JPH03118440A - Element analyzing apparatus having laser device - Google Patents

Abstract

PURPOSE:To automate the operation of analyzing device by imparting the moving distance and the direction of a solid-state sample to a laser controller from the controller of the analyzing apparatus. CONSTITUTION:An X-Y stage 1 mounting a solid-state sample 12 and a laser device 7 are automatically controlled with a laser controller 5. Various commands are imparted to the controller 5 from a work station 11, and the operation of the system as a whole and data arrangement are performed. A switching valve 12 wherein the internal flow paths can be switched between a solid-line connecting state and a broken- line connecting state alternately is provided. At the time of measurement, the internal flow path is made to be in the broken-line connecting state. Then, Ar gas (c) is made to flow through the flow path by way of a first connecting port 21a of the valve 12 a second connecting port 21b the solid-state sample 2 a third connecting port 21c a fourth connecting port 21d an analyzing device 8. Thus the evaporated sample 2 is conveyed into the device 8. Then, the laser emitting time interval and the moving distance of the sample 2 are set in the station 11. The laser emitting time interval is imparted to the device 7 or the moving distance of the sample 2 is imparted to the controller 5. Thus the operation can be automated.

Description

[Detailed Description of the Invention] <Industrial Application Field> The present invention relates to an elemental analyzer having a laser device, and more specifically, to an elemental analyzer that uses a laser in a solid sample introduction system. Concerning control of time intervals and solid sample movement.

<Prior Art> Apparatuses for irradiating a solid sample with a laser to vaporize the sample and then introducing the sample into an analyzer for elemental analysis have been known.

FIG. 5 is a diagram showing the configuration of such a conventional apparatus, in which 1 is an XY stage on which a solid sample 2 is placed;
A pulse motor 3 for movement in the X-axis direction and a pulse motor 4 for movement in the Y-axis direction allow movement in two-dimensional directions, X and Y. The solid sample 2 is specifically placed inside a sample cell.

These pulse motors 3 and 4 are adapted to move the XY stage 1 in any direction in response to a movement signal from an operation mechanism 6 provided within the laser controller 5.

The laser controller 5 has a built-in driver for the pulse motors 3 and 4, and can directly drive the pulse motors 3 and 4. Reference numeral 7 denotes a laser device, which irradiates the solid sample 2 with a laser beam from, for example, the z-axis direction. Reference numeral 1 denotes an XY stage on which a solid sample 2 is placed, and can be moved in two-dimensional directions of X and Y by a pulse motor 3 for movement in the X-axis direction and a pulse motor 4 for movement in the Y-axis direction. The solid sample 2 is specifically placed inside a sample cell.

Reference numeral 8 denotes an analyzer which takes a solid sample vaporized by laser irradiation into the analyzer and performs mass spectrometry using At gas as a carrier, and 9 is a controller of the analyzer 8.

In the apparatus configured as described above, the XY stage 1 is moved in any direction using the operating mechanism 6 such as a bush switch or a joystick.

In actual operation, after the operator confirms the position of the solid sample on the monitor 10, the analyzer 8 starts analysis.
Start data import. Next, the solid sample 2 is irradiated with a laser beam from the laser device 7, the XY stage 1 is moved as necessary, the position of the solid sample 2 is shifted, and the laser is irradiated again to a location away from the previously irradiated position. .

By irradiating this laser, the position of the solid sample is shifted by about 0.
2mm), then irradiates the laser again for a certain period of time (several seconds to several tens of seconds) by operating a switch.
0 seconds) several times to several dozen times.

<Problems to be Solved by the Invention> However, in the conventional example described above, the operator manually controls the interval of laser emission and the distance by which the solid sample is shifted. This lick relies on the operator's experience and intuition, is not reproducible, and requires skill. In addition, skill is required to emit laser light a large number of times in a short period of time, and there are also problems such as contamination of the analyzer if the flow path of the connection port is not changed in a timely manner.

The present invention was made in view of this situation, and its object is to provide an elemental analyzer having a laser device that can be operated automatically by simply setting the laser irradiation range, sample movement pattern, distance, etc. in a program. Our goal is to provide the following.

