JP2628037B2 - Automatic gas analyzer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for measuring a specific component in a gas produced by a gas separation device or a specific component in a gas discharged from an industrial gas using device. The present invention relates to an automatic gas analyzer.

[Conventional technology]

When a gas is produced industrially by various gas separation devices, it is necessary to analyze and measure the component composition of the gas to determine the quality of the product. If the purity of the product gas is high, it is impossible to measure the base component of the gas with high accuracy. Therefore, the amount of trace components contained in the product gas is conventionally analyzed and measured and displayed. In order to continuously analyze and measure the trace gas, various trace component analyzers such as a yellow phosphorescent trace trace oxygen meter are used.

By the way, in recent years, automatic operation including start-up and stop of the gas separation device has been performed by employing a computer control device or the like in the gas separation device.

[Problems to be solved by the invention]

However, the analytical instruments used in these methods require operations such as introduction of sample gas, purging, flow rate setting, and scale range switching at the start of use, and sometimes the composition of the production gas is reduced when the gas separator is started up. Since it is unknown, the handling operation required skill to protect the analytical instrument. In addition, since this is a final quality control operation, this operation has conventionally been excluded from automation.

Accordingly, the present invention automatically introduces a sample gas into an analytical instrument, purges, sets a flow rate, switches a scale range, and periodically performs a calibration operation, thereby reducing maintenance work of the analytical instrument due to an incorrect handling operation. It is an object of the present invention to provide an automatic gas analyzer capable of shortening the rise time of an analytical instrument up to analytical measurement, improving the reliability of the instrument, and achieving fully automatic operation of the gas separator. Another object of the present invention is to provide a similar automatic gas analyzer for an analyzer that measures a specific component in a gas discharged from an industrial gas using device.

[Means for solving the problem]

In order to achieve the above object, the present invention relates to an automatic gas analyzer for measuring a specific component in a gas produced by a gas separation device or a specific component in a gas discharged from an industrial gas use device. And a purge gas introduction channel for introducing a single component gas having a known component composition, and a calibration gas introduction channel for introducing a standard gas. A sample gas flow controller for controlling the sample gas to an arbitrary flow rate in the sample gas introduction flow path, a single component gas flow controller for controlling the single component gas to an arbitrary flow rate in the purge gas introduction flow path,
Along with providing a calibration gas flow controller for controlling the standard gas to an arbitrary flow rate in the calibration gas introduction flow path,
The sample gas introduction flow path is provided with a three-way switching electromagnetic valve that switches to the analyzer side and to the discharge side when the sample gas has a high concentration equal to or higher than a predetermined value during sample gas analysis measurement, and when the sample gas is not analyzed, A switching solenoid valve for opening and closing these flow paths is provided in each of the purge gas introduction flow path and the calibration gas introduction flow path, and a signal notifying the operation state from the gas separation device or the industrial gas use device, a signal from the analyzer, A controller that transmits a signal for operating the three-way switching valve and both switching valves based on at least one of the signals stored in advance, and a transmission signal from the controller,
By switching operation of the three-way switching solenoid valve between the analyzer side and the discharge side and opening and closing switching operation of both switching solenoid valves, the gas of each flow path whose flow is controlled is introduced alone or mixed and introduced into the analyzer. It is characterized by.

(Operation)

With the above configuration, a signal notifying the operation state from the gas separation device or the industrial gas use device, a signal from the analyzer,
Based on the signal stored in advance, the sample gas or single-component gas is introduced into the analyzer automatically or independently according to the concentration of the analytical component, or mixed at an arbitrary mixing ratio, or used for calibration. Since gas can be automatically introduced into the analyzer for analysis, purge, standby, calibration, start-up measurement, and steady-state operation measurement can be automatically performed.

〔Example〕

Hereinafter, an embodiment of the automatic gas analyzer of the present invention will be described with reference to the drawings.

The automatic gas analyzer of the present embodiment measures a specific component in a gas produced by a gas separator (not shown) or a specific component in a gas discharged from an industrial gas using device (not shown). In the analyzer 1, a sample gas introduction channel 3 for introducing a sample gas to be analyzed through a flow meter 2 is provided.
And a purge gas (single component gas) introduction flow path 4 for introducing a single component gas whose component composition is known, and a calibration gas (standard gas) introduction flow path 5 for introducing a standard gas are connected and connected. Have been.

Each of these flow paths is provided with a flow controller for arbitrarily controlling the gas flow rate of each flow path. That is, a sample gas flow rate controller 6 for controlling the sample gas introduced into the analyzer 1 to an arbitrary flow rate is provided in the sample gas introduction flow path 3, and a single component gas is provided in the purge gas introduction flow path 4 for arbitrary flow rate. A single component gas flow controller 7 for controlling the flow rate is provided, and a calibration gas flow controller 8 for controlling the standard gas to an arbitrary flow rate is provided in the calibration gas introduction flow path 5.

