WO2018193495A1 - 発光分光分析装置 - Google Patents

発光分光分析装置 Download PDF

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Publication number
WO2018193495A1
WO2018193495A1 PCT/JP2017/015471 JP2017015471W WO2018193495A1 WO 2018193495 A1 WO2018193495 A1 WO 2018193495A1 JP 2017015471 W JP2017015471 W JP 2017015471W WO 2018193495 A1 WO2018193495 A1 WO 2018193495A1
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WO
WIPO (PCT)
Prior art keywords
gas
pressurizer
gas supply
discharge chamber
discharge
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Application number
PCT/JP2017/015471
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English (en)
French (fr)
Japanese (ja)
Inventor
晶 菅瀬
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株式会社島津製作所
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 株式会社島津製作所 filed Critical 株式会社島津製作所
Priority to CN201780089644.4A priority Critical patent/CN110546485B/zh
Priority to JP2019513512A priority patent/JP6897763B2/ja
Priority to PCT/JP2017/015471 priority patent/WO2018193495A1/ja
Priority to TW107111780A priority patent/TWI672485B/zh
Publication of WO2018193495A1 publication Critical patent/WO2018193495A1/ja

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
    • G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges

Definitions

  • the present invention relates to an emission spectroscopic analysis apparatus that excites a solid sample by discharge and performs spectroscopic measurement of the emitted light.
  • an emission spectroscopic analyzer In an emission spectroscopic analyzer, generally, a solid sample, which is a metal or nonmetal, is given energy by arc discharge or spark discharge to evaporate and evaporate the sample, and the emitted light is introduced into a spectrometer. A spectral line having a wavelength peculiar to the element is extracted and detected (for example, see Patent Document 1).
  • an emission spectroscopic analyzer using a spark discharge as an excitation source is capable of highly accurate analysis. For example, in a production plant such as a steel material or a non-ferrous metal material, a composition analysis in a produced metal body is performed. Widely used.
  • the configuration of a conventional general emission spectroscopic analyzer is shown in FIG.
  • the emission spectroscopic analysis apparatus includes an excitation unit 210 that excites and emits a solid sample S, a spectroscopic unit 220 that detects light emitted from the sample S by wavelength dispersion, and a control / processing unit that performs control and data processing of each unit. 230.
  • the excitation unit 210 includes a discharge generation unit 211, an electrode rod 212, a discharge chamber 213, a sample mounting plate 214, and a condenser lens 215.
  • the discharge chamber 213 is provided with an analysis opening opened obliquely upward and a light guide hole 213a for taking out light from the discharge chamber 213, and a sample is provided above the discharge chamber 213 so as to cover the analysis opening.
  • a mounting plate 214 is detachably attached.
  • the sample mounting plate 214 has a central opening 214a smaller than the sample S. By placing the sample S on the sample mounting plate 214 so as to cover the central opening 214a, the lower surface ( A part of the surface to be analyzed) is exposed inside the discharge chamber 213.
  • an electrode rod 212 for discharge is disposed with its tip directed toward the central opening 214a.
  • the discharge generator 211 applies a pulsed high voltage to the electrode bar 212 in synchronization with a predetermined frequency (for example, 400 Hz).
  • the sample S such as iron or non-ferrous metal is excited to emit light by the spark discharge from the electrode rod 212.
  • Light emitted by excitation light emission of the sample S passes through a light guide hole 213 a provided in the discharge chamber 213, is collected by the condenser lens 215, and is introduced into the spectroscopic unit 220 through the entrance slit 221.
  • the spectroscopic unit 220 includes a diffraction grating 222 for wavelength-dispersing light from the sample S in order to obtain spectral lines having wavelengths unique to a plurality of elements, Exit slits 223a, 223b, and 223c disposed at positions where spectral lines of wavelengths reach, and a plurality of photodetectors (usually photomultiplier tubes) 224a disposed behind the exit slits 223a, 223b, and 223c. 224b and 224c.
