JP3204106B2 - measuring device - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an analyzer or a measuring device such as a gas chromatograph or a mass spectrometer.

[0002]

2. Description of the Related Art Generally, in a gas chromatograph apparatus, a column is housed in an oven and subjected to temperature control up to about 450 ° C. After performing gas chromatographic analysis at a high temperature by such temperature control, if the column is to be replaced, first, the temperature of the oven must be lowered to such a degree that the operator can be touched. When the column is replaced, the carrier gas must also be stopped.

On the other hand, an adsorbent exists on the inner surface of a gas chromatograph column, and this adsorbent rapidly deteriorates when exposed to air at a high temperature. Therefore, the carrier gas must always flow through the column while the temperature of the column is high.

Accordingly, when the column is to be replaced as described above, first, the temperature of the column (oven) is lowered while flowing a carrier gas through the column, and the temperature of the column is lowered to such an extent that the adsorbent does not deteriorate. It is necessary to perform an ordered operation to stop the carrier gas for the first time.

[0005]

Conventionally, such a column exchange operation has been performed manually by a user of the gas chromatograph apparatus. That is, the control temperature of the oven is set to room temperature (or lower) while allowing the carrier gas to flow through the column. After confirming that the temperature of the oven has been sufficiently lowered by a thermometer provided in the oven temperature control unit, the carrier gas is stopped by operating the carrier gas control unit, the oven is opened, and the column is replaced.

The manual operation by the operator as described above is troublesome, and sometimes an operation error may occur. Also,
If you want to hurry the column change, the operator must be by the instrument until the oven cools down.

[0007] Such maintenance work is necessary for many analyzers and measurement devices, and the original analysis,
Nowadays, the measurement task has been considerably automated by the introduction of a computer, and this is a burden on the operator.
The present invention has been made in order to solve such a problem, and an object of the present invention is to provide a measuring device that automates a maintenance operation so that it can be easily performed.

[0008]

SUMMARY OF THE INVENTION The present invention has been made in order to solve the above-mentioned problems, and it is an object of the present invention to provide a method for moving an apparatus from a measurable state to a maintainable state, or vice versa. For a measuring device that needs to go through a plurality of states requiring a point-and-go relationship, a) state changing means for changing the state of the apparatus; b) state detecting means for detecting the state of the apparatus; c) detected state State determination means for determining whether or not the state corresponds to any of the plurality of states; andd) a state change when the state of the apparatus is determined to correspond to any of the plurality of states by the state determination means. State control means for changing the apparatus to the next state determined by the temporal sequence.

[0009]

DESCRIPTION OF THE PREFERRED EMBODIMENTS For example, when the apparatus is shifted from a measurable state to a maintainable state, the state control means performs the following maintenance shift processing. The following process is started by a command such as a key operation, a mouse operation, and a voice input by the operator. In the present measurement apparatus, as described above, the temporal relationship between a plurality of states (this is called a state change schedule) is given in advance. This may be provided in a state held in a non-volatile storage means, or may be held in a rewritable storage means to allow a change by an operator.

[0010] When the maintenance transition process is started, the state control means first detects the current state of the apparatus by using the state detection means, and determines whether the current state corresponds to any of the predetermined states. The state is determined by the state determination means. If it is determined that the state corresponds to any one of the states, the state of the apparatus is changed using the state changing means so as to set the apparatus to the next state determined by the temporal relationship. Thus, the state of the device is sequentially changed according to the state change schedule,
Eventually, the device is ready for maintenance. During this time, the operator does not need to be involved at all and can leave the apparatus. Therefore, it is desirable that the operator be notified by a lamp, a buzzer, or the like when maintenance is possible. The procedure is the same when the apparatus is shifted from a state in which maintenance can be performed to a state in which measurement can be performed.

In the above processing, if it is determined that the current state of the apparatus is not any of the predetermined states, the state control means may generate an abnormal signal.

