WO2016194084A1

WO2016194084A1 - Injection method and injection device

Info

Publication number: WO2016194084A1
Application number: PCT/JP2015/065671
Authority: WO
Inventors: 賢一大林
Original assignee: 株式会社島津製作所
Priority date: 2015-05-29
Filing date: 2015-05-29
Publication date: 2016-12-08

Abstract

Provided are an injection method and an injection device, whereby pressure in a container can be prevented from increasing when a liquid is injected into the container. Before a needle 41 is inserted into a container 100 having a seal member 120 that is attached to an opening 110, and a liquid is injected into the container, a through hole is formed in the seal member 120. Consequently, when the liquid is injected into the container 100, since air in the container 100 can be released to the atmosphere through the through hole previously formed in the seal member 120, pressure in the container 100 can be prevented from increasing.

Description

Injection method and injection apparatus

The present invention relates to an injection method and an injection device for injecting a liquid into a container having a seal member attached to an opening.

A container that contains a liquid such as a sample may be used in a state where its opening is sealed by a sealing member such as a septum. As an apparatus for handling this type of container, an injection apparatus that dispenses liquid by inserting a needle so as to penetrate a seal member and sucking or injecting liquid through the needle is known.

For example, in the apparatus disclosed in Patent Document 1 below, a needle is inserted into a container containing a sample so as to penetrate the seal member, and the tip of the needle is immersed in the sample in the container. The In this state, after the sample is sucked from the tip of the needle, the needle is removed from the container. Then, the needle is moved to the injection position, and the sample is dispensed by discharging the sample from the needle at the injection position.

When the opening of the container is sealed with the seal member, the inside of the container is kept substantially sealed by the seal member coming into close contact with the outer peripheral surface of the needle when the needle is inserted into the container. For this reason, when the sample in the container is sucked into the needle in this state, the inside of the container becomes a negative pressure, and an accurate amount of the sample may not be sucked.

Therefore, in the apparatus disclosed in Patent Document 1 below, a groove is formed on the outer peripheral surface of the needle. As a result, even when the needle is inserted into the container, the inside of the container and the atmosphere communicate with each other through a groove formed on the outer peripheral surface of the needle, thereby preventing negative pressure in the container. be able to.

JP 2007-107918 A

As described above, Patent Document 1 proposes a configuration in which the shape of the needle is changed so that the pressure in the container does not become too low compared to the atmospheric pressure when the sample in the container is sucked with the needle. Has been. On the other hand, when the dispensing destination of the liquid such as the sample sucked into the needle is in a container whose opening is sealed by the seal member, the sample is injected into the container through the needle. May be too high compared to atmospheric pressure.

That is, when the liquid is injected into the container through the needle with the needle inserted into the container so as to penetrate the seal member, the space in the container decreases by the amount of the injected liquid, The pressure in the container increases. Furthermore, when the volatility of the liquid is high, the pressure in the container is further increased. And since the temperature rises as the pressure in the container increases, the volatilization of the liquid is further promoted, and pressurization in the container may proceed.

When the pressure in the container rises as described above, when the needle is subsequently removed from the container, the liquid injected into the container is formed in the through-hole formed in the seal member when the needle is inserted There is a risk of jumping out. Since some liquids injected into the container contain components harmful to the human body, it is very dangerous for the liquid to jump out of the container. In addition, when the liquid jumps out from the container, the amount of liquid injected from the needle does not match the amount of liquid remaining in the container, so that an accurate analysis result may not be obtained.

The present invention has been made in view of the above circumstances, and an object thereof is to provide an injection method and an injection device capable of preventing the pressure in the container from increasing when a liquid is injected into the container. And

(1) The injection method according to the present invention includes a drilling step and an injection step. In the perforating step, a through hole is formed in the seal member attached to the opening of the container. In the injection step, after the drilling step, a needle is inserted into the container so as to penetrate the seal member, and a liquid is injected into the container through the needle, and then the needle is inserted from the container. Pull out.

