JP6281441B2 - Process gas chromatograph and temperature adjustment method for temperature raising tank - Google Patents

Description

  The present invention relates to a process gas chromatograph and a temperature adjustment method for a temperature raising tank.

  A gas chromatograph is a gas analyzer that separates and detects multi-component gas mixtures and volatile liquids for each single component, and has a wide measurement range and can simultaneously measure multi-components without interference. It is a representative analyzer. Utilizing this advantage, process gas chromatographs are widely used in industrial fields such as petrochemistry, petroleum refining, metal refining, and inorganic chemistry.

  For example, Patent Document 1 discloses a process gas chromatograph technique for the purpose of rapid cooling of the above-described column thermostat and which has greatly improved the analysis structure. Not only in the thermostatic bath, but also in the temperature rising bath, it is important to quickly cool the temperature in the bath after the analysis to a low temperature before the analysis in terms of improving the analysis throughput.

  An example of a temperature rising pattern for each analysis cycle of the temperature rising tank in the process gas chromatograph described above is shown in FIG. 5 as a conventional example. FIG. 5 shows a temperature change pattern (OT01) of the heating tank for each analysis cycle (period) with the time axis on the horizontal axis and the temperature on the vertical axis. According to FIG. 5, in the process gas chromatograph, after the temperature rising pattern by temperature adjustment is completed (t01), the temperature rising tank starts rapid cooling, and the temperature of the temperature rising tank is changed to the next flow in the analysis cycle of the next flow path. It is rapidly lowered to the initial path control temperature T01. At this time, the temperature of the heating tank must be the next flow path initial control temperature T01 by the analysis start time t02 of the next flow path.

  If the temperature of the temperature raising tank does not fall to the next flow path initial control temperature T01 at the next flow path analysis start time t02, an alarm is generated at the point indicated by A01, and the analysis is forcibly stopped. On the other hand, if the temperature of the temperature raising tank has reached the next channel initial control temperature T01, the analysis cycle of the next channel is executed.

  FIG. 6 shows a processing procedure of a temperature adjustment (hereinafter simply referred to as temperature control) program for that purpose. According to FIG. 6, after the temperature control by the temperature rising pattern defined in advance is completed (step S201 “YES”), the elapsed time is confirmed (step S202), and if it is not the next flow path analysis start time (step S203). “NO”), the elapsed time is confirmed again (step S202). When the next flow path analysis start time has elapsed (step S203 “YES”), the temperature of the temperature rising tank is confirmed again (step S204). If the difference between the temperature rising temperature and the next flow path initial temperature is within a certain range. (Step S205 “YES”), analysis of the next flow path is started (Step S206). On the other hand, if the difference is not within a certain range (“NO” in step S205), an alarm is generated (step S207), and the analysis is forcibly stopped (step S208).

Japanese Patent Application Laid-Open No. 8-086781

  According to the above-described conventional temperature control program, the process gas chromatograph forcibly terminates the analysis when the initial control temperature necessary for executing the analysis of the next channel is not reached by the analysis start time t02 of the next channel. The operator needs to wait until the cooling end time t03 and perform an operation for starting the analysis again.

  The present invention has been made in order to solve the above-described problems. When the initial control temperature necessary for execution of the next analysis cycle has not been reached by the start time of the next analysis cycle, the analysis is forced. It is an object of the present invention to provide a process gas chromatograph capable of improving analysis throughput without stopping, and a temperature adjusting method for a temperature raising tank.

  In order to solve the above-described problems, the present invention provides a process gas chromatograph for performing component analysis of a sample by heating and cooling a temperature rising tank based on a predetermined temperature control pattern for each analysis cycle. When the sensor unit that measures the temperature of the warm bath, the timer unit that measures the elapsed time when the temperature rise control based on the temperature control pattern ends, and the timer unit detect the start time of the next analysis cycle In addition, when the temperature of the heating chamber measured by the sensor unit has not reached the initial control temperature necessary for execution of the next analysis cycle, the next analysis cycle is executed after alarm notification. And a control unit that controls to delay by a predetermined allowable waiting time.

  In the present invention, the controller starts the cooling after the temperature increase control based on the temperature control pattern is finished, and the cooling is completed when the sensor unit is cooled beyond the initial control temperature required for the next analysis cycle. When the temperature control is detected again, the timer unit detects the start time of the next analysis cycle during the stabilization waiting period until the initial control temperature is reached by the temperature control again. Control is performed such that execution of the next analysis cycle is delayed by a first allowable waiting time until the waiting period ends.

