TWI672485B - Emission spectroscopy device - Google Patents

Abstract

The light emitting spectroscopic analysis device is provided with: a discharge chamber that excites the sample by generating an internal discharge; a pressurizer as a container for containing a liquid; a gas supply source filled with an inert gas compressed to an atmospheric pressure or more; One end of the gas supply pipe is connected to the gas supply source and the other end is connected to the discharge chamber. The gas discharge pipe is connected to the discharge chamber at one end and the other end is opened into the liquid in the pressurizer. The exhaust line is at one end. It is arranged in the pressurizer above the liquid level and the other end is opened to the outside of the pressurizer; the pressure sensor measures the pressure of the inert gas in the gas supply pipe; and the warning component The user is warned when the measured value obtained by the pressure sensor exceeds a predetermined value.

Description

Luminescence spectroscopic analysis device

The present invention relates to a light emission spectroscopic analysis device that excites and emits a solid sample by electric discharge and performs spectroscopic measurement of the light emitted.

In a light emission spectroscopic analysis device, an arc discharge, a spark discharge, or the like is usually used to apply energy to a solid sample that is a metal or a nonmetal, thereby evaporating and vaporizing the sample, and exciting the light. Spectral lines having wavelengths peculiar to each element are taken out after detection in the spectroscope (for example, refer to Patent Document 1). In particular, a light-emitting spectroscopic analysis device using a spark discharge as an excitation source can perform high-precision analysis. Therefore, for example, it is widely used for the composition of a produced metal body in a production plant such as a steel material or a non-ferrous metal material. analysis.

The configuration of a conventional general light emission spectroscopic analysis device is shown in FIG. 3. The light emission spectroscopic analysis device includes an excitation unit 210 for exciting and emitting solid sample S, a spectroscopic unit 220 for detecting wavelength dispersion of light emitted from the sample S, and a control / processing unit 230 for each unit. Control and data processing.

The excitation unit 210 includes a discharge generating unit 211, an electrode rod 212, a discharge chamber 213, a sample mounting plate 214, and a condenser lens 215. Provided in the discharge chamber 213 An analysis opening opened obliquely upward and a light guide hole 213a for taking out light from the discharge chamber 213. The sample mounting plate 214 is detachably mounted on the upper portion of the discharge chamber 213 so as to cover the analysis opening. The sample mounting plate 214 has a central opening 214a smaller than the sample S, and the sample S is placed on the sample mounting plate 214 so as to cover the central opening 214a of the sample mounting plate 214. Part of the lower surface (analyzed surface) of S is exposed to the inside of the discharge cell 213. The electrode rod 212 for discharging is arranged inside the discharge chamber 213 with its tip facing the central opening 214a.

The discharge generator 211 applies a high pulse-like voltage to the electrode rod 212 in synchronization with a predetermined frequency (for example, 400 Hz). Samples S such as iron or non-ferrous metals are excited to emit light by spark discharge from the electrode rod 212. The light emitted by the excitation light emission of the sample S passes through the light guide hole 213a provided in the discharge chamber 213, is collected by the condenser lens 215, and is then introduced into the beam splitter 220 through the entrance slit 221.

As disclosed in Patent Document 1, etc., the spectroscopic section 220 has a diffraction grating 222 for dispersing the wavelength of light from the sample S in order to obtain a spectral line with a wavelength unique to each of the plurality of elements, and is disposed at each An exit slit 223a, an exit slit 223b, an exit slit 223c, and a plurality of photodetectors (usually photomultiplier tubes) arranged behind the exit slits 223a, 223b, and 223c at positions where the spectral line of the wavelength reaches ) 224a, 224b, 224c. The light incident from the excitation unit 210 through the entrance slit 221 into the spectroscopic unit 220 is wavelength-dispersed by the diffraction grating 222, and the wavelength-dispersed light passes through the exit slits 223a, 223b, Light in a predetermined wavelength range of 223c is detected by each of the photodetectors 224a, 224b, and 224c.

Each photodetector (224a, 224b, 224c) detection signals are input to the control and processing unit 230 through the analog / digital (A / D) conversion unit 225, and a certain data content is obtained by performing a predetermined data processing. The intensity of the spectral line of an element, and a quantitative analysis of each element and the like are performed according to it.

