JPH061263B2 - Chromatographic analysis system - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to a chromatographic analysis device, and more particularly to a chromatographic analysis system suitable for automation.

[Background of the Invention]

Chromatographic analyzers are generally characterized by a large number of functional units such as sample introduction device, separation device, detection device, recording device, etc., and their configuration changes depending on the sample, analysis purpose, and scale. This point is also important.

In a communication system, a method of defining a main station and a secondary station to perform communication control is generally used, and a method of setting a station number has been conventionally used.

However, in the conventional method, the system configuration is fixed, and when changing, the setting must be changed.

In addition, in order to minimize setting changes, there is a method in which the main station attempts communication with units that may be connected and checks whether there is a connection, but this is related to the power-on sequence of each unit.
It is a complicated procedure.

In JP-A-59-53924, when a terminal is initially connected, an address registration request is issued from the terminal to a node to which the terminal is connected, and the node sends a permission response and an address table loading. The network address management method is described in which the user of the terminal determines the logical address to be registered by itself from the address table and performs the logical address registration operation. However, in this method, since the user is involved in address registration, there is a possibility that an erroneous operation or an operation omission may occur.

Further, in Japanese Patent Laid-Open No. 60-14367, each module sends ID information to a system control unit by a system initialization command signal SYR (which is sent after power is turned on or at the time of total system reset such as system rebuilding). An information processing system including a control unit is described.
However, with this system, it is not possible to add a new module while the system is operating, and it is necessary to perform a total system reset once, so chromatographic analysis involving many precision instruments that require time to stabilize. It was unsuitable to apply to the system.

[Object of the Invention]

An object of the present invention is to provide a chromatographic analysis system capable of automatically constructing a system by communication.

[Outline of Invention]

In the present invention, when the power is turned on from the secondary station to the main station,
By transmitting operable information including the station number and model code, the master station can grasp the system configuration without an instruction from the operator. At this time, the main station displays the station number and other information contained in the operable information transmitted from a plurality of secondary stations on the screen, and the operator can easily know the system state by the display, The system can be booted only by confirmation.

That is, the present invention comprises a plurality of units required for chromatographic analysis, such as a sample introduction device, a separation device, a measurement device, and a data processing device, and a system is constructed by connecting each unit by communication and controlling it integrally. In the chromatographic analysis system, one of the plurality of units constituting the system is operated as a main station and the other units are operated as secondary stations, and the plurality of units are provided with station number setting means It has a communication form that identifies it by the set station number, and each secondary station
When the power supply to the own station is turned on and it becomes possible to operate, the main station automatically displays the operable information including at least the station number of the own station and the model code indicating what kind of device the own station is. Of the system based on the station number of the secondary station recognized as means for incorporating the secondary station in the control target based on the operable information including the received station number. And a means for displaying the configuration.

Example of Invention

The constitution of the liquid chromatograph is shown in FIGS. 10 and 11. Although FIG. 10 shows the simplest configuration,
Depending on the method of analysis, various peripheral devices are connected as shown in FIG. 11 for analysis.

In FIG. 10, the solvent pump 17 continues to flow the solvent reagent 8 through the column at a constant flow rate, and when the analytical sample is injected into the separation column 11 by the manual sampler 18, the analysis sample is temporally separated by the separation column 11, and the separation column is separated. It is eluted from 11.

The separated liquid is measured by the detector 6, and the data processing unit 7 performs analog recording of the detector output, peak judgment,
Calculate the content, etc.

In order to perform correct analysis even with such a simple configuration, the data processing device which is the system controller,
Continue monitoring during analysis for:

Abnormal increase in hydraulic pressure due to clogging of piping tube. Liquid pressure drops due to liquid leakage. Insufficient solvent reagents. The light source lamp of the detector is broken.

If even one of these is found to be abnormal during the analysis, the obtained analytical data cannot be used correctly and is treated as abnormal data.

Further, FIG. 11 shows the most complicated analysis system, including a gradient programmer 50 for changing the concentration of a solvent, an autosampler 60 for automatically injecting an analysis sample, a column thermostat 70 for controlling the temperature of the column, and a reaction reagent 12. A reaction pump 80 for mixing, a reaction tank 90 for accelerating reaction color development by heating, a detector 6 for measuring a reacted sample, and a data processing unit 7 for quantifying contained components from a signal from the detector.
It is composed of

In this system as well, in order to perform an accurate analysis, all the units constituting the system must be operating properly.

Further, in this system, the concentration control of the solvent by the gradient programmer 50, the supply of the analytical sample by the autosampler 60, and the start of calculation of the data processing unit 7 must be correctly synchronized.

The system control function monitors the state of each unit and synchronizes the units.

In the chromatographic analysis system of the present invention, each unit is connected by a communication line 30 as shown in FIG.
A system control function is added to the data processing unit 7, and the data processing unit controls each unit via the communication circuit 30. In FIG. 1, each unit constituting the system is provided with a communication line drive circuit (FIG. 2), and sends and receives commands and data by serial communication.

