JPH0829432A - Automatic sample preparing device - Google Patents

Abstract

PURPOSE:To completely automate a series of processes for preparation from a solid sample to a sample solution. CONSTITUTION:In the circumference of a handling robot 21 traveling on a rail 13, a heating melting part 35, air/water cooling part 20, dilution/constant volume part 31, stirring part 16, and filtering parts 12, 25 are furnished. These parts are controlled by a control part (personal computer) to operate in accordance with predetermined conditions, and operation of the handling robot 21 is controlled to sequentially transfer vessels containing a solid sample or sample solution between respective parts and then place them at a specified analysis- waiting position.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an automatic sample preparation device for preparing a solid sample into a sample solution which can be analyzed by a chemical analyzer.

[0002]

2. Description of the Related Art Methods for analyzing solid samples include so-called instrumental analysis methods such as arc emission spectroscopy and so-called chemical analysis methods such as inductively coupled plasma (ICP) emission spectroscopy. . In the instrumental analysis method, generally, a solid sample can be analyzed in a lump state, but in chemical analysis, the solid sample is heated and dissolved with an acid or the like, and then the solution is analyzed.

The chemical analysis has an advantage that a multi-component mixed sample such as a standard solution for preparing a calibration curve can be easily prepared by adding a solution or the like, but a pretreatment for making the sample into a solution is required. Becomes The solution of a solid sample is usually performed by putting the sample in an acid solution such as hydrochloric acid or nitric acid and heating it. Actually, before and after that, the sample is weighed, fractionated, added with acid, heated and dissolved. Many processes such as cooling, addition of additives, constant volume of solution, filtration, etc. are required. Each of these treatments requires a dedicated instrument or device (for example, acid vapor is generated during heating and melting, so
Draft chambers are required), and many processes require complicated and delicate work. Therefore, performing these manually is very complicated and time consuming. Further, when a large number of samples must be analyzed promptly, it is necessary to prepare the number of instruments in each process and prepare the sample solution in advance.

[0004]

Although attempts to automate such a complicated and time-consuming sample preparation process have been made in the past, the conventional automatic sample preparation apparatus has only a part of the above-mentioned series of steps. Even if it is the target, or if it is a plurality of steps, one of the steps is omitted or simplified, such as omitting the filtration process. However, a simplified automatic sample preparation device requires human intervention in the middle of the process, which does not result in great labor saving. Further, there is a problem that the applicable sample is limited by the simplified automatic sample preparation device. For example, an automatic solutionizer without the filtration step can handle only a sample with no residue.

Further, with respect to each treatment, the conventional sample preparation device or manual operation has the following problems.
First, regarding solutionization of a solid sample, conventionally, mineral acids (inorganic acids) such as hydrochloric acid, nitric acid, and sulfuric acid have been used, and heating has been performed to increase the dissolution rate and speed up the process. Further, by arranging a plurality of containers on a metal plate heated by a gas burner, an electric heater or the like and heating them simultaneously, it is possible to shorten the time in the case of processing a plurality of samples.
Since acid vapor or gases such as NOx and SOx are generated during heating, these are heated in the draft chamber, and the air is exhausted from the draft chamber by the exhaust fan. However, such a conventional apparatus or system has the following problems.

(1) Since the heating device is large, the heat radiated from the heating device is also large. Therefore, in order to avoid the influence of the heat, another processing device or the like cannot be placed around the heating device, which requires a large space. (2) Metals such as iron and aluminum are used for the draft chamber, heating source, etc., but these are corroded by acid vapor generated from the heated sample solution and have low durability Can not). A method of minimizing the generation of acid vapor by reducing the heat source can be considered, but this method sacrifices the sample processing speed (or the number of samples that can be processed within a predetermined time). (3) In order to prevent this, it is necessary to clean the inside of the draft chamber frequently. (4) When the draft chamber is evacuated, the draft chamber has a negative pressure, and dust from the outside enters the draft chamber, enters the sample solution, and deteriorates the analysis accuracy. (5) On the contrary, toxic gas such as acid vapor leaks from the draft chamber to a small extent and deteriorates the surrounding work environment.

[0007] Next, regarding the constant volume treatment, a marked line is conventionally drawn in advance at a predetermined volume position of a glass container such as a volumetric flask, and a diluent is added to a sample solution placed up to the position below the marked line. In addition, the method of stopping the addition of the diluting solution at the time when the liquid surface (more precisely, the meniscus of the liquid surface) coincides with the marked line was taken. If this is done manually, it is necessary to bring the eye to the position of the marked line and the height of the liquid surface, and since the coincidence between the two is delicate, it is a complicated and time-consuming process. Was there. There is also a problem in that it varies from operator to operator.

[0008] On the other hand, in the case of performing automatically, simply,
(Since the size of the container is not generally constant), always use the same container, install a liquid level sensor at the liquid level position where the specified volume is reached, and stop the addition when the liquid level is detected. The method of doing was taken. However, when another sample is set to a constant volume, the inside of the container must be washed once with the same diluent, and an automatic washing device must be incorporated for complete automation. Moreover, the next sample cannot be charged until the processing cycle of charging, dissolving, and cleaning one sample is completed, which is extremely inefficient. Further, as a sensor for detecting the meniscus on the liquid surface, conventionally, a contact type sensor has been used in which an electrode is placed at a predetermined height and the time at which the liquid contacts the electrode is electrically detected. However, also in this case, the contamination of the sample solution poses a problem when the volume of another sample is fixed. Further, there is a problem that the sensor malfunctions when the liquid surface vibrates due to the dropping of the diluent.

If a separate container is used for each sample in order to prevent contamination, the height of the marked line differs from container to container as described above, so it should be judged that the volume has become constant only by the height of the liquid surface. Therefore, it is necessary to detect the coincidence between the marked line and the liquid surface. In this case, both the mark sensor (a non-contact type sensor is used to prevent contamination) and the liquid level sensor are required. However, when the volume is constant, the mark line and the liquid level are almost at the same position. Since the surface sensor detects the mark line and the liquid level sensor and the mark sensor are at the same height, there is a possibility of malfunction due to mutual interference between them.

Next, regarding the filtration treatment, a filtration method or a centrifugation method has been conventionally used as a method for separating a solid-liquid from a mixture of a solid and a liquid. However, centrifugation cannot be said to be a complete solid-liquid separation, only by separating solid and liquid into respective layers. Further, although filtration can perform complete solid-liquid separation, in order to completely recover both solids and liquids, the sample container is washed and the sample is completely discharged onto the filter paper, and It is necessary to wash the solids remaining in the solution and collect the liquid adhering to the surface of the solids as a filtrate. Since such an operation is extremely complicated, the conventional automatic filtration device is intended to collect only one of the filtrate and the residue, and cannot collect both the filtrate and the residue. .

The present invention has been made in order to solve these problems, and its purpose is to be able to deal with various purposes (filtrate, residue, etc.) analysis, and to be highly automated, Moreover, it is to provide an automatic sample preparation device with due consideration given to safety and durability.

