JP3844053B2 - Liquid passage device for liquid sample measurement - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a liquid passing device that constitutes a sample introduction unit in various measuring instruments used for liquid component detection, concentration measurement, and the like, including liquid chromatography and flow injection devices.
[0002]
[Prior art]
In general, in liquid chromatography, flow injection devices, etc., a liquid sample is quantified by introducing it from a sample supply port through an introduction channel to a metering valve, and the quantified liquid sample is separated by switching the channel of the metering valve. A method is often used in which a specific component is detected through a required separation or reaction process in the measurement system together with the carrier liquid from the transfer channel. The remainder of the liquid sample that has become surplus by quantification by the metering valve is discharged through a discharge channel located on the extension of the introduction channel via the metering valve. Generally, a suction pump is provided in the discharge channel. The liquid sample is drawn into the metering valve and the remaining part is sucked and discharged by the suction force.
[0003]
However, if the liquid sample contains contaminants or insoluble substances, or contains substances that become insoluble over time under the measurement conditions, these contaminants and insoluble substances are likely to adhere to the introduction path, and these redissolved substances are dissolved again. Or the composition of the liquid sample used for the next measurement changes due to re-dispersion, or the amount of the liquid sample used for the measurement fluctuates due to the obstruction of the flow due to accumulated insoluble matter or the volume change of the quantitative valve, The reliability of the measured value is impaired, and when the adhesion is significant, there is a problem that the introduction path is blocked and measurement is impossible. Therefore, as a means for coping with these problems, conventionally, when a liquid sample containing a contaminant or insoluble matter is to be measured, before the insoluble matter in the liquid sample is removed by filter filtration or centrifugation in advance. In general, a method is used in which treatment is performed and measurement is interrupted at a stage where a contaminant or insoluble matter adheres to each site to some extent and the deposit is removed.
[0004]
[Problems to be solved by the invention]
However, the pretreatment method such as filter filtration or centrifugation described above is excellent in that it removes the problematic factors in advance, but the work process is increased and the operation becomes complicated, and a small amount of It is difficult to apply to samples and is not effective for components that become insoluble during measurement. On the other hand, the method of removing contaminants and insoluble substances when they have adhered to a certain extent is also complicated in operation and requires constant monitoring of the degree of adhesion, and it is efficient to interrupt the measurement at each removal operation. As a result, there is a hindrance to continuous and quick measurement, and maintenance personnel must be secured, leading to an increase in measurement cost.
[0005]
In the present invention, in view of the above situation, even when a liquid sample containing a pollutant and an insoluble material is used as a measurement target as a liquid sample measuring device, the contaminant and the insoluble material are attached to the introduction path. Accumulation can be effectively suppressed, high reliability and accuracy can be measured, and there is no need for special preprocessing or complicated work operations. The purpose is to provide something that requires less burden.
[0006]
[Means for Solving the Problems]
  In order to achieve the above object, a liquid sample measuring device according to claim 1 of the present invention is provided with a reference numeral in the drawing, and the liquid sample S is supplied from the sample supply port 1.As a liquid column sandwiched between the front and rear air layers AIn the liquid passing device that flows into the metering valve 3 through the introduction channel 2 and sends a fixed amount of the liquid sample S1 in the valve 3 to the measuring system M by switching the channel of the metering valve 3, the liquid sample S Contrary to the introduction path, there is provided a reverse feeding means P1 for sending the liquid to the sample supply port 1 through the metering valve 3 and the introduction flow path 2.And this reverse feed meansP1As a result, the liquid head side and the remaining portion S2 of the liquid column that have not been supplied to the sample measurement system are fed back, and the cleaning liquid W is sent out to the sample supply port 1 through the quantitative valve 3 and the introduction flow path 2. Not configured asIt is characterized by that.
[0007]
  As a preferred embodiment of the liquid sample measuring device according to claim 1, in the invention of claim 2, a suction / discharge port 4 is provided in the vicinity of the sample supply port 1, and the reverse feeding means. A configuration having suction / discharge means P2 for discharging the liquid fed back by P1 from the suction / discharge port 4 is adopted..
