WO2022190466A1 - 元素分析装置、元素分析装置の操作方法及び元素分析装置の動作プログラム - Google Patents
元素分析装置、元素分析装置の操作方法及び元素分析装置の動作プログラム Download PDFInfo
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- WO2022190466A1 WO2022190466A1 PCT/JP2021/042816 JP2021042816W WO2022190466A1 WO 2022190466 A1 WO2022190466 A1 WO 2022190466A1 JP 2021042816 W JP2021042816 W JP 2021042816W WO 2022190466 A1 WO2022190466 A1 WO 2022190466A1
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- Prior art keywords
- purge gas
- flow path
- heating furnace
- resistance
- sample
- Prior art date
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- 238000004458 analytical method Methods 0.000 title claims description 46
- 238000000034 method Methods 0.000 title claims description 3
- 238000010926 purge Methods 0.000 claims abstract description 114
- 238000010438 heat treatment Methods 0.000 claims abstract description 78
- 238000007872 degassing Methods 0.000 claims abstract description 61
- 238000005086 pumping Methods 0.000 claims abstract description 15
- 238000007599 discharging Methods 0.000 claims description 8
- 238000000921 elemental analysis Methods 0.000 claims description 8
- 238000003795 desorption Methods 0.000 claims 2
- 239000007789 gas Substances 0.000 description 114
- 239000012159 carrier gas Substances 0.000 description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 229910002804 graphite Inorganic materials 0.000 description 10
- 239000010439 graphite Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001745 non-dispersive infrared spectroscopy Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Definitions
- the present invention relates to an elemental analyzer that analyzes elements contained in a sample based on sample gas generated by heating the sample.
- a sample is placed in a graphite crucible installed in a heating furnace, and an electric current is passed through the graphite crucible to generate heat, thereby heating the sample.
- the heating furnace is opened and the graphite crucible is replaced for each analysis. Before that, it is necessary to perform a degassing (purging) to exhaust the residual gas in the heating furnace.
- conventional elemental analyzers are provided with a pumping channel for pumping a purge gas, which is an inert gas such as He or Ar, from a cylinder to a heating furnace, and a discharge channel for discharging the purge gas pumped to the heating furnace.
- a purge gas is circulated in the heating furnace, and the residual gas is discharged together with the purge gas.
- Patent Document 1 Japanese Utility Model Laid-Open No. 5-33057
- a configuration has been conceived in which an ejector pump is connected to the rear end of the discharge passage, and the remaining gas is discharged from the heating furnace by suction in a short period of time. rice field.
- the present invention provides an elemental analyzer that can shorten the time required for degassing without sacrificing analysis accuracy, and can also moderate the consumption of purge gas at that time. It is intended as much as possible.
- an elemental analysis apparatus includes a heating furnace for heating a sample to generate a sample gas, an analysis section for analyzing elements contained in the sample based on the sample gas, and a purge gas circulated to a degassing mechanism for discharging residual gas in the heating furnace, wherein the degassing mechanism communicates a pumping passage for pumping a purge gas to the heating furnace with the outside air, and the heating furnace It is characterized by comprising a discharge passage for discharging the purge gas pressure-fed inside to the outside air, and a purge gas flow rate adjustment mechanism for changing the passage resistance of the discharge passage in a plurality of stages or continuously. .
- the flow path resistance of the discharge flow path is first reduced and the purge gas is flowed, so that the degassing is almost completed in a short time, and then the gas is discharged.
- the internal pressure of the heating furnace can be raised by the boosting action of the flow path resistance while degassing, and immediately after degassing, a state in which stable analysis can be performed can be achieved. can.
- the discharge passage has a first exhaust passage and a second exhaust passage provided parallel to each other, and the purge gas flow rate adjustment mechanism
- the purge gas flow rate adjustment mechanism may include an on-off valve that changes the flow path resistance of the discharge flow path in two stages by opening and closing the second exhaust path.
- the heating furnace communicates with the outside air through the second exhaust passage, and the purge gas flows while being maintained at substantially atmospheric pressure. Even if the flow rate is smaller than before, the same degassing effect can be obtained in the same time. This was discovered by the inventors for the first time. According to that knowledge, when the same flow rate of purge gas is flowed through the heating furnace, the pressure is in the atmospheric pressure state when the heating furnace is in an atmospheric pressure state and when it is in a pressurized state with a higher pressure than that. It has been found that the degassing effect is greater in the case of
- the flow path resistance of the discharge flow path is maintained at a low state for a certain period of time and then changed to a high state, the flow path resistance of the discharge flow path will be high at the end of degassing, and heating will occur. Since the pressure in the furnace is in a high state, it is possible to proceed smoothly to the next analysis step.