According to such a configuration, the through hole is formed in the seal member before the needle is inserted into the container having the seal member attached to the opening and the liquid is injected. Thereby, when the liquid is injected into the container, the air in the container can be released into the atmosphere from the through-hole formed in the sealing member in advance, and thus the pressure in the container is prevented from rising. Can do. Therefore, even when the volatility of the liquid is high, the liquid injected into the container can be prevented from jumping out when the needle is removed from the container after the liquid is injected.

(2) In the drilling step, after inserting the needle into the container so as to penetrate the seal member, the needle is removed from the container, thereby forming a through hole in the seal member. Also good.

According to such a configuration, the needle is inserted into and removed from the container to form a through-hole in the seal member, and then the needle is reinserted into the container. Liquid is injected into the inside. That is, a through hole can be formed in the seal member using a needle for injecting liquid into the container. Thereby, it is not necessary to separately provide a member for forming the through hole in the seal member, and the through hole can be formed in the seal member with a simple configuration.

(3) In the perforating step, the operation of inserting and withdrawing the needle from and into the container may be repeated a plurality of times.

According to such a configuration, the through-hole is formed in the seal member by repeating the operation of inserting and withdrawing the needle into and from the container a plurality of times. Therefore, when the needle penetrates the same position on the seal member a plurality of times, a larger through hole is formed. On the other hand, when the needle passes through different positions in the seal member a plurality of times, a plurality of through holes are formed. In any case, when the liquid is injected into the container, the air in the container can be easily released into the atmosphere from the through-hole formed in the seal member in advance. It is possible to effectively prevent the rise.

(4) In the drilling step, the needle may be inserted into and removed from the container by moving the needle to a specific position in the horizontal direction and then moving the needle along the axis. In this case, in the injection step, the needle may be moved along the axis while the needle is maintained at the specific position in the horizontal direction.

According to such a configuration, the needle is inserted into and removed from the container at a specific position in the horizontal direction, so that the through hole is formed in the seal member, and then the needle is not moved in the horizontal direction. Liquid is injected into the container through the needle. Thereby, the operation for forming the through hole in the seal member is simplified, and the time until the liquid injection is completed can be shortened.

When the operation of inserting and withdrawing the needle into and out of the container is repeated a plurality of times at the specific position in the horizontal direction, if the needle position accuracy is high, the needle penetrates the same position in the seal member a plurality of times. A larger through hole is formed. On the other hand, when there is variation in the position accuracy of the needle, a plurality of through holes are formed by allowing the needle to penetrate a plurality of different positions in the seal member a plurality of times.

(5) The injection device according to the present invention includes a container holding unit, an injection mechanism, an injection control unit, and a perforation control unit. The container holding unit holds a container having a seal member attached to the opening. The injection mechanism has a needle and a moving mechanism for moving the needle, and injects a liquid into the container via the needle. The injection control unit moves the needle with the moving mechanism, thereby inserting the needle into the container so as to penetrate the seal member, and injecting liquid into the container through the needle Then, the needle is removed from the container. The perforation control unit forms a through hole in the seal member before the needle is inserted into the container by the injection control unit.

(6) The perforation control unit moves the needle with the moving mechanism to insert the needle into the container so as to penetrate the seal member, and then removes the needle from the container. Thus, a through hole may be formed in the seal member.

(7) The perforation control unit may repeat the operation of inserting and withdrawing the needle into and from the container a plurality of times.

(8) The perforation control unit may insert and remove the needle with respect to the container by moving the needle along an axis at a specific position in the horizontal direction. In this case, the injection control unit may move the needle along the axis while maintaining the needle at the specific position in the horizontal direction.

According to the present invention, when the liquid is injected into the container, the air in the container can be released into the atmosphere from the through-hole formed in the sealing member in advance. Can be prevented.