[0008]
  Further claims3The invention of claim 12In the liquid sample measuring apparatus, the sample supply port 1 and the suction / discharge port 2 are provided in the vicinity of the bottom of the recess 5 that opens upward, and the cleaning liquid W that has been fed back by the back feeding means P1 is A configuration is adopted in which a liquid pool is formed in the recess 5 and is set to be discharged from the suction / discharge port 4. Further claims4The invention of claim 1 to claim 13In the liquid sample measuring device, the reverse feeding means P1 is a reversible pump that also serves as a sample suction means that sucks the liquid sample S introduced from the sample supply port 1 and draws it into the metering valve 3. It is supposed to be.
[0009]
DETAILED DESCRIPTION OF THE INVENTION
As described above, the present invention allows a liquid sample to flow into the metering valve from the sample supply port via the introduction channel, and by switching the channel of the metering valve, a certain amount of liquid sample in the valve is measured. Contrary to the liquid sample introduction path, the liquid flow apparatus is provided with a reverse feeding means for feeding the liquid to the sample supply port through the metering valve and the introduction flow path.
[0010]
In such a liquid flow device, the liquid head of the liquid sample introduced from the sample supply port exceeds the inside of the quantitative valve, reaches the inside of the flow path on the extension through the valve of the introduction passage, By switching the flow path of the quantitative valve, only the amount in the valve is transferred to another transfer flow path toward the measurement system, so that the surplus of quantitative flow flows as the remainder on the liquid head side and the tail side of the original liquid column. Remain on the road. Conventionally, the remaining part of the liquid sample is discharged from the flow path on the extension of the introduction passage by switching the flow path of the quantitative valve after sending a certain amount of liquid sample to the measurement system. In the case of liquid samples containing substances and insoluble substances, contaminants and insoluble substances remain on the introduction passage and the inner wall of the metering valve, and these remain dry until the next liquid sample to be measured is supplied. A hard solidified layer will be formed.
[0011]
However, in the liquid flow device of the present invention, after a fixed amount of the liquid sample is sent to the measurement system, the reverse flow unit is operated together with the switching of the flow path of the quantitative valve, whereby the remaining portion of the liquid sample is removed from the quantitative valve and the introduction flow. It can be sent back to the sample supply port through the path and discharged from the sample supply port side. Then, by reverse feeding of the remaining portion of the liquid sample, the contaminants and insoluble matter adhering to the introduction passage and the inner wall surface of the metering valve come into contact with the remaining liquid sample again before being hardened and solidified. It is re-dissolved or re-dispersed and discharged together with the remaining portion, thereby suppressing adhesion residue on the introduction path.
[0012]
Such a reverse feeding means is not particularly limited, but preferably uses pumps such as a tube pump, a syringe pump, a plunger pump, etc., and pressurizes from the downstream side of the introduction path or from the sample supply port side. What is necessary is just to set so that the remainder of the said liquid sample may be sent back by suction. If a tube pump, syringe pump, or the like used for the reverse feeding means by pressure from the downstream side of the introduction path is made to be a reversible specification, the liquid sample introduced from the sample supply port is sucked together with the function of the reverse feeding means. Thus, it can also serve as a sample suction means for drawing into the metering valve.
[0013]
Further, in this reverse feeding means, in addition to the reverse feeding of the remaining portion of the liquid sample, it is recommended that the cleaning liquid is fed into the introduction path from the downstream side (back feeding) by the pump or the like. That is, among the contaminants and insoluble matter adhering to the inner wall surface of the introduction passage and the metering valve, the portion that could not be transferred into the remaining liquid sample to be fed back is brought into contact with the cleaning liquid. Therefore, it is possible to more reliably prevent adhesion and adhesion to the introduction path. Thus, the cleaning liquid may be sent (reversely fed) simultaneously with the reverse feeding of the remaining portion of the liquid sample, or separately after the reverse feeding of the remaining portion of the liquid sample is completed. For simultaneous liquid feeding, for example, the suction pipe of the pump is connected to a cleaning liquid tank, the cleaning liquid is sucked by the operation of the pump and sent to the introduction path, and the pressure causes the remainder of the liquid sample in the path to advance. It can be set so that the sample is fed to the sample supply port side.