- the purge gas flow path restricting mechanism is configured to be switchable between an operating state in which the flow rate is restricted and a non-operating state in which the flow rate is not restricted.
- the purge gas flow path limiting mechanism when the flow path resistance of the discharge flow path is low, the purge gas flow path limiting mechanism is in an operating state, and when the flow path resistance of the discharge flow path is high, the purge gas flow path limiting mechanism is in a non-operating state.
- Such a configuration is conceivable.
- the purge gas flow control mechanism when the purge gas is discharged, the purge gas flow control mechanism is operated to maintain the flow resistance of the discharge flow passage in a low state for a certain period of time, and then change the flow resistance to a high state.
- a method for operating an elemental analyzer characterized by Further, in the present invention, when the purge gas is discharged, the purge gas flow rate adjusting mechanism is operated to keep the flow path resistance of the discharge flow path low for a certain period of time, and then change the flow path resistance to a high state. It may be an operation program of an elemental analyzer characterized in that it causes a computer to exhibit the function of performing the analysis.
- FIG. 4 is an operation explanatory view showing the flow of purge gas during the degassing operation of the elemental analyzer in the same embodiment
- FIG. 4 is an operation explanatory view showing the flow of purge gas during the degassing operation of the elemental analyzer in the same embodiment
- FIG. 4 is an operation explanatory view showing the flow of purge gas during the degassing operation of the elemental analyzer in the same embodiment
- FIG. 4 is an operation explanatory view showing the flow of purge gas during the degassing operation of the elemental analyzer in the same embodiment
- FIG. 4 is an operation explanatory diagram showing the flow of carrier gas and sample gas during analysis of the elemental analyzer in the same embodiment. Experimental result data showing the effect of the same embodiment.
- an elemental analysis apparatus 100 heats a metal sample, a ceramic sample, or the like (hereinafter simply referred to as a sample), and generates a gas (hereinafter referred to as a sample gas) at that time.
- a sample gas a gas
- the type, amount, ratio, etc. of the elements contained in the sample can be quantified, and roughly includes the following parts.
- a heating furnace 1 for heating the sample.
- an analysis unit 2 for analyzing the sample gas generated in the heating furnace 1;
- a sample gas delivery mechanism 3 for introducing a carrier gas, which is an inert gas such as He or Ar, into the heating furnace 1 and delivering the sample gas to the analysis section 2 together with the carrier gas.
- the heating furnace 1 heats a sample, for example, by heating a graphite crucible 11 containing the sample.
- the heating furnace 1 is opened so that it is divided into upper and lower parts, and in this open state, the graphite crucible 11 can be inserted therein. Further, the graphite crucible 11 is sandwiched between a pair of electrodes, and configured to heat the crucible 11 by applying current to the crucible 11 from these electrodes.
- the analysis unit 2 measures, for example, the concentrations (amounts) of O, H and N contained in the sample by measuring CO, N2 and H2 in the sample gas, Although not shown, it includes a plurality of NDIRs (non-dispersive infrared gas analyzers), TCDs (thermal conductivity detectors), an oxidizer, a gas remover, and the like. For details of these, the description in JP-A-2013-250061 and the like is used.
- the sample gas delivery mechanism 3 includes a carrier gas introduction path 31 for delivering the carrier gas to the heating furnace 1 and a sample gas delivery path for delivering the sample gas generated in the heating furnace 1 to the analysis unit 2 together with the carrier gas. 32.
- the carrier gas introduction path 31 is mainly composed of a piping member, and its starting end is connected to a high-pressure gas cylinder (not shown), which is a carrier gas supply source, and its terminal end is provided in the heating furnace 1. connected to the inlet.
- a pressure regulating valve (not shown) is provided upstream of the carrier gas introduction passage 31.
- the sample gas delivery path 32 is mainly composed of a piping member, and its starting end is connected to the gas outlet provided in the heating furnace 1, and its terminal end is connected to the analysis section 2.
- a dust filter (not shown) is provided on the sample gas delivery path 32 to filter out soot and the like contained in the sample gas.