In the light emission spectroscopic analysis device as described above, the influence of gas components in the discharge chamber 213 on the analysis result is suppressed, or the discharge is stabilized to improve the analysis accuracy, and the light having a wavelength in the vacuum ultraviolet region is not attenuated and introduced to In the spectroscope (spectroscopy section 220), and to prevent deterioration of the analysis accuracy caused by microparticles originating from the sample that evaporate due to discharge remaining in the discharge chamber 213, etc., the purity of the sample is measured with high purity Argon is introduced into the discharge chamber 213. Therefore, the discharge chamber 213 is connected to a gas supply pipe 242 for supplying argon gas from a gas supply source 241 such as a gas storage tank to the discharge chamber 213, and a gas discharge pipe for discharging gas from the discharge chamber 213. Road 245. The gas supply pipe 242 is provided with an on-off valve 243 and a flow rate adjustment valve 244, and the control / processing unit 230 or a user drives these valves to perform the introduction of argon gas into the discharge chamber 213.

Furthermore, in order to prevent a decrease in the purity of argon gas caused by the inflow of air from the surroundings, the pressure in the discharge chamber 213 must be maintained at a pressure higher than the atmospheric pressure. Therefore, the end of the gas exhaust pipe 245 is not opened to the atmosphere, but is introduced into a container called a pressurizer 246, and opens into a liquid 246a such as water or oil contained in the pressurizer 246. At this time, the gas introduced into the pressurizer 246 from the end of the gas discharge line 245 is discharged to the outside through the exhaust line 247 provided in the pressurizer 246. Furthermore, one end of the exhaust pipe 247 is disposed at a level higher than the liquid level in the pressurizer 246. Further above, the other end is opened to the atmosphere outside the pressurizer 246.

Some of the sample-derived particles evaporated in the discharge chamber 213 are captured by the liquid 246 a in the pressurizer 246, but most of them pass through the pressurizer 246. Therefore, in order to prevent the particles from being released indoors, the exhaust gas from the pressurizer 246 is usually released to the outside through an exhaust device, or as shown in FIG. 3, passed through a filter provided on the exhaust pipe 247 248 and released indoors.

[Prior Art Literature]

[Patent Literature]

[Patent Document 1] Japanese Patent Laid-Open No. 2001-83096

When the filter 248 is used as described, the filter must be replaced periodically. If it is continued to be used without replacement, there is a possibility that the exhaust gas flow rate from the pressurizer 246 decreases due to the clogging of the filter 248 and eventually does not flow at all. In addition, even when the exhaust gas is discharged to the outside through the exhaust device without using a filter, for example, particles of the evaporated sample may accumulate in the flow path of the exhaust device or may be used in a cold area. There is a possibility that the end of the pipe that discharges the exhaust gas to the outside freezes, and the exhaust gas from the pressurizer 246 may not flow.

If the backlog of exhaust gas from the pressurizer 246 is caused by the clogging of such a flow path, the gas flow path from the gas supply source 241 to the pressurizer 246 (that is, the gas supply line 242, The internal pressure of the discharge chamber 213, the gas exhaust pipe 245, and the pressurizer 246) increases, and pressure may be generated at the moment the sample S is removed from the sample mounting plate 214 after the measurement is completed. Fluid in the vessel 246 The body 246a flows back into the discharge chamber 213 and contaminates the inside of the discharge chamber 213, and the like.

The present invention has been made in view of this point, and it is an object of the present invention to provide a light emission spectroscopic analysis device that does not cause a failure caused by a clogging of an exhaust flow path from a pressurizer as described above.

The light-emitting spectroscopic analysis device of the first invention, which is formed to solve the above-mentioned problems, includes: a) a discharge chamber that emits light to excite a sample by generating an internal discharge; b) a pressurizer as a container for storing a liquid; c ) A gas supply source filled with an inert gas compressed to an atmospheric pressure or more; d) a gas supply pipeline, one end of which is connected to the gas supply source and the other end of which is connected to the discharge chamber; e) a gas discharge pipeline, One end is connected to the discharge chamber, and the other end is opened into the liquid in the pressurizer; f) an exhaust line, one end is disposed in the pressurizer above the liquid level of the liquid , The other end opens toward the outside of the pressurizer; g) a pressure sensor that measures any of the gas supply line, the discharge chamber, the gas exhaust line, or the pressurizer The pressure of the inert gas in the internal space; and h) a warning component, when the measured value obtained by the pressure sensor exceeds a predetermined regulation Warn the user when the value is set.