[0012]

The automatic sample preparation device according to the present invention made to solve the above problems is an automatic sample preparation device for preparing a sample solution from a solid sample that can be analyzed by a chemical analyzer. A) A heating / dissolving section for adding a acid to a solid sample and heating it to create a sample solution; b) a cooling section for cooling the sample solution; and c) ensuring that the cooled sample solution has a prescribed volume. Add a diluting solution to a constant volume, d) a stirring part to stir the sample solution, e) a filtering part to filter the sample solution and separate it into a filtrate and a residue, and f) a solid sample or sample. A handling robot that has a hand that holds a predetermined container containing a solution and that moves on a rail that is provided between the above-mentioned parts arranged at predetermined positions; and g) the above-mentioned parts operate under preset conditions. Control the solid sample or sample solution After the container sequentially transported between the various parts, is characterized in that a control unit for controlling the operation of the handling robot to place a predetermined analysis waiting position.

The heating and dissolving part is a) a microwave heating device for heating a container containing a solid sample and an acid, b) a heating chamber surrounding the container, and c) an upper part of the heating chamber. An openable and closable cap with a steam outlet, d) a connection channel that connects to the acid vapor outlet of the cap when the cap is closed and connects to a water flow aspirator, and e) a gas in the connection channel due to the water flow. And an aspirator for mixing the sucked gas with water.

Further, while using a container having a simulated reference line at a predetermined distance from the position of the liquid surface which is the target of constant volume, the constant volume section detects a) the simulated reference line. The simulated level sensor, b) the liquid level sensor provided at the predetermined distance from the simulated level sensor, and c) the simulated level sensor and liquid level sensor at the specified distance. The automatic sample preparation device may include a sensor moving device that moves the device as it is.

Further, the above-mentioned filtering section has: a) a funnel for holding the cartridge type filter paper in an airtight manner; b) a suction chamber in which the lower part of the funnel is airtightly enclosed and the lower part is opened; and c) air in the suction chamber is sucked. It is possible to simultaneously mount a suction pump that operates, d) a filtrate container that receives the filtered sample solution, and a washing liquid container that receives the washing liquid that is used to wash the residue left on the filter paper. And a container stand that hermetically closes the lower part of the suction chamber when it rises, and the control unit controls the handling robot such that e) the processing in the filtering unit is performed after the processing in the constant volume unit. At the same time, f) When the sample solution is collected, the filtrate container is put into the suction chamber, and when washing the residue, the washing liquid container is put into the suction chamber, and the raising and lowering and rotation of the container stand are controlled. As an automatic sample preparation device It may be.

[0016]

In the automatic sample preparation device according to the present invention, the control unit controls the handling robot so that the container containing the solid sample or the sample solution is heated and dissolved, the cooling unit, the constant volume unit, the stirring unit and the filtration unit. Then, the sample solution thus prepared is placed at a predetermined analysis waiting position. Moreover, since the control unit controls the individual processing in each unit,
An automated sample preparation process is possible without the need for operator intervention. By automatically collecting the sample solution from this analysis waiting position by an autosampler or the like which is an analyzer or its peripheral device, it is possible to completely automate sample preparation to analysis.

Further, in the heating and melting section of the automatic sample preparation device according to the second aspect, since the microwave heating method is adopted, wasteful heat generation is minimized, and the processing speed is sacrificed. Without doing so, the heating device can be made as small as possible. In addition, since the acid vapor generated during heating is guided from the cap to the water flow aspirator and dissolved in water as it is for recovery, a large draft chamber is not required,
There are no problems of leakage or surrounding corrosion.

In the constant volume section of the automatic sample preparation device according to the third aspect, since the liquid level sensor comes to a predetermined liquid level position when the pseudo mark line sensor detects the pseudo mark line, both sensors are provided. It is possible to accurately detect whether or not the liquid surface has reached a predetermined position determined for each container without causing a problem of interference between them. As a result, it is possible to perform an automated constant volume that does not vary by the operator. Also, because a separate container can be used for each sample,
Highly accurate analysis can be performed without worrying about contamination between samples.

In the filtration section of the automatic sample preparation device according to the fourth aspect, the cartridge type filter paper is kept airtight in the funnel,
Since the suction chamber is airtightly closed at the lower part of the suction chamber by the container stand, high-speed filtration can be performed by sucking the inside of the suction chamber with the suction pump. Next, since the container stand can be raised and lowered and rotated, the filtrate container and the washing liquid container can be alternately housed in the suction chamber. When the filtrate container is placed in the suction chamber, the filtrate can be recovered from the sample solution. Since this apparatus employs a so-called dry filtration system in which the constant volume treatment is performed in the constant volume section and then the filtration section is performed, the residue is not washed when the filtrate is collected. Next, the container stand is moved up and down and rotated to place the washing liquid container in the suction chamber and the residue on the filter paper is washed to collect the residue (solid component in the sample solution) this time. Thus, in the automatic sample preparation device according to claim 4, both the filtrate and the residue can be completely recovered.

[0020]

EXAMPLE A fully automatic sample preparation device for an ICP emission spectroscopic analyzer, which is an example of the present invention, will be described with reference to FIGS. As shown in FIG. 5, the fully-automatic sample preparation device L of the present embodiment is arranged beside the sample table M of the ICP emission spectrum analyzer J, and the prepared sample is placed on the sample table M by an autosampler described later. The sample preparation process including the pre-treatment up to and the post-treatment of the sample for which the analysis has been completed is automatically performed. Note that K is an automatic standardization unit, A is an ICP control personal computer, D is a data transmission personal computer, F is a sample preparation device control personal computer, and H is a weighing personal computer (I is an electronic balance). All of these computers are dedicated work desks,
Placed on racks such as B, C, E, G, and CR respectively
It is equipped with a T, a printer and the like.

The appearance of this apparatus is shown in FIG. 3 (overall plan view) and FIG.
(Overall side view). Regarding the internal structure not shown here, the layout of the foundation members on the floor is shown in FIG. 2, and the layout of the equipment above it is shown in FIG. 1, respectively. As shown in FIG. 2, the solvent tank 55 for the autosampler, the solvent supply pump 56 for the autosampler, the distribution board unit 38, the robot control unit 40, the parallel movement device control unit 41, the acid tank 42, the additive tank 4
3, ion exchange water tank 44, ion exchange water pump, filtration pump, wash water pump 45, cooling water circulation unit 4
6, ion exchange water production unit 54, sequencer 48,
49, uninterruptible power supply 50, cooling fan 47 and other basic members are installed.

On these base members, as shown in FIG. 1, an autosampler 10 (having a turntable 11) at a position closest to the sample table M of the ICP emission spectrum analyzer J, and sample preparation. Various devices and units related to the above are arranged. A robot moving rail 13 is laid in the center of the floor, and the handling robot 2 is placed on the rail 13.
1 moves. Around the robot moving rail 13, in addition to the automatic sampler 10 described above, the filter unit A12 and the filter paper cartridge holder 1 are rotated counterclockwise.
4, filter paper supply unit 15, stirring unit 16, beaker holder 17, beaker supply unit 18, flask rack 19, cooling unit 20, flask holding holder 2
2, filter paper rack 23, water drop removal unit 24, filtration unit B25, two microwave type sample dissolution apparatus 3
5 (36 is an acid vapor discharge cap), 5 electric burets 34 for acid addition, an acid addition unit (remaining drop receiver) 3
3, Y addition unit (remaining drop receiver) 32, dilution constant volume electric buret 31, Y addition electric buret 30, manipulator rail 29, beaker unloading manipulator 2
8, a waiting beaker stocker 27 for analysis, and a manipulator 26 for moving the beaker are arranged. In addition, two analyzed beaker racks 37 are provided from the tip end portion of the manipulator rail 29 along the side surface on the outside of the main body.

