JP2007163189A - Weighing method, weighing device and preprocessing apparatus for sample analysis - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To improve the accuracy of the preprocessing of weighing and the working environment by inhibiting the flying up of the sample. <P>SOLUTION: The weighing device 44 is provided with a sample supply means for supplying a sample to the extraction vessel 48, while the sample vessel 47 is tilted to the prescribed angle while rotating, a measurement means for supplying sample to the extraction vessel 48 and for measuring the sample, and the control means 44c for controlling the sample supply means so as to be a previously set weighing value. The sample vessel 48 is tilted to the prescribed angle and is rotated by the sample supply means, the sample stored in the sample vessel 47 is supplied to the extraction vessel 48 set to the measurement means, and the sample supply means is controlled so as to be the sample weighted value of the previously set weighted value, based on the measurement information. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to, for example, a weighing method, a weighing apparatus, and a sample analysis pretreatment apparatus for measuring a weight of a sample in a process of performing a pretreatment for soil analysis.

For example, in the soil analysis pretreatment process, the rotating operation of the motor is converted into a swiveling operation in the fixed sample container, the vibration is applied by the vibrator, and the sample is supplied to the extraction container. Tilt and adjust the angle / vibration frequency when the first sample falls into the extraction container, supply at the speed appropriate for the sample, measure this sample with a scale, and when the required amount is reached, Stop supplying. In addition, there is a type in which the volume corresponding to the specific gravity of the reagent is measured with a reagent pump with respect to the measured sample weight, the reagent is supplied to the sample from the nozzle, and the amount of the sample and the reagent is measured with a scale ( For example, Patent Document 1).
JP2003-161680

  However, because the sample container is vibrated with a vibrator and the sample is supplied to the extraction container, a large amount of sample may drop at once, and the variation is large, and the accuracy of measuring the required sample amount may be inferior. there were.

  In addition, since the sample container is vibrated by the vibrator, the sample rises due to the vibration, and the working environment is deteriorated.

  The present invention has been made in view of this point, and an object thereof is to provide a weighing method, a weighing apparatus, and a sample analysis pretreatment apparatus that can improve the accuracy of pretreatment of a sample.

  In order to solve the above problems and achieve the object, the present invention is configured as follows.

  According to the first aspect of the present invention, the sample container is tilted and rotated by a predetermined angle by the sample supply means, the sample stored in the sample container is supplied to the extraction container set in the measurement means, and based on the measurement information in advance. The weighing method is characterized in that the sample supply means is controlled so as to have a set sample weighing value.

  The invention according to claim 2 sets the sample container supplied with the sample to the measuring means, measures the measured value of the sample, and actually injects the chemical solution having the set weight concentration from the measurement result of the measured value of the sample The weighing method is characterized in that the amount is set, and the chemical solution is supplied by controlling the chemical solution supply means so that the set amount of the actually injected chemical solution is obtained.

  The invention according to claim 3 is characterized in that the sample supply means tilts the supply port of the sample container as a fulcrum and rotates about the supply port of the sample container as an axis. It is a weighing method.

  The invention according to claim 4, wherein the sample container is tilted to a first inclination, rotated at a first speed to supply a sample and perform rough weighing, and when the weighing exceeds the rough weighing value The sample container is returned from the first inclination to the second inclination, the rotation is reduced to a second speed slower than the first speed, the sample is supplied, and a fine weighing is performed. 4. The weighing method according to claim 1, wherein when the supply weighing value before the weighing value is exceeded, the rotation of the sample container is stopped.

  The invention according to claim 5 includes a sample supply means for supplying the sample to the extraction container by tilting and rotating the sample container at a predetermined angle, a measurement means for supplying the sample to the extraction container and measuring, and the measurement information And a control means for controlling the sample supply means so as to obtain a preset weight value of the sample based on the weighing apparatus.

  The invention according to claim 6 includes a chemical solution supply means for supplying a chemical solution to an extraction container containing a sample, a measurement means for measuring a measured value of the sample in the sample container, and a set weight based on a measurement result of the measured value of the sample. A weighing apparatus comprising: setting means for setting an actual injection amount of the chemical liquid to be a concentration; and control means for controlling the chemical liquid supply means so as to be the actual liquid injection amount of the set chemical liquid It is.