  In the present invention, the control unit starts the cooling after the temperature increase control based on the temperature control pattern is finished, and the timer unit detects the start time of the next analysis cycle during the cooling period. A period until the controller detects the completion of cooling that has been cooled beyond the initial control temperature required for the next analysis cycle and starts temperature control again, and a stabilization waiting period until the initial control temperature is reached by temperature control again Are controlled so as to delay the execution of the next analysis cycle until a second allowable waiting time obtained by summing up and.

  The present invention is a temperature adjustment method for the temperature raising tank in a process gas chromatograph for performing component analysis of a sample by raising and cooling the temperature raising tank based on a predetermined temperature adjustment pattern for each analysis cycle, A first step of measuring the temperature of the temperature raising tank, a second step of measuring elapsed time upon completion of the temperature rise based on the temperature adjustment pattern, and a start time of the next analysis cycle in the second step When the temperature of the heating tank measured in the first step has not reached the initial control temperature necessary for execution of the next analysis cycle, the alarm And a third step of controlling to delay the execution of the analysis cycle by a predetermined allowable waiting time.

  According to the present invention, when the initial control temperature necessary for execution of the next analysis cycle has not been reached by the start time of the next analysis cycle, the analysis throughput can be improved without forcibly stopping the analysis. A fast process gas chromatograph and a method for adjusting the temperature of the heating tank can be provided.

It is a figure which shows the external appearance structure of the process gas chromatograph which concerns on embodiment of this invention. It is a block diagram which shows the internal structure of the electric circuit part of FIG. It is a flowchart which shows operation | movement of the process gas chromatograph which concerns on embodiment of this invention. It is a figure which shows an example of the temperature rising pattern for every analysis cycle of the temperature rising tank in the process gas chromatograph which concerns on embodiment of this invention. It is a figure which shows an example of the temperature rising pattern for every analysis cycle of the temperature rising tank in the conventional gas chromatograph. It is a flowchart which shows the process sequence of the temperature control by the conventional temperature control program.

  DESCRIPTION OF EMBODIMENTS Hereinafter, embodiments for carrying out the present invention (hereinafter referred to as “embodiments”) will be described in detail with reference to the accompanying drawings. Note that the same number is assigned to the same element throughout the description of the embodiment.

(Configuration of the embodiment)
FIG. 1 is a diagram showing an external structure of a process gas chromatograph 1 according to the present embodiment, and shows a state where a front door of a container in which each device is stored is opened.

  According to FIG. 1, reference numeral 10 denotes an electric circuit unit. For example, a microprocessor is mounted, and signal amplification, waveform processing, temperature control described later, communication processing with the outside, and the like are performed. Details of the internal configuration of the electric circuit unit 10 will be described later with reference to FIG.

  Reference numeral 11 denotes a terminal portion, which is a connecting portion by wiring between the gas chromatograph main body and the outside. Reference numeral 12 denotes a thermostatic bath, the temperature in the bath is set to a constant value, and the temperature adjustment is controlled to about a set temperature ± 0.03 degrees by PID (Proportional Integral Derivative) control. Various detectors, columns, and switching valves are arranged in the tank.

  Reference numeral 13 denotes a temperature raising tank, and the inside of the tank is controlled by a temperature control program over a wide temperature range. The temperature inside the tank is maintained uniformly by an air bath and a stirring fan system. Reference numeral 14 denotes a flow rate adjusting valve, which includes a pressure reducing valve for carrier gas, a pressure gauge, and a pressure reducing valve for purge air.

  Reference numeral 15 denotes an analyzer sampling unit. The analyzer sampling unit 15 houses a filter, a sampling pressure reducing valve, a flow meter, a flow path switching valve, and the like.

  The internal configuration of the electric circuit unit 10 is shown in FIG. 2, the electric circuit unit 10 includes an analysis execution control unit 100, a temperature control unit 101, a sensor unit 102, a timer unit 103, and a notification unit 104.

  The sensor unit 102 acquires temperature information of the temperature raising tank 13 measured by a temperature sensor such as an externally connected thermocouple and outputs the temperature information to the analysis execution control unit 100. The timer unit 103 performs time monitoring, measures elapsed time when the temperature control based on the temperature control pattern by the temperature control unit 101 ends, and outputs the measured elapsed time to the analysis execution control unit 100.