As shown in FIG. 6, the handling robot 21 has one parallel movement part a, five rotation axes b to f, and one.
It is provided with one opening / closing part g and two hand parts 57 and 58. The hands 57 and 58 are given the degree of freedom of movement and orientation in a two-dimensional plane by the three rotation axes c, d, and e, and by rotating around the vertical rotation axis b, the above-mentioned respective processes are performed. It is possible to access the department. As described above, due to the large number of degrees of freedom, the handling robot can move extremely freely, and the sample can be smoothly transferred between the respective parts. The first hand portion 57 is provided horizontally from the tip of the arm, and the second hand portion 58 is provided vertically downward from that. The lower second hand portion 58 is used only for taking in and out the sample dissolving flask 2 from the flask rack 19, and after carrying it by the flask holding holder 22 described later, the first hand portion on the tip side is all. Use 57.

As described above, in the apparatus of this embodiment, since each processing unit is rationally arranged around the robot moving rail 13, the handling robot 21 moves on the robot moving rail 13 and the sample solution is moved. A flask containing
By moving the beaker or the like between these parts, the sample preparation from the solid sample to the sample solution that can be analyzed by the ICP emission spectroscopic analyzer J can be fully automated.

The entire automatic sample preparation device has a substantially hermetically sealed structure in order to prevent volatilization of acid vapor from the device to the outside and invasion of dust from the outside to the inside of the device and to consider safety. . As shown in FIGS. 3 and 4, the roof is provided with two exhaust ducts 51, and an air exhauster 52 is used to forcibly exhaust the internal air. Further, an alarm panel 39 is provided on the side surface, and when various troubles described later occur, the unit in which the trouble has occurred and the details of the trouble are
An alarm lamp (and an alarm buzzer in some cases) provided for each is used to alert the worker.

I in the fully-automatic sample preparation device of this embodiment
The outline of the procedure of processing the sample before and after the CP analysis is as follows.

(1) Register the sample on the personal computer for weighing (2) Set the processing conditions of each processing unit for each sample on the personal computer for the sample preparation device (3) Weigh and sample the sample (4) Set the dissolution container (5) Set the dissolution container in the dissolution device (6) Add acid (7) Heat and dissolve (8) Cool (air / water cooling) (9) Add additives (10) ) Constant volume (11) Stir (12) Filter (13) Transfer the filtrate to the analyzer (keep the residue) (14) Perform analysis (15) Store the analyzed sample

The above processes will be described in detail below.

(1) Registration of Sample First, the sample name or number of the sample to be analyzed is registered in the personal computer F (FIG. 5) for controlling the fully automatic sample preparation device. This data is a personal computer D for data transmission
Is transmitted to the personal computer H for controlling the weighing unit and the personal computer A for controlling the ICP emission spectrum analyzer.

(2) Setting of processing conditions of each processing section for each sample Next, processing conditions such as heating power in the heating / dissolving section, filtration section, heating time, filtration time, etc. for each registered sample are respectively set. Set it on the personal computer F for controlling the sample preparation device. At the time of this setting, a list of samples registered in (1) above appears on the CRT, and a list of processing units and a list of processing conditions selectable in each processing unit are displayed. Therefore, the operator can easily set conditions simply by selecting them with a mouse or the like.

(3) Weighing / Distribution of Sample After registering a sample name, setting conditions, etc., a solid sample to be analyzed is sampled and weighed by an electronic balance I. The weighed solid sample is put in the sample dissolution flask 2 shown in FIG. As will be described later, the sample dissolving flask 2 is provided with an Al ribbon as a simulated reference line 3 at a position below the reference line 1 for constant volume and separated by a predetermined distance Lf.

(4) Sample set The sample dissolving flask 2 containing the weighed solid sample is
First, the flask is set at the flask setting position (recess) 102 of the flask cartridge 104 as shown in FIG. Further, the flask cartridge 104 is attached to the flask rack 19.
Then, the flask rack 19 is set on the flask rack base 103 of the fully-automatic sample preparation device (101 is a handle). As shown in FIG. 1, in this embodiment, two flask racks 103 are prepared, and 30 flasks for sample dissolution 2 are placed on one flask rack 19 as shown in FIG. 8A. Therefore, a total of 60 samples can be prepared. Therefore, the addition and replacement of the sample during the preparation of the sample can be performed by replacing only the flask cartridge 104.

After the solid sample is set as described above, the operator operates the sample preparation device controlling personal computer F,
Start the automatic sample preparation process.

(5) Changeover of flask First, the sample preparation apparatus control personal computer F controls the handling robot 21 shown in FIG. 6 to place the flask rack 19 on the first flask setting position 102 to be processed. Move the hands 57 and 58 to move the second
The hand portion 58 holds the upper portion of the set sample dissolution flask 2. Then, by lifting the second hand portion 58 upward, the sample dissolving flask 2 is pulled out upward, and the flask holding holder 22 (Fig. 9 (a),
(B)). Therefore, the second hand portion 58 is once opened and the sample dissolving flask 2 is released. Next, the first hand portion 57 again holds the sample dissolving flask 2 again.

(6) Acid addition The handling robot 21 holding the sample dissolving flask 2 by the first hand portion 57
It is set on the parallel movement rack 162 of the acid addition unit shown in FIG. When the flask sensor 161 detects the setting of the sample dissolving flask 2, the parallel moving device 163 moves the sample dissolving flask 2 to just below the acid addition nozzle 164, and the acid of the acid prepared in advance in the sample preparation device controlling personal computer F is changed. Acid is added through the acid addition nozzle 164 of the electric acid addition buret 34 according to the type and the addition amount. In the case of adding a plurality of acids, the sample dissolving flask 2 is continuously moved to directly below another acid addition nozzle 164, and the acids are added in the same manner. Since the fully-automatic sample preparation device of this example is equipped with five electric burets 34 for acid addition (FIG. 1),
Up to 5 acids or acid solutions can be added in any order. When the addition of all the acids is completed, the handling robot 21 sets the parallel movement rack 162 on which the sample dissolving flask 2 is placed to its original position (FIGS. 13A and 13B).
Return to.

For the sake of safety, the present acid addition unit is provided with the following various devices. First, an optical flask sensor 161 using infrared rays or the like is provided so that the acid is not injected when the sample dissolving flask 2 is not on the parallel moving rack 162. Receivers 33 are provided directly below the acid addition nozzles 164, respectively.
Residual drops dropped from the tip of No. 4 are prevented from flowing out of the system. In addition, the remaining amount sensor is used for each acid tank 42
The alarm panel 39 is provided when the remaining amount of acid becomes low.
(Fig. 4).

