JPH04204155A - Sample injecting apparatus - Google Patents

Abstract

PURPOSE:To make it possible to inject the same sample into two measuring systems at the same time by one injecting operation by rotating a rotor by a specified angle, and switching the internal flow paths. CONSTITUTION:Under the state wherein an apparatus is turned OFF, the liquid in the first moving phase which is introduced through an introducing flow path C for liquid to be measured is discharged from a moving-phase lead-out flow path D. At the same time, the second moving phase which is introduced from a moving-phase introducing flow path E is discharged from a moving-phase lead-out flow path F. Liquid to be measured which is introduced from an introducing flow path A for the liquid to be measured is discharged from a sample lead-out flow path B. At the same time, the other flow is discharged from the flow path B. In this way, measuring pipes 74 and 75 are filled with the liquid to be measured. When a rotor is rotated by 45 degrees in the direction of a thick arrow, the first moving phase which is introduced through the flow path C is discharged through the flow path D and sent into the first measuring system. The second moving phase from the flow path E is discharged from the flow path F. In this way, two sample groups are filled by the first operation, and the same sample can be injected into two measuring systems at the same time.

Description

Detailed Description of the Invention <Industrial Application Field> The present invention is installed in a liquid chromatograph or an ion chromatograph, and injects two components with different physical properties into two chromatographs at the same time in one injection operation. The present invention relates to a sample injection device that enables measurement in two separation modes.

<Prior Art> FIG. 4 is an explanatory diagram of the configuration of an ion chromatograph equipped with such a sample injection device. In this diagram,
1a is a tank in which a mobile phase made of, for example, a carbonate solvent is stored;
1b is a cypress in which a scavenger liquid is stored; 2a and 2b are liquid pumps; 3 is a sample injection device; 4 is a separation column filled with, for example, an anion exchange resin with a low ion exchange capacity; 5 is, for example, an ion exchange membrane 5a The suppressor has an interior divided into an inner chamber 5b and an outer chamber 5C, and 6 is a detector, for example, a conductivity detector.

In the ion chromatograph having the configuration as shown in FIG. 4, initially, the sample injection device 3 is off and its internal flow path is connected with the broken line. Furthermore, when the pump 2a is driven, the mobile phase in the tank la flows from the first boat 3a to the second port 3b of the sample injection device 3 to the separation column 4 to the inner chamber 5b of the suppressor 5 to the detector 6 to the discharge port ( (not shown).

Further, when the pump 2b is driven, the scavenger liquid in the tank 1b is discharged from an outlet (not shown) through the outer chamber 5b of the suppressor 5. Therefore, the cations contained in the mobile phase flowing in the inner chamber 5b are ion-exchanged via the ion exchange membrane 5a, and the conductivity background of the eluent is reduced.

On the other hand, when the sample to be measured is injected from the fourth boat 3d of the sample injection device 3 using the syringe 3h, the sample is transferred from the fourth boat 3d of the sample injection device 3 to the groove 31” to the third boat 3.
C → Measuring tube 3g → 6th port 3f → Flows through the groove 3m-, filling the measuring tube 3g. In this state, the sample injection device 3 is turned on and its internal flow path is switched to the solid line connection state. Then, the sample to be measured in the measuring tube 3g is transported by the mobile phase to the separation column 4, where it is separated into chromatography columns. The sample to be measured thus separated is detected by the detector 6 via the inner chamber 5b of the suppressor 5.

<Problems to be Solved by the Invention> However, in the conventional example described above, in order to measure components with different properties (for example, an anion and a cation) contained in the same sample, it is necessary to measure only one component. After completing one component, the mobile phase and separation column were changed and the other component was measured.

For this reason, measurement requires a long time, and if the components in the sample are likely to denature or change in composition, this poses a major problem in terms of measurement accuracy and reproducibility.

On the other hand, attempts have also been made to prepare two chromatography apparatuses and inject the same sample into each measurement system for measurement. However, in order to automate the process, it is necessary to prepare two automatic injection devices, and there are also disadvantages in that two samples to be measured must be prepared for the two autosamplers.

The present invention has been made in view of the drawbacks of the conventional example, and an object of the present invention is to provide a sample injection device that can simultaneously inject the same sample into two measurement systems with -1 injection operations. .

Means for Solving the Problems> The present invention is characterized by a sample injection device having a disk-shaped fixed valve seat and a disk-shaped rotor disposed opposite to the fixed valve seat. , first to tenth holes drilled along the circumference of the fixed valve seat, and first holes formed in an arc shape at equal intervals and provided on a surface of the rotor that is in contact with the fixed valve seat. ~ a fourth groove, and a fifth groove formed in an elongated shape in the center of the rotor;
a first metering tube connected to the second hole and the fifth hole and having a constant internal volume; a second metering tube connected to the seventh hole and the tenth hole and having a constant internal volume; a liquid to be measured introduction channel connected to the first hole, a liquid to be measured outlet channel connected to the sixth hole, a first mobile phase introduction channel connected to the fourth hole, and a first mobile phase introduction channel connected to the eighth hole. a second mobile phase introduction channel connected to the hole, a first mobile phase outlet channel connected to the third hole, and a second mobile phase outlet channel connected to the ninth hole; The rotor is rotated by 45 degrees to switch the internal flow path.

Solid line example> The present invention will be described in detail below with reference to the drawings. 1st
The figure is a perspective view of the configuration of an embodiment of the present invention, in which (1) shows a disk-shaped fixed valve seat, and (2) shows a disk-shaped disk-shaped valve made of, for example, ceramic, which is arranged opposite to the fixed valve seat. Showing the rotor. In addition, in FIG. 1, 7a~
7j are the first to tenth holes provided in the fixed valve seat 71;
-7n are first to fourth grooves formed in the shape of a circle provided on the surface of the rotor 72 that is in contact with the fixed valve seat 71;
7r is a fifth groove formed in the center of the rotor 72 in an elongated shape.