As described above, the inert gas is supplied into the discharge chamber from the gas supply source through the gas supply pipe, and the inert gas is further supplied from the discharge chamber through the gas discharge pipe, the pressurizer, and the exhaust pipe. In a light emission spectroscopic analyzer having a function of external discharge, if a blockage occurs in the flow path of the exhaust gas from the pressurizer, the pressure in the flow path of the inert gas from the gas supply source to the pressurizer via the discharge chamber Rise abnormally. Therefore, in the above-mentioned first invention, the pressure sensor is used for the flow path of the inert gas, that is, in the internal space of any one of a gas supply pipe, a discharge chamber, a gas discharge pipe, or a pressurizer. The pressure of the inert gas is measured, and a warning is issued to the user when the obtained measured value exceeds a predetermined value. Thereby, the user can immediately know that a blockage has occurred in the flow path of the exhaust gas from the pressurizer. For example, it is possible to replace the filter provided on the flow path of the exhaust gas or to perform exhaust equipment including the flow path. Measures such as inspection and maintenance. As a result, problems such as backflow of liquid in the pressurizer as described above can be prevented in advance.

In addition, a light-emitting spectroscopic analysis device of a second invention formed to solve the above-mentioned problems includes: a) a discharge chamber that emits light to excite a sample by generating an internal discharge; b) a pressurizer as a container for storing a liquid C) a gas supply source filled with an inert gas compressed above atmospheric pressure; d) a gas supply pipe, one end of which is connected to the gas supply source, and the other end opened toward the discharge chamber; e) a gas discharge tube Circuit, one end opens toward the discharge chamber, and the other end faces The liquid in the pressurizer is opened; f) an exhaust pipe, one end of which is arranged in the pressurizer above the liquid level of the liquid, and the other end is opened to the outside of the pressurizer; g) a flow sensor that measures the flow of the inert gas in the gas supply line, the gas exhaust line, or the exhaust line; and h) a warning component, The sensor warns the user when the measured value obtained by the sensor is lower than a predetermined value.

As described above, the inert gas is supplied into the discharge chamber from the gas supply source through the gas supply pipe, and the inert gas is further supplied from the discharge chamber through the gas discharge pipe, the pressurizer, and the exhaust pipe. In a light emission spectroscopic analysis device having an external discharge function, if a blockage occurs in a flow path of exhaust gas from a pressurizer, the flow rate of the inert gas in the gas supply pipe, the discharge pipe, and the exhaust pipe Falling abnormally. Therefore, in the second invention, the flow rate of the inert gas in the gas supply pipe, the gas exhaust pipe, or the exhaust pipe is measured by a flow sensor, and the measured value obtained is low when Warn the user at a predetermined value. Thereby, the user can immediately know that a blockage has occurred in the flow path of the exhaust gas from the pressurizer. For example, it is possible to replace the filter provided on the flow path of the exhaust gas or to perform exhaust equipment including the flow path. Measures such as inspection and maintenance. As a result, problems such as backflow of liquid in the pressurizer can be prevented in advance.

Furthermore, as the warning means in the first or second invention, a warning means may be considered in a case where a measured value obtained by the pressure sensor exceeds a predetermined value, or Measured value obtained by the flow sensor When the value is lower than a predetermined value, the meaning or the clogging in the flow path of the exhaust gas from the pressurizer is output to the monitor screen in the form of text or graphics, or in the form of sound. The form is output from the speaker. In addition, it is not limited to these warning members, and the warning member may be set when a measured value obtained by the pressure sensor exceeds a predetermined value or obtained by the flow sensor. When the measured value is lower than the predetermined value, turn on the light or sound the buzzer.

It is desirable that the light emission spectroscopic analysis device according to the first or second invention is further provided with a flow rate adjustment valve provided in the gas supply line, and the pressure sensor or the flow rate A sensor is disposed between the flow regulating valve on the gas supply pipe and the discharge chamber.

The light emission spectroscopic analysis device according to the first or second invention may include a gas supply stop means in addition to or in place of the warning means, and the gas supply stop means may be provided by the When the measured value obtained by the pressure sensor exceeds a predetermined value, or when the measured value obtained by the flow sensor is lower than a predetermined value, the discharge from the gas supply source to the discharge is stopped. Supply of inert gas in the chamber.