  When the timer unit 103 detects the start time of the next analysis cycle, the analysis execution control unit 100 determines the initial control necessary for executing the next analysis cycle based on the temperature of the heating tank 13 measured by the sensor unit 102. When the temperature has not been reached, the alarm unit 104 is controlled to notify the alarm. Then, control is performed so that execution of the next analysis cycle is delayed by a predetermined allowable waiting time. Note that the notification unit 104 can include an LCD (Liquid Crystal Display) or the like that displays a message in addition to notifying an alarm.

  For this reason, the analysis execution control unit 100 and the temperature adjustment control unit 101 function in cooperation so that “the timer unit detects the rise time measured by the sensor unit when it detects the start time of the next analysis cycle. Control that delays the execution of the next analysis cycle by a predetermined permissible waiting time after alarm notification when the temperature of the hot bath has not reached the initial control temperature necessary for the execution of the next analysis cycle. Part ".

  The analysis execution control unit 100 starts cooling after the temperature control based on the temperature control pattern by the temperature control unit 101 is finished, and the sensor unit 102 is cooled beyond the initial control temperature necessary for the next analysis cycle. When the completion of cooling is detected, the temperature control is started again, and when the timer unit 103 detects the start time of the next analysis cycle during the stabilization wait period until the initial control temperature is reached by the second temperature control, the stabilization wait period ends. Control may be performed so that the execution of the next analysis cycle is delayed by a first allowable waiting time until the time (time Ta in FIG. 4A described later).

  Further, the analysis execution control unit 100 starts cooling after the temperature increase control based on the temperature control pattern by the temperature control unit 101 is finished, and the timer unit 103 detects the start time of the next analysis cycle during the cooling period. In addition, the period until the sensor unit 102 detects the completion of cooling that has been cooled beyond the initial control temperature necessary for the next analysis cycle and starts temperature control again, and the temperature reaches the initial control temperature by the temperature control again. Control may be performed so that the execution of the next analysis cycle is delayed until a second allowable waiting time obtained by adding the waiting periods (time Tb + Tc in FIG. 4B described later).

(Operation of the embodiment)
The operation of the process gas chromatograph 1 according to the present embodiment will be described below with reference to the flowchart of FIG. According to FIG. 3, after the temperature increase pattern control by the temperature control unit 101 ends (step S <b> 101 “YES”), the analysis execution control unit 100 checks the elapsed time by the timer unit 103 (step S <b> 102). If the analysis start time (next analysis cycle) of the next channel has not been reached (step S103 “NO”), the analysis execution control unit 100 confirms the elapsed time monitored by the timer unit 103 again. (Step S102).

  When the timer unit 103 detects the next flow path analysis start time (step S103 “YES”), the analysis execution control unit 100 confirms the temperature of the heating tank 13 by the sensor unit 102 (step S104), and the heating tank 13 It is determined whether or not the difference between this temperature and the initial control temperature of the next flow path is within a certain range (step S105). If the difference is within a certain range (step S105 “YES”), the analysis execution control unit 100 starts the analysis of the next flow path as it is (step S106). If the difference is outside the certain range (step S105 “NO”). The alarm unit 104 is driven to generate an alarm (step S107).

  Subsequently, the analysis execution control unit 100 checks the temperature of the temperature rising tank 13 measured by the sensor unit 102 (step S108), and the difference between the temperature of the temperature rising tank 13 and the initial control temperature of the next flow path is within a certain range. It is determined whether it is within (step S109). If the difference is within a certain range (step S109 “YES”), the analysis execution control unit 100 starts the analysis of the next flow path from that point (step S106). If the difference is outside the certain range (step S109 “ NO "), the elapsed time monitored by the timer unit 103 is confirmed (step S110).

  Then, the analysis execution control unit 100 monitors the maximum allowable waiting time for a time corresponding to one analysis cycle (period) (step S111). Here, if the time for one analysis cycle has not elapsed (step S111 “NO”), the process of confirming the temperature of the heating tank 13 is executed again (step S108), and the maximum time for one analysis cycle is reached. If the allowable waiting time has elapsed (step S111 “YES”), the alarm unit 104 is driven to generate an alarm (step S112), and control for forcibly stopping the analysis is performed (step S113).

(Effect of embodiment)
As described above, according to the process gas chromatograph 1 according to the present embodiment, when the start time of the next analysis cycle is detected, the measured temperature of the heating tank 13 is necessary for the execution of the next analysis cycle. When the initial control temperature has not been reached, after the alarm is notified, control of the execution of the next analysis cycle is delayed so as to allow the waiting time. The event that the analysis process stops without satisfying the initial control temperature necessary for the execution of the cycle is less likely to occur. Therefore, the throughput for analysis is improved.

