JPH0943111A - Sample vial and sample introducing device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a sample vial which does not require the vertical movement of the plunger of a syringe, fixed amount sucking operation, nor cleaning operation and has excellent determining accuracy and a sample introducing device using the sample vial. SOLUTION: A sample vial 1 has a narrow hole 1b bored through the main body of the vial 1, tapered recessed sections provided at both end sections of the hole 1b, and a thin vent hole 1f bored through the main body. A sample introducing device is provided with sample vials 1, a turntable 8 to which the sample vials 1 are attached, a needle 7 which is connected to a mobile phase or a pipeline through which a solvent is transported under pressure on one side, another needle 9 which is connected to another pipeline through which a sample is introduced to an analyzer on the other side, and a driving mechanism which drives the needles 7 and 9 to both sides of the thin hole 1b sections of the vials 1.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample vial for containing a sample when introducing the sample into an analyzer such as a chromatograph (gas chromatograph or liquid chromatograph), and more particularly to a sample vial having a self-weighing function. The present invention relates to a sample introduction device using the sample vial.

[0002]

2. Description of the Related Art When a sample is introduced into a sample analyzer such as a gas chromatograph or a liquid chromatograph, a large number of sample vials containing the sample are placed side by side in a rack.
While automatically controlling the syringe installed in the sample introduction device, operations such as suction of the sample by the needle, movement to the injection port, injection, withdrawal of the needle, and washing of the needle are performed. In this case, the sample introduction device is composed of a syringe having various capacities, a needle provided in the syringe, a sample loop for measuring the sample amount, a switchable port valve, a cleaning port, and the like. . The sample is injected into the injection port by piercing the septum with the needle and pushing the plunger of the syringe.

[0003]

In the conventional sample introducing device, a syringe is used for the fixed amount and introduction of the sample as described above, and the sample must be introduced by the vertical movement of the plunger. Therefore, a mechanical error will be added to the quantitativeness of the sample amount. In particular, in the case of microquantification, it is even more difficult to ensure the accuracy when injecting the amount determined by the vertical movement of the plunger. In addition, when introducing a sample into an analyzer such as a chromatogram,
Even if the needle is moved to the sample vial, lowered, aspirated, raised, moved, lowered to the injection port, injected, pulled up, moved to the washing port, etc., it is complicated but much complicated. Operations are required.

The present invention has been made by paying attention to the above-mentioned problems, and requires no vertical movement of the plunger of the syringe, does not require a fixed amount suction operation, is excellent in fixed amount accuracy, and does not require a washing operation. An object is to provide a vial and a sample introduction device using the sample vial.

[0005]

[Means for Solving the Problems] That is, in order to solve the above-mentioned problems, the present invention provides that a sample vial is formed by penetrating pores in the main body, and the main body at both ends of the pores. Is characterized in that a taper-shaped concave portion is provided around the periphery thereof, and the main body portion is provided with pores for venting air different from the pores. Further, the sample introduction device is formed by penetrating through the pores in the main body, and the taper-shaped recesses are provided in the main body at both ends of the pores. A sample vial having holes for venting air separate from the pores, a turntable or a rack for mounting the sample vial, and one of them is connected to a pipeline for pumping a mobile phase or a solvent. A needle, a needle connected to a conduit for introducing a sample into the analyzer, and a drive mechanism for driving the two needles to positions on both sides of the pore portion of the sample vial. It is characterized by being done.

[0006]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, specific embodiments of the present invention will be described with reference to the drawings. FIG. 1 is a vertical sectional view of a sample vial of the present invention. In this sample vial 1, a pore 1b is vertically penetrated in a central portion of a main body 1a. Then, the upper and lower body portions 1a of the pores 1b have a taper-shaped recess 1 around the periphery thereof.
c and 1d are provided, and a constant space 1e is formed below the lower taper-shaped recess 1d. Further, in the main body portion 1a of the sample vial 1, finer pores 1f for air venting are provided in parallel with the pores 1b. The air vent hole 1f is formed above the space 1e. The material of the sample vial 1 can be made of resin, glass, metal or the like.
The air vent holes 1f may be provided between the tapered recesses 1c and 1d when the space 1e is not provided.

As described above, the sample vial 1
When the fine pores 1b are formed in the main body 1a of the above, the volume V of the fine pores 1b (area of the fine pores 1b × length of the fine pores 1b) is processed with high precision. When the hole 1b is difficult to be machined with high accuracy, a slightly thicker hole may be bored and a capillary (capillary tube) may be embedded therein. Alternatively, the pores 1b and the air vent pores 1f may be laser-processed. By the way, the volume V of the pore 1b is 1 μl (1
mm ³ ), the diameter is 357 μm (0.357 mm) when the length L of the pore 1b is 10 mm.

Next, the septums 2 and 3 are placed on the upper and lower sides of the sample vial 1, and the upper caps 4 are placed on the upper side of the septum 2 and the lower side of the septum 3, respectively.
Also, the lower cap 5 is fitted into the main body 1a to such an extent that it is slightly pressed. The upper cap 4 and the lower cap 5 are provided with holes 4a and 5a at their central portions so as not to interfere with needles 7 and 9 described later.

Next, the operation of putting a liquid sample into the sample vial 1 will be described. That is, as shown in FIG. 2, the upper septum 2 and the upper cap 4 are removed. Then, the needle 6 of the syringe is used to insert the liquid sample into the pores 1b formed in the main body 1a. In this case, the taper-shaped recess 1d provided on the lower side of the main body 1a, the space 1e, and the taper-shaped recess 1c on the upper side are filled with the sample. The air remaining in the space 1e is discharged from the air venting pores 1f as indicated by the arrow. Then, when the sample is filled to the upper side, the upper septum 2 is placed, and the upper cap 4 is fitted from the upper side. The upper and lower recesses 1c and 1d and the space 1e are filled with the excess sample.