(7) Heating and Dissolving The handling robot 21 then lifts the sample-dissolving flask 2 containing the sample and the acid from the parallel moving rack 162, and the microwave-type sample dissolving device 3 shown in FIG.
Then, the sample is conveyed to No. 5 and inserted into the sample hole 131. A magnetron 132 is provided at the bottom of the sample hole 131, and a recess for accommodating the bottom of the sample dissolving flask 2 is provided in the magnetron 132. Sample hole 13
An acid vapor discharge cap 36 that can be opened and closed is provided on the upper portion of 1. The acid vapor discharge cap 36 is rotationally driven by an air cylinder 134.
4 is controlled by the personal computer F for controlling the sample preparation device.
A gas discharge pipe 137 is provided on the top of the acid vapor discharge cap 36.
The gas exhaust pipe 137 is connected to the water flow aspirator 133 when the acid vapor exhaust cap 36 closes the sample hole 131.
It is connected to 36. Water aspirator 13
3 is connected between the tap 138 and the drain 139 of the tap water, and an electromagnetic valve is also used as a valve (not shown) for opening and closing the tap water so that it can be controlled by the personal computer F for controlling the sample preparation device. .

When the sample dissolving flask 2 is inserted into the sample hole 131 by the handling robot 21, the acid vapor discharging cap 36 is closed. Further, the water valve for the water flow aspirator is opened, and the water flow aspirator 1
33 starts suctioning. Then, the magnetron 132 heats the sample dissolution flask 2 in accordance with the power and time preset in the sample preparation apparatus control personal computer F in (2) above. As a result, the sample in the sample dissolving flask 2 is dissolved by the acid or acid solution added in (6) above.

Acid vapor (NOx, SOx generated during dissolution)
Etc.) from the acid vapor discharge cap 36 to the gas discharge pipe 13
7 and the fixed exhaust pipe 136 through the water flow aspirator 13
3 and is dissolved in water by the water flow aspirator 133. The water in which the acid is dissolved is sent from the drain port 139 to a predetermined tank, where it is temporarily stored and then collectively subjected to an appropriate post-treatment.

The acid vapor discharge cap 36 is handled by the handling robot 21 even after the dissolution is completed.
It is kept closed until just before picking up the acid, and the acid vapor generated during that time is fully discharged by the residual heat. As shown in FIG. 1, the fully-automatic sample preparation device of this embodiment is provided with two microwave type sample dissolution devices 35, which are used alternately for each sample.

The microwave heating has high heating efficiency and can shorten the dissolution time of the solid sample.
Even in the method in which the sample dissolving flasks 2 are serially processed one by one as in the present embodiment, it is possible to obtain a heating efficiency equivalent to that when a large number of flasks are processed at once by a heating device such as a conventional gas burner or electric heater. You can

Further, in the microwave type heating device,
Since the heat dissipation from the heating portion is suppressed to a minimum, the acid vapor discharging cap 36 can be made of a plastic material (Teflon or the like) having excellent acid resistance and processability.

Since the acid vapor discharge cap 36 only covers a small portion around the opening of the sample dissolution flask 2, it does not require a large exhaust fan such as a draft chamber, and is operated by the water pressure of purified water for general use. Water Stream Aspirator 1
With only 33, the acid vapor generated from the sample solution can be sufficiently sucked. Further, since the sucked acid vapor is mixed and stirred with water (tap water) by the water flow aspirator 133, it is sufficiently dissolved in water. This facilitates post-treatment of toxic gas.

(8) Cooling In the fully-automatic sample preparation apparatus of this embodiment, rapid heating of the sample solution after heating and dissolution avoids inconveniences such as strain in the flask and change in the quality of the solution. The system is air-cooled and then water-cooled.

The handling robot 21 conveys the sample dissolving flask 2 after the heating and dissolving treatment to the cooling unit 20 shown in FIG.
Set to. In the cooling unit 20, first, the electric air-cooling fan 142 is operated for a preset time in the sample preparation device control personal computer F to air-cool the sample dissolution flask 2 (state on the right side in FIG. 11). After that, the flask elevating device 141 lowers the flask holder 144, and the water cooling tank 1
It is immersed in 43 (state on the left side of FIG. 11). Water cooling tank 143
Inside, the sample dissolving flask 2 is similarly cooled by the circulating water 145 for a time set in advance in the sample preparation apparatus control personal computer F. When the water cooling is completed, the flask elevating device 141 raises the flask holder 144 and returns it to the original position (state on the right side in FIG. 11). The water cooling tank 14
The cooling water 145 of No. 3 is the cooling water circulation unit 46 (FIG. 2).
It is circulated and cooled by.

(9) Water Drop Removal The handling robot 21 has the water drop removal unit 2 shown in FIGS. 9 (c) and 9 (d) showing the sample dissolving flask 2 after water cooling.
4 and inserts it into the water drop removing rubber hole 121 and pulls it out. By this operation, water droplets adhering to the outer surface of the sample dissolving flask 2 during the water cooling are removed. The removed water drops fall into the water drop receiving tank 122 and are discharged from the drain 123.

(10) Addition of Additives Here, the sample solution after cooling is added with ICP, if necessary.
An internal standard element (yttrium Y is used in this example) used in an emission spectroscopic analyzer or the like is added.

Next, the handling robot 21 sets the sample dissolving flask containing the sample solution on the parallel moving rack 178 of the Y addition unit shown in FIG. The flask sensor 16 indicates that the sample dissolving flask 2 has been set.
When 1 is detected, the parallel moving device 176 moves the parallel moving rack 178, and moves the sample dissolving flask 2 to just below the Y addition nozzle 177. The Y-addition electric burette 30 drops the amount of Y (yttrium) solution preset in the sample preparation device control personal computer F in the above step (2) onto the sample dissolution flask 2. The Y solution is held in the additive tank 43, and a predetermined amount is added by the Y addition electric buret 30.

This addition unit is also provided with the same safety device as the acid addition unit (6).

(11) Dilution / constant volume In the fully automatic sample preparation apparatus of this embodiment, the sample dissolution flask 2 using heat-resistant and acid-resistant glass was used as a constant-volume container to prevent contamination of the sample during constant volume. To prevent this, a separate sample dissolution flask 2 is used for each sample. Therefore, in FIG.
As shown in (a), each sample dissolution flask 2 is provided with a simulated reference line 3 made of an Al ribbon below the constant volume reference line 1 by a fixed distance Lf. Then, a method is adopted in which both the marked line 1 of the sample dissolution flask 2 and the sample liquid surface are detected for each sample, and the constant volume is detected by matching both.

Therefore, the dilution / constant volume unit shown in FIG.
As shown in FIG. 6, a sensor stand 172 is provided next to the flask stand 311 and the pillar of the sensor stand 172 is
The elevator 174 holding the liquid level sensor 173 and the simulated gauge sensor 175 was made to move up and down. Both sensors 173,
175 is fixed above and below a U-shaped sensor arm 303 fixed to the elevator 174.
The distance between 3 and 175 is set to the above distance Lf. As described above, since the dilution / constant volume unit detects both the simulated reference line 3 of the sample dissolution flask 2 and the sample liquid surface at different positions, malfunction due to mutual interference between the two sensors 173 and 175 can be prevented. A capacitance type sensor can be used as the liquid level sensor, and an optical sensor such as an infrared sensor can be used as the lower simulated gauge line sensor 175 that detects the simulated gauge line (Al ribbon) 3. Detection signals from the respective sensors 173 and 175 are transmitted to the sample preparation device control personal computer F, and an elevating motor (not shown) housed in the elevator 174 is controlled by the sample preparation device control personal computer F. .