It is the schematic which showed the structural example of the injection apparatus which concerns on one Embodiment of this invention. It is the block diagram which showed the structural example of the control part. It is the schematic which showed the flow of operation | movement of the needle at the time of dispensing. It is the schematic which showed the flow of operation | movement of the needle at the time of dispensing. It is the schematic which showed the flow of operation | movement of the needle at the time of dispensing. It is the schematic which showed the flow of operation | movement of the needle at the time of dispensing. It is the schematic which showed the flow of operation | movement of the needle at the time of dispensing. It is the schematic which showed the flow of operation | movement of the needle at the time of dispensing. It is the flowchart which showed the flow of the process by the control part at the time of dispensing.

1. Configuration of Injection Device FIG. 1 is a schematic diagram illustrating a configuration example of an injection device 1 according to an embodiment of the present invention. This injection device 1 is an autosampler device for automatically injecting a liquid sample into an analyzer such as a gas chromatograph or a liquid chromatograph, for example, in order to pre-process the sample, a reaction reagent is applied to the sample. It can be used as a liquid injection mechanism for mixing or injecting a solvent for dilution into a standard sample for preparing a calibration curve. The autosampler device can inject the liquid sample after the pretreatment into the analyzer. The injection device 1 performs an operation for dispensing the container 100, for example, during the execution of the pretreatment. The injection device 1 includes a container housing part 2, a container holding part 3, an injection mechanism 4, and the like.

The container 100 is a bottomed cylindrical vial with one end closed. A seal member 120 is attached to the opening 110 formed at the other end of the container 100. The seal member 120 is a septum formed of an elastic body such as rubber, and the container 100 is sealed by being attached to the opening 110.

A plurality of containers 100 can be stored in the container storage unit 2. Various types of containers 100 such as an empty container 101, a container 102 in which a liquid sample to be analyzed is enclosed, and a container 103 in which a standard sample is enclosed are appropriately accommodated in the container accommodation unit 2. The empty container 101 is, for example, a new container 100 in which a through hole has never been formed in the seal member 120.

The container holding unit 3 holds the container 100. Specifically, the container 100 is held by the container holding unit 3 in such a posture that the container 100 extends in the vertical direction D1 and the seal member 120 is positioned on the upper side. The container 100 held by the container holding part 3 is conveyed by the conveying apparatus (not shown) from the container accommodating part 2, for example. In the example of FIG. 1, an empty container 101 is conveyed to and held by the container holding unit 3.

The injection mechanism 4 includes a needle 41 and a moving mechanism 42. The needle 41 is an elongated tubular member, and is held by the moving mechanism 42 in such a posture that the axis L extends in the vertical direction D1. The lower end of the needle 41 is formed in a sharp shape. The moving mechanism 42 is configured to include, for example, a motor and a gear (both not shown), and can move the needle 41 in the vertical direction D1 and the horizontal direction D2.

As shown in FIG. 1, when the needle 41 is moved horizontally to the upper side of the container 100 held by the container holding unit 3 and then moved downward, the seal member 120 attached to the container 100 is moved to the needle. 41 penetrates. Thereby, the tip of the needle 41 can be inserted into the container 100.

Although not shown in FIG. 1, a suction position for sucking a liquid into the needle 41 is set in the injection device 1. When dispensing, first, the needle 41 moves to the suction position, and then the liquid is sucked into the needle 41. Then, as shown in FIG. 1, the needle 41 moves to the injection position, which is a specific position in the horizontal direction, and the needle 41 is inserted into the container 100 so as to penetrate the seal member 120. Then, the liquid is injected into the container 100.

As the liquid sucked by the needle 41 at the suction position, a diluent can be exemplified. However, the liquid sucked into the needle 41 is not limited to the diluted liquid, and the liquid sample is transferred from the container 102 to the needle by moving the

containers

102, 103, etc. accommodated in the container accommodating portion 2 to the aspirating position. The standard sample may be sucked into the needle 41 from the container 103. The liquid sample sealed in the container 102 may not be the sample itself but a liquid in which a highly volatile solvent is mixed with the sample.

When the diluent is sucked into the needle 41 and dispensed into the empty container 101, and the standard sample in the container 103 is dispensed into the container 101, a standard sample diluted with the diluent can be generated. The standard sample diluted in this way is used as a calibration curve sample when preparing a calibration curve.