[0014]
Such a cleaning liquid is preferably a liquid component that is the same or similar to the liquid medium of the liquid sample to be measured, but is not limited thereto, and has good solubility and dispersibility in the contaminants and insoluble materials, and Any liquid component that does not adversely affect the measurement can be used without any particular limitation. In addition, if necessary, the cleaning liquid may contain a component that helps dissolve and disperse the contaminants and insoluble matter, such as a surfactant.
[0015]
On the other hand, the remainder of the liquid sample fed back to the sample supply port side and the discharge of the cleaning liquid may be performed manually using a pipette, a dropper, etc., but a suction discharge port is provided near the sample supply port, A configuration in which the suction and discharge is automatically performed by suction and discharge means such as a suction pump through a pipe from the suction and discharge port is preferable. Thus, since contaminants and insoluble matter in the liquid sample may adhere to the vicinity of the sample supply port, more preferably, it is provided near the bottom of the recess that opens the sample supply port and the suction / discharge port upward, A configuration is recommended in which the cleaning liquid that has been sent back forms a liquid pool in the recess, and is then discharged and removed from the suction outlet. The position of the suction / discharge port is not particularly limited. However, if the suction / discharge port is set at the same height as the sample supply port or slightly higher, it is easy to perform suction and discharge of the liquid that has been sent back to the sample supply port.
[0016]
In order to form the cleaning liquid pool in the recess as described above, it is only necessary to set a transport speed difference or an operating time difference between the reverse feeding means and the suction / discharge means. That is, if the discharge speed by the suction discharge means is made smaller than the reverse speed by the reverse feed means, a liquid pool is generated in the recess due to the difference in the transport speed. Alternatively, the operation of the suction / discharge means may be delayed with respect to the reverse feeding means, and the suction / discharge may be performed after the cleaning liquid has accumulated in the recess. In the initial stage of reverse feeding, where the remaining portion of the liquid sample is sent to the sample supply port, in order to reduce the contamination of the recess by the liquid sample, the suction is performed against the reverse feeding speed by the reverse feeding means, contrary to the above. It is desirable to set a large discharging speed by the discharging means.
[0017]
The liquid sample is introduced into the sample supply port by storing the liquid sample in the recess using a liquid dropping tool such as a pipette or a dropper, or by supplying the sample at the lower end of a tube body such as a capillary tube holding the liquid sample. What is necessary is just to make it fit to an opening | mouth and to draw in to a fixed quantity valve | bulb by sample suction means, such as the said pump. When the liquid sample is filled in the quantitative valve, this is detected by an appropriate detection means such as a liquid identification sensor based on the transmitted light intensity, and the sample suction means is stopped based on the detection signal. A certain amount of liquid sample is sent to the measurement system by switching the flow path. The flow control of the metering valve after the liquid feeding to the measurement system and the operation control of the reverse feeding means and the suction / discharge means may be performed by the timer setting input to the control device in advance.
[0018]
As the constant volume valve, those generally used for liquid chromatography, flow injection devices, etc. can be used, and the type thereof is not particularly limited. In addition, the material of the constituent members such as the sample supply port, the suction / discharge port, and the introduction flow path is not particularly limited. However, since metal may cause corrosion depending on the type of liquid sample, for example, silicon rubber, vinyl chloride resin, polyolefin Synthetic resins such as fluororesins and fluororesins are preferred. Of these, fluororesins, polypropylene, and polyethylene are recommended because of their excellent chemical resistance. In particular, fluororesins and polypropylene have the advantage of being capable of autoclaving.
[0019]
Next, a liquid sample measuring device for measuring a liquid sample according to an embodiment of the present invention will be specifically described with reference to the drawings. Needless to say, the liquid passing device of the present invention is not limited to this embodiment.