- this elemental analysis apparatus 100 pumps the carrier gas, which is also a purge gas, into the heating furnace 1, and discharges unnecessary substances such as residual gas in the heating furnace 1 to the outside air together with the carrier gas.
- a degassing mechanism 4 is further provided. Although the degassing mechanism 4 will be described in detail below, the carrier gas may also be referred to as a purge gas for ease of understanding.
- the degassing mechanism 4 communicates the pressure-feeding passage 41 for pressure-feeding the purge gas to the heating furnace 1 with the heating furnace 1 and the outside air so that the purge gas pressure-fed into the heating furnace 1 is removed by the outside air. and a purge gas flow control mechanism 43 that changes the flow resistance of the discharge flow path 42 in two steps.
- the carrier gas introduction path 31 also functions as the pressure-feed flow path 41 , but the pressure-feed flow path 41 may be provided separately from the carrier gas introduction path 31 .
- the discharge channel 42 is mainly composed of a piping member, and its starting end is connected to a predetermined point in the middle of the sample gas delivery channel 32, and its terminal end is open to the outside air.
- a switching valve V4 which is a three-way valve, is provided at this connection point, and the gas in the heating furnace 1 is discharged to the outside air through the discharge passage 42, or is analyzed through the sample gas delivery passage 32. It is configured so that it can be selected either to be introduced into the mechanism.
- the discharge channel 42 is branched into a first exhaust channel 421 and a second exhaust channel 422 from the middle.
- the flow path resistance of the first exhaust path 421 is configured to be higher than the flow path resistance of the second exhaust path 422 .
- the purge gas flow rate adjusting mechanism 43 is provided on the second exhaust path 422 and has an on-off valve V1 that changes the flow path resistance of the discharge path 42 in two stages. That is, when the opening/closing valve V1 is opened, the passage resistance of the discharge passage 42 decreases and a large flow of purge gas flows, and when the opening/closing valve V1 is closed, the passage resistance increases and a small flow of purge gas flows. is configured to flow.
- a purge gas flow rate limiting mechanism 44 that regulates the maximum flow rate of the purge gas that flows during degassing, and a resistance adding mechanism 7 that operates during depressurization, which will be described later, are provided in series on the pressure feed passage 41. There is.
- the purge gas flow rate limiting mechanism 44 includes a capillary C3 that is a resistance flow path provided on the pressure-feed flow path 41 .
- a bypass is provided in parallel with the capillary C3, and the bypass is provided with an on-off valve V3.
- the on-off valve V3 When the on-off valve V3 is closed, the purge gas passes only through the capillary C3 and is flow controlled by its resistance, that is, the purge gas flow rate limiting mechanism 44 is in operation.
- the on-off valve V3 is open, the purge gas mainly passes through the bypass passage with almost no resistance, and the flow rate is not controlled.
- the resistance adding mechanism 7 increases the flow path resistance of the pressure-feeding flow path 41, and specifically, includes a capillary C2 which is a resistance flow path provided on the pressure-feeding flow path 41.
- a bypass is provided in parallel with the capillary C2, and the bypass is provided with an on-off valve V2.
- the on-off valve V2 When the on-off valve V2 is closed, the purge gas passes only through the capillary C2 and the flow path resistance is added, that is, the additional resistance adjusting mechanism 7 is in operation.
- the on-off valve V2 is open, the purge gas passes through the bypass path with almost no resistance, and flow path resistance is not applied, that is, the resistance adding mechanism 7 is in a non-operating state.
- a command device for electrically controlling the on-off valve.
- This command device comprises, for example, a so-called computer having a CPU, memory, A/D converter, D/A converter, various input/output means, etc., and the CPU and its peripheral devices cooperate according to the program stored in the memory. By operating, a command signal is sent to each of the valves described above to control their operation.
- the switching valve V5 is operated to purge the analysis section 2 at the same time.
- the degassing operation includes an initial pressurization operation to pressurize the heating furnace 1, a depressurization operation to release the pressure of the heating furnace, and a high-speed degassing operation in which a purge gas is supplied while the pressure furnace 1 is maintained at a low pressure (here, atmospheric pressure).
- An operation and a pre-analysis degassing operation in which a purge gas is flowed while the heating furnace 1 is at a high pressure required for analysis are performed in this order before analysis.
- each valve is automatically controlled by a command signal from the command device.
- an empty graphite crucible 11 is set in the heating furnace 1 before the degassing operation starts.
- an initial pressurization operation is performed for a short time (for example, 2 seconds).
