaning container 3A or 3B from above. The needle 73 enters the cleaning container 3A or 3B, so that a sample or the like adhering to its peripheral surface is washed away.
After injecting a sample into the injection port 74 by the needle 73, for example, the needle 73 is cleaned in the cleaning container 3A or 3B. Alternatively, the needle 73 is cleaned in the cleaning container 3A or 3B before the step of collecting a next sample. Also in this case, the cleaning container 3A or 3B to be utilized for cleaning is filled with a cleaning liquid before the needle 73 is cleaned in the cleaning container 3A or 3B. The needle 73 is cleaned by the cleaning liquid by accessing the cleaning container 3A or 3B from above. The needle 73 enters the cleaning container 3A or 3B, so that a sample or the like adhering to its peripheral surface is washed away. Alternatively, the needle 73 sucks and discharges the cleaning liquid in the cleaning container 3A or 3B, so that the inside of the needle 73 is cleaned.
When the pump 75A or the pump 75B is driven, and an additional cleaning liquid is supplied to the cleaning container 3A or 3B, the cleaning liquid in the cleaning container 3A or 3B overflows from the upper end of the cleaning container 3A or 3B. The overflowing cleaning liquid flows into the inner space 20 of the rinse port main body 2. The cleaning liquid that has flowed into the inner space 20 flows into the liquid drainage tube 55 via the liquid drainage port 23. The cleaning liquid that has flowed into the liquid drainage tube 55 is collected in the liquid drainage tank 77.
In the present embodiment, the cleaning containers 3A, 3B are individually detachable from the rinse port main body 2 as described above. Therefore, different types of materials can be used as a material for the cleaning container 3A and a material for the cleaning container 3B. As the materials for the cleaning containers 3A, 3B, PEEK (polyetheretherketone), stainless and ceramic can be used, for example. As one example, a combination of PEEK being used as a material for the cleaning container 3A and stainless being used as a material for the cleaning container 3B is possible.
In the present embodiment, PPS (Poly Phenylene Sulfide) is used as a material for the rinse port main body 2. It is desirable that the rinse port main body 2 has excellent chemical resistance because the rinse port main body 2 receives an overflowing cleaning liquid from the cleaning containers 3A, 3B. While metal such as stainless may be used as a material for the rinse port main body 2 from this point of view, PPS is used in the present embodiment from the viewpoint of processability.
As shown in
When the cleaning containers 3A, 3B are fastened to the rinse port main body 2, an operator can attach and detach the cleaning containers 3A, 3B by making a tool be engaged with the upper ends of the cleaning containers 3A, 3B. The grooves 32A, 32B at the upper ends of the cleaning containers 3A, 3B also serve as flow paths from which a cleaning liquid flows when the cleaning liquid overflows.
Next, the configuration of a rinse port cover 4 will be described.
As shown in
As shown in
As shown in
As shown in
In the present embodiment, two types of cover caps 45, 45A can be utilized. As shown in
Differently from the cover cap 45 shown in
As a material for the rinse port cover 4 and the cover caps 45, 45A, PP (polypropylene) or PE (polyethylene) is used, for example.
The structure for exhausting gas vaporized from the rinse port 1 will be described next with reference to
As shown in the diagram, the main body upper portion 21 of the rinse port main body 2 is arranged in the first region A1. The cooling system 78 is attached to the casing 701 in the first region A1. Further, although not shown in
As shown in
As shown in
As shown in
Further, an external gas exhaust passage 708 is connected to the gas exhaust chamber 705 at a position farther downstream than the exhaust fan 707. As shown in
With above-mentioned configuration, the gas in the gas exhaust region 706 is exhausted outwardly of the autosampler 7 through the external gas exhaust passage 708 by the pressure generated by the gas exhaust fan 707. That is, when the gas exhaust fan 707 is driven, the gas in the inner space 20 of the rinse port 1 is exhausted outwardly of the autosampler 7 via the gas exhaust port 201, the unit gas exhaust passage 200, the gas exhaust port 202, the gas exhaust opening 703, the gas exhaust region 706 and the external gas exhaust passage 708.
As described above, the autosampler 7 of the present embodiment is sectioned into the first region A1 in which the injection port 74, the needle 73 and the unit opening 210 are arranged and the second region A2 in which the gas exhaust fan 707 is arranged by the boundary portion 702. The inner space 20 of the rinse port 1 is connected to the gas exhaust region 706 of the second region A2 through the unit gas exhaust passage 200 in the rinse port 1. The gas in the inner space 20 of the rinse port 1 is exhausted due to a negative pressure generated by the gas exhaust fan 707 to the gas exhaust region 706 in the second region A2 through the unit gas exhaust passage 200 and the gas exhaust opening 703 provided at the boundary portion 702.
The gas in the rinse port 1 is exhausted due to a negative pressure generated by the gas exhaust fan 707 to the second region A2 through the unit gas exhaust passage 200 in the rinse port 1, so that the gas in the rinse port 1 is prevented from flowing out from the unit opening 210. Thus, the gas that has flowed out from the unit opening 210 is prevented from filling the first region A1. Even in a case where a highly corrosive liquid such as chlorine is used as the cleaning liquid, a vaporized gas is prevented from filling the first region A1. Thus, rusting of a metallic member in the first region A1 due to a highly corrosive gas is prevented.
With the autosampler 7 of the present embodiment, the gas that flows out from the rinse port 1 does not fill the first region A1. Therefore, it is not necessary to provide a gas exhaust fan at the side surface of the casing 701 of the autosampler 7 and ventilate the first region A1 as conventionally done, and a period of time required to ventilate the first region A1 is shortened. Further, because the autosampler 7 does not ventilate the first region A1 by a gas exhaust fan, cooling performance of the first region A1 is not lowered.