[0020]
In FIG. 1, reference numeral 10 denotes a liquid chromatography sample injection portion, which is opened at the bottom of a recess 5 that opens upward in a trumpet shape, with a sample supply port 1 opened at the center, and at a slightly higher side. And a suction discharge port 4. An introduction flow path 2 extending in the vertical direction is connected between the sample supply port 1 and the metering valve 3 disposed below, and the sample suction means is disposed on the extension of the introduction flow path 2 via the metering valve 3. A cleaning liquid supply path 6 connected to the cleaning liquid tank T1 is provided via a reversible syringe pump P1 serving as a reverse feeding means. The suction / discharge port 4 is provided with a suction / discharge path 7 connected to the waste liquid tank T2 via a syringe pump P2 serving as a suction / discharge means.
[0021]
The metering valve 3 is connected to a transfer channel 8 that is oblique to the vertical channel composed of the introduction channel 2 and the cleaning liquid supply channel 6, and the former vertical channel is driven by the rotation of the metering valve 3. The connection state of the latter and the connection state of the latter transfer channel 8 are set to switch to the connection state of only the transfer channel 8. The lower side of the transfer channel 8 is connected to a measurement system (not shown), and the carrier liquid C is constantly flowing toward the measurement system. In addition, a liquid identification sensor 9 for detecting the presence or absence of the liquid sample S based on the transmitted light intensity is attached in the vicinity of the connection portion of the cleaning liquid supply path 6 to the quantitative valve 3. Reference numeral 20 denotes a capillary tube that supplies the liquid sample S to the sample supply port 1.
[0022]
In the above-described configuration, when necessary measurement such as the component concentration of the liquid sample S is performed, first, as shown in FIG. 2A, the capillary tube 20 holding the liquid sample S with the pumps P1 and P2 stopped. Is inserted into the sample supply port 1 at the bottom of the recess 5. At this time, the metering valve 3 is in a position where the vertical flow path connecting the introduction flow path 2 and the cleaning liquid supply path 6 communicates and the transfer flow path 8 communicates. Then, when the pump P1 operates in the suction direction, the liquid sample S flows from the sample supply port 1 into the introduction flow path 2 as shown in FIG. 2B, and flows as shown in FIG. 2C. It is drawn into the metering valve 3. In the state before the start of the injection of the liquid sample S, the cleaning liquid W fed back during the previous measurement remains to a position slightly exceeding the metering valve 3 as shown in FIG. By the operation in the suction direction, the liquid sample S is simultaneously returned to the cleaning liquid tank T1 while the air layer A is maintained between the liquid sample S and the liquid head.
[0023]
As shown in FIG. 2 (C), when the liquid head (lower end) of the introduced liquid sample S passes through the metering valve 3 and enters the cleaning liquid supply path 6, this is detected by the liquid identification sensor 9. Based on the detected signal, the pump P1 is stopped and the metering valve 3 is operated to switch the flow path, and a fixed amount of the liquid sample S1 in the metering valve 3 is communicated as shown in FIG. It is pushed by the carrier liquid C in the transfer channel 8 and flows into the transfer channel 8 as shown in FIG. 2E, and is sent to the measurement system. At this time, as shown in FIG. 2 (E), the remaining liquid sample S2 remains in the introduction channel 2 and the portion near the metering valve 3 of the cleaning liquid supply channel 6, and the blocked flow in the metering valve 3 is blocked. The carrier liquid C remains in the road space.
[0024]
  Next, with a predetermined time lag from the transfer of the liquid sample S1 to the transfer channel 8, FIG.F) And the flow path is switched again, and the pump P1 rotates in the reverse direction to operate in the pressurizing direction, and at the same time, the pump P2 of the suction / discharge means operates. As a result, the remaining liquid sample S2 remaining in the introduction flow path 2 and the cleaning liquid supply path 6 isAs shown in Fig. 2 (G)It is sent back together with the carrier liquid C in the metering valve 3 and sent out to the sample supply port 1 through the introduction flow path 2. At the initial stage of this reverse sending, the suction speed by the pump P2 is reversed by the pump P1. Since it is set to be larger than the feeding speed, as shown in FIG. 2 (H), it flows into the suction discharge port 4 without causing a liquid pool in the recess 5, and is discharged to the waste liquid tank T2 through the suction discharge port 7. .