According to this configuration, when a blockage occurs in the flow path of the exhaust gas from the pressurizer, the supply of the inert gas is automatically stopped, so that the inert gas can be prevented even when the user is not in the vicinity of the device. The pressure has risen further.

In addition, the light emission spectroscopic analysis device according to the first or second invention may be configured to include a gas emission member whose measured value obtained by the pressure sensor exceeds a predetermined value. Case, or by the When the measured value obtained by the flow sensor is lower than a predetermined value, an inert gas is discharged from the gas exhaust pipe or the pressurizer to the outside.

In addition, instead of the gas discharge member, the gas discharge line or the pressurizer may be provided with a pressure increase of the inert gas to be opened, and the gas discharge line may be opened. Or a configuration of a relief valve which releases an inert gas in the pressurizer to the outside.

According to this configuration, when a blockage occurs in the flow path of the exhaust gas from the pressurizer, the inert gas is discharged from the gas exhaust line or the pressurizer by the gas release member or the release valve. Therefore, even when the user is located away from the device, the abnormal rise in the pressure of the inert gas can be eliminated immediately.

As described above, according to the light-emitting spectroscopic analysis device of the present invention including the above configuration, for example, when the filter is clogged as described above, the sample particles are deposited in the exhaust device, or the pipeline is frozen. When a blockage in the flow path of the exhaust gas from the pressurizer is detected, the meaning is detected based on the measurement value of the pressure sensor or the flow sensor, and the user is warned, or the supply of the inert gas is stopped, Or vent the inert gas outside the device. Therefore, it is possible to prevent an undesired pressure rise, and to avoid problems such as a backflow of liquid in the pressurizer.

110, 210‧‧‧Excitation Department

111, 211‧‧‧discharge generation unit

112, 212‧‧‧ electrode rods

113, 213‧‧‧discharge chamber

113a, 213a‧‧‧light guide hole

114, 214‧‧‧sample mounting plate

114a, 214a‧‧‧Central opening

115, 215‧‧‧ condenser lens

120, 220‧‧‧Spectral Division

121, 221‧‧‧ entrance slit

122, 222‧‧‧diffraction grating

123a ~ 123c, 223a ~ 223c‧‧‧ exit slit

124a ~ 124c, 224a ~ 224c‧‧‧Light detector

125, 225‧‧‧A / D conversion department

130‧‧‧Control‧Processing Section (Warning part)

131‧‧‧ Input Department

132‧‧‧Output section (warning part)

141, 241‧‧‧Gas supply source

142, 242‧‧‧‧Gas supply pipeline

143, 243‧‧‧ On-off valve

144, 244‧‧‧ flow regulating valve

145, 245‧‧‧‧gas exhaust pipeline

146, 246‧‧‧Pressurizer

147, 247‧‧‧ exhaust pipe

148, 248‧‧‧ filters

151‧‧‧Pressure sensor

152‧‧‧ Diverter

153‧‧‧Flow path switching valve

230‧‧‧Control‧Processing Department

246a‧‧‧Liquid

Ar‧‧‧Argon

S‧‧‧Sample

FIG. 1 is a schematic configuration of a light emission spectroscopic analysis apparatus according to an embodiment of the present invention. Illustration.

FIG. 2 is a schematic configuration diagram of a light emission spectroscopic analysis device according to another embodiment of the present invention.

FIG. 3 is a schematic configuration diagram of a conventional emission spectroscopic analysis device.

Hereinafter, the light-emitting spectroscopic analysis device of the present invention will be described with examples. FIG. 1 is a diagram showing a configuration of a main part of a light emission spectroscopic analysis apparatus according to this embodiment. In addition, constituent elements that are the same as or corresponding to those in FIG. 3 described above are denoted by the same two-digit symbols, and descriptions thereof are appropriately omitted.

The main difference between the light emission spectroscopic analysis device of this embodiment and the conventional light emission spectroscopic analysis device is that the pressure sensor 151 is provided on the gas flow path from the gas supply source 141 to the pressurizer 146 through the discharge chamber 113. . When a blockage occurs in the exhaust line 147 for exhausting the gas in the pressurizer 146 or the filter 148 provided on the exhaust line 147, the inert gas (here, argon) cannot be blocked. Since the pressurizer 146 is appropriately discharged, the pressure in the gas flow path rises. Therefore, the pressure in the gas flow path is monitored by the pressure sensor 151, so that a blockage generated in the exhaust line 147 or the filter 148 can be detected immediately.