In addition, the operating mode suitable for the analytical method and the analytical sample must be designated for each unit, but the system of the present invention is configured so that each unit is set by communication from the data processing unit. Has only the data set in the data processing unit, and the operability is improved because it is not necessary to operate each unit individually.

The information that the data processing unit 7 communicates with each unit via the communication line has the following contents.

<Control of auto sampler (automatic sample supply device)> i) Confirmation of device status Confirm the presence or absence of energized state and abnormal state.

ii) Indication of sample number The sample number to be injected into the column is indicated, and the autosampler sucks the sample of the specified number and injects it into the column.

iii) Instruction of injection amount Indicate the amount to be aspirated from the sample cup and injected into the column.

iv) Injection start instruction Instruct to start injection under the conditions specified in i) to iii).

v) Instructions for cleaning and maintenance operations <Control of gradient programmer> i) Device status check Check the energization status and the pressure status of the pump and valve.

ii) Program transfer of mixing ratio The program of the mixing ratio and flow rate of the separation reagent is transferred to the gradient controller, and when the gradient controller receives an operation start instruction, the mixing ratio and flow rate of the separation reagent are controlled according to this program.

iii) Operation start instruction iv) Operation stop instruction v) Cleaning and other maintenance operation instructions <Reaction pump control> i) Confirmation of equipment state Energization state, confirmation of pressure state of reaction pump ii) Flow rate instruction of reaction reagent Indicating the flow rate of the reaction reagent, the reaction pump sends the specified amount of the reaction reagent.

iii) Pump operation start instruction iv) Pump operation stop instruction <Control of column constant temperature bath> i) Device state confirmation Temperature state confirmation (heater disconnection, temperature runaway) ii) Column temperature column constant temperature bath Controls the column temperature to the indicated temperature.

<Reaction tank control> i) Confirmation of apparatus state Confirmation of reaction vessel temperature state ii) Indication of reaction temperature The reaction vessel controls the temperature of the reaction vessel to the instructed temperature.

<Detector control> i) Device status check Check the energized state and lamp disconnection.

ii) Indication of measurement wavelength Indicate the measurement wavelength of the photometer.

iii Analysis start instruction In response to the measurement start instruction, the detector starts measurement under the specified conditions and sends measurement data to the data processing device at regular intervals.

iv) Analysis end instruction In order to smoothly execute such communication, the present invention adopts a communication system form in which the data processing unit 7 having a system control function is a communication main station and the other units are secondary stations. The communication line control is also performed by the data processing unit 7, which is the main station.

FIG. 3 shows the basic structure of each unit constituting the system of the present invention. Each unit has a mechanism section 154 for executing the function of the unit, a control section 153 for controlling the unit,
Communication control unit 150 for controlling communication, communication interface 31, station number setting switch 1 for setting unit number of unit
52, a model code memory 151 storing a model code of the unit.

The station number setting switch 152 is set so that the same number does not exist in the same system when the unit is connected.

When the power supply to each secondary station is turned on, the control unit 153 reads the model code memory 151 and the station number setting switch 152 and sends this value to the main station at the same time as the READY command to notify the main station of the connection. Incorporate the unit into the system.

Thus, each unit has a communication function and a station number setting switch.

The station number setting switch is set when the unit is connected to the system, the chromatographic data processing device that is the main station is number 0, and each other unit is the secondary station, so it is a value other than 0 and does not overlap. Set.

The commands, data, and timings between the units are exchanged by exchanging the data of the communication block as shown in FIG.

The structure of this communication block is generally used in communication, but in this case, communication is not possible unless the station number of the partner station is known.

When there are various combinations such as in a chromatograph, the method of setting the station number is not preferable, especially when it is necessary to connect multiple units of the same model in a large system.
Station number is fixed to the model (one station number is assigned to one model) in the system number collision occurs.

In the system of the present invention (FIG. 1), in order to eliminate this inconvenience, the station number is not set according to the model, and the main station is “0” and the secondary station is a non-overlapping number other than “0”. I decided to do it.

Therefore, the data processing device, which is the main station, is in a state where the station number and the number of units of each connected secondary station are unknown.

Therefore, a communication block called operational information (Fig. 5)
It is configured to start communication from the secondary station to the main station, which has only the station number when the power is turned on.

When the main station receives this operable information, it can know the station number and model of the secondary station that transmitted the operable information. This operable information is sent from all secondary stations when the power is turned on. Therefore, the master station can grasp the system configuration at this point.

FIGS. 6, 7, and 8 show the operation when the power is turned on. The unit with the station number 0 set becomes the main station and waits for operation information transmission from the secondary station and operation by the operator.

When the operator instructs START, the START command is transmitted by communication to the station that has received the operable information.

Similarly, other system control is also performed via communication with the station that has received the operable information.

Also, the unit whose station number is set to a value other than 0 becomes the secondary station and sends operable information as shown in Fig. 5 to the station (main station) with station number 0. Operate.

When the master station receives the operable information from the secondary station, it displays the station number and model code of the secondary station as shown in the display example of FIG.