[0025]
  In the above reverse feeding process, the cleaning liquid W in the cleaning liquid tank T1 is sucked up by the pump P1, and the introduction channel 2 and the cleaning liquid supply are simultaneously performed while the air layer A is maintained between the preceding liquid sample S2. The vertical flow path connecting the paths 6 is fed back upward. Thus, at the stage where all of the preceding remaining liquid sample S2 is discharged from the suction discharge port 4, the suction speed by the pump P2 becomes smaller than the reverse feed speed by the pump P1, and this difference in transport speed causes the difference in FIG.)As shown, the cleaning liquid W is discharged from the suction outlet 4 while forming a liquid pool in the recess 5.
[0026]
  AndAs shown in Fig. 2 (J)A predetermined amount of the cleaning liquid W is discharged from the suction discharge port 4.AndAmplifier P1 stops andInWhen the pump P2 is stopped, the pump P1 operates in the suction direction, and the cleaning liquid W that has reached the sample supply port 1 is removed.As shown in Fig. 2 (K)When the liquid head (upper end) is pulled back to a position slightly higher than the metering valve 3, the pump P1 is stopped and enters a standby state for the next measurement.
[0027]
According to the above configuration, the contaminants and insoluble matter adhering to the inner wall surface of the introduction passage 2 and the metering valve 3 are returned to the remaining liquid sample S2 again before being hardened by the reverse feeding of the remaining liquid sample S2. Contaminants and insoluble matters that have contacted, re-dissolved or re-dispersed in the liquid, discharged together with the remaining portion S2, and then could not be transferred into the remaining liquid sample S2 by the cleaning liquid W fed back. Since the cleaning liquid W is dissolved or dispersed in the liquid and discharged and removed, adhesion and adhesion to the introduction path is reliably prevented. In addition, the difference in transport speed between the pumps P1 and P2 is changed in the reverse feeding process, and the remaining liquid sample S2 is sucked and discharged without causing a liquid pool in the recess 5, and then the cleaning liquid W that is fed backward is the recess 5 Therefore, the remaining liquid sample S2 is prevented from being contaminated by the remaining liquid sample S2 in the vicinity of the sample supply port 1, and the cleaning liquid W is pooled even if there is some contamination. Thus, it is surely removed by re-dissolution or re-dispersion.
[0028]
Therefore, according to this liquid passing device, as in the prior art, pretreatment for removing insoluble matters in the liquid sample is performed in advance by filtering or centrifuging, or contaminants and insoluble matters are adhered to each part to some extent. There is no need to perform complicated work operations such as interrupting measurement and removing deposits at the stage, and highly reliable and accurate measurement can be performed very efficiently. On the other hand, in the configuration of the above embodiment, the pump P1 has a reversible specification, and the liquid sample S introduced from the sample supply port 1 is quantified by sucking the liquid sample S introduced from the sample supply port 1 along with the function as a means for reversely feeding the remaining liquid sample S2 and the cleaning liquid W. Since the function as the sample aspirating means for drawing into the valve 3 is also used, the overall apparatus configuration is very simple and functionally integrated, and the equipment cost burden as a liquid passing apparatus can be reduced.
[0029]
The configuration of the sample injection unit 10 is not particularly limited, but for example, a unit type as shown in FIGS. 3 and 4 is preferable. That is, the sample injection portion 10 shown in FIGS. 3 and 4 includes a port union 11, a port 12, a port nut 13, a fixing nut 14, and a packing 15, and a mounting frame recessed in a circular shape on the liquid chromatography main body side. A unit that can be easily attached to and detached from the unit 21 is configured. As for the material of these constituent members, the packing 15 is made of silicon rubber, but the other members 11 to 14 are all made of fluororesin or polypropylene.
[0030]
As shown in FIGS. 5A to 5C, the port union 11 has a stepped portion between a large-diameter upper half portion 11a and a small-diameter lower half portion 11b. 11c, an injection hole 24 along the axial center and a discharge hole 25 at an eccentric position are vertically penetrated. A circular recess 26 and a circular small recess 27 concentrically provided on the bottom surface are provided on the upper surface. In addition, pipe connection screw holes 24 a and 25 a for the injection hole 24 and the discharge hole 25 are opened on the lower surface. As shown in FIG. 5C, the lower half portion 11b of the port union 11 has a shape obtained by cutting a part of a circle along the tangential direction.