  • Light incident on the spectroscopic unit 220 from the excitation unit 210 through the entrance slit 221 is wavelength-dispersed by the diffraction grating 222, and a predetermined wavelength range in which the wavelength-dispersed light passes through the exit slits 223a, 223b, and 223c.
  • a predetermined wavelength range in which the wavelength-dispersed light passes through the exit slits 223a, 223b, and 223c. are detected by the photodetectors 224a, 224b, and 224c.
  • Detection signals obtained by the respective photodetectors 224a, 224b, and 224c obtained by measuring the sample are input to the control / processing unit 230 via the A / D conversion unit 225, and are included by performing predetermined data processing.
  • the intensity of the spectral line of a certain element having a quantity is obtained, and based on this, quantitative analysis or the like for each element is executed.
  • the influence of the gas components in the discharge chamber 213 on the analysis result is suppressed, the discharge is stabilized to improve the analysis accuracy, and the light having a wavelength in the vacuum ultraviolet region is attenuated.
  • the sample is measured. High purity argon gas is introduced into the discharge chamber 213.
  • the discharge chamber 213 includes a gas supply conduit 242 for supplying argon gas from a gas supply source 241 such as a gas cylinder to the discharge chamber 213, and a gas exhaust conduit for discharging gas from the discharge chamber 213. H.245 is connected.
  • An open / close valve 243 and a flow rate adjusting valve 244 are provided on the gas supply line 242, and the argon gas is introduced into the discharge chamber 213 by being driven by the control / processing unit 230 or the user. .
  • the discharge chamber 213 must be maintained at a pressure higher than the atmospheric pressure in order to prevent a decrease in argon gas purity due to the inflow of air from the surroundings.
  • the end of the gas discharge conduit 245 is not opened to the atmosphere, but is led to a container called a pressurizer 246 and opened in a liquid 246 a such as water or oil accommodated in the pressurizer 246.
  • the gas introduced into the pressurizer 246 from the end of the gas discharge conduit 245 is discharged to the outside through the exhaust conduit 247 provided in the pressurizer 246.
  • One end of the exhaust pipe 247 is disposed above the liquid level in the pressurizer 246, and the other end is opened to the atmosphere outside the pressurizer 246.
  • the exhaust from the pressurizer 246 is discharged to the outside via the exhaust equipment or provided on the exhaust pipe 247 as shown in FIG. It is common to discharge indoors through a filter 248.
  • the filter 248 When using the filter 248 as described above, periodic filter replacement is required. If the filter 248 continues to be used without being replaced, the exhaust flow rate from the pressurizer 246 may be reduced due to clogging of the filter 248 and may eventually not flow at all. Also, even when exhaust is released outdoors through an exhaust facility without using a filter, for example, evaporated sample particulates accumulate in the flow path of the exhaust facility, or exhaust is emitted outdoors in a cold region. For example, the end of the pipe line for freezing may freeze, and the exhaust from the pressurizer 246 may not flow.
  • the gas supply path from the gas supply source 241 to the pressurizer 246 that is, the gas supply conduit 242, the discharge chamber 213, and the gas
  • the pressure in the discharge pipe 245 and the internal space of the pressurizer 246 increases, and the liquid 246a in the pressurizer 246 flows back into the discharge chamber 213 at the moment when the sample S is removed from the sample mounting plate 214 after the measurement is completed.
  • problems such as contamination of the discharge chamber 213 may occur.
  • the present invention has been made in view of the above points, and an object of the present invention is to provide an emission spectroscopic analyzer that does not cause problems due to clogging of the exhaust passage from the pressurizer as described above. There is to do.