  The invention according to claim 7 is characterized in that the sample supply means includes an inclination means for inclining the supply port of the sample container around a fulcrum, and a rotation means for rotating about the supply port of the sample container. 6. The weighing apparatus according to claim 5, wherein

The invention according to claim 8, wherein the control means controls the sample supply means, the sample container is tilted to a first inclination, rotated at a first speed, and a sample is supplied to roughly measure the weight. Done
When the weighing exceeds the rough weighing value, the sample container is returned from the first inclination to the second inclination, and the rotation is reduced to a second speed slower than the first speed to supply the sample. 8. The weighing apparatus according to claim 5, wherein fine weighing is performed and rotation of the sample container is stopped when weighing exceeds a supply weighing value before a set weighing value.

  The invention according to claim 9 is a sample analysis pretreatment apparatus comprising the weighing apparatus according to any one of claims 5 to 8.

  The invention according to claim 10 is the sample analysis pretreatment apparatus according to claim 9, wherein the sample is soil.

  With the above configuration, the present invention has the following effects.

  In the first and fifth aspects of the present invention, the sample container is tilted and rotated at a predetermined angle, and the sample is supplied to the extraction container so as to have a preset value of the supplied sample based on the measurement information. The sample can be supplied little by little and the sample supply amount can be adjusted, so that the accuracy of sample pretreatment is improved. Further, by supplying the sample in small amounts, the sample can be prevented from flying up and the working environment is improved.

  In the invention according to claim 2 and claim 6, the actual solution volume of the drug solution having the set weight concentration is set from the measurement result of the measured value of the sample, and the drug solution is set to the set actual solution volume of the drug solution By controlling the supply means and supplying the chemical solution, the pretreatment accuracy of the sample is improved.

  In the inventions of claim 3 and claim 7, the supply port of the sample container is always positioned on the extraction container by inclining the supply port of the sample container around the fulcrum and rotating around the supply port of the sample container. By doing so, scattering of the sample can be prevented, and the sample can be reliably supplied to the extraction container.

  In the invention according to claim 4 and claim 8, the sample container is tilted to the first inclination, rotated at the first speed, the sample is supplied and a rough weighing is performed, and the rough weighing value is measured. If exceeded, return the sample container from the first tilt to the second tilt, reduce the rotation to the second speed slower than the first speed, supply the sample, perform fine weighing, and the weighing is set When the supply weighing value before the value is exceeded, the sample can be accurately supplied to the extraction container by stopping the rotation of the sample container.

  The invention according to claim 9 is provided with the weighing device according to any one of claims 5 to 8, and the pretreatment accuracy of the sample is improved in the pretreatment of the sample analysis.

  In the invention according to claim 10, the sample is soil, and the pretreatment accuracy of the sample is improved in the pretreatment of soil analysis.

  Hereinafter, embodiments of the weighing method, the weighing apparatus, and the sample analysis pretreatment apparatus of the present invention will be described. However, the embodiments of the present invention show the most preferable embodiments of the present invention, and the present invention is not limited thereto. Not.

  1 to 4 show the configuration of the sample analysis pretreatment apparatus. FIG. 1 is a plan view, FIG. 2 is a front view, FIG. 3 is a left side view, and FIG.

  This sample analysis pretreatment device 1 shows a sample that is sampled with a pipette in order to perform various tests on soil as a sample, but performs various tests such as a chemical experiment or a water quality test, a microorganism test, etc. Applicable to.

  This sample analysis pretreatment apparatus 1 includes a frame 2, and a caster 3 with an adjuster is provided at the lower part of the frame 2 so that it can be smoothly moved and adjusted in height. Yes. The frame 2 includes a front-stage processing unit 20 and a rear-stage processing unit 30 that are divided into two.

  An air device 21, a pump 22, and the like are disposed at the lower part of the upstream processing unit 20, and a chemical tank 23 is stored on the chemical tank storage rack 99. The chemical tank storage rack 99 can be taken in and out of the lower part of the pre-treatment unit 20. When the chemical liquid in the chemical tank 23 runs out, the chemical tank storage rack 99 is pulled out and replaced with a new chemical tank 23.