As shown in FIG. 14, when the additive addition process is completed, the parallel moving device 176 further moves the parallel moving rack 178 to move the sample dissolving flask 2 to directly below the dilution water adding nozzle 171. . As shown in FIG. 16, the sample dissolving flask 2 has a dilution water addition nozzle 171.
The computer F for controlling the sample preparation device drives the elevating motor in the elevator 174, and the sensor arm 303
Move up and down. Meanwhile, the personal computer F for controlling the sample preparation device monitors the signal from the simulated reference line sensor 175, and when the simulated reference line sensor 175 detects the simulated reference line 3, the lifting motor is stopped and the sensor arm 303 is kept at that position. Fix it. As a result, the upper liquid level sensor 173 is stopped at the marked line 1 of the sample dissolving flask 2.

Next, the personal computer F for controlling the sample preparation device
Until the liquid level in the sample dissolving flask 2 reaches the marked line 1 (that is, until the liquid level sensor 173 at the marked position detects the liquid level of the sample) by driving the dilution constant volume electric buret 31. Ion-exchanged water in the exchanged water tank 44 is dropped from the dilution water addition nozzle 171 into the sample dissolving flask 2 to dilute and adjust the volume. At this time, in order to shorten the time required for constant volume, rapid injection up to a preset amount (amount smaller than a predetermined constant volume). However, when injected rapidly like this, the liquid surface vibrates greatly,
Since the liquid level sensor 173 cannot correctly detect the height of the liquid surface, the liquid is gradually injected thereafter. In this embodiment, such an injection speed control function is provided in the dilution constant volume electric buret 31 shown in FIG. In the ion exchange water tank 44, the ion exchange water production unit 54 and the ion exchange water pump 45 constantly
Make sure that a certain amount or more of ion-exchanged water can be stored.

The liquid level sensor 173 is the sample dissolving flask 2
Electric burette for dilution constant volume 3 when the liquid level inside is detected
1 stops the dropping of ion-exchanged water. This completes the dilution and constant volume of the sample solution. When the dilution / constant volume of one sample dissolution flask 2 is completed, as shown in FIG. 17, the flask stand moving plate 312 moves by a predetermined distance, and the next sample dissolution flask 2 moves to the dilution water addition nozzle 1
It is placed just below 71. In this way, the dilution and constant volume of many samples are processed continuously.

The dilution / constant volume unit is also provided with the same safety device as in the case of the acid addition (6).

Upon completion of this dilution / constant volume process, the parallel moving device 176 sets the parallel moving rack 178 (and the sample dissolving flask 2 set therein) to the original position (FIG. 14).
State). As a result, the handling robot 2
1 can hold the sample dissolving flask 2.

(12) Stirring Dilution so that no error due to concentration segregation occurs during analysis.
The sample solution after the constant volume is sufficiently stirred by the stirring unit 16.

The handling robot 21 conveys the sample dissolving flask 2 containing the diluted and fixed volume sample solution to the stirring unit 16 (FIG. 12). Stirring unit 16
In the above step (2), stirring is performed for a preset time in the sample preparation device control personal computer F.

(13) Filtration In the fully-automatic sample preparation device of the present embodiment, in order to omit the washing of the residue when collecting the filtrate, a so-called dry filtration system is adopted in which the sample solution is filtered after a fixed volume to obtain the filtrate. ing. Therefore, the filtration unit of this embodiment is configured as follows. First, when the residue is analyzed separately from the filtrate, it is necessary to wash the residue. Therefore, in the apparatus of this example, as shown in FIG. 19, the residue is separated from the container 9 for receiving the filtration. Container (drain funnel) for receiving washing liquid 19
9 was prepared, and the filtrate at the time of filtration and the washing liquid at the time of washing were received in separate containers 9, 199, respectively. Then, a turntable 191 for alternately setting these containers 9, 199 in the filtration chamber 184, and
Air cylinder 197 and rotary motor 1 for raising and lowering it
86 is provided. Further, in order to shorten the filtration time, the suction filtration method was adopted, and the suction port 198 was provided in the filtration chamber 184. The container 199 for receiving the washing liquid is a discharge funnel, and the drain port 20 is provided at the bottom thereof so that the washing liquid of the residue can be immediately discharged.
0 is set.

Further, the funnel is divided into a filtration chamber 184 and a funnel taper frame 182 so that the filter paper cartridge 8 can be replaced for each sample, and the funnel taper frame 182 is raised by the funnel lifting air cylinder 196 to raise the filtration chamber. 1
It was lifted from 84 and the filter paper cartridge 8 was set in between. Filtration chamber 184 after setting the filter paper
The close contact between the filter paper cartridge 8 and the funnel taper frame 182 is maintained by the dead weight of the funnel taper frame 182 (therefore, a weight is added to the funnel taper frame 182) and the O-ring 183. An O-ring 185 is also provided at the lower edge of the filtration chamber 184, which ensures the close contact between the filtration chamber 184 and the turntable 191.

The filter paper 8 is of a cartridge type so that it can be easily handled by the handling robot 21. As shown in FIG. 7C, the filter paper cartridge 8 has a filter paper 5
Is sandwiched between a filter paper fixing ring 4 and a filter paper supporter 6 and fixed to a filter paper holder 7. A large number of filter paper cartridges 8 are prepared in the filter paper supply unit. As shown in FIG. 20, the filter paper supply unit is provided with three filter paper cartridge holders 14 each capable of storing a maximum of 100 filter paper cartridges 8. The three filter paper cartridge holders 14 have different types (A, B
(3 types of C and C), a filter paper cartridge 8 in which filter papers (fifth kind of filter paper) of 5) are set, and the sample preparation device controlling personal computer F stores one of the filter paper cartridge holders 1.
By operating the air cylinder 212 of No. 4, the filter paper cartridge 8 according to the preset conditions can be supplied. The filter paper cartridge 8 is taken out by pushing the push rod 211 with the air cylinder 212 and pushing out the filter paper cartridge 8. A robot 21 for handling the extruded filter paper cartridge 8
And feed it to the filtration unit (FIGS. 18 and 19). Further, a filter paper cartridge sensor 214 is provided, and when the number of filter paper cartridges 8 falls below a predetermined number, an alarm panel 39 is displayed, and when the filter paper cartridges 8 of the filter paper cartridge holder 14 are exhausted, other filter paper cartridge holders 14 are automatically provided. The filter paper cartridge 8 is taken out.