The operator confirms the display of the main station, confirms whether it is in the intended configuration, confirms the unit of this connection, and if it is the intended configuration, press the START switch to the unit of the main station. Gives a start instruction such as pressing.

By this operation, the whole system can be started.

An analysis flow chart is shown in FIG. 12, and when the power is turned on, the system configuration is performed in step 100.

This system configuration is automatically performed by the data processing unit, which is the main station, by receiving operable information from the gradient programmer, which is the secondary station, and the operator can display the necessary units in the system by displaying the data on the data processing device. , It ends by checking whether it is in the operable state.

Next, the pump and the heater are preliminarily operated for stabilization.

Next, it is judged in step 102 whether or not the operator has instructed to start the analysis, and if there is an instruction to start the analysis, the analysis is started. Analysis starts with sample injection of the autosampler, and in synchronism with this, calculation of solvent concentration control and data processing starts. When the analysis of one analysis sample is completed, the autosampler injects the next analysis sample to start the next analysis.

When the communication response from any unit is not returned during the analysis or the error information is returned to the data processing device which is the main station, an error is displayed and the analysis ends.

When the analysis is completed, the operation of each unit is stopped by leaving the solvent pump in order to eliminate clogging of the piping.

After the washing time has elapsed, the solvent pump is also stopped to complete the entire operation.

〔The invention's effect〕

As described above, according to the present invention, the system configuration can be easily changed and the unnecessary units are not turned on, and the system can be automatically configured by turning on only the necessary units.

Further, according to the present invention, since the state of the unit forming the system can be known when the power source of the unit forming the secondary station is turned on, it is possible to reduce the frequency of erroneous operation and erroneous analysis.

Further, according to the present invention, since the system configuration is automatically confirmed when the power to the unit forming the secondary station is turned on,
Since it is not necessary to input system configuration information, it is easy to add or reduce the system and change the unit.

Furthermore, according to the present invention, since the operation is simple, operation mistakes are reduced.

[Brief description of drawings]

FIG. 1 is a diagram showing the communication connection of a unit, FIG. 2 is a transmission / reception interface for communication, FIG. 3 is a diagram showing the basic structure of each unit constituting an analysis system, FIG. 4 is a communication block configuration diagram, FIG. Fig. 5 is an operational information communication block configuration diagram, Fig. 6 is a processing flow chart of each unit when the power is turned on, Fig. 7 is a processing flow chart of the main station when the power is turned on, and Fig. 8 is a flow chart when the power is turned on. Processing flow chart of the next station, FIG. 9 is a diagram showing an example of a system configuration display screen, FIG.
FIG. 0 is a block diagram of a simple chromatograph, FIG. 11 is a block diagram of a complicated chromatograph, and FIG. 12 is a diagram showing an operation flow chart of the analysis system. 1 ... Gradient programmer, 2 ... Autosampler, 3
... column constant temperature tank, 4 ... reaction pump, 5 ... reaction tank, 6 ... detector, 7 ... data processing unit, 8 ... solvent reagent, 9 ... analysis sample, 10 ... heater, 11 ... separation column, 12 ... reaction reagent, 13 ... Heater, 14 ... Reaction coil, 15 ... Waste liquid,
17 ... Solvent pump, 18 ... Manual sampler, 30 ... Communication line, 31 ... Transmission / reception interface, 40 ... Transmission signal,
41 ... Reception signal, 42 ... DC power supply, 43 ... Transmission / reception circuit power supply, 44 Reception phototransistor collector resistance, 4
5 ... Receiving light emitting diode current limiting resistor, 46 ... Receiving photocoupler, 47 ... Transmitting light emitting diode current limiting resistor, 48 ... Transmitting photocoupler, 50 ... Gradient programmer, 60 ... Autosampler, 70 ... Column thermostat,
80 ... Reaction pump, 90 ... Reaction tank, 150 ... Communication control section, 151 ... Model code memory, 152 ... Station number setting switch, 153 ... Control section, 154 ... Mechanical section

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Momohachi Yoshihara, 882 Ichimo, Katsuta-shi, Ibaraki Hitachi, Ltd., Naka Factory, Ltd. Naka Factory (56) Reference JP 58-56099 (JP, A) JP 59-53924 (JP, A) JP 60-14367 (JP, A)

Claims (1)

[Claims] 1. A chromatograph comprising a plurality of units required for chromatographic analysis, such as a sample introduction device, a separation device, a measurement device, and a data processing device, and each system being connected by communication to integrally control the chromatograph. In the graph analysis system, one of the plurality of units constituting the system is operated as a main station and the other units are operated as secondary stations, and the plurality of units are each provided with station number setting means. Each secondary station has a communication mode that is identified by the station number set in, and when it becomes operable after the power to its own station is turned on,
It is equipped with a means to automatically transmit at least the station number of its own station and a model code to the master station, and the master station identifies the model of the secondary station and the station number based on the received station number and model code. It is provided with means for recognizing and automatically incorporating the secondary station into a control target, and means for displaying the system configuration based on the station number and / or model code of the recognized secondary station. Characteristic chromatographic analysis system.