  • An emission spectroscopic analysis apparatus made to solve the above-mentioned problems, a) a discharge chamber in which a sample is excited to emit light by generating discharge inside; b) a pressurizer that is a container containing a liquid; c) a gas supply source filled with an inert gas compressed above atmospheric pressure; d) a gas supply line having one end connected to the gas supply source and the other end connected to the discharge chamber; e) a gas exhaust line having one end connected to the discharge chamber and the other end opened to the liquid in the pressurizer; f) an exhaust pipe having one end disposed above the liquid level of the liquid in the pressurizer and the other end opened to the outside of the pressurizer; g) a pressure sensor that measures the pressure of the inert gas in the internal space of any of the gas supply line, the discharge chamber, the gas discharge line, or the pressurizer; h) warning means for issuing a warning to the user when the measured value by the pressure sensor exceeds a predetermined value;
  • the inert gas is supplied from the gas supply source to the discharge chamber via the gas supply line, and further, the inert gas is supplied from the discharge chamber to the gas discharge line, the pressurizer, and the exhaust line.
  • the emission spectroscopic analysis apparatus having a function of discharging the gas to the outside, when clogging occurs on the flow path of the exhaust from the pressurizer, the flow path of the inert gas from the gas supply source through the discharge chamber to the pressurizer Pressure rises abnormally. Therefore, in the first aspect of the invention, the pressure of the inert gas in the internal space of any one of the flow paths of the inert gas, that is, the gas supply conduit, the discharge chamber, the gas discharge conduit, or the pressurizer is measured.
  • the user can immediately know that clogging has occurred on the flow path of the exhaust gas from the pressurizer.
  • the filter provided on the flow path of the exhaust gas can be replaced or the exhaust gas including the flow path can be replaced. It is possible to take measures such as inspection and maintenance of equipment. As a result, it is possible to prevent problems such as the backflow of the liquid in the pressurizer as described above.
  • an emission spectroscopic analyzer made to solve the above problems is a) a discharge chamber in which a sample is excited to emit light by generating discharge inside; b) a pressurizer that is a container containing a liquid; c) a gas supply source filled with an inert gas compressed above atmospheric pressure; d) a gas supply line having one end connected to the gas supply source and the other end opened to the discharge chamber; e) a gas exhaust line having one end opened in the discharge chamber and the other end opened in the liquid in the pressurizer; f) an exhaust pipe having one end disposed above the liquid level of the liquid in the pressurizer and the other end opened to the outside of the pressurizer; g) a flow rate sensor for measuring a flow rate of the inert gas in the gas supply line, the gas discharge line, or the exhaust line; h) warning means for issuing a warning to the user when the measured value by the flow sensor falls below a predetermined value; It is good also as what is characterized by
  • the inert gas is supplied from the gas supply source to the discharge chamber via the gas supply line, and further, the inert gas is supplied from the discharge chamber to the gas discharge line, the pressurizer, and the exhaust line.
  • the emission spectroscopic analyzer having a function of discharging the gas to the outside, when clogging occurs on the flow path of the exhaust from the pressurizer, the gas supply pipe, the discharge pipe, and the inert gas in the exhaust pipe The flow rate drops abnormally. Therefore, in the second aspect of the invention, the flow rate of the inert gas in the gas supply pipe, the gas discharge pipe, or the exhaust pipe is measured by a flow sensor, and the obtained measurement value is lower than a predetermined value. If this happens, a warning is issued to the user.
  • the user can immediately know that clogging has occurred on the flow path of the exhaust gas from the pressurizer.
  • the filter provided on the flow path of the exhaust gas can be replaced or the exhaust gas including the flow path can be replaced. It is possible to take measures such as inspection and maintenance of equipment. As a result, it is possible to prevent problems such as the backflow of the liquid in the pressurizer described above.
  • the warning means in the first invention or the second invention when the measured value by the pressure sensor exceeds a predetermined value, or the measured value by the flow sensor falls below a predetermined value. In such a case, it may be possible to output the fact or the fact that clogging has occurred on the flow path of the exhaust from the pressurizer on the screen of the monitor as characters or graphics, or output from the speaker as sound. Further, the present invention is not limited thereto, and the warning means is used when the measured value by the pressure sensor exceeds a predetermined value, or when the measured value by the flow sensor falls below a predetermined value. It is good also as what makes it light or sounds a buzzer.