The dilution liquid is a highly volatile liquid containing, for example, hexane and acetone. In the diluted solution, hexane and acetone are mixed at a volume ratio of 1: 1, for example. However, the diluting solution is not limited to such a liquid, and may be, for example, diethyl ether, pyridine, acetonitrile, or dichloromethane. The liquid sucked by the needle 41 is not limited to a highly volatile liquid, and may be a low volatile liquid.

2. Configuration of Control Unit FIG. 2 is a block diagram illustrating a configuration example of the control unit 5. The operation of the injection device 1 according to the present embodiment is controlled by a control unit 5 including, for example, a CPU (Central Processing Unit). The control unit 5 functions as an injection control unit 51, a perforation control unit 52, and the like when the CPU executes a program.

The injection control unit 51 controls the operation of the pump 43 provided in the injection mechanism 4 in addition to the moving mechanism 42. The pump 43 communicates with the needle 41, and in the operation of sucking the liquid into the needle 41 (suction operation), the operation of injecting the liquid sucked into the needle 41 into the container 100 (injection operation), and the like. Driven by.

The perforation controller 52 controls the operation of the moving mechanism 42 to form a through hole in the seal member 120 of the container 100 held by the container holder 3. The processing by the perforation control unit 52 is performed before the needle 41 is inserted into the container 100 by the injection control unit 51.

3. Operation at the time of dispensing FIGS. 3A to 3F are schematic views showing the flow of operation of the needle 41 at the time of dispensing. FIG. 4 is a flowchart showing a flow of processing by the control unit 5 at the time of dispensing. Hereinafter, the operation during dispensing will be described in detail with reference to FIGS. 3A to 3F and FIG.

When dispensing a liquid to the container 100 held by the container holding unit 3, first, the needle 41 is moved to the suction position by the moving mechanism 42 (step S101). Then, by driving the pump 43 at the suction position, the liquid to be dispensed is sucked in advance into the needle 41 (step S102: suction step).

Thereafter, the needle 41 is moved to the injection position as shown in FIG. 1 by moving the needle 41 in the horizontal direction by the moving mechanism 42 (step S103). In this state, the perforation control unit 52 moves the needle 41 along the axis L by the moving mechanism 42 to perform an operation for forming a through hole in the seal member 120 attached to the opening 110 of the container 100. Performed (step S104: drilling step).

Specifically, as shown in FIG. 3A, the perforation control unit 52 moves the needle 41 downward along the axis L at the injection position. As a result, the needle 41 is inserted into the container 100 so as to penetrate the seal member 120. Thereafter, as shown in FIG. 3B, the perforation control unit 52 moves the needle 41 upward along the axis L.

Thereby, the needle 41 is removed from the container 100, and the through hole 121 is formed in the seal member 120. A series of drilling operations as shown in FIGS. 3A and 3B are repeated a plurality of times. That is, the perforation control unit 52 repeats the operation of inserting and withdrawing the needle 41 from the container 100 a plurality of times.

Next, the injection control unit 51 moves the needle 41 along the axis L with the moving mechanism 42 while maintaining the needle 41 at the injection position in the horizontal direction, and drives the pump 43 to thereby move the inside of the container 100. An operation for injecting the liquid is performed (step S105: injection step). That is, after the drilling step, the injection step is performed without moving the needle 41 in the horizontal direction.

Specifically, as shown in FIG. 3C, the injection control unit 51 moves the needle 41 along the axis L downward. As a result, the needle 41 is inserted into the container 100 so as to penetrate the seal member 120. At this time, the needle 41 penetrates the seal member 120 at a position different from the through-hole 121 formed in the seal member 120 by the drilling operation due to the needle 41 being slender and easily bent. For the same reason, when the drilling operation is repeated a plurality of times as described above, a plurality of through holes 121 are formed in the seal member 120.

The tip position of the needle 41 inserted into the container 100 during the injection operation may be lower than the tip position of the needle 41 inserted into the container 100 during the drilling operation. That is, as long as the through hole 121 can be formed in the seal member 120 during the drilling operation, the insertion amount of the needle 41 into the container 100 may be smaller than that during the injection operation.