[0031]
As shown in FIGS. 6A to 6C, the port 12 is a member constituting the recess 5 that opens upward in a trumpet shape. In addition to having a circumferential groove 12b into which the O-ring 16 is fitted, a channel groove 28 extending in the radial direction from the bottom hole 5a of the recess 5 is formed in the circular bulging portion 12c on the lower surface. The lower end of the port 12 is liquid-tightly fitted to the circular recess 26 of the port union 11 via the O-ring 16, and the flow channel 28 is formed in the discharge hole 25 of the port union 11 in this fitted state. It comes to communicate.
[0032]
In addition, the packing 15 has a circular thick plate shape, and has a center hole 15a constituting the sample supply port 1, and the upper side of the center hole 15a is formed to have a large diameter. By fitting into the recess 27, the center hole 15 a communicates concentrically with the bottom hole 5 a of the recess 5 of the port 12 and the injection hole 24 of the port union 11. Then, as shown by the phantom line in FIG. 3, when the tip of the capillary tube 20 is inserted into the center hole 15a, the upper side of the center hole 15a is held in the capillary so that the tip can be tightened and held liquid-tight by its own elasticity. The diameter is set slightly smaller than that of the tube 20.
[0033]
As shown in FIG. 3, the port nut 13 includes a female screw 22 b corresponding to the male screw 22 a of the upper half portion 11 a of the port union 11, and has a pressing flange portion 13 a on the inner peripheral upper edge. Further, by screwing and tightening to the port union 11 in which the packing 15 is fitted, the pressing flange portion 13a is pressed against the flange portion 12a of the port 12 to prevent the port 12 from coming off. The fixing nut 14 includes a female screw 23 b corresponding to the male screw 23 a of the lower half portion 11 b of the port union 11.
[0034]
In order to attach the unit of the sample injection unit 10 to the liquid chromatography body, the lower half portion 11b of the port union 11 with the port nut 13 screwed to the port union 11 fitted with the port 12 and the packing 15 is screwed. Is inserted into the holding hole 21a of the mounting frame 21 from above, locked to the periphery of the holding hole 21a by the step portion 11c, and the fixing nut 14 is screwed into the lower half portion 11b from below and tightened. What is necessary is just to clamp the periphery of the holding hole 21a between the part 11c and the nut 14 for fixation. In addition, the shape of the holding hole 21a of the mounting frame 21 corresponds to a shape in which a circular part of the lower half portion 11b of the port union 11 is cut away, so that the port union 11 to be inserted is oriented in a certain direction. In addition, the rotation of the port union 11 is prevented when the fixing nut 14 is screwed.
[0035]
In such a unit configuration, it can be easily removed from and attached to the main body of a measuring apparatus such as liquid chromatography for periodic cleaning, inspection, member replacement, etc. Therefore, there is an advantage that it is possible to surely clean every corner, and it is only necessary to replace a member that has been damaged or deteriorated, thereby reducing maintenance and inspection costs.
[0036]
【The invention's effect】
  According to the first aspect of the present invention, after a certain amount of liquid sample is sent to the measurement system as a liquid passing device that constitutes a sample introduction part in various measuring instruments used for component detection, concentration measurement, etc. of the liquid sample, quantitative determination is performed. Operate the reverse feed means along with the switching of the valve flow path,Not sent to measurement systemThe rest of the liquid sampleWith reverse feed of cleaning liquidIs sent to the sample supply port through the metering valve and the introduction channel.OutDischarge from the sample supply port side.RukaTherefore, even if the liquid sample to be measured contains pollutants and insoluble substances, it is possible to effectively suppress the accumulation of these pollutants and insoluble substances on the introduction path, thereby achieving high reliability and accuracy. Measurement ofThe That is, the contaminants and insoluble matter adhering to the introduction passage and the inner wall surface of the metering valve are brought into contact with the remaining liquid sample again before being hardened and solidified and re-dissolved or re-dispersed in the liquid. In addition to being discharged together with the remainder, the contaminants and insoluble matter that could not be dissolved or dispersed in the remainder of the liquid sample, as well as contamination caused by the remainder of the liquid sample, are dissolved or dispersed in the cleaning liquid. Can be removed reliably.Moreover,There is provided an apparatus capable of performing measurement efficiently without requiring any special pretreatment or complicated work operation, and having a simple apparatus configuration and less equipment burden.