  A sample rack 40, a lid 41, an extraction rack 42, a shaking rack 43, a weighing device 44, a liquid injection device 45, a transport mechanism 46, and the like are provided in the middle of the front processing unit 20. The sample rack 40 can be taken in and out, and a plurality of sample containers 47 each containing a sample are set in the sample rack 40 side by side. On the lid base 41, a plurality of lids 49 of the extraction container 48 are set side by side. A plurality of empty extraction containers 48 are set side by side in the extraction rack 42, covered with a sample and a chemical solution, and transported from the start station A to the shaking station B by the transport mechanism 46. The transport mechanism 46 includes a roller transport base 46a and an air cylinder 46b. An extraction rack 42 is set on the roller transport base 46a, and the extraction rack 42 is transported by the operation of the air cylinder 46b. The shaking station B is provided with a shaking table 43. The shaking table 43 holds the lid 49 of the extraction container 48 from above and shakes to shake the sample and the chemical solution placed in the extraction container 48. The weighing device 44 includes a supply mechanism 44a and a weighing mechanism 44b, measures the sample in the sample container 47, and puts the sample into the extraction container 48. The liquid injection device 45 puts a predetermined amount of the chemical into the extraction container 48 containing the sample.

  A pre-stage working robot device 24 is provided at the top of the pre-stage processing unit 20. The former stage work robot device 24 is constituted by a three-axis robot, and includes a drive shaft 24a, a guide shaft 24b, a moving shaft 24c, a robot 24d, and a drive motor 24e. The drive shaft 24a and the guide shaft 24b are arranged in parallel, and a moving shaft 24c is stretched over the drive shaft 24a and the guide shaft 24b. As the drive motor 24e, for example, a servo motor is used, and when the drive motor 24e is driven, the drive shaft 24a rotates in the positive direction or rotates in the negative direction so that the moving shaft 24c moves along the drive shaft 24a and the guide shaft 24b. Go forward and backward. The robot 24d has a horizontal movement motor 24d1 and a vertical movement motor 24d2, and moves back and forth along the movement axis 24c by driving the horizontal movement motor 24d1, and can move in the vertical direction by driving the vertical movement motor 24d2. It has become. For example, stepping motors are used as the horizontal movement motor 24d1 and the vertical movement motor 24d2.

  The robot 24d sets the empty extraction container 48 of the extraction rack 42 to the weighing mechanism 44b of the weighing apparatus 44, and carries the sample container 47 containing the sample of the sample rack 40 to the supply mechanism 44a of the sample supply apparatus 44, thereby measuring the weighing apparatus. When the supply of the sample at 44 is completed, the extraction container 48 containing the sample is carried to the liquid injection device 45, and the sample container 47 is returned to the original sample rack 40. Further, when the supply of the chemical solution to the extraction container 48 in which the sample is placed in the liquid injection device 45 is completed, the extraction container 48 is returned to the original position of the extraction rack 42 and the lid 49 is inserted into the extraction container 48.

  A control device 31, an emergency stop button 32, and the like are disposed below the post-processing unit 30. The control device 31 automatically controls the sample analysis pretreatment device 1 based on the program, and the emergency stop button 32 is forcibly stopped by pressing the emergency stop button 32 when, for example, an abnormality occurs. Can do.

  A filtration rack 60, a pipette rack 61, a pipette discarding section 62, a transport mechanism 63, and the like are provided in the middle of the post-processing section 30. In the filtration rack 60, a plurality of filtration containers 64 are set side by side. In the pipette rack 61, a plurality of pipettes 65 are set side by side. From the pipette discarding unit 62, the used pipette 65 is discarded. The extraction rack 42 is transported from the shaking station B to the filtration station C by the transport mechanism 63 and transported from the filtration station C to the end station D. That is, the transport mechanism 63 is composed of a roller transport base 63a and air cylinders 63b and 63c, and transports the extraction rack 42 of the station B that is shaken by the operation of the air cylinder 63b onto the roller transport base 63a of the filtration station C for extraction. The extraction rack 42 containing the container 48 is stopped at the filtration work position. When the filtration operation is completed, the air rack 63c is operated to convey the extraction rack 42 of the filtration station C onto the roller conveyance table 63a of the termination station D, and the pretreatment is completed. The extraction container 48 is discarded from the extraction rack 42, and an empty extraction container 48 is placed in the extraction rack 42 and set in the start station A.