Thereafter, as shown in FIG. 3D, the injection control unit 51 drives the pump 43 to inject the liquid into the container 100 through the needle 41. In this example, about 500 μl of a diluent corresponding to about ¼ of the volume is injected into a container 100 having a volume of about 2 ml. When the liquid is injected into the container 100, the space in the container 100 is reduced by the amount of the injected liquid. However, as shown by an arrow A1 in FIG. Can escape into the atmosphere.

Thereafter, the injection control unit 51 moves the needle 41 upward by the moving mechanism 42 to remove the needle 41 from the container 100. At this time, in the present embodiment, before the tip of the needle 41 is completely removed from the container 100, the movement of the needle 41 is temporarily stopped as shown in FIG. 3E (step S106). In this state, the tip of the needle 41 is not in the liquid in the container 100 but is located in the space in the container 100 (the space above the liquid).

Then, when the pump 43 is driven in this state, the air in the container 100 is sucked into the needle 41 as shown by the arrow A2 in FIG. 3E (step S107). Thereby, the air in the container 100 can be released not only from the through hole 121 but also from the needle 41.

Thereafter, as shown in FIG. 3F, the injection control unit 51 moves the needle 41 upward again by the moving mechanism 42, whereby the needle 41 is completely removed from the container 100 (step S108). At this time, a through hole 122 is newly formed in the seal member 120 at a position different from the through hole 121 formed during the drilling operation.

4). Operation and Effect (1) In this embodiment, before the liquid is injected by inserting the needle 41 into the container 100 in which the sealing member 120 is attached to the opening 110, as shown in FIGS. 3A and 3B, the sealing is performed. A through hole 121 is formed in the member 120. 3D, when the liquid is injected into the container 100, the air in the container 100 can be released into the atmosphere from the through-hole 121 formed in the seal member 120 in advance. It is possible to prevent the internal pressure from increasing. Therefore, even when the liquid is highly volatile, the liquid injected into the container 100 is prevented from jumping out when the needle 41 is removed from the container 100 after the liquid is injected as shown in FIG. 3F. can do.

(2) In particular, in the present embodiment, as shown in FIGS. 3A and 3B, after the through hole 121 is formed in the seal member 120 by inserting and removing the needle 41 from the container 100, 3C, the needle 41 is inserted again into the container 100, and liquid is injected into the container 100 through the needle 41 as shown in FIG. 3D. That is, the through hole 121 can be formed in the seal member 120 using the needle 41 for injecting the liquid into the container 100. Thereby, it is not necessary to separately provide a member for forming the through hole 121 in the seal member 120, and the through hole 121 can be formed in the seal member 120 with a simple configuration.

(3) In this embodiment, the operation of inserting and removing the needle 41 as shown in FIGS. 3A and 3B into and out of the container 100 is repeated a plurality of times, so that the through hole 121 is formed in the seal member 120. It is formed. When the position accuracy of the needle 41 varies due to the needle 41 being slender and easily bent as in this embodiment, the needle 41 penetrates different positions in the seal member 120 a plurality of times. Thus, a plurality of through holes 121 are formed. 3D, when the liquid is injected into the container 100, the air in the container 100 can be easily released into the atmosphere from the plurality of through holes 121 formed in advance in the seal member 120. Therefore, it is possible to effectively prevent the pressure in the container 100 from increasing.

(4) Moreover, in this embodiment, after the through-hole 121 is formed in the seal member 120 by inserting and withdrawing the needle 41 from the container 100 at a specific position (injection position) in the horizontal direction, The liquid is injected into the container 100 through the needle 41 without moving the needle 41 in the horizontal direction. Thereby, the operation for forming the through hole 121 in the seal member 120 is simplified, and the time until the liquid injection is completed can be shortened.