  In addition, according to the above-described embodiment, the allowable waiting time indicated by the time until the difference between the temperature of the temperature raising tank 13 and the initial control temperature of the next flow path falls within a certain range is analyzed up to one from the occurrence of the alarm. Although it is specified up to the period, this length may be arbitrary. In addition, by applying the analysis start delay at the start of the first analysis, the operator can immediately start the analysis without waiting for the temperature of the heating chamber 13 to stabilize, such as immediately after the process gas chromatograph 1 is turned on. Become.

(Modification)
By the way, in the process gas chromatograph 1, in an operating environment in which the outside air temperature greatly changes, a preparation period for the next analysis cycle from the start of cooling after the end of the control based on the temperature control pattern to the end of cooling (the cooling in FIG. 5). The waiting time C01) is also different. Therefore, in order to further improve the analysis throughput, it is necessary to optimally tune the driving state in consideration of the operating environment such as the weather. FIGS. 4A and 4B show an example of the temperature rising pattern for each analysis cycle of the temperature rising tank 13 in that case.

  4 (a) and 4 (b), the vertical axis indicates the temperature change pattern of the heating tank 13 and the initial control temperature, and the time axis (horizontal axis) indicates whether the temperature is being increased or is being prepared. The status and the temperature control ON / OFF status are shown. FIG. 4A shows the case where the next analysis cycle arrives during the stabilization wait time after the temperature adjustment is turned on after the cooling period, and FIG. 4B shows the next state when the temperature adjustment is in the OFF state during the cooling. Each operation timing when an analysis cycle arrives is shown.

  According to FIG. 4A, the cooling period (preparation period) for the next analysis cycle is started at the timing T1 of the temperature rise control end based on the temperature control pattern. At this time, the temperature control is OFF. At timing T2, the completion of cooling that has been cooled beyond the initial control temperature required for the next analysis cycle is detected. At this time, the temperature control is turned ON to start the temperature control again. The analysis execution control unit 100 executes the next analysis cycle by releasing the stabilization wait at the timing T4 when the stabilization wait time Ta reaching the initial control temperature is completed by the temperature control again. That is, even if the start time of the next analysis cycle is detected at the timing T3, the analysis execution control unit 100 executes the next analysis cycle until the timing T4 at which the stable waiting time Ta (first allowable waiting time) is completed. Delay. In other words, it is possible to drive in consideration of the operating environment such as the weather by tuning the stable waiting time Ta.

  On the other hand, according to FIG. 4B, the cooling period (preparation period) for the next analysis cycle is started at the timing T5 of the temperature increase control end based on the temperature control pattern. At this time, the temperature control is OFF. At timing T6, the next analysis cycle is detected, and at timing T7, the completion of cooling that has been cooled beyond the initial control temperature required for this analysis cycle is detected. When the completion of cooling is detected, the analysis execution control unit 100 detects the completion of cooling from the timing T6 when the next analysis cycle is detected to the timing T7 when the temperature adjustment is started again, and the temperature again Control is performed so that the execution of the next analysis cycle is delayed until the allowable waiting time (second allowable waiting time Tb + Tc) obtained by summing the stabilization waiting period Tc to reach the initial control temperature by the adjustment, that is, the timing T8. That is, the operation considering the operating environment can be performed by tuning the allowable waiting time Tb + Tc.

(Effect of modification)
As described above, according to the process gas chromatograph 1 according to the modification of the present embodiment, the next analysis cycle has arrived during the stabilization waiting time after the temperature control is turned on during the preparation period for executing the next analysis cycle. In some cases, the analysis throughput is improved by delaying the execution of the analysis until the end of the stable waiting time (first allowable waiting time), and the operation such as weather is adjusted by adjusting the allowable waiting time. Operation that is not affected by the environment becomes possible. In addition, when the next analysis cycle arrives at the time of temperature control OFF during the preparation period of the next analysis cycle, the total time required for the temperature control ON from the arrival of the analysis cycle and the stable waiting time (second tolerance) By delaying the execution of the analysis cycle by (waiting time), the analysis throughput can be improved, and by adjusting the allowable waiting time, driving that is not affected by the operating environment such as the weather becomes possible.