  On the upper part of the rear stage processing unit 30, a rear stage working robot apparatus 25 is provided, and an operation unit 26 is provided. The operation unit 26 is configured by a touch panel, for example. The rear work robot device 25 is constituted by a three-axis robot, and includes a drive shaft 25a, a guide shaft 25b, a moving shaft 25c, a robot 25d, and a drive motor 25e. The drive shaft 25a and the guide shaft 25b are arranged in parallel, and a moving shaft 25c is stretched over the drive shaft 25a and the guide shaft 25b. As the drive motor 25e, for example, a servo motor is used, and when the drive motor 25e is driven, the drive shaft 25a is rotated in the positive direction or rotated in the negative direction so that the moving shaft 25c is moved along the drive shaft 25a and the guide shaft 25b. Go forward and backward. The robot 25d has a horizontal movement motor 25d1 and a vertical movement motor 25d2, and moves forward and backward along the movement axis 25c by driving the horizontal movement motor 25d1, and can move in the vertical direction by driving the vertical movement motor 25d2. It has become. For example, stepping motors are used as the horizontal movement motor 25d1 and the vertical movement motor 25d2.

  The robot 25d holds the two pipettes 65 of the pipette rack 61, inserts the two pipettes 65 from the lids 48 of the two extraction containers 48 stored in the extraction rack 42, and sucks the sample in the extraction container 48. And the sample is supplied to the two filtration containers 64 of the filtration rack 60. When the filtration in the filtration container 64 is completed, the two pipettes 65 are carried to the pipette disposal unit 62 and discarded.

  As shown in FIG. 1, the sample analysis pretreatment apparatus 1 of this embodiment includes a start station A, a shaking station B, a filtration station C, and an end station D arranged in a straight line as viewed from above, and an extraction rack. 42 can carry each station linearly. In addition, the sample rack 40, the lid 41, and the weighing device 44 are arranged on one side of the start station A and the shaking station B, and the liquid injection device 45 and the drive motor 24e of the front work robot device 24 are arranged on the other side, A filtration rack 60, a pipette rack 61 and a pipette disposal unit 62 are arranged on one side of the filtration station C and the end station D, and a drive motor 25e of the rear stage work robot device 25 is arranged on the other side to effectively use the space. It is a compact arrangement.

  Next, the weighing device 44 will be described in detail with reference to FIGS. FIG. 5 is a plan view of the weighing device, FIG. 6 is a front view of the weighing device, FIG. 7 is a diagram showing the setting state of the sample container, FIG. 8 is a diagram showing the basic operation of the weighing device, and FIG. FIG. 10 is a diagram showing a cap of a sample container according to another embodiment, FIG. 11 is a flowchart of the operation of the weighing device, and FIG. 12 is a diagram showing the operation of the weighing device.

  The weighing device 44 includes a supply mechanism 44a, a weighing mechanism 44b, and a control means 44c. A sample container 47 is set in the supply mechanism 44a by a robot 24d, and an extraction container 48 is set in the weighing mechanism 44b by a robot 24d. Set.

  The supply mechanism 44a constitutes sample supply means for supplying the sample to the extraction container 48 by rotating the sample container 47 at a predetermined angle, moving means 44a1 for reciprocating the initial position and the supply position of the sample container 47, and the sample Inclination means 44a2 for inclining the supply port 47a1 of the container 47 around the fulcrum, and rotation means 44a3 for rotating about the supply port 47a1 of the sample container 47 as an axis. The moving means 44a1 is composed of, for example, a stepping motor, and moves the entire supply mechanism 44a along the guide 44d to move the sample container 47 to the initial position shown in FIGS. 8 (a) and 8 (b) and FIGS. The supply position shown in d) is reciprocated. The tilting means 44a2 is composed of, for example, a stepping motor, and rotates the support shaft portion 44e of the sample container 47 via the gear mechanism 44h to supply the supply port 47a1 of the sample container 47 as shown in FIGS. 8 (b) to (c). Tilt to the fulcrum. The rotating means 44a3 is composed of, for example, a stepping motor, and rotates the holding portion 44f of the sample container 47 via the timing belt 44g to rotate around the supply port 47a1 of the sample container 47 as shown in FIG. 8 (d). .

  The weighing mechanism 44b constitutes a measuring means for supplying a sample to the extraction container 48 and measuring it, and is composed of, for example, an electronic balance, and the measurement information is sent to the control means 44c. The control means 44c is provided in the control device 31, and the control device 31 is provided with a storage means 44i. In the storage means 44i, the weighed value of the sample to be supplied and the injection amount of the reagent are registered in advance. The setting to the storage means 44i is performed by an operator through the operation unit 26.