FIG. 2 is a diagram for explaining the operation of the embodiment of the present invention, in which (1) shows the state where the sample collection device is on, and (
2) shows the state in which the sample collection device is off. Also,
In FIG. 2, 7 is the fixed valve seat 71 and the rotor 72.
The joint surfaces 74 and 75 each have a constant internal volume. In the second measuring tube, A indicates a flow path for introducing a liquid to be measured, B indicates a flow path for discharging a liquid to be measured, C and E indicate channels for introducing a mobile phase, and D and F indicate channels for discharging a mobile phase.

Initially, the sample introduction device of the embodiment of the present invention is turned off, and the second
The state is shown in Figure (2). In this state, the first mobile phase introduced from the sample liquid introduction flow FIIIC is
It passes through the fourth hole 7d, the groove 71, and the third hole 7c, and is discharged from the mobile phase derivation channel. At the same time, the second mobile phase introduced from the mobile phase introduction channel E is transferred from the eighth hole 7h to the groove 7n to the ninth
It is discharged from the mobile phase deriving channel F through the hole 71. Also,
The liquid to be measured introduced from the liquid to be measured introduction flow path A enters from the first hole 7a and is divided into two streams at the groove 7, and the negative flow is connected to the second hole 7b = first measuring tube 74. →The sample is discharged from the sample outlet B through the fifth hole 7e, the liquid 7m, and the sixth hole 7f. At the same time, the other flow is discharged from the sample outlet channel B via the 10th hole 7j -> the second measuring tube 75 -> the 7th hole 7g -> the 7m - 6th hole 7f. In this way, the metering tube 7
The liquid to be measured is filled at 4.75.

In this state, when the sample introduction device according to the embodiment of the present invention is turned on and rotated by 45 degrees in the direction of the bold line arrow in FIG. 2(2), it becomes the state shown in FIG. 2(1). In this state, the first mobile phase introduced from the measurement liquid introduction channel C is transferred to the fourth hole 7d.
-+ Lecture 7! - 5th hole 7e → 1st measuring tube 74 → 2nd hole 7b
→To the groove 7=Through the third hole 7c, the sample is discharged from the sample outlet channel and sent to the first measurement system. Further, the second mobile phase introduced from the mobile phase introduction channel E is transferred from the 8th hole 7h to the liquid 7m to the 7th hole 7g to the second measuring tube 75 to the 10th hole 7j-+
Spring n → passes through the ninth hole 71 and is discharged from the mobile phase derivation channel F.

In this way, it is possible to fill two sample loops in one operation and inject the same sample into two measurement systems simultaneously.

On the other hand, the liquid to be measured introduction channel A is connected to the mobile phase derivation channel B via the first hole 7a, the first hole 7r, and the sixth hole 7f. Therefore, the liquid to be measured remaining in the liquid to be measured can be washed out with the cleaning liquid when the valve is on (ie, the state shown in FIG. 2(1)).

FIG. 5 is a diagram showing a state in which the embodiment of the present invention is applied to an autosampler. In the figure, the same symbols as in FIG. 2 are used with the same meanings, and the operation of the sample collecting device 73 is It is exactly the same as Figure 2. In addition, lc and ld are sample bottles, 8
9 is a flow path switching valve, and 9 is a syringe. By using an autosampler with such a configuration, samples for two measurement systems can be sampled from one sample bottle in one sampling.

In addition, samples can be injected into two measurement systems by simply switching the sample injection device 7 once.

Note that the present invention is not limited to the above-described embodiments, and can be modified in various ways.

<Effects of the Invention> According to the present invention as described in detail above, a sample injected from one sample injection boat is simultaneously filled into two sample loops, and the same sample is placed in two measurement systems. They can be injected at the same time.

[Brief explanation of the drawing]

Fig. 1 is a perspective view of the structure of the embodiment of the present invention, Fig. 2 is an explanatory diagram of the operation of the embodiment of the present invention, Fig. 3 is an illustration of an example of use of the embodiment of the present invention, and Fig. 4 is an illustration of an example of use of the conventional example. It is a diagram. la, lb...tank, 2a, 2b...liquid pump, 3
... Sample injection device, 4... Separation column, 5... Suppressor, 6... Detector, 7... Joint surface of fixed valve seat and rotor, 71... Rotor, 72... Fixed valve seat, 74.75... Metering tube, 7a to 7j... Hole, 7 to 7r... Groove, A... Mobile phase introduction channel, B... Mobile phase outlet channel, C, E...Measurement liquid 'introduction channel, D,
F...Measurement liquid outlet channel,

Claims (1)

[Claims] a disk-shaped fixed valve seat; a disk-shaped rotor disposed opposite to the fixed valve seat; first to tenth holes bored along the circumference of the fixed valve seat; first to fourth grooves formed in an arc shape at equal intervals provided on the surface in contact with the fixed valve seat; a fifth groove formed in an elongated shape in the center of the rotor; and the second groove. hole and fifth
a first metering tube connected to the hole and having a constant internal volume; a second metering tube connected to the seventh hole and the tenth hole and having a constant internal volume; and a cover connected to the first hole. a measurement liquid introduction channel, a measurement liquid introduction channel connected to the sixth hole, a first measurement liquid introduction channel connected to the fourth hole, and a measurement liquid introduction channel connected to the eighth hole. 2 mobile phase introduction channels, a first mobile phase outlet channel connected to the third hole, and a second mobile phase outlet channel connected to the ninth hole, and the rotor
A sample injection device characterized in that it is rotated to switch internal flow paths.