[0012]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An example in which the present invention is applied to a gas chromatograph will be described with reference to FIGS. As shown in FIG. 1, the gas chromatograph device 10 includes a column 12 housed in an oven 11, a sample introduction unit 13 provided at an inlet of the column 12, a detection unit 14 provided at an outlet of the column 12, and a gas chromatograph. The control unit 15 controls the entire system 10. The sample introduction section 13 includes a carrier gas cylinder 20, a flow controller (FLC) 21, a vaporization chamber (SVP) 22, and the like. The control section 15 includes a sample introduction control circuit 25 for controlling these. The sample introduction control circuit 25 controls the pressure of the vaporization chamber 22 (that is, the column inlet pressure), the temperature of the vaporization chamber 22, the flow rate of the carrier gas, and the like. The control unit 15 further includes an oven control circuit 26 for controlling the oven 11, a detection unit control circuit 27 for controlling the detection unit 14 and processing a signal from the detection unit 14, and a central unit for performing various operations described below. A processing circuit 28 is included. Among them, the sample introduction control circuit 25, the oven control circuit 26, and the detection unit control circuit 27 constitute a state changing unit in the present invention.

The outline of the operation when gas chromatograph analysis is performed by the gas chromatograph device 10 is as follows. Operation panel 16 connected to central processing circuit 28
When the operator inputs or selects various analysis conditions and instructs the start of the analysis work, the central processing circuit 28 causes the sample introduction control circuit 25 and the oven control circuit 26 according to a program stored in a storage device (not shown). Then, a control signal is sent to the detection unit control circuit 27, and the temperature control of the vaporization chamber 22, the oven 11, and the detection unit 14 is started. When these temperatures reach the predetermined values, the central processing circuit 28 prompts the operator to inject the sample. If you are using an automatic sample injector,
The control unit 15 automatically injects a sample by sending a signal to the control unit of the automatic sample injection device. Thereafter, the central processing circuit 28 controls the carrier gas flow rate, the oven temperature, and the like to perform gas chromatographic analysis in accordance with given conditions, and fetches a detection signal from the detection unit 14 to perform analysis.

After the completion of such analysis, the column 12
When exchanging, the operator operates the operation panel 16
Give instructions to perform maintenance for column replacement. When this instruction is issued, the central processing circuit 28 performs control as shown in the flowchart of FIG. 2 and shifts the apparatus 10 to a state where the column can be replaced. That is, first, a predetermined control target temperature TT is transmitted to the oven control circuit 26 (step S1). The control target temperature TT is set to room temperature or a temperature lower than room temperature. As a result, the oven control circuit 26 stops energizing the heater, and starts forced air cooling by the fan. The central processing circuit 28 then determines the transition temperature T
G is set (S2). The transition temperature TG is a limit temperature at which the supply of the carrier gas to the column 12 may be stopped when the temperature of the column 12 becomes equal to or lower than the temperature TG. The transition temperature TG may be a predetermined value, or the operator may be able to appropriately input a value corresponding to the column 12.

Thereafter, the central processing circuit 28 sends the temperature of the column 12 (that is, the oven 1) from the oven control circuit 26.
(T1) is sequentially received (S3), and it is determined whether the temperature T0 of the column 12 has fallen below the transition temperature TG (S4). As long as T0> TG, the oven control circuit 26 continues the control for lowering the temperature of the column 12.

When T0 ≦ TG, the central processing circuit 2
8 transmits the target value PT of the pressure in the vaporization chamber 22 to the sample introduction control circuit 25 (S5). The control target pressure PT is set to the atmospheric pressure or a pressure lower than the atmospheric pressure. As a result, the sample introduction control circuit 25 gradually reduces the flow rate of the carrier gas. Next, the central processing circuit 28 sets the end pressure PG (S6). The end pressure PG is a limit pressure at which the column 12 may be removed when the pressure in the vaporization chamber 22 falls below this value. As in the case of the temperature control, the central processing circuit 28 waits until the measured pressure P0 of the vaporization chamber 22 becomes the end pressure PG (S7, S8).

When P0≤PG, the central processing circuit 2
8 outputs a preparation completion signal (S9). As a result, a warning is issued by a lamp, a buzzer, or the like on the operation panel 16 to notify the operator that the column can be replaced.

The above description is about the case where the column 12 is replaced. Next, an example where the glass insert of the vaporizing chamber 22 is replaced will be described with reference to the flowchart of FIG. Silica wool is inserted into the glass insert so that the injected liquid sample is uniformly vaporized. When replacing the glass insert, the pressure in the vaporizing chamber 22 must be kept close to the atmospheric pressure so that the silica wool does not fly out. In order to reduce the pressure in the vaporization chamber 22, the carrier gas must be stopped. At that time, the temperature of the column 12 needs to be reduced as described above.
In addition, the temperature of the glass insert must be sufficiently lowered so that the operator does not get burned.