A three-way switching solenoid valve 9 is provided in the sample gas introduction flow path 3 to switch to the analyzer 1 side and to the discharge side when the sample gas has a higher concentration than a predetermined level during sample gas analysis measurement and when the sample gas is not analyzed. However, a switching electromagnetic valve 10 for opening and closing the flow path 4 is provided in the purge gas introduction flow path 4, and a switching electromagnetic valve 11 for opening and closing the flow path 5 is provided in the calibration gas introduction flow path 5. .

Further, in order to operate each of the flow controllers 6, 7, 8 and each of the switching solenoid valves 9, 10, 11, a controller 12 for transmitting a signal thereto is provided. This controller
12, a signal is input in advance and stored, or a signal notifying the operation state from the gas separation device or the industrial gas use device or a signal from the analyzer 1 is stored together with or instead of the storage. input. Then, based on at least one of these signals, the controller 12 monitors the indicated value of the analyzer 1 and the measurement time, and issues an instruction for switching each flow path and controlling and mixing the flow rate of each gas.
The signals are transmitted to the flow controllers 6, 7, 8 and the switching solenoid valves 9, 10, 11.

Then, each of the flow controllers 6, 7, 8 receives the transmission signal to arbitrarily control the gas flow rate of each flow path. In addition, by receiving this transmission signal, the three-way switching solenoid valve 9 performs a switching operation between the analyzer side and the discharging side, and both switching solenoid valves 10 and 11 perform an opening and closing switching operation, thereby controlling each of the flow rates. Analyzer 1 by mixing or mixing gas in flow path
Let me introduce you.

A back pressure control valve 13 is provided between the analyzer 1 and the flow meter 2. A pressure reducing valve is provided in the sample gas introduction passage 3.
14 and an on-off valve 17, a pressure reducing valve 15
And a switching valve 18, and a pressure reducing valve 16 and a calibration gas cylinder 19 are provided in the calibration gas introduction flow path 5, respectively.

As the analyzer 1, an instrument for analyzing and measuring various trace components is mainly an object of the present invention. For example, a yellow phosphorus emission trace oxygen meter, a trace moisture meter, or a volatile inorganic hydride measurement by a mercury-ultraviolet absorption method Device.

Next, a case where a specific component in a gas produced by a gas separator is measured by the automatic gas analyzer configured as described above will be described as follows.

When Analytical Measurement is Not Performed on the Gas Production Line (Standby State) The switching solenoid valve 10 is opened, and a single-component purge gas whose component composition is known from another gas production line or the like via the purge gas introduction flow path 4 ( Zero gas) to analyzer 1
The flow rate is set by a flow rate setting device built in the analyzer 1, the scale range is switched, and the like, each device is put into an operating state, and the calibration of the meter is completed.

That is, at the time of non-analytical measurement of the sample gas, the sample gas introduction flow path 3 opens the on-off valve 17 and switches the three-way switching solenoid valve 9 to the discharge side, and the flow controller 6 provides an arbitrary mixing ratio to the flow rate of the purge gas. The calibration gas introduction flow path 5 is similarly set to be in the discharge state, and the flow rate controller 8 measures the flow rate necessary for analysis and measurement, and closes the switching electromagnetic valve 11.

After performing the above operations by manual operation, the apparatus enters a standby state, and enters a next measurement start step by a start signal of the gas separation apparatus.

When starting the analytical measurement of the gas production line (at the time of starting the apparatus) The purge gas introduction flow path 4 is kept as it is, the three-way switching solenoid valve 9 of the sample gas introduction flow path 3 is switched to the analyzer 1 side, and the gas production is started. A sample gas of unknown composition in the line is introduced and mixed with the purge gas. The flow rate at this time is an amount set by the flow rate controllers 6 and 7, and is set, for example, to have an equal mixing ratio. The indicated value of the analyzer 1 is monitored by the controller 12, and when the rate of change of the indicated value and / or a certain absolute value reaches a preset value, a signal is sent from the controller 12 immediately and the three-way switching solenoid valve 9 is operated. Is switched to the discharge side to protect the component to be measured from becoming a high concentration so that the performance of the analyzer 1 is not hindered. Then, after a certain period of time, the three-way switching solenoid valve 9 is switched again to the analyzer 1 side by a signal from the controller 12, and
The indicated value is monitored in the same manner.

As a result, if the change rate and / or the absolute value of the indicated value is lower than the set value, the controller 12 measures the duration of the change, and elapses a predetermined time to check the stability of the analysis value. Later, the operation proceeds to the steady operation measurement. That is, the switching electromagnetic valve 10 of the purge gas introduction flow path 4 is closed, and only the sample gas flows to the analyzer 1. At this time, the indicated value of the analyzer 1 is continuously monitored by the controller 12, and when the rate of change and / or the absolute value different from the set value at the time of the previous mixing reaches the set value, the purge gas introduction flow path is returned again. The switching electromagnetic valve 10 of 4 is opened, and the purge gas and the sample gas are mixed and flow to the analyzer 1. When the rate of change and / or the absolute value reaches the set value at the time of the previous mixing, the introduction of the sample gas is stopped, and the state returns to the state where only the purge gas is introduced.