  The control unit 44c controls the moving unit 44a1, the tilting unit 44a2, and the rotating unit 44a3 of the supply mechanism 44a so as to obtain a preset weighed sample value based on the measurement information.

  Next, the operation of the weighing device 44 will be described with reference to FIGS. The operator registers the inspection items and the number of samples as samples on the touch panel of the operation unit 26, and for example, the soil weighing value and the reagent injection amount are registered in advance in the inspection items. For example, a soil weighing value of 1.0 g and a reagent injection amount of 10 ml (10 ml is assumed to be 10 g, assuming a specific gravity of 1) are registered.

  When the operation is started, the robot 24d sets the sample container 47 and the extraction container 48 in the weighing device 44 [FIG. 11 (a), FIG. 12 (a)]. Next, the sample container 47 moves forward while tilting to an initial tilt (a tilt that does not spill soil). Further, a zero reset signal is transmitted to the electronic balance of the weighing mechanism 44b [FIG. 11 (b), FIG. 12 (b)].

  The sample container 47 tilts to tilt 1, rotates at a speed of 1, and roughly weighs to drop the soil [FIG. 11 (c), FIG. 12 (c)]. The values of slope 1 and speed 1 are adjustment values that can be adjusted and set, for example, when the apparatus is shipped. The measured value of the electronic balance is constantly taken in via communication until the weighing is completed.

  When the weighing exceeds the weighing value 1 (for example, 80 to 90% of the set weighing value), the sample container 47 returns to the inclination 2, and the fine weighing is performed to reduce the rotation to the speed 2 and drop the soil [FIG. 11 (d) , FIG. 12 (d)]. The values of the weighing value 1, the slope 2, and the speed 2 are adjustment values that can be adjusted and set. For example, the values are adjusted when the device is shipped.

  When the weighing exceeds the drop weighing value before the set weighing value, the rotation of the sample container 47 stops and returns to the initial tilt position [FIG. 11 (e), FIG. 12 (e)]. The value of the drop weighing value before the set weighing is an adjustment value that can be adjusted and set, for example, at the time of shipment of the apparatus. When stopped after reaching the set weighing value, the weighing value will exceed, so it is predicted in advance how much soil will fall after stopping and stopped in advance. If the drop weighing value before the set weighing is not reached even after a certain time has elapsed, an error notification is given when the time is over.

  The sample container 47 is retracted to the origin position, and the weighing value is received from the electronic balance [FIGS. 11 (f) and 12 (f)]. When the received weighing value exceeds the weighing error requested by the customer, the weighing error is notified.

  Thus, the weighing value is affected by the tilt angle and rotation speed of the sample container 47. Therefore, the sample container 47 is tilted to the first tilt and rotated at the first speed to supply the sample. If the weighing exceeds the rough weighing value, the sample container 47 is returned from the first inclination to the second inclination, and the rotation is reduced to the second speed slower than the first speed to supply the sample. If the weighing exceeds the supply weighing value before the set weighing value, the rotation of the sample container 47 is stopped to accurately supply the sample from the sample container 47 to the sample container 48. it can.

  Further, the sample container 47 is rotated by tilting to a predetermined angle, and the sample is supplied to the extraction container 48 so as to have a preset value of the supplied sample based on the measurement information, thereby supplying the sample little by little, and The supply amount of the sample can be adjusted, and the preprocessing accuracy of weighing is improved. Further, by supplying the sample in small amounts, the sample can be prevented from flying up and the working environment is improved.

  In addition, by inclining the supply port 47a1 of the sample container 47 as a fulcrum and rotating around the supply port 47a1 of the sample container 47, the supply port 47a1 of the sample container 47 is always located on the extraction container 48, so that the sample The sample can be reliably supplied to the extraction container 48.

  In this embodiment, as shown in FIGS. 9 (a) to 9 (c), the sample container 47 has a configuration in which a cap 47a is covered on a container body 47b, and a conical shape having a supply port 47a1 at the tip of the cap 47a. The aperture shape is formed as follows. The sample can be supplied little by little by supplying the sample from the supply port 47a1 of the cap 47a and reducing the supply port 47a1. As shown in FIG. 10, the cap 47a may be formed in a conical throttle shape having a supply port 47a1 at the tip, and a spiral groove 47a2 may be formed inside the cap 47a. The spiral groove 47a2 spirals in the same direction as the rotation direction when the sample is supplied, and is formed continuously to the supply port 47a1. The cross-sectional shape of the spiral groove 47a2 is formed in a U-shaped cross section as shown in FIG. 10C, but it may be a V-shaped cross section and is not particularly limited. As described above, when the spiral groove 47a2 is formed inside the cap 47a, the sample is guided by the spiral groove 47a2 by rotating the sample container 47 and moved to the supply port 47a1, and the sample is not clogged. A sample can be dropped and supplied from the mouth 47a1.