(Temperature adjustment method for temperature riser)
For example, as shown in FIG. 1, the temperature adjustment method for the temperature raising tank according to the present embodiment is performed by heating and cooling the temperature raising tank 13 based on a predetermined temperature control pattern for each analysis cycle. It is the temperature adjustment method of the said heating tank in the process gas chromatograph 1 which performs analysis. For example, as shown in FIG. 3, the temperature adjustment method is triggered by the first step (S104, S108) for measuring the temperature of the temperature raising tank and the termination of the temperature raising control based on the temperature control pattern. When the start time of the next analysis cycle is detected in the second step (S102, S110) for measuring time and in the second step, the temperature of the heating tank measured in the first step is A third step of performing control so as to delay execution of the next analysis cycle by a predetermined allowable waiting time after alarm notification when the initial control temperature necessary for execution of the next analysis cycle has not been reached. (S105 to S113).

  According to the method for adjusting the temperature of the heating tank 13 in the process gas chromatograph 1 according to the present embodiment, it is measured when the electric circuit unit 10 (analysis execution control unit 100) detects the start time of the next analysis cycle. If the temperature of the heated tank has not reached the initial control temperature required for the next analysis cycle, control is performed so that the execution of the next analysis cycle is delayed by a predetermined allowable waiting time after alarm notification. By doing so, the throughput of the analysis can be improved.

  As mentioned above, although this invention was demonstrated using embodiment, it cannot be overemphasized that the technical scope of this invention is not limited to the range as described in the said embodiment. It will be apparent to those skilled in the art that various modifications or improvements can be added to the above-described embodiments. Further, it is apparent from the scope of the claims that the embodiments added with such changes or improvements can be included in the technical scope of the present invention.

  DESCRIPTION OF SYMBOLS 1 ... Process gas chromatograph, 10 ... Electric circuit part, 11 ... Terminal part, 12 ... Constant temperature bath, 13 ... Temperature rising tank, 14 ... Flow control valve, 15 ... Analyzer sampling part, 100 ... Analysis execution control part, 101 ... Temperature Key control unit, 102 ... sensor unit, 103 ... timer unit, 104 ... notification unit

Claims (4)

It is a process gas chromatograph for performing component analysis of a sample by heating and cooling a heating tank based on a predetermined temperature control pattern for each analysis cycle,
A sensor unit for measuring the temperature of the heating tank;
A timer unit for measuring elapsed time triggered by the end of temperature rise control based on the temperature control pattern;
When the timer unit detects the start time of the next analysis cycle, the temperature of the heating tank measured by the sensor unit has not reached the initial control temperature necessary for the execution of the next analysis cycle. A control unit that controls to delay the execution of the next analysis cycle by a predetermined allowable waiting time after alarm notification;
A process gas chromatograph characterized by comprising: The controller is
The cooling is started after the temperature increase control based on the temperature control pattern is completed, and the temperature control is started again when the sensor unit detects the completion of the cooling that has exceeded the initial control temperature required for the next analysis cycle. And when the timer unit detects the start time of the next analysis cycle during the stabilization waiting period until the initial control temperature is reached by temperature control again, the first waiting time until the stabilization waiting period ends. 2. The process gas chromatograph according to claim 1, wherein control is performed so that execution of the next analysis cycle is delayed by an allowable waiting time. The controller is
The cooling is started after the temperature raising control based on the temperature control pattern is completed, and the sensor unit is necessary for the next analysis cycle when the timer unit detects the start time of the next analysis cycle during the cooling period. A second period obtained by adding the period from the completion of cooling that has exceeded the initial control temperature to the start of temperature adjustment to the start of temperature adjustment again, and the stabilization waiting period to reach the initial control temperature by the second temperature adjustment. 2. The process gas chromatograph according to claim 1, wherein execution of the next analysis cycle is delayed until a permissible waiting time. A method for adjusting the temperature of the temperature-raising tank in a process gas chromatograph for performing component analysis of a sample by heating and cooling the temperature-raising tank based on a predetermined temperature control pattern for each analysis cycle,
A first step of measuring the temperature of the heating tank;
A second step of measuring the elapsed time triggered by the end of the temperature rise control based on the temperature control pattern;
When the start time of the next analysis cycle is detected in the second step, the temperature of the heating tank measured in the first step reaches the initial control temperature necessary for the execution of the next analysis cycle. If not, after the alarm notification, a third step of controlling to delay the execution of the next analysis cycle by a predetermined allowable waiting time;
A method for adjusting the temperature of the heating tank, characterized by comprising:

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