In addition, the pressure sensor 151 may be provided in each of the constituent elements constituting the argon flow path, that is, any of the gas supply pipe 142, the discharge chamber 113, the gas discharge pipe 145, and the pressurizer 146. One in. However, in the discharge chamber 113, On the further downstream side, fine particles of the evaporated sample are suspended in argon. Therefore, from the viewpoint of avoiding the influence of the fine particles on the measured value, it is desirable to provide a pressure sensor 151 on the upstream side of the discharge chamber 113. . In addition, the pressure in the flow path on the upstream side is higher than the flow rate control valve 144, and even if the exhaust line 147 or the filter 148 is clogged as described above, the pressure fluctuation range is smaller than the downstream side. Therefore, in the light emission spectroscopic analysis device of this embodiment, the pressure sensor 151 is disposed at a position further downstream than the flow rate adjustment valve 144 on the gas supply pipe 142.

The detection signal from the pressure sensor 151 is sent to the control and processing unit 130. In addition, the detection signals from the photodetector 124a, 124b, and 124c of the spectroscopic section 120 are input to the control / processing section 130 via the A / D conversion section 125. The control and processing unit 130 includes dedicated hardware or general-purpose hardware (such as a personal computer) or a combination thereof, and is further connected to an input unit 131 including a keyboard and the like, and an output unit 132 including a monitor or a speaker. The control and processing unit 130 performs a predetermined data processing based on the detection signals from the pressure sensor 151 or the photodetector 124a, the photodetector 124b, and the photodetector 124c, and performs a discharge generating unit 111 and an on-off valve 143. And flow control valve 144. Furthermore, in this embodiment, the control and processing unit 130 and the output unit 132 cooperate to function as a warning means in the present invention.

Next, a basic operation flow when measuring a sample in the light emission spectroscopic analysis device of this embodiment will be described. First, the user sets the sample S on the sample mounting plate 114 of the excitation section 110, and then performs a predetermined operation using the input section 131, thereby instructing the control and processing section 130 to purge the discharge chamber 113 Start. Then, the control / processing unit 130 opens the on-off valve 143 provided in the gas supply line 142 from the gas supply source 141 to the discharge chamber 113, and flushes the air inside the discharge chamber 113 with argon.

The flow rate of argon gas at this time is adjusted by a flow rate adjustment valve 144. The flow regulating valve 144 includes a needle valve for reducing the flow rate of the fluid flowing in the gas supply pipe 142, and a dial for adjusting the opening degree of the needle valve. The user manually operates the scale. To change the opening of the needle valve, thereby adjusting the flow rate of argon gas. In addition, a reference of a flow rate obtained when the dial is rotated at various angles is described around the scale, and the flow rate is set to a relatively high value (for example, 5 L / min) when the sample measurement is performed. Otherwise, set to a relatively low value (for example, 1 L / min). Hereinafter, the former is referred to as a state where the flow is "high", and the latter is referred to as a state where the flow is "low". Furthermore, at the start point of the flushing operation, the flow rate is set to "low".

Thereafter, at a point in time when a predetermined time has elapsed since the flushing of the discharge chamber 113 was started, the user operates the dial provided on the flow adjustment valve 144 to make the argon flow rate "high", and then, uses the input The unit 131 performs a predetermined operation and instructs the control / processing unit 130 to execute the sample measurement. Then, the control / processing unit 130 controls the discharge generating unit 111, thereby applying a high pulse-like voltage to the electrode rod 112 from the discharge generating unit 111, and exciting and emitting the sample S by the spark discharge from the electrode rod 112. . The luminous light obtained at this time passes through the light guide hole 113a provided in the discharge chamber 113, is collected by the condenser lens 115, and is emitted toward the beam splitter 120. The light emitted from the excitation unit 110 enters the beam splitting unit 120 through the entrance slit 121, Wavelength dispersion is performed by the diffraction grating 122. The light in the predetermined wavelength range of the wavelength-dispersed light passes through the exit slit 123a, the exit slit 123b, and the exit slit 123c, and is performed by the photodetector 124a, the photodetector 124b, and the photodetector 124c. Detection.