  • the emission spectroscopic analyzer according to the first invention or the second invention further includes a flow rate adjusting valve provided on the gas supply pipe, and the pressure sensor or the flow sensor is provided on the gas supply pipe. It is desirable that the flow control valve is disposed between the discharge chamber and the discharge chamber.
  • the emission spectroscopic analyzer according to the first invention or the second invention may be used when the measured value by the pressure sensor exceeds a predetermined value, or by the flow sensor.
  • Gas supply stop means may be provided for stopping supply of inert gas from the gas supply source to the discharge chamber when the measured value falls below a predetermined value.
  • the emission spectroscopic analysis apparatus may be configured such that the measured value by the pressure sensor exceeds a predetermined value, or the measured value by the flow sensor falls below a predetermined value.
  • the gas discharge pipe or the gas discharge means for discharging the inert gas from the pressurizer may be provided.
  • the gas discharge conduit or the pressurizer is opened as the pressure of the inert gas increases, and the inert gas in the gas discharge conduit or the pressurizer is opened. It is also possible to provide a relief valve that discharges to the outside.
  • the inert gas when clogging occurs on the flow path of the exhaust from the pressurizer, the inert gas is discharged from the gas discharge conduit or the pressurizer by the gas discharge means or the relief valve. Therefore, even when the user is away from the apparatus, the abnormal increase in the pressure of the inert gas can be solved immediately.
  • the emission spectroscopic analysis apparatus As described above, according to the emission spectroscopic analysis apparatus according to the present invention having the above-described configuration, for example, due to the clogging of the filter as described above, the accumulation of sample fine particles in the exhaust facility, or the freezing of the pipeline.
  • clogging occurs on the flow path of the exhaust from the pressurizer, this is detected based on the measured value of the pressure sensor or flow sensor, and a warning is given to the user, or the supply of inert gas is stopped, The inert gas is discharged outside the apparatus. Therefore, an undesired increase in pressure can be prevented, and problems such as backflow of liquid in the pressurizer can be avoided.
  • FIG. 1 is a schematic configuration diagram of an emission spectroscopic analyzer according to an embodiment of the present invention.
  • 1 is a schematic configuration diagram of a conventional emission spectroscopic analyzer.
  • FIG. 1 is a diagram showing a main configuration of an emission spectroscopic analyzer according to the present embodiment.
  • subjected and description is abbreviate
  • the main difference between the emission spectroscopic analysis apparatus according to this embodiment and the conventional emission spectroscopic analysis apparatus is that a pressure sensor 151 is provided on a gas flow path from the gas supply source 141 to the pressurizer 146 through the discharge chamber 113. It is.
  • the pressurizer 146 provides an inert gas (here, argon gas). Is not properly discharged, the pressure in the gas flow path increases. Therefore, by monitoring the pressure in the gas flow path with the pressure sensor 151, it is possible to immediately detect clogging occurring in the exhaust pipe 147 or the filter 148.
  • the pressure sensor 151 may be provided in any of the components constituting the argon gas flow path, that is, the gas supply pipe 142, the discharge chamber 113, the gas discharge pipe 145, and the pressurizer 146. .
  • the pressure is more upstream than the discharge chamber 113 from the viewpoint of avoiding the influence of the fine particles on the measurement value. It is desirable to provide the sensor 151.
  • the upstream side of the flow rate adjusting valve 144 has a higher pressure in the flow path than the downstream side, and even if the exhaust pipe 147 or the filter 148 is clogged as described above, the pressure fluctuation range is on the downstream side. Smaller. Therefore, in the emission spectroscopic analysis apparatus according to this embodiment, the pressure sensor 151 is disposed at a position downstream of 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 / processing unit 130. Further, detection signals from the photodetectors 124 a, 124 b, and 124 c of the spectroscopic unit 120 are input to the control / processing unit 130 via the A / D conversion unit 125.