Means for Solving the Problems> The present invention provides an apparatus for performing elemental analysis by irradiating a solid sample with a laser beam from a laser device and introducing the vaporized solid sample into an analyzer, in which the solid sample is placed in an XY a stage, a laser controller that automatically controls the stage and the laser device, a workstation that gives various commands to the controller of the analysis device, operates the entire system and organizes data, and first to fourth connection ports. and a switching valve whose internal flow path is alternately switched to send the sample to the analyzer, and the workstation is provided with a laser emission time interval, a moving distance of the solid sample, and a range to be irradiated with the laser. At the same time, the laser emission time interval inputted from the workstation is given to the laser device via the controller of the analyzer, and the moving distance and direction of the solid sample are determined by the analyzer's controller. The above-mentioned problem is solved by allowing the laser controller to send the signal from the controller to the laser controller.

Function> The present invention functions as follows. That is, the operator informs the workstation of the analysis conditions, laser irradiation starting point, laser irradiation pattern, and laser irradiation range.

Once the number of laser irradiations and the moving distance of the solid sample are set, these data are entered into the controller of the analyzer. As a result, the laser emission time interval and the moving distance of the solid sample inputted from the workstation are provided from the controller to the laser controller.

Here, when the operator presses a key in the desired direction on the control panel 6 (or when the workstation instructs the analyzer controller to start analysis), the controller starts operating. is detected and sends a signal to the laser controller to operate the pulse motor and laser device at the next timing, thereby controlling the operation of the pulse motor and laser device.

As a result, the analyzer starts analysis, and after a predetermined period of time elapses, the laser is irradiated at a predetermined position on the solid sample.
The pulse motor operates to move the XY stage by a set distance in the X or Y direction. Next, the laser is irradiated at the position after the movement and a set time has elapsed since the previous laser irradiation. A synchronization signal is sent from the laser device to the controller each time the laser is emitted. This allows the controller to monitor the number of times the laser is emitted.

<Example> Hereinafter, the present invention will be described in detail using the drawings. 1st
The figure is an explanatory diagram of the configuration of an embodiment of the present invention, and in the figure, the same symbols as in FIG. 5 are used with the same meaning, and repeated explanation here will be omitted. Further, 11 is a workstation of the analyzer 8, and 12 is a switching valve having first to fourth connection ports 12a to 12d and whose internal flow path is alternately switched between a solid line connection state and a broken line connection state. That is, during non-measurement, the switching valve 12 is off and the internal flow path is in a solid line connection state. Therefore, Ar gas is directly supplied to the analyzer 8,
No vaporized sample is provided. Further, during measurement, the switching valve 12 is turned on and the internal flow path is connected to the broken line.

Therefore, the Ar gas is
1a → 2nd connection 21b → solid sample 2 → switching valve 12
It flows through the flow path from the third connecting hole 21c to the fourth connecting hole 21d to the analyzer 8, and transports the vaporized sample to the analyzer 8.

Furthermore, the workstation 11 provides various commands to the controller 9 of the analyzer 8, and also operates the entire system and organizes data. Furthermore, the laser emission time interval and the moving distance of the solid sample 2 (or XY stage 1) are set. Further, the laser emission time interval inputted from the workstation 11 is given to the laser device 7 via the controller 9, and the moving distance of the solid sample 2 is given to the laser device 7 via the controller 9.
is given to the laser controller 5 from. As the operating mechanism 6, four keys are used to manually move the XY stage 1 forward, backward, left and right.

The operator inputs the analysis conditions, laser irradiation start point, laser irradiation pattern, laser irradiation range,
and the moving distance of the solid sample, these data enter the controller 9 of the analyzer 8. As a result, the laser emission time interval and the movement 1ull of the solid sample 2 inputted from the workstation 11 are given from the controller 9 to the laser controller 5.

Here, when the operator presses a key in the desired direction on the operating mechanism 6 (or when the workstation instructs the analyzer controller to start analysis), the controller 9 starts operating. is detected, a signal is sent to the laser controller 5 to operate the pulse motors 3 and 4 and the laser device 7, and the operations of the pulse motors 3 and 4 and the laser device 7 are controlled at the following timing.

As a result, when a predetermined period of time has elapsed after the analyzer started analysis, the laser is irradiated to a predetermined position on the solid sample 2, and then the pulse motor 3.4 operates to move the XY stage a preset distance in the X direction or in the Y direction. Next, the laser is irradiated at the position after the movement after a set time has elapsed since the previous laser irradiation. A synchronization signal is sent from the laser device 7 to the controller 9 every time the laser is irradiated. This allows the controller 9 to monitor the number of times the laser is emitted. This series of sequences is repeated as many times as necessary. During this time, the solid sample irradiated with the laser is vaporized, and A
The gas enters the analyzer 8 using r gas as a carrier, and elemental analysis is performed.