[0037]
According to the second aspect of the present invention, there is provided the liquid passing device capable of efficiently discharging and removing the liquid fed back by the back feeding means from the suction outlet.
[0039]
  Claim3According to the invention, in the liquid passing device described above, the sample supply port and the suction / discharge port are provided in the vicinity of the bottom of the recess that opens upward, and due to a difference in transport speed or an operation time difference between the reverse feeding unit and the suction / discharge unit. Since the cleaning liquid fed back by the back feeding means is set to be discharged from the suction discharge port after forming a liquid pool in the recess, contamination by the remaining liquid sample in the vicinity of the sample supply port Is suppressed, and even if there is some contamination, it is reliably removed by re-dissolving or re-dispersing in the cleaning liquid pool.
[0040]
  Claim4According to the invention, the liquid passing device includes the reversible pump that also serves as the sample suction unit that sucks the liquid sample introduced from the sample supply port by the reverse feeding unit and draws it into the metering valve. However, it is very simple and functionally organized, so that the equipment cost burden can be reduced.
[Brief description of the drawings]
FIG. 1 is a schematic view schematically showing a liquid passing device for measuring a liquid sample according to an embodiment of the present invention.
FIG. 2 is a schematic view showing the liquid passing operation by the liquid passing device in order of steps (A) to (L).
FIG. 3 is a longitudinal sectional view showing a configuration example of a sample injection unit of the liquid passing device.
FIG. 4 is a partially longitudinal front view showing the sample injection part in an exploded manner.
FIGS. 5A and 5B show a port union of the sample injection section, where FIG. 5A is a plan view, FIG. 5B is a longitudinal sectional view, and FIG. 5C is a bottom view.
6A and 6B show a port of the sample injection section, where FIG. 6A is a plan view, FIG. 6B is a longitudinal sectional view, and FIG. 6C is a bottom view.
[Explanation of symbols]
1 Sample supply port
2 Introduction channel
3 Metering valve
4 suction outlet
5 recess
6 Cleaning liquid supply path
7 Suction discharge path
8 Transfer channel
9 Liquid identification sensor
10 Sample injection part
S liquid sample
S1 A certain amount of liquid sample
S2 The remaining liquid sample
P1 Syringe pump (reversible pump that serves both as a reverse feed means and a sample suction means)
P2 Syringe pump (suction / discharge means)
T1 cleaning liquid tank
T2 Waste liquid tank
W Cleaning solution

Claims (4)

The liquid sample is introduced into the metering valve through the introduction channel as a liquid column sandwiched between the air layers before and after the sample supply port, and a certain amount of liquid sample in the valve is measured by switching the channel of this metering valve In the liquid passing device to send to the system
Wherein the liquid as opposed to the introduction path of the liquid sample have a backhaul means feeding through metering valve and the introduction channel to the sample-supplying port,
With this reverse feeding means, the liquid head side and the remainder on the tail side of the liquid column that have not been fed to the sample measurement system are fed back, and the cleaning liquid is sent to the sample supply port through the quantitative valve and the introduction channel. liquid passage device for a liquid sample measurement ing is configured.   The liquid sample measurement passage according to claim 1, further comprising a suction / discharge port provided in the vicinity of the sample supply port, and having a suction / discharge unit for discharging the liquid fed back by the back-feeding unit from the suction / discharge port. Liquid device. The sample supply port and the suction / discharge port are provided in the vicinity of the bottom of the recess that opens upward, and the cleaning liquid that has been fed back by the reverse feeding means forms a liquid reservoir in the recess and is discharged from the suction / discharge port. The liquid passing device for liquid sample measurement according to claim 2, which is set as described above. 4. The liquid sample measuring passage according to claim 1, wherein the reverse feeding unit includes a reversible pump that also serves as a sample suction unit that sucks a liquid sample introduced from a sample supply port and draws the liquid sample into a quantitative valve. Liquid device.

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