FIG. 3A is a partial plan view of the sample vial 1 attached to the turntable 8.
FIG. 3B is a partially sectional front view. That is, turn
A plurality of holes 8a are formed on the same circumference of the bull 8, and a large number of the sample vials 1 containing the sample are fitted into these holes 8a. A needle 7 for sending the mobile phase from the pump side is arranged above the sample vial 1, and a needle 9 for introducing the sample and the mobile phase into a column (not shown) is provided below the sample vial 1. Are arranged.
These needles 7 and 9 are provided with a cleaning unit (not shown) and a turret.
A drive mechanism for reciprocating up and down the sample vial 1 installed in the table 8 and a drive mechanism for piercing the septums 2 and 3 at both ends of the fine pore portion 1b are provided, as described later.

In order to introduce a sample from the sample vial 1 into an analyzer (not shown), these needles 7 and 9 penetrate the septums 2 and 3 from above and below, respectively, as shown in FIG. The taper-shaped recesses 1c and 1d provided on the upper and lower sides of the portion 1a are inserted, and the upper and lower pores 1b are contacted. Then, if a mobile phase or a solvent is sent from the pump to the upper needle 7, a certain amount of the sample stored in the pores 1b of the main body 1a of the sample vial 1 is transferred to the lower needle 9 to the analyzer. be introduced. That is, at the time of introducing the sample in this case, the sample in the pore 1b portion (portion of length L) provided in the sample vial 1 is introduced into the analyzer (upper and lower concave portions 1c and 1d and the space portion 1e). Since the sample remains as it is), it can be introduced with extremely high accuracy.
When the sample was introduced, the positions of the needles 7 and 9 were the pores 1.
Even if the position is slightly deviated from the position of b, it can be absorbed by the tapered recesses 1c and 1d provided above and below the pores 1b of the main body 1a, so that it is not necessary to strictly consider the positioning accuracy.

As mentioned above, the sample vial 1
Are installed in the turntable 8 and, when a sample is introduced from one sample vial 1, they are arranged above and below the sample vial 1.
The dollars 7 and 9 are moved to the washing section for washing, while the turntable 8 is rotated by one vial to introduce the next sample. In this way, the samples contained in the sample vials 1, 1, ... Installed in the turntable 8 can be successively introduced into the analyzer. That is, in the sample introducing device using the sample vial 1, like the sample introducing device using a conventional syringe, the needle is moved to the sample vial, lowered, aspirated, raised, moved, lowered to the injection port, There is no need to repeat operations such as pouring, pulling up, moving to a cleaning port, etc.
Intermittent rotation of the bull 8 and the needles 7 arranged above and below,
Since only the cleaning operation of 9 and the reciprocating motion are sufficient, the operation is extremely simple and easy. When the sample vial 1 is stored, it may be stored in a rack or the like that moves in a fixed direction instead of the turntable 8.

[0013]

As described in detail above, according to the sample vial and the sample introduction device of the present invention, it is not necessary to introduce the sample by the vertical movement of the plunger of the syringe as in the prior art, so that the plunger vertical drive device is It becomes unnecessary.
In addition, since the volume of the fine hole portion of the sample vial itself is constant and the sample of the constant volume portion of the fine hole is introduced, the quantitative function becomes unnecessary. That is, the quantification accuracy is related to the volume of the pores (capillary tubes) formed in the sample vial. Therefore, the finer the pores (capillary tubes), the longer the length, and thus the quantitative accuracy can be improved. By making the sample vial of this invention disposable, it is not necessary to wash the vial. Further, in the sample introducing device using this sample vial, like the sample introducing device using a syringe, movement of the needle to the sample vial, lowering, suctioning, raising, moving, lowering to the injection port, injection, pulling up. Since a device for performing operations such as moving to a cleaning port, etc. is unnecessary, the sample introduction device can be manufactured at low cost.

[Brief description of drawings]

FIG. 1 is a vertical sectional view of a sample vial of the present invention.

FIG. 2 is a vertical cross-sectional view showing a method for putting a sample into a sample vial of the present invention.

FIG. 3 (A) is a partial plan view of the sample vial of the present invention attached to a turntable, and FIG. 3 (B) is a partial sectional front view.

FIG. 4 is a longitudinal sectional view showing a method for introducing a sample contained in a sample vial of the present invention into an analyzer.

[Explanation of symbols]

 1 Sample Vial 1a Sample Vial Main Body 1b Pore 1c, 1d Tapered Recess 1f Air Venting Pore 2, 3 Septum 4, 5 Cap 7, 9 Needle 8 Turntable

Claims (2)

[Claims] 1. A main body is formed by penetrating through a fine hole, and the main body at both ends of the fine hole is provided with a tapered recess around the main body. A sample vial, characterized in that it is provided with pores for venting air that are separate from the pores. 2. A main body part is formed by penetrating through a fine hole, and the main body part at both ends of the fine hole is provided with a taper-shaped concave portion, and the main body part is further provided with the thin portion. A sample vial having holes for venting air separate from the holes, a turntable or rack for installing the sample vial, and one of which is connected to a pipeline for pumping a mobile phase or a solvent.
And a needle connected to a conduit for introducing a sample into the analyzer, and a drive mechanism for driving the two needles to positions on both sides of the pore portion of the sample vial. A sample introduction device characterized in that