The set values of these indicated values are purge gas (zero gas)
And the flow rate distribution of the sample gas and the purge gas and the scale range of the analyzer 1. Also, the rate of change is determined in relation to the set value and predicts and protects the scale over of the analytical instrument. Thus, the sample gas of unknown composition is automatically and safely analyzed and measured.

Continuous Analysis and Measurement of Gas Production Line After starting the analysis and measurement of the production line as described above, the indicated value of the analyzer 1 is continuously monitored by the controller 12 to control the state of the gas production line. That is, an alarm is issued to the outside by an alarm set value provided separately, or a stop signal is sent to the gas separation device to stop the device. Further, in this situation, the analyzer measurement of the gas production line is stopped, and the above-mentioned standby state is set to protect the analyzer 1.

Calibration of analyzer In the stand-by state after the manual operation described above or the continuous analysis measurement state, the sample gas or purge gas periodically introduced into the analyzer 1 and the standard gas are automatically switched to calibrate the analyzer 1. Done. That is, the three-way switching solenoid valve 9 or the switching solenoid valve 10 and the switching solenoid valve 11 are automatically switched when the set time has elapsed, and the calibration gas (standard gas) adjusted to the optimum flow rate by the flow controller 8 is analyzed by the analyzer. At this time, the value previously stored in the controller 12 is compared with the component composition of the calibration gas. As a result of this comparison,
If there is a difference between them, the controller 12 emits an alarm sound. After the alarm is generated, calibration is performed manually.

As described above, according to the automatic gas analyzer of the present embodiment, when a target component having a concentration higher than the maximum scale range comes in the trace component analyzer, the dilution is performed with the dilution gas (purge gas) composed of a single component. The operation to be performed is performed automatically, so that the analyzer can be protected. That is, purge, wait,
Calibration, start-up measurement, and steady-state operation measurement can be performed automatically.

〔The invention's effect〕

According to the automatic gas analyzer of the present invention, various gases are introduced into the analyzer in response to the operating state of the gas separation device or the industrial gas using device by the above-described configuration, and the analysis, calibration, and purge steps are automatically performed. Therefore, the following effects can be obtained.

Purging, standby, calibration, start-up measurement, and steady-state operation measurement can be performed automatically.

It is possible to automatically prevent a high concentration of the component to be measured from being introduced into the analyzer, so that the performance of the analyzer is not hindered.

The start-up time of the analyzer until analysis measurement can be reduced.

The automatic calibration of the analyzer increases the reliability of the instrument.

Automated analytical measurement is possible without any modification to commercially available analytical instruments.

By providing a large number of purge gas introduction channels and changing the flow rate distribution with the sample gas, the apparent scale range can be further automatically expanded.

[Brief description of the drawings]

FIG. 1 is a system diagram showing one embodiment of the automatic gas analyzer of the present invention. 1 ... Analyzer, 2 ... Flow meter, 3 ... Sample gas introduction passage, 4 ... Purge gas introduction passage, 5 ... Calibration gas introduction passage, 6,7,8 ... Flow controller 9 ... 3-way switching solenoid valve, 1
0,11… Switching solenoid valve, 12 …… Controller

Claims (1)

(57) [Claims] 1. An automatic gas analyzer for measuring a specific component in a gas produced by a gas separation device or a specific component in a gas discharged from an industrial gas use device, a sample gas introduction for introducing a sample gas to be analyzed. A flow path, a purge gas introduction flow path for introducing a single component gas having a known component composition, and a calibration gas introduction flow path for introducing a standard gas are joined to be connected to an analyzer, and the sample gas introduction flow is connected. A sample gas flow controller for controlling the sample gas at an arbitrary flow rate in the flow path; a single component gas flow controller for controlling the single component gas at an arbitrary flow rate in the purge gas introduction flow path; In addition to providing a calibration gas flow rate controller for controlling the standard gas to an arbitrary flow rate in the path, and the sample gas introduction flow path, the sample gas has a high concentration of a predetermined level or more during the sample gas analysis measurement with the analyzer side. Edge A three-way switching solenoid valve for switching to a discharge side during sample gas non-analytical measurement; A signal indicating the operating status of the separation device or industrial gas using device,
A controller for transmitting a signal for operating the three-way switching valve and the two-way switching valve based on at least one of a signal from the analyzer and a signal stored in advance; By switching operation of the switching electromagnetic valve between the analyzer side and the discharge side and opening / closing operation of both switching electromagnetic valves, the gas in each flow path whose flow rate is controlled is solely or mixed and introduced into the analyzer. And an automatic gas analyzer.