As the container 9 for receiving the filtrate, a beaker made of poly was used for convenience of use in the subsequent analysis (FIG. 7).
(B)). All the other parts are made of resin such as vinyl chloride or Teflon in consideration of acid resistance, or the surface of metal is coated with resin.
The beaker 9 used here is stored in a beaker unit. As shown in FIG. 21, the beaker unit of this embodiment is provided with two beaker holders 17, and a maximum of 100 beakers 9 can be stored. The handling robot 21 grips the lower part of the beaker 9 protruding from the lower part of the beaker holder 17 and pulls it out of the beaker holder 17. Then, it is once placed on the beaker holding table 223, held again so as to grasp the central portion of the beaker 9, and then conveyed to the filtration unit (FIGS. 18 and 19). As a result, the beakers 9 can be reliably taken out one by one. First, hold the bottom of the beaker 9 and hold the beaker holder 1
The reason for removing from 7 is that if the center part is grasped when pulling out the beaker 2, two beakers may be pulled out at a time. Conversely, set the beaker 9 in the filtration unit while holding the lower part of the beaker 9. This is because the beaker 9 may roll over. Further, the beaker sensor 221 is provided in the beaker holder 17, and when the remaining amount of the beaker 9 becomes low, a warning to that effect is displayed on the alarm panel 39 and the beaker 9 is automatically taken out from another beaker holder 17. There is.

The filtration operation is as follows. The handling robot 21 sets the sample dissolving flask 2 for which the stirring process has been completed in the flask holder 181. The handling robot 21 then takes out the beaker 9 from the beaker holder 17 of the beaker supply unit 18 and places it on the outside (right side in FIG. 19) of the turntable 191. After the beaker 9 is set on the turntable 191, the turntable lifting air cylinder 197 once lowers the turntable 191 and the turntable rotation motor 186 rotates the turntable 191 to move the beaker 9 to the filtration chamber 1.
Move it just below 84. Then, the turntable elevating air cylinder 197 raises the turntable 191 to set the beaker 9 in the filtration chamber 184.

With the funnel lifting air cylinder 196 raising the funnel taper frame 182, the handling robot 2
1 takes out the filter paper cartridge 8 set in the filter paper cartridge holder 14 of the filter paper supply unit 15 and sets it in the funnel position on the filtration chamber 184. When the funnel lifting air cylinder 196 lowers the funnel taper frame 182, the filter paper cartridge 8 is sandwiched and fixed between the funnel taper frame 182 and the filtration chamber 184.

In this state, a suction pump is used to filter the chamber 1.
While sucking the air in 84, the flask holder 181 is rotated by the flask holder rotation motors 193 and 194 to make the sample dissolution flask 2 sideways (2a → 2b), and the sample solution in the sample dissolution flask 2 is filtered with a filter paper 8 Pour onto the top and filter. After a predetermined time, the flask holder rotation motor 19
3, 194 are further operated to completely invert the sample dissolving flask 2 (2c), and all the sample solution is discharged onto the filter paper 8. Thus, the discharge of the sample solution onto the filter paper 8 is 2
Since it is carried out gradually in stages, the scattering of the sample solution is minimized.

Then, after the suction pump is operated for a predetermined time, the suction pump is stopped and the filtration is completed. After a predetermined time, when the pressure in the filtration chamber 184 returns to normal pressure, the turntable 191 is lowered by the turntable lifting air cylinder 197, and the turntable rotation motor 18
The filtrate beaker 9 is brought to the outside of the turntable 191 by 6. As a result, the drain funnel 199 is set in the filtration chamber 184.

Even if the sample dissolving flask 2 is completely inverted as shown by 2c in FIG. 18, the residue remains on the inner wall of the sample dissolving flask 2. A flask washing nozzle 187 is provided to wash off the residue on the filter paper 8.
First, the flask holder elevating air cylinder 195 raises the flask holder 181 (2d), and the nozzle rotation motor 188 rotates the flask washing nozzle 187,
Bring it just below the mouth of the sample dissolution flask 2. next,
The flask holder 181 is lowered so that the sample dissolving flask 2 covers the flask washing nozzle 187. In this state, the washing water pump 45 jets the ion-exchanged water from the washing nozzle 187 for a predetermined time, and the sample dissolving flask 2
The inner wall of the sample is washed to wash away all the residue in the sample dissolving flask 2 on the filter paper 8. When the inside of the sample dissolving flask 2 has been washed, the flask holder 181 and the washing nozzle 187 are returned to their original positions.

Next, the funnel washing shower 189 is set on the funnel taper frame 182 by the shower rotation motor 190. Then, the washing water pump 45 spouts ion-exchanged water from the funnel washing shower 189 for a predetermined time, and the filter paper 8
Wash the upper residue. At this time, the ejection time of the ion-exchanged water is arbitrarily set according to the amount of the residue and the like to prevent insufficient cleaning of the residue. In addition, the washing liquid is the drainage port 2 of the drainage funnel 199.
Direct discharge from 00 with an aspirator.

When the washing of the residue on the filter paper 8 is completed, the funnel washing shower 189 is returned to its original position and the filtration chamber 1
After waiting for a predetermined time until the inside of 84 returns to the normal pressure, the turntable 191 is lowered by the turntable lifting air cylinder 197. Further, the funnel elevating air cylinder 196 raises the funnel taper frame 182, and the handling robot 21 transports the filter paper cartridge 8 to the filter paper rack 23 by the operation reverse to that of the above setting and stores it. Further, the sample dissolving flask 2 is conveyed to the flask holding holder 22 by the handling robot 21, held there, and then returned to the flask rack 19.

Also in the present filtration unit, a flask sensor, a filter paper sensor and a beaker sensor are provided as safety devices so that the filtration operation is not started when an alarm occurs in any of the sensors.

(14) Transport to the analyzer The beaker 9 containing the sample solution after filtration is handled by the handling robot 21 by the turntable 19 of the filtration unit.
1 is conveyed from above to the position of the beaker moving manipulator 26 at the tip of the analysis-waiting beaker stocker 27. Here, the beaker 9 is transferred from the handling robot 21 to the beaker moving manipulator 26, and the beaker 9 is conveyed to the next position by the beaker moving manipulator 26 moving on the rail 232.

Considering that when the sample analysis takes a long time, the ICP emission spectroscopic analyzer J waits for the analysis, and as shown in FIG.
In 7, it is possible to wait up to 10 samples for analysis.
When the ICP emission spectroscopic analyzer J is stopped, the beakers 9 are stored in the analysis-waiting beaker stocker 27, and when the number of analysis-waiting beakers 9 exceeds the analysis-waiting beaker stocker 27, a new sample is added. It does not start the preparation process. The presence / absence of the analysis-waiting beakers 9 and the number thereof (if present) are detected by a beaker sensor 231 provided beside the beaker stocker 27.

A place called a suction position is provided at a predetermined position of the beaker stocker 27. When the beaker 9 is placed at this suction position, the sample solution is sucked from the auto sampler 10. The movement of the beaker 9 in the analysis waiting state to this suction position is performed by sliding the beaker 9 with the other analysis waiting beakers 9 by means of a belt conveyor.

(15) Analysis The sample solution in the beaker 9 set at the suction position on the beaker stocker 27 is analyzed. In addition, the sample inhalation during analysis can be used during manual analysis as well.
The autosampler 10 was used, and the sample suction tube was moved to the suction position. First, the sample solution in the beaker 9 at the suction position is sucked by the autosampler 10 and supplied to the sample stand M of the ICP emission spectrum analyzer J. At this time, the solvent used in the auto sampler 10 is automatically supplied by the solvent tank 55 for the auto sampler and the solvent supply pump 56 for the auto sampler so that a constant amount or more is constantly stored.