The central processing circuit 28 executes these conditions in order according to the flowchart of FIG. That is, first, the oven control circuit 26 controls the control target temperature TCT.
And the control target temperature TVT to the sample introduction control circuit 25 (step S11). In both cases, similarly to the control target temperature TT, the temperature is set to room temperature or lower. The control of the temperature of the oven 11 and the control of the pressure of the vaporization chamber 22 (steps S12 to S18) are performed in the above steps S1 to S18.
This is the same as the processing in S9. The control of the temperature of the vaporization chamber 22 is also the same as the temperature control of the oven 11 described above. First, the end vaporization chamber temperature TVG is set (S22), and the central processing circuit 28 sets the measured temperature TV0 of the vaporization chamber 22 to the value TVG. Wait until it reaches (S23, S24).

When the pressure in the vaporizing chamber 22 becomes equal to or lower than the predetermined end pressure PVG and the temperature reaches the predetermined end temperature TVG,
The central processing circuit 28 outputs a ready signal (S19, S19).
20) Notify the operator that the glass insert can be replaced.

As described above, when performing maintenance such as replacement of the column 12 in the gas chromatograph apparatus 10 of the present embodiment, the operator only needs to give one instruction from the operation panel 16 and then the apparatus itself. Controls the oven temperature, carrier gas pressure, etc. in the correct order and automatically transitions to a state where maintenance is possible.

[Brief description of the drawings]

FIG. 1 is a schematic configuration diagram of a gas chromatograph apparatus according to one embodiment of the present invention.

FIG. 2 is a flowchart of a process performed by a central processing circuit when shifting to a column replaceable state.

FIG. 3 is a flowchart of a process performed by a central processing circuit when shifting to a state in which a glass insert can be replaced.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 10 ... Gas chromatograph apparatus 11 ... Oven 12 ... Column 13 ... Sample introduction part 14 ... Detection part 15 ... Control part 16 ... Operation panel 22 ... Vaporization chamber

──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int.Cl. ⁷ , DB name) G01N 30/02 G01N 27/62 G01N 30/12 G01N 30/54

Claims (2)

(57) [Claims] 1. An oven accommodating a column for gas chromatography, a vaporization chamber for vaporizing a sample and introducing it into the column, a temperature control means for controlling the temperature of the oven, and a supply of a carrier gas to the column. A measuring device having gas supply control means for controlling the temperature of the oven; a pressure detecting means for detecting the pressure of the vaporization chamber; and At a certain time, when a signal instructing the start of maintenance of the oven is given, the temperature of the oven decreases while operating the gas supply control means so that a carrier gas having a flow rate equal to or more than a predetermined flow rate flows through the column. Operating the temperature control means as follows,
When the temperature of the oven is lower than a predetermined temperature, the gas supply control unit is operated so that the flow rate of the carrier gas is reduced. When the pressure of the vaporization chamber is lower than a predetermined pressure, maintenance preparation is performed. A measuring device comprising a state control means for outputting a signal indicating completion. 2. An oven accommodating a column for gas chromatography, a vaporization chamber for vaporizing a sample and introducing it into the column, an oven temperature control means for controlling the temperature of the oven, and controlling the temperature of the vaporization chamber. A gas supply control means for controlling the supply of the carrier gas to the column; an oven temperature detection means for detecting the temperature of the oven; A vaporization chamber temperature detecting means for detecting a temperature, a pressure detecting means for detecting a pressure of the vaporization chamber, and a signal instructing a start of maintenance of the vaporization chamber when the apparatus is in a measurable state are given. When the oven is operated, the gas supply control means is operated so that a carrier gas having a flow rate equal to or higher than a predetermined flow rate flows through the column. Operating the oven temperature control means and the vaporization chamber temperature control means so that the temperature and the temperature of the vaporization chamber decrease, and when the oven is in a state of a temperature lower than a first predetermined temperature, the flow rate of the carrier gas Operating the gas supply control means so as to decrease, when the vaporization chamber is in a state where the pressure is lower than a predetermined pressure and lower than a second predetermined temperature, a signal indicating completion of maintenance preparation is issued. A measuring device comprising a state control means for outputting.