Once the sample measurement is completed, the user operates the dial of the flow control valve 144 again to return the argon flow to "low". Then, the sample S is replaced, or the position or direction of the sample S on the sample mounting plate 114 is changed so that an area not to be measured in the measurement surface of the sample S is exposed from the central opening 114a. Thereafter, the user operates the dial of the flow rate adjustment valve 144 again to make the argon gas flow rate “high”, and uses the input unit 131 to instruct the control and processing unit 130 to execute the measurement of the sample.

Thereafter, the above-mentioned sample replacement or position change and sample measurement are performed alternately, and at the time point when all the required measurements are completed, the user instructs the control and processing unit 130 via the input unit 131 on the discharge chamber 113. Rinse is over. Then, the control / processing unit 130 closes the on-off valve 143 of the gas supply pipe 142 and stops the introduction of argon gas into the discharge chamber 113.

In the light emission spectroscopic analysis device of this embodiment, the gas supply tube is monitored by the pressure sensor 151 during the period from the start of the flushing of the discharge chamber 113 to the end of the flushing with the sample measurement as described above. Pressure inside the road 142. That is, the detection signal from the pressure sensor 151 is sent to the control / processing unit 130 at predetermined time intervals, and the control / processing unit 130 sequentially determines whether the measured value of the pressure obtained based on the detection signal exceeds a predetermined value. The upper limit. When it is determined that the measured value exceeds the upper limit value, it is emitted from a speaker of the output unit 132. A warning sound, and a message notifying the user that there is a blockage in the exhaust flow path (ie, the exhaust line 147 and the filter 148) from the pressurizer 146 is displayed on the monitor provided in the output section 132 Screen.

Furthermore, even when the exhaust from the pressurizer 146 is performed normally, the pressure in the gas supply line 142 is different between when the argon flow rate is "high" and when it is "low". That is, the internal pressure of the gas supply line 142 is relatively high when the flow rate is "high", and the internal pressure is relatively low when the flow rate is "low". Therefore, as the upper limit value, it is desirable to individually set the upper limit value applied when the flow rate is "high" and the upper limit value applied when the flow rate is "low". The upper limits may be set by the user from the input section 131 during the measurement, or may be set at the time of shipment from the factory of the device, and stored in the memory in the control and processing section 130.

As mentioned above, although the form for implementing this invention was demonstrated using the specific example, this invention is not limited to the said example, It can change suitably within the range of the summary of this invention. For example, in the above example, it is assumed that the flow path of the exhaust gas from the pressurizer is blocked based on the detection value of the pressure sensor, but a flow sensor may be provided instead of the pressure sensor. Composition. In this case, the flow sensor is provided in any one of the gas supply pipe 142, the gas exhaust pipe 145, and the exhaust pipe 147. When the flow sensor detects the Warn the user when the flow is below a predetermined lower limit.

In addition to the warning to the user or replacing the warning as described above, the measurement value of the pressure sensor may exceed the predetermined upper limit value or the measurement value of the flow sensor may be lower than the predetermined lower limit value. In the case of the control, the processing unit 130 is turned off An on-off valve 143 provided in the gas supply line 142 stops the supply of argon gas. According to this configuration, when the exhaust gas from the pressurizer 146 does not flow normally, the supply of argon gas to the discharge chamber 113 is automatically stopped. Therefore, even when the user is not in the vicinity of the device, it can be prevented A further rise in the pressure of argon.

In addition, as shown in FIG. 2, a shunt pipe 152 and a flow path switching valve 153 may be provided on the gas exhaust pipe 145. When the measured value of the pressure sensor 151 exceeds a predetermined upper limit value or the flow rate is sensed. When the measured value of the device is lower than the predetermined lower limit value, the control and processing unit 130 switches the flow path switching valve 153, so that the argon gas discharged from the discharge chamber 113 is directed toward the shunt pipe 152 instead of being added. The presser 146 flows. According to this configuration, when clogging occurs in the exhaust line 147 or the filter 148, argon gas is automatically discharged from the gas exhaust line 145 to the outside, so even when the user is located away from the device , Can also immediately reduce the pressure in the flow path. In addition, it is also possible to provide a configuration in which a release valve (drain valve) for escaping gas from the gas discharge line 145 when the pressure is abnormally increased is used instead of the branch pipe 152 and the flow path switching valve 153 described above. . The release valve is normally closed by the force of a spring. However, if the pressure exceeds the force of the spring due to an increase in the internal pressure, the valve is opened. As a result, the gas in the gas exhaust pipe 145 Argon is exhausted to the outside. In addition, when the flow path switching valve 153 or the release valve is provided, in order to prevent particles of the sample contained in the exhaust gas from the discharge chamber 113 from being discharged to the periphery of the device, it is desirable to remove the particles from the shunt pipe. The exhaust gas from 152 or the release valve is sent to the specified recovery container instead of the atmosphere.