When the sample solution is analyzed by the ICP emission spectroscopic analyzer J, the result is displayed on the CRT of the personal computer A for controlling the analyzer and printed out if necessary. Furthermore, it is also possible to send the data to a higher-level computer or the like after the data transmission personal computer D has performed a weighing correction and the like on the analysis result.

(16) Storage of Analyzed Samples When the analysis is completed, the belt conveyor of the beaker stocker 27 is rotated to move the beaker 9 containing the analyzed sample solution from the suction position, and to sequentially store the next sample solution. Set the beaker 9 to the suction position.

As shown in FIGS. 22 and 23, the beaker 9 for which analysis has been completed is sequentially moved from the suction position to the beaker unloading manipulator 28 by the belt conveyor, and when it reaches the end, it is unloaded. Manipulator 2
It is gripped by 8. The carry-out manipulator 28 holding the beaker 9 is lifted by the manipulator lifting device 241 (FIG. 23 (b)). As a result, the beaker 9 is transported laterally along the manipulator rail 29 (FIG. 23 (a)) to the analyzed beaker rack 37, where it is stored. This analyzed beaker rack 37 has a maximum of 7
0 samples can be stored. The analyzed beaker rack 37 is provided with a beaker sensor, and when the number of stored beakers is exceeded, preparation of a new sample is not started. In addition, the analyzed beaker rack is provided on the outer side surface of the main body in order to prevent acids from entering the facility due to the fall of the beaker.

As described above, in the fully-automatic sample preparation apparatus of this embodiment, the handling robot 21 is used to sequentially transfer the sample between the respective processing units, so that a series of solid samples can be analyzed. Treatments are performed serially for one sample and sequentially for multiple samples. All of these operations are performed by the two sequencers 48, 49, the robot control unit 40, the parallel movement device control unit 41, and the sample preparation device that controls these and sets the processing conditions and the like of the device of each processing unit. All are automatically performed by the control personal computer F. Further, alarms such as abnormality of each unit equipped with the sensor and each device are all displayed on the CRT of the alarm panel 39 and the sample preparation device controlling personal computer F. Furthermore, in order to perform the minimum processing to avoid the risk of power failure,
An uninterruptible power supply 50 is provided.

In the fully automatic sample preparation device of this embodiment, 1
The time required to prepare one sample is about 40 minutes, but each processing unit is independent, and each heating / melting, cooling, and filtration processing unit, which requires a long processing time, requires 2 units each.
Since the set is provided, the preparation of another sample can be started while the preparation of one sample is performed (sequential progress), and the interval is as short as about 7 minutes. Therefore, even if the number of analysis samples is large, efficient analysis with a short sample waiting time becomes possible.

[0080]

In the automatic sample preparation device according to the present invention, the control unit controls the handling robot so that the container containing the solid sample or the sample solution is heated and dissolved, the cooling unit, the constant volume unit, the stirring unit, It sequentially transfers between the respective parts of the filtration part, and also controls the individual processing in each part. Then, the sample solution prepared by each treatment is automatically placed in a predetermined analysis waiting device. This allows fully automated sample preparation without the need for operator intervention. Furthermore, by automatically collecting the sample solution from this analysis waiting position by an autosampler, which is an analyzer or its peripheral device, it is possible to completely automate the process from sample preparation to analysis.

Further, in the heating and melting section of the automatic sample preparation device according to the second aspect, since the microwave heating method is adopted, wasteful heat generation is minimized, and the processing speed is sacrificed. Without doing so, the heating device can be made as small as possible. Further, since the local exhaust is adopted in which the acid vapor generated at the time of heating is guided from the cap to the water flow aspirator, a large draft chamber is not required, and the problems of acid vapor leakage and surrounding corrosion do not occur. Further, the recovered acid vapor is dissolved in water as it is by the water flow aspirator, which facilitates treatment of harmful acid vapor.

In the constant volume section of the automatic sample preparation device according to the third aspect, the liquid level sensor comes to a predetermined liquid level position when the simulated marked line sensor detects the simulated marked line. The problem of sensor interference does not occur, and it is possible to accurately detect whether or not the liquid surface has reached a predetermined position defined for each container. As a result, it is possible to perform an automated constant volume that does not vary by the operator. Moreover, since a separate container can be used for each sample, there is no concern about contamination between samples, and highly accurate analysis can be performed.

In the filtration section of the automatic sample preparation device according to the fourth aspect, since the suction filtration is performed, the filtration can be processed at a high speed. Further, when the filtrate container on the container stand is placed in the suction chamber, the filtrate can be recovered from the sample solution, and then the container stand is raised and lowered and rotated to place the washing liquid container in the suction chamber, and the filter paper The residue (solid component in the sample solution) can now be recovered by washing the above residue. Thus, in the automatic sample preparation device according to claim 4, both the filtrate and the residue can be completely recovered.

[Brief description of drawings]

FIG. 1 is a plan view of an upper portion of a fully automatic sample preparation device for an ICP emission spectroscopic analyzer which is an embodiment of the present invention.

FIG. 2 is a plan view of a lower portion of the fully automatic sample preparation device according to the embodiment.

FIG. 3 is a plan view of the roof of the fully-automatic sample preparation device of the example.

FIG. 4 is a side view of the entire fully-automatic sample preparation device of the embodiment.

FIG. 5 is a plan view showing an example of the arrangement of a fully automatic sample preparation device and an ICP emission spectroscopic analysis device of the embodiment, and a personal computer for controlling them.

FIG. 6 is a side view of the handling robot and a plan view of a hand unit.

FIG. 7 is a perspective view (a) of a sample dissolving flask, a perspective view (b) of a beaker, and an exploded perspective view (c) showing a configuration of a cartridge filter.

FIG. 8 is a plan view (a) and a side view (b) of the flask rack.

9A and 9B are a plan view (a), a side view (b), and a plan view (c) and a side view (d) of a water drop removing unit, respectively.

FIG. 10 is a plan view (a) and a vertical sectional view (b) of the sample heating / melting apparatus.

FIG. 11 is a vertical sectional view of the cooling unit.

FIG. 12 is a side view of the stirring unit.

FIG. 13 is a side view (a) and a plan view (b) of the acid addition unit.

FIG. 14 is a side view (a) and a plan view (b) of an additive addition and dilution constant volume unit.

FIG. 15 is a schematic configuration diagram showing an overall configuration of a constant volume unit.

FIG. 16 is a side view showing the configuration of the main part of the constant volume unit.

FIG. 17 is a front view showing a state of continuous processing in the constant volume unit.

FIG. 18 is a front view of the filtration unit.

FIG. 19 is a side view of the filtration unit.

FIG. 20 is a plan view (a) and a side view (b) of the filter paper supply unit.

FIG. 21 is a plan view (a) and a side view (b) of the beaker supply unit.

FIG. 22 is a side view (a) and a plan view (b) of a beaker stocker waiting for analysis.

FIG. 23 is a plan view (a) and a side view (b) of the analyzed beaker unloading device.