  Next, the liquid injection device 45 will be described in detail with reference to FIGS. FIG. 13 is a plan view of the liquid injection device, FIG. 14 is a view showing a set state of the extraction container, FIG. 15 is a view showing the liquid injection state, and FIG. 16 is a flowchart of the operation of the liquid injection device.

  The liquid injection device 45 includes a supply mechanism 45a and a weighing mechanism 45b. The supply mechanism 45a is provided with a chemical solution supply nozzle 50, and an extraction container 48 is set in the weighing mechanism 45b by a robot 24d. The supply mechanism 45a constitutes a chemical solution supply unit.

  The supply mechanism 45a has moving means 45a1 for reciprocating the chemical solution supply nozzle 50 between the drain discharge position and the supply position. This moving means 45a1 is composed of, for example, an air cylinder, and the chemical liquid supply nozzle 50 is retracted to the drain discharge position, advances during the chemical liquid supply, moves the chemical liquid supply nozzle 50 to the supply position, and supplies the chemical liquid to the extraction container 48. Supply. When the chemical solution supply nozzle 50 is retracted to the drain discharge position, the chemical solution that drops from the chemical solution supply nozzle 50 is discarded from the drain discharge unit 51.

  The weighing mechanism 45b constitutes a measuring means for supplying the measuring solution to the extraction container 48 for measurement, and is constituted by, for example, an electronic balance, and the measurement information is sent to the control means 44c. The control unit 44c includes a setting unit that sets an actual injection liquid amount that becomes a set weight concentration from the measurement result of the weighed value, and a supply mechanism that configures the chemical liquid supply unit so that the actual liquid injection amount of the set chemical liquid is obtained Control 45a.

  Next, the operation of the liquid injection device 45 will be described with reference to FIG. As a step before the liquid injection device 45 is operated, the robot 24d sets the extraction container 47 in the weighing device 44 as shown in FIGS. 5 to 11 (step a1). In the weighing device 44, a zero reset signal is transmitted to the electronic balance, and the actual injection liquid amount that becomes the set weight concentration is set in the control means 44c from the measurement result of the soil weighing value. As a requirement for accuracy, there is a weight concentration ratio of the soil liquid in addition to the soil weighing error. For example, in the case of setting 1.0 g of soil and 10 ml of liquid injection, it is required to be “weight concentration 10% (error ± 5%)”. Therefore, if the weighed value of the soil is 1.1 g, it is necessary to inject 11 ml, and the necessary actual amount of solution is calculated by the control means 44c from the result of weighing the soil and the set reference weight concentration. (Step a2).

  Then, in the liquid injection device 45, reagent injection is started. When the amount of dropped liquid before the actual liquid volume is exceeded, liquid injection is stopped (step a3). The amount of dropped liquid before the actual liquid volume is an adjustment value that can be adjusted and set, for example, when the apparatus is shipped. As in the case of weighing the soil, if the liquid injection is stopped after reaching the actual liquid injection volume, it will be over. Therefore, it is predicted in advance how much the reagent will be dropped after the liquid injection is stopped and stopped in advance.

  The control means 44c receives the amount of liquid injection, and notifies the error by the display device 90 when the weight concentration ratio of the soil liquid exceeds a set value, for example, 10% ± 5%. Further, for each sample specimen, the measured value of the soil, the amount of liquid to be poured, and the weight concentration are displayed on the display device 90 and recorded by the recording device 91 (step a4). Then, the robot 24d returns the extraction container 48 to the extraction rack 42 (step a5).

  In this way, the actual injection amount of the chemical solution with the set weight concentration is set from the measurement result of the sample weighing value by the weighing mechanism 45b, and the supply mechanism 45a is controlled so as to become the set actual injection amount of the chemical solution. By supplying the chemical solution, the pretreatment accuracy of the liquid injection is improved.