  • the control / processing unit 130 is configured by dedicated hardware, general-purpose hardware (such as a personal computer), or a combination thereof, and further includes an input unit 131 including a keyboard and an output unit 132 including a monitor and a speaker. Is connected.
  • the control / processing unit 130 executes predetermined data processing based on detection signals from the pressure sensor 151 and the photodetectors 124a, 124b, and 124c, as well as a discharge generation unit 111, an on-off valve 143, and a flow rate adjustment valve. 144 and the like are controlled.
  • the control / processing unit 130 and the output unit 132 cooperate to function as warning means in the present invention.
  • the user sets the sample S on the sample mounting plate 114 of the excitation unit 110 and then performs a predetermined operation with the input unit 131 to instruct the control / processing unit 130 to start purging the discharge chamber 113.
  • the control / processing unit 130 opens the opening / closing valve 143 provided in the gas supply conduit 142 from the gas supply source 141 to the discharge chamber 113, and purges the air inside the discharge chamber 113 with argon gas.
  • the flow rate of the argon gas is adjusted by the flow rate adjusting valve 144.
  • the flow rate adjusting valve 144 has a needle valve for restricting the flow rate of the fluid flowing through the gas supply pipe 142 and a dial for adjusting the opening of the needle valve, and the user manually operates the dial.
  • the flow rate of the argon gas can be adjusted by changing the opening of the needle valve.
  • a guideline of the flow rate obtained when the dial is rotated at various angles is described around the dial, and the flow rate is a relatively high value (for example, 5 L / L) when performing sample measurement. min), otherwise it is set to a relatively low value (eg 1 L / min).
  • the former is referred to as a “high” state
  • the latter is referred to as a “low” state.
  • the flow rate is set to “low” at the start of the purge operation.
  • the user operates the dial provided on the flow rate adjustment valve 144 to set the argon gas flow rate to “high”, and then the input unit 131.
  • a predetermined operation is performed to instruct the control / processing unit 130 to execute sample measurement.
  • the control / processing unit 130 controls the discharge generation unit 111 to apply a pulsed high voltage from the discharge generation unit 111 to the electrode bar 112 and excite the sample S by the spark discharge from the electrode bar 112. Make it emit light.
  • the emitted light obtained at this time passes through a light guide hole 113 a provided in the discharge chamber 113, is condensed by the condenser lens 115, and is emitted to the spectroscopic unit 120.
  • the emitted light emitted from the excitation unit 110 enters the spectroscopic unit 120 through the entrance slit 121 and is wavelength-dispersed by the diffraction grating 122.
  • the wavelength-dispersed light light in a predetermined wavelength range passes through the exit slits 123a, 123b, and 123c, and is detected by the photodetectors 124a, 124b, and 124c.
  • the user When one sample measurement is completed, the user operates the dial of the flow rate adjusting valve 144 again to return the argon gas flow rate to “low”. Then, the sample S is exchanged, or the position and orientation of the sample S on the sample mounting plate 114 are changed so that the region of the measurement surface of the sample S that has not been used for measurement is exposed from the central opening 114a. Or Thereafter, the user operates the dial of the flow rate adjusting valve 144 again to set the argon gas flow rate to “high”, and instructs the control / processing unit 130 to execute sample measurement using the input unit 131.
  • the user sets the discharge chamber 113 in the control / processing unit 130 via the input unit 131. Instructs the end of purging. Then, the control / processing unit 130 closes the open / close valve 143 of the gas supply conduit 142 and stops introducing argon gas into the discharge chamber 113.
  • the pressure in the gas supply pipe 142 is monitored by the pressure sensor 151 from the start of the purge of the discharge chamber 113 accompanying the sample measurement as described above to the end of the purge.
  • the detection signal from the pressure sensor 151 is sent to the control / processing unit 130 at a predetermined time interval, and the control / processing unit 130 sets the measured value of the pressure obtained from the detection signal to a predetermined upper limit value. It is sequentially judged whether or not it exceeds.