Further, as described above, the rinse port main body 2 has the unit opening 210 through which the needle 73 passes when accessing the cleaning containers 3A, 3B. Further, the rinse port 1 has the rinse port cover 4 that covers the unit opening 210 while enabling the needle 73 to access the cleaning containers 3A, 3B.
Because the autosampler 7 in the present embodiment has the rinse port cover 4 that covers the unit opening 210 of the rinse port 1, the gas in the rinse port 1 is further prevented from filling the first region A1. Rusting of a metallic member in the first region A1 due to a highly corrosive gas is effectively prevented.
Further, the rinse port cover 4 is provided on the path through which the needle 73 passes when accessing the cleaning containers 3A, 3B and has the cover caps 45, 45A provided to enable the needle 73 to access the cleaning containers 3A, 3B.
Because the rinse port cover 4 has the cover cap 45 on the path through which the needle 73 passes, the gas in the rinse port 1 is further prevented from filling the first region A1. Further, while a portion through which the needle 73 passes in the rinse port cover 4 may be contaminated by a sample or the like, it is possible to remove a contaminated portion by replacing the cover caps 45, 45A.
Further, because the cover cap 45 has an insertion hole 451 through which the needle 73 passes, the inner space 20 in the rinse port 1 is separated from the first region A1 except for a portion including the insertion hole 451 through which the needle 73 passes.
Further, the cover cap 45A has the hole region 452 in which a hole through which the needle 73 passes and which is formed when the cover cap 45A is pierced by the needle 73. A hole through which the needle passes is not present until the needle 73 passes through. The inner space 20 in the rinse port 1 is more effectively separated from the first region A1. The gas in the rinse port 1 is further effectively prevented from flowing into the first region A1.
Further, as described above, the autosampler 7 has the external gas exhaust passage 708 through which the gas flowing into the gas exhaust region 706 from the inner space 20 due to a negative pressure generated by the gas exhaust fan 707 is sent outwardly of the autosampler 7. The gas that has flowed into the gas exhaust region of the second region A2 is further sent outwardly of the autosampler 7. A member in the second region A2 is also prevented from being contaminated by gas.
In the following paragraphs, non-limiting examples of correspondences between various elements recited in the claims below and those described above with respect to various preferred embodiments of the present disclosure are explained. In the above-mentioned embodiment, the rinse port 1 is an example of a cleaning unit, and the rinse port main body 2 is an example of a unit main body. Further, the gas exhaust port 201 is an example of a partition wall opening.
As each of constituent elements recited in the claims, various other elements having configurations or functions described in the claims can be also used.
While the rinse port 1 is configured to have the two cleaning containers 3A, 3B by way of example in the above-mentioned embodiment, the number of cleaning containers is not limited to this. The number of cleaning containers stored in the rinse port 1 may be one or three or more.
While the gas exhaust port 202 and the gas exhaust opening 703 are connected directly to each other by way of example in the above-mentioned embodiment, the gas exhaust port 202 and the gas exhaust opening 703 may be connected to each other through a tube, a pipe, etc. Further, while the gas exhaust port 201 that is a partition wall opening is provided at the upper end of the partition wall 203 in the above-mentioned embodiment, a partition wall opening does not have to be provided at the upper end of the partition wall 203. A partition wall opening may be a hole provided in the vicinity of the upper portion of the partition wall 203.
While the unit opening 210 is covered by the rinse port cover 4 by way of example in the above-mentioned embodiment, the rinse port cover 4 is not required. Even in a case where the rinse port cover 4 is configured not to be attached, gas is prevented from filling the first region A1 due to a negative pressure generated by the gas exhaust fan 707. For example, attachment or non-attachment of the rinse port cover 4 may be selected based on whether a highly corrosive cleaning liquid is used.
In the above-mentioned embodiment, the gas in the inner space 20 of the rinse port 1 is exhausted to the gas exhaust region 706 in the second region A2 due to a negative pressure generated by the gas exhaust fan 707. As another method, the gas in the rinse port 1 may be exhausted to the second region A2 due to a positive pressure generated by the gas exhaust fan. In this case, two passages connecting the second region A2 to the inner space 20 are prepared. A fan is arranged in the second region A2, and a positive pressure is generated in the inner space 20 through one passage by a positive pressure generated by the fan. The gas in the inner space 20 is exhausted to the second region A2 through the other passage by a positive pressure generated by the fan. Also with this method, the gas in the rinse port 1 can be prevented from filling the autosampler 7.
Filing Document | Filing Date | Country | Kind |
---|---|---|---|
PCT/JP2018/039391 | 10/23/2018 | WO |
Publishing Document | Publishing Date | Country | Kind |
---|---|---|---|
WO2020/084696 | 4/30/2020 | WO | A |
Number | Name | Date | Kind |
---|---|---|---|
20090041622 | Maeda | Feb 2009 | A1 |
20130019697 | McKeen | Jan 2013 | A1 |
20130067997 | Ebsen | Mar 2013 | A1 |
20190072577 | Konishi | Mar 2019 | A1 |
Number | Date | Country |
---|---|---|
2017-207391 | Nov 2017 | JP |
Entry |
---|
International Search Report for corresponding Application No. PCT/JP2018/039391, dated Dec. 11, 2018. |
Written Opinion for corresponding Application No. PCT/JP2018/039391, dated Dec. 11, 2018 (Machine Translation). |
Number | Date | Country | |
---|---|---|---|
20210389283 A1 | Dec 2021 | US |