  When the medium solution in the liquid injection device 45 is finished, the robot 24d takes out the lid 49 from the lid base 41 and inserts it into the extraction container 48 as shown in FIGS. The lid 49 is integrally formed of rubber and includes a cylindrical portion 49a, an upper film 49b, and a lower film 49c. Cross cuts 49b1 and 49c1 are formed in the upper film 49b and the lower film 49c, and a pipette insertion hole 49c2 is formed in the lower film 49c. Thus, the lid 49 inserted into the extraction container 48 is formed with the cuts 49b1 and 49c1 in the upper film 49b and the lower film 49c, and the lid 49 of the extraction container 48 is shaken as shown in FIG. Even if the sample and the chemical solution are stirred while being pressed by the table 43, the lid 49 can prevent the sample from blowing up and prevent contamination due to the ejection.

  Next, the filtration device 70 will be described in detail with reference to FIGS. 19 is a plan view of a state in which a pipette is held by a robot, FIG. 20 is a side view of a state in which a pipette is held by a robot, FIG. 21 is a view showing a pipette setting state, FIG. 22 is a view showing a liquid injection state, FIG. 23 is a diagram showing the operation of the filtration device.

  The filtration device 70 includes an extraction container 48, a pipette 65, a filtration container 64, and a robot 24d that is a pipette transport mechanism. As shown in FIGS. 17 and 18, the extraction container 48 has a lid 49 in which a cut is formed. The robot 24d includes a rotary shaft 25d11 in the vertical direction, an arm 25d12 provided on the rotary shaft 25d11, and a pipette holder 25d13 provided on the arm 25d12. Two extraction pipes 71 are attached to the pipette holding portion 25d13, and the tip end portion 71a of the extraction pipe 71 is inserted into the upper portion 65a of the pipette 65. The supernatant sample can be extracted.

  Next, the operation of the filtration device 70 will be described with reference to FIG. The robot 25d holds and carries the two pipettes 65 of the pipette rack 61 [FIGS. 23 (a), (b)], and the two pipettes from the lids 49 of the two extraction containers 48 stored in the extraction rack 42 65 is inserted, and the sample of the supernatant of the extraction container 48 is aspirated and extracted [FIG. 23 (c)], and the sample is supplied to the two filtration containers 64 of the filtration rack 60 [FIG. 23 (d)]. When the filtration in the filtration container 64 is completed, the two pipettes 65 are carried to the pipette disposal unit 62 and discarded [FIG. 23 (e)].

In the filtration station C, a jammer plate 72 is disposed above the extraction container 48 as shown in FIG. An opening 72a is formed in the jammer plate 72, and the opening 72a is formed in a size that allows the pipette 65 to be inserted and restricts the lifting of the extraction container 48. Therefore, the robot 24d is operated to insert the tip portion 65b of the pipette 65 from the opening 72a of the jammer plate 72, and the tip portion 65b of the pipette 65 is connected to the upper membrane 49b of the lid 49 without removing the lid 49 from the extraction container 48. The sample in the extraction container 48 can be extracted by inserting from the cuts 49b1 and 49c1 in the lower membrane 49c, and the pipette 65 can be lifted to supply the sample to the filtration container 64. Even when the extraction container 48 is lifted when the pipette 65 is lifted, the lifting of the extraction container 48 can be restricted by the jammer plate 42 provided above the extraction container 48 to prevent the extraction pipe 48 from being lifted.
Thus, without removing the lid 49 from the extraction container 48, the pipette 65 can be inserted from the notch of the lid 49 to extract the sample from the extraction container 48, and the sample can be supplied to the filtration container 64, which can be automated. Processing speed is improved.

  Further, the robot 24d rotates the rotary shaft 25d11 in the vertical direction, holds the pipette 65 with the pipette holder 25d13 of the arm 25d12 provided on the rotary shaft 25d11, and extracts the sample of the extraction container 48 easily and reliably. Can be supplied to the filtration container 64, which can be automated and the processing speed can be improved. In addition, multiple pipettes 65 can be held at the same time, and samples from multiple extraction containers 48 can be extracted and supplied to multiple filtration containers 64. Multiple filtration processes can be performed in a single operation, reducing processing time. Processing speed is improved.

  The present invention can be applied to, for example, a weighing method, a weighing apparatus, and a sample analysis pretreatment apparatus for measuring a weight of a sample in a process of performing a pretreatment for soil analysis, and can improve the pretreatment accuracy of the weighing, In addition, the working environment can be improved by preventing the sample from flying up.