Claims (8)

A luminescence spectroscopic analysis device includes: a) a discharge chamber that causes a sample to emit light by generating an internal discharge; b) a pressurizer as a container for holding a liquid; c) a gas supply source filled with a compressed gas Inert gas above atmospheric pressure; d) gas supply pipe, one end is connected to the gas supply source, and the other end is connected to the discharge chamber; e) gas discharge pipe, one end is connected to the discharge chamber, and the other end Open to the liquid in the pressurizer; f) an exhaust line, one end of which is disposed in the pressurizer above the liquid level of the liquid, and the other end of The outside is opened; g) a pressure sensor that measures the inert gas in the internal space of any one of the gas supply pipe, the discharge chamber, the gas discharge pipe, or the pressurizer; Pressure; h) a warning component that warns a user when a measured value obtained by the pressure sensor exceeds a predetermined value; and a flow regulating valve provided on the gas supply pipeline, the pressure sensing The device is arranged in the gas supply pipe Between the flow regulating valve on the road and the discharge chamber. The light emission spectroscopic analysis device according to item 1 of the scope of patent application, in addition to or in place of the warning part, includes a gas supply stop part which is obtained from the pressure sensor. Measured value exceeded When the value exceeds a predetermined value, the supply of the inert gas from the gas supply source to the discharge chamber is stopped. The light emitting spectroscopic analysis device according to item 1 of the scope of patent application, in addition to or in place of the warning part, includes a gas emission part, and the gas emission part is measured by the pressure sensor. When the value exceeds a predetermined value, an inert gas is discharged from the gas exhaust pipe or the pressurizer to the outside. According to the light emission spectroscopic analysis device according to item 1 of the scope of patent application, in addition to or in place of the warning member, a release valve is provided in the gas exhaust line or the pressurizer, and The release valve is opened as the pressure of the inert gas rises, and releases the inert gas in the gas discharge line or the pressurizer to the outside. A luminescence spectroscopic analysis device includes: a) a discharge chamber that causes a sample to emit light by generating an internal discharge; b) a pressurizer as a container for holding a liquid; c) a gas supply source filled with a compressed gas Inert gas above atmospheric pressure; d) gas supply pipe, one end is connected to the gas supply source, and the other end is opened to the discharge chamber; e) gas discharge pipe, one end is opened to the discharge chamber, and the other end Open to the liquid in the pressurizer; f) an exhaust line, one end of which is disposed in the pressurizer above the liquid level of the liquid, and the other end of Externally open g) a flow sensor that measures the flow of the inert gas in the gas supply line, the gas exhaust line, or the exhaust line; and h) a warning component, Warn the user when the measured value obtained by the sensor is lower than a predetermined value; and a flow regulating valve is provided on the gas supply pipe, and the flow sensor is disposed on the gas supply pipe Between the flow regulating valve and the discharge chamber. The luminescent spectroscopic analysis device according to item 5 of the scope of application for a patent, in addition to or in place of the warning member, includes a gas supply stop member, which is obtained from the flow sensor. When the measured value is lower than a predetermined value, the supply of the inert gas from the gas supply source to the discharge chamber is stopped. The light emitting spectroscopic analysis device according to item 5 of the scope of patent application, in addition to or in place of the warning part, includes a gas emission part, and the gas emission part is a measured value obtained by the flow sensor. When the value is lower than a predetermined value, an inert gas is discharged from the gas exhaust pipe or the pressurizer to the outside. According to the light emission spectroscopic analysis device according to item 5 of the scope of patent application, in addition to or in place of the warning member, a release valve is provided in the gas exhaust line or the pressurizer, and The release valve is opened as the pressure of the inert gas rises, and releases the inert gas in the gas discharge line or the pressurizer to the outside.