- the purge gas flow rate limiting mechanism 44 and the resistance adding mechanism 7 are put into a non-operating state by opening the on-off valves V3 and V2, respectively. Further, the purge gas flow rate control mechanism 43 is brought into a state in which the on-off valve V1 is closed and the purge gas flows only through the capillary C1, that is, the flow resistance of the exhaust flow channel 42 is large.
- an on-off valve (not shown) provided at the base of the pressure-feeding channel 41 is opened, and the purge gas flows into the heating furnace 1 from the pressure-feeding channel 41 and is discharged from the exhaust channel 42 .
- an on-off valve (not shown) provided at the base of the pressure-feeding channel 41 is opened, and the purge gas flows into the heating furnace 1 from the pressure-feeding channel 41 and is discharged from the exhaust channel 42 .
- High pressure eg, 80 kPa
- the purge gas flow rate is substantially determined only by the flow resistance of the capillary C ⁇ b>1 of the purge gas flow rate adjusting mechanism 4 .
- the channel resistance of the capillary C1 in this embodiment is set lower than those of the other capillaries C2 and C3 (the specific magnitude relationship of the channel resistance in this embodiment is C2>C3>C1 ), the purge gas flow rate is greater than during the depressurization operation and high-speed degassing operation, which will be described later.
- a depressurization operation is performed for a short time (for example, 1 second).
- the purge gas flow rate limiting mechanism 44 and the resistance adding mechanism 7 are in an operating state with their open/close valves V3 and V2 closed, respectively.
- the purge gas flow rate control mechanism 43 is brought into a state in which the on-off valve V1 is opened and is not affected by the flow resistance of the capillary C1, that is, the flow resistance of the exhaust flow passage 42 is low.
- the pressurizing furnace 1 is in a state of almost zero flow resistance, while the pressure feed flow path 41 side has high flow resistance due to the series connection of the capillaries C2 and C3, while the exhaust flow path 42 side has almost no flow resistance. From the high pressure state during pressure operation, the atmospheric pressure at the connection destination of the exhaust passage 42 is reached.
- the purge gas flow rate is substantially determined by the series flow resistance of the capillaries C2 and C3, but since the series flow resistance is considerably larger than the flow resistance of the capillary C1, the purge gas flow rate is considerably higher than that during the initial pressurization operation. Few.
- a high speed degassing operation is performed for a predetermined time (for example, 30 seconds).
- the on-off valve V2 of the resistance adding mechanism 7 is opened and becomes non-operating.
- flow path resistance is generated by the capillary C3 of the purge gas flow rate limiting mechanism 44, while on the side of the exhaust flow path 42, there is almost no flow path resistance. It is maintained at atmospheric pressure as it is during operation.
- the purge gas flow rate is determined by the flow resistance of the capillary C3, which is set to be greater than the flow resistance of the capillary C1. more than during operation.
- the pre-analysis degassing operation is performed for a predetermined time (for example, 5 seconds).
- a predetermined time for example, 5 seconds.
- the on-off valve V3 of the purge gas flow rate limiting mechanism 44 is opened to be in a non-operating state, and the on-off valve V1 of the purge gas flow rate adjusting mechanism 43 is closed.
- the purge gas flows only through the capillary C1, that is, the flow path resistance of the exhaust flow path 42 is large. This state is the same state as the initial pressure operation.
- the pressurization furnace 1 is brought to a high pressure (for example, 80 kPa) based on the pressure regulating valve (not shown) at the base of the pumping passage 41, as in the initial pressurization operation.
- the purge gas flow rate is the same as that during the initial pressurization operation.
- the graphite crucible 11 is heated while it is empty.
- the reason for heating in this way is to detach hydrogen (H), oxygen (O), and nitrogen (N) adsorbed on the inner wall of the graphite crucible 11 and the heating furnace 1, so that they can be reliably discharged by the purge gas.
- the predetermined time for each operation may be changed by an operator or the like by inputting it into the command device each time analysis is performed.
- the switching valve V4 is switched to open to the sample gas delivery path 32 side.
- the degassing operation is completed, and as shown in FIG. 6, the carrier gas passes through the heating furnace and is introduced into the analysis section 2, thereby enabling analysis.
- the analysis operation starts.
- the pressure of the heating furnace 1 is brought close to the atmospheric pressure (actually, almost atmospheric pressure), and the purge gas is flowed at a high speed degassing operation.
- the flow path resistance of the discharge flow path 