It is a top view of a sample analysis pretreatment apparatus. It is a front view of a sample analysis pretreatment apparatus. It is a left view of a sample analysis pretreatment apparatus. It is a right view of a sample analysis pretreatment apparatus. It is a top view of a weighing apparatus. It is a front view of a weighing apparatus. It is a figure which shows the set state of a sample container. It is a figure which shows the basic operation | movement of a weighing apparatus. It is a figure which shows a sample container. It is a figure which shows the cap of the sample container of other embodiment. It is a flowchart of operation | movement of a weighing apparatus. It is a figure which shows operation | movement of a weighing apparatus. It is a top view of a liquid injection apparatus. It is a figure which shows the set state of an extraction container. It is a figure which shows an injection state. It is a flowchart of operation | movement of a liquid injection apparatus. It is a side view of the extraction container which has a lid | cover. It is a figure which shows the lid | cover which has a cross-shaped cut. It is a top view of the state holding a pipette with a robot. It is a side view of the state holding a pipette with a robot. It is a figure which shows the set state of a pipette. It is a figure which shows an injection state. It is a figure which shows operation | movement of a filtration apparatus.

Explanation of symbols

1 Sample analysis pretreatment equipment
2 Frame
20 Pre-processing section
30 Post-processing section
24 Pre-stage robot
25 Rear-stage robot
40 Sample rack 41 Lid
42 Extraction rack
43 Shaking table
44 Weighing equipment
45 Injection device
46 Transport mechanism
47 Sample container
48 Extraction container
49 lid
60 Filtration rack
61 Pipette rack
62 Pipette disposal section
63 Transport mechanism
64 Filtration container
65 Pipette
70 Filtration equipment
A Start station
B Shaking station
C Filtration station
D End station

Claims (10)

The sample container is tilted and rotated by a predetermined angle by the sample supply means, and the sample stored in the sample container is supplied to the extraction container set in the measurement means,
A weighing method, characterized in that the sample supply means is controlled so as to obtain a preset sample weighing value based on the measurement information. Set the sample container to which the sample has been supplied to the measuring means, and measure the measured value of the sample.
Set the actual injection volume of the chemical solution that will be the set weight concentration from the measurement result of the weighing value of the sample,
A weighing method, characterized in that the chemical solution is supplied by controlling the chemical solution supply means so as to obtain the set actual injection amount of the chemical solution.   2. The weighing method according to claim 1, wherein the sample supply means is inclined with the supply port of the sample container as a fulcrum and rotates around the supply port of the sample container. The sample container is tilted to the first tilt, rotated at the first speed, and the sample is supplied for rough weighing,
When the weighing exceeds the rough weighing value, the sample container is returned from the first inclination to the second inclination, and the rotation is reduced to a second speed slower than the first speed to supply the sample. Weigh finely,
4. The weighing method according to claim 1, wherein the rotation of the sample container is stopped when weighing exceeds a supply weighing value before a set weighing value. A sample supply means for supplying the sample to the extraction container by tilting and rotating the sample container at a predetermined angle;
Measuring means for supplying and measuring a sample to the extraction container;
Control means for controlling the sample supply means so as to have a preset sample weighing value based on the measurement information;
A weighing apparatus comprising: A chemical supply means for supplying the chemical to the extraction container containing the sample;
A measuring means for measuring the weighing value of the sample in the sample container;
Setting means for setting the actual liquid injection amount of the chemical solution having the set weight concentration from the measurement result of the weighing value of the sample;
And a control means for controlling the chemical liquid supply means so as to obtain the set actual liquid injection amount of the chemical liquid. The sample supply means includes
Inclining means for inclining the supply port of the sample container to a fulcrum;
Rotating means for rotating the supply port of the sample container as an axis;
6. The weighing apparatus according to claim 5, further comprising: Controlling the sample supply means by the control means;
The sample container is tilted to the first tilt, rotated at the first speed, and the sample is supplied for rough weighing,
When the weighing exceeds the rough weighing value, the sample container is returned from the first inclination to the second inclination, and the rotation is reduced to a second speed slower than the first speed to supply the sample. Weigh finely,
8. The weighing device according to claim 5 or 7, wherein when the weighing exceeds a supply weighing value before a set weighing value, the rotation of the sample container is stopped.   9. A sample analysis pretreatment device comprising the weighing device according to claim 5. 10. The sample analysis pretreatment apparatus according to claim 9, wherein the sample is soil.