The specific operation sequence is as follows.

■Set analysis conditions etc. on the workstation 11.

The laser emission starting point is set by manually operating the XY stage 1.

(2) The operator selects the direction of movement of the solid sample 2 by pressing a key switch on the operating mechanism 6 or instructing the start of analysis from the workstation 11.

(2) Set the switching valve 21 to measurement mode (that is, switch the internal flow path of the switching valve 21 from the solid line connection state to the broken line connection state.

■Analyzer 8 starts analysis (starts scan)
.

(2) After a predetermined time has elapsed from the start of analysis, a laser is emitted to the solid sample 2, and a synchronization signal is sent from the laser device 7 to the controller 9.

■When the synchronization signal is input to the controller 1-roller 9, the analyzer controller controls the laser controller 5 and
The Y stage 1 is automatically determined by the workstation 11 based on the specified irradiation pattern, and moves in the specified direction by a distance set on the workstation 11.

FIGS. 2 to 4 are diagrams showing the trajectory of laser irradiation,
In the figure, 2 is the solid sample, the black circle is the laser irradiation position, and A is the laser irradiation start point. In FIG. 2, since the preset laser irradiation pattern is a straight line, after the laser irradiation starting point A, the laser is irradiated on the - straight line at equal intervals.

The direction of movement at this time is automatically determined based on parameters such as the set irradiation pattern and irradiation interval.

The laser irradiation pattern (miracle) is not limited to the one shown in Figure 2, but can be modified in various ways, such as the one shown in Figure 3.
It may be done as shown in the figure or FIG.

That is, FIGS. 3 and 4 are diagrams showing the miracle of laser irradiation. In the case of Fig. 3, a certain rectangular surface is sequentially irradiated with a laser, starting from the laser irradiation starting point A and automatically determined from parameters such as the laser irradiation pattern and irradiation interval, which are not set in advance. The laser is irradiated according to the moving direction and irradiation interval. Moreover, the case of FIG. 4 shows the case where the laser irradiation pattern is not set so that the laser irradiation pattern is sequentially irradiated onto the circular noodles. <Effects of the Invention> According to the present invention as described in detail above, an elemental analyzer having a laser device includes an XY stage on which a solid sample is placed, and a laser controller that automatically controls the stage and the laser device. , a workstation that gives various commands to the control, operates the entire system and organizes data, and has first to fourth connection ports, and the internal flow path is alternately switched between a solid line connection state and a broken line connection state. A switching valve is provided, and the laser emission time interval and the movement distance of the solid sample are set in the workstation, and the laser emission time interval inputted from the workstation is transmitted to the laser apparatus through the controller of the analysis apparatus. Since the moving distance of the solid sample is configured to be given from the controller of the analyzer to the laser controller, the following effects (1) to (4) can be obtained.

■Measurement is easy and the set values are reproducible. Therefore, a large number of samples can be measured with good reproducibility.

■Automation dramatically reduces erroneous operations and prevents damage to valuable samples.

■Measurement time can be shortened because the irradiation speed can be easily increased.

[Brief explanation of drawings]

FIG. 1 is an explanatory diagram of the configuration of an embodiment of the present invention, and FIGS.
The figure shows a laser irradiation pattern (trajectory), and FIG. 5 is a diagram illustrating the configuration of a conventional example. 1...XY stage, 2...solid sample, 3.4...pulse motor, 5...laser controller, 6...operation Mechanism 7... Laser device, 8... Analyzer, 9... Analyzer controller, 11.
...Workstation, 12...Switching valve

Claims (1)

[Claims] In an apparatus that performs elemental analysis by irradiating a solid sample with laser light from a laser device and introducing the vaporized solid sample into an analyzer, an XY stage on which the solid sample is placed, the stage, and the laser device are automatically controlled. A laser controller, a workstation that gives various commands to the controller of the analyzer, operates the entire system and organizes data, and has first to fourth connection ports, and the internal flow path is alternately switched. The workstation is equipped with a switching valve for transporting the sample to the analyzer, and a pattern indicating the laser emission time interval, the moving distance of the solid sample, and which area to irradiate with the laser is set on the workstation. A laser emission time interval input from the analyzer is provided to the laser device via a controller of the analyzer, and a moving distance and direction of the solid sample are provided from the controller of the analyzer to the laser controller. An elemental analyzer with a device.