  • a warning sound is emitted from the speaker of the output unit 132 and the exhaust passage from the pressurizer 146 (that is, the exhaust pipe 147 and the filter 148).
  • a message for notifying the user that clogging has occurred is displayed on a monitor screen provided in the output unit 132.
  • the pressure in the gas supply pipe line 142 differs depending on whether the argon gas flow rate is “high” or “low” even when the exhaust from the pressurizer 146 is normally performed. That is, when the flow rate is “high”, the internal pressure of the gas supply pipe 142 is relatively high, and when the flow rate is “low”, the internal pressure is relatively low. Therefore, it is desirable that the upper limit value applied when the flow rate is “high” and the upper limit value applied when the flow rate is “low” are individually set as the upper limit value. These upper limit values may be set by the user from the input unit 131 at the time of measurement, or may be set at the time of shipment of the apparatus from the factory and stored in the memory in the control / processing unit 130. Good.
  • this invention is not limited to said example, A change is suitably permitted in the range of the meaning of this invention. It is.
  • clogging of the flow path of the exhaust gas from the pressurizer is detected based on the detection value of the pressure sensor, but a flow rate sensor may be provided instead of the pressure sensor.
  • the flow rate sensor is provided in any one of the gas supply line 142, the gas discharge line 145, and the exhaust line 147, and the flow rate detected by the flow rate sensor is below a predetermined lower limit value. It is assumed that a warning is issued to the user in the event of a failure.
  • the processing unit 130 may close the on-off valve 143 provided in the gas supply conduit 142 to stop the supply of argon gas. According to such a configuration, when the exhaust from the pressurizer 146 stops flowing normally, the supply of argon gas to the discharge chamber 113 is automatically stopped, so even when the user is not near the apparatus. Further increase in the pressure of argon gas can be prevented.
  • a branch pipe 152 and a flow path switching valve 153 are provided on the gas discharge pipe 145, and the measured value of the pressure sensor 151 exceeds a predetermined upper limit value or the measured value of the flow sensor.
  • the control / processing unit 130 switches the flow path switching valve 153 so that the argon gas discharged from the discharge chamber 113 is not on the pressurizer 146 but on the branch tube 152 side. You may make it flow.
  • the exhaust pipe 147 or the filter 148 is clogged, the argon gas is automatically discharged from the gas discharge pipe 145 to the outside. Even in the place, the pressure in the flow path can be immediately reduced.
  • a relief valve for allowing gas to escape from the gas discharge pipe 145 when the pressure rises abnormally may be provided.
  • This relief valve is normally closed by the force of a spring, but when the pressure higher than the force of the spring is applied due to an increase in internal pressure, the valve opens and, as a result, a gas exhaust line 145 is opened. The argon gas inside is discharged to the outside.
  • the branch pipe 152 or the relief valve is used. It is desirable to send the exhaust gas to a predetermined collection container instead of the atmosphere.

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  • Health & Medical Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
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  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
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PCT/JP2017/015471 2017-04-17 2017-04-17 発光分光分析装置 WO2018193495A1 (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
CN201780089644.4A CN110546485B (zh) 2017-04-17 2017-04-17 发光分光分析装置
JP2019513512A JP6897763B2 (ja) 2017-04-17 2017-04-17 発光分光分析装置
PCT/JP2017/015471 WO2018193495A1 (ja) 2017-04-17 2017-04-17 発光分光分析装置
TW107111780A TWI672485B (zh) 2017-04-17 2018-04-03 發光分光分析裝置

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Application Number Priority Date Filing Date Title
PCT/JP2017/015471 WO2018193495A1 (ja) 2017-04-17 2017-04-17 発光分光分析装置

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WO2018193495A1 true WO2018193495A1 (ja) 2018-10-25

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JP (1) JP6897763B2 (zh)
CN (1) CN110546485B (zh)
TW (1) TWI672485B (zh)
WO (1) WO2018193495A1 (zh)

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