[Explanation of symbols]

1 ... Mark line 2 ... Sample dissolving flask 3 ... Constant volume simulated mark line 4 ... Filter paper fixing ring 5 ... Filter paper 6 ... Filter paper supporter 7 ... Filter paper holder 8 ... Filter paper cartridge 9 ... Analytical beaker 10 ... Autosampler 11 ... Turn Table 12 ... Filtration unit A 13 ... Robot moving rail 14 ... Filter paper cartridge holder 15 ... Filter paper supply unit 16 ... Stirring unit 17 ... Beaker holder 18 ... Beaker supply unit 19 ... Flask rack 20 ... Cooling unit 21 ... Handling robot 22 ... Holding flask Replacement holder 23 ... Filter paper rack 24 ... Water drop removing unit 25 ... Filtration unit B 26 ... Manipulator for moving beaker 27 ... Waiting beaker stocker 28 ... Manipulator for carrying out beaker 29 ... Manipulator rail 30 ... Electric buret 31 for Y addition ... Diluting constant volume Electric burette 32 ... Y addition position (remaining drop receiving beaker) 33 ... Acid addition position (remaining drop receiving beaker) 34 ... Acid addition electric buret 35 ... Microwave type sample dissolving device 36 ... Acid vapor discharge cap 37 ... Analyzed Beak rack 38 ... Distribution board unit 39 ... Alarm panel 40 ... Robot control unit 41 ... Rail control unit 42 ... Acid tank 43 ... Additives tank 44 ... Ion exchange water tank 45 ... Ion exchange water pump, filtration pump, washing water pump 46 ... Cooling water circulation unit 47 ... Cooling fan 48 ... Sequencer B 49 ... Sequencer A 50 ... Uninterruptible power supply 51 ... Exhaust port 52 ... Exhaust fan 53 ... Stand leg 54 ... Ion exchange water production unit 55 ... Solvent tank 56 for autosampler ... Solvent supply pump for autosampler 57 ... 1st han 58: Second hand 101: Handle 102 ... Flask setting position 103 ... Flask rack stand 104 ... Flask rack cartridge 105 ... Cartridge stopper 111 ... Flask holding stand 121 ... Water drop removing rubber hole 122 ... Water drop receiving tank 123 ... Drain 131 ... Sample hole 132 ... Magnetron 133 ... Aspirator 134 ... Cap opening / closing air cylinder 135 ... Connecting rod 136 ... Fixed exhaust pipe 137 ... Gas exhaust pipe 138 ... Water faucet 139 ... Drainage port 141 ... Flask lifting device 142 ... Air cooling fan 143 ... Water cooling Tank 144 ... Flask holder 145 ... Circulating water 151 ... Stand 152 ... Manipulator 161 ... Flask sensor 162 ... Parallel movement rack 163 ... Parallel movement device 164 ... Acid addition nozzle 171 ... Dilution water addition nozzle 1 2 ... Sensor stand 173 ... Liquid level sensor 174 ... Elevator 175 ... Simulated mark line sensor 176 ... Parallel moving device 177 ... Y addition nozzle 178 ... Parallel moving rack 181 ... Flask holder 182 ... Funnel taper frame 183 ... O-ring 184 ... Filtration chamber 185 ... O-ring 186 ... Turntable rotation motor 187 ... Flask washing nozzle 188 ... Nozzle rotation motor 189 ... Funnel washing shower 190 ... Shower rotation motor 191 ... Turntable 192 ... Turntable lifting rail 193 ... Flask holder rotation motor (1) 194 ... Flask holder rotation motor (2) 195 ... Flask holder lifting air cylinder 196 ... Funnel lifting air cylinder 197 ... Turntable lifting air cylinder 198 ... Suction port 199 ... Drain funnel 200 ... Drain port 211 ... Shu rod 212 ... Air cylinder 213 ... Stocker upper lid 214 ... Filter paper cartridge sensor 221 ... Beaker sensor 222 ... Stocker upper lid 223 ... Beaker holding table 231 ... Beaker sensor 232 ... Manipulator rail 233 ... Manipulator moving motor 241 ... Manipulator lifting device A ... ICP control personal computer. (Including printer and CRT) B ... Working table for ICP C ... PC rack D ... Data transmission PC (including printer and CRT) E ... PC rack F ... PC for sample preparation device control (including printer and CRT) G … Working machine for balance H… PC for weighing (including printer and CRT) I… Electronic balance J… ICP emission spectroscopic analyzer K… Automatic standardization unit L… Automatic sample preparation device

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Tetsuro Kitade 1-chome, Kawasaki-dori, Mizushima, Kurashiki City Kawatetsu Techno-Research Corp.

Claims (4)

[Claims] 1. An automatic sample preparation device for preparing a sample solution that can be analyzed by a chemical analyzer from a solid sample, comprising: a) a heating dissolution section for preparing a sample solution by adding an acid to a solid sample and heating. And b) a cooling section for cooling the sample solution, c) a constant volume section for adding a diluting solution so that the cooled sample solution has a predetermined volume, and a d) a stirring section for stirring the sample solution. , E) Between the above-mentioned parts arranged at predetermined positions, which are equipped with a filtering part for filtering the sample solution and separating it into a filtrate and a residue, and f) a hand for holding a predetermined container holding the solid sample or sample solution. G) a handling robot that moves on the rails installed on the rail, and g) control the above-mentioned parts so that they operate under preset conditions, and transfer the container containing the solid sample or sample solution between the parts. , Handle it so that it is put in the designated analysis waiting position. An automatic sample preparation device, comprising: a control unit that controls the operation of the robot. 2. The heating and dissolving part is a) a microwave heating device for heating a container containing a solid sample and an acid; b) a heating chamber surrounding the container; An openable and closable cap with a steam outlet, d) a connection channel that connects to the acid vapor outlet of the cap when the cap is closed and connects to a water flow aspirator, and e) a gas in the connection channel due to the water flow. The automatic sample preparation device according to claim 1, further comprising: a water flow aspirator that sucks the gas and mixes the sucked gas with water. 3. A container having a simulated reference line at a position separated from the position of the liquid surface, which is the target of constant volume, by a predetermined distance is used, and the constant volume section detects a) the simulated reference line. The simulated level sensor, b) the liquid level sensor provided at the predetermined distance from the simulated level sensor, and c) the simulated level sensor and liquid level sensor at the specified distance. The automatic sample preparation device according to claim 1, further comprising: a sensor moving device that moves the device as it is. 4. The filter section comprises: a) a funnel that holds a cartridge-type filter paper in an airtight manner; b) a suction chamber that airtightly encloses the lower part of the funnel and the lower part is open; and c) sucks air in the suction chamber. It is possible to simultaneously mount a suction pump that operates, d) a filtrate container that receives the filtered sample solution, and a washing liquid container that receives the washing liquid that is used to wash the residue left on the filter paper. And a container stand that hermetically closes the lower part of the suction chamber when it rises, and the control unit controls the handling robot so that e) the process in the constant volume unit is followed by the process in the filter unit. At the same time, f) controlling the raising and lowering and rotation of the container stand so that the filtrate container is put in the suction chamber when the sample solution is collected and the washing liquid container is put in the suction chamber when the residue is washed. The automatic sample preparation device described.