5. Modified Example Similarly to the above embodiment, even when the operation of inserting and removing the needle 41 from and into the container 100 is repeated a plurality of times at a specific position (injection position) in the horizontal direction, the position of the needle 41 If the accuracy is high, the needle 41 penetrates the same position in the seal member 120 a plurality of times. Even in such a case, since the drilling operation is repeated a plurality of times, a larger through-hole 121 is formed. Therefore, when the liquid is injected into the container 100, the air in the container 100 can be easily released into the atmosphere from the through-hole 121 formed in the seal member 120 in advance, so that the pressure in the container 100 increases. Can be effectively prevented.

However, when the needle 41 is moved horizontally along the axis L after the needle 41 is moved horizontally to a position different from the injection position, it does not penetrate the seal member 120. The structure which forms the hole 121 may be sufficient.

In the above embodiment, a configuration has been described in which a series of drilling operations as shown in FIGS. 3A and 3B are repeated a plurality of times. However, the configuration is not limited to such a configuration, and a configuration in which the punching operation is performed only once may be used.

In the above-described embodiment, the configuration in which the through hole 121 is formed in the seal member 120 using the needle 41 after the liquid is sucked into the needle 41 at the suction position has been described. However, the present invention is not limited thereto, and the liquid may be sucked into the needle 41 at the suction position after the through hole 121 is formed in the seal member 120 using the needle 41.

The operations shown in steps S106 and 107 in FIGS. 3E and 4 can be omitted. In other words, the configuration may be such that after the liquid is injected into the container 100 through the needle 41, the needle 41 is removed from the container 100 without stopping.

The drilling operation may be performed using a member different from the needle 41 used for the injection operation. Further, the liquid injection destination from the needle 41 is not limited to the empty container 101. The injection apparatus according to the present invention is not limited to a gas chromatograph or a liquid chromatograph autosampler, but can be applied to other analysis apparatuses such as a liquid injection mechanism of an automatic pretreatment apparatus.

DESCRIPTION OF SYMBOLS 1 Injection apparatus 2 Container accommodating part 3 Container holding part 4 Injection mechanism 5 Control part 41 Needle 42 Moving mechanism 43 Pump 51 Injection control part 52 Punch control part 100-103 Container 110 Opening part 120 Seal member 121 Through-hole 122 Through-hole

Claims

A drilling step of forming a through hole in a seal member attached to the opening of the container;
After the drilling step, an injection step of inserting a needle into the container so as to penetrate the seal member, injecting a liquid into the container through the needle, and then withdrawing the needle from the container An injection method comprising:
In the drilling step, the needle is inserted into the container so as to penetrate the seal member, and then the needle is removed from the container to form a through hole in the seal member. The injection method according to claim 1.
3. The injection method according to claim 2, wherein, in the perforating step, the operation of inserting and withdrawing the needle from and into the container is repeated a plurality of times.
In the drilling step, after the needle is moved to a specific position in the horizontal direction, the needle is moved along the axis to be inserted into and removed from the container,
The injection method according to claim 2 or 3, wherein, in the injection step, the needle is moved along an axis while maintaining the needle at the specific position in a horizontal direction.
A container holding unit for holding a container having a seal member attached to the opening;
An injection mechanism having a needle and a moving mechanism for moving the needle, and injecting a liquid into the container via the needle;
By moving the needle with the moving mechanism, the needle is inserted into the container so as to penetrate the seal member, and after injecting liquid into the container through the needle, the needle is inserted into the container from the container. An injection controller for removing the needle;
An injection apparatus comprising: a perforation control unit that forms a through hole in the seal member before the needle is inserted into the container by the injection control unit.
The perforation control unit moves the needle with the moving mechanism, thereby inserting the needle into the container so as to penetrate the seal member, and then removing the needle from the container. The injection device according to claim 5, wherein a through hole is formed in the seal member.
The injection device according to claim 6, wherein the perforation control unit repeats the operation of inserting and withdrawing the needle into and from the container a plurality of times.
The perforation control unit moves the needle along the axis at a specific position in the horizontal direction, thereby inserting and withdrawing the needle from and into the container,
The injection device according to claim 6 or 7, wherein the injection control unit moves the needle along an axis while maintaining the needle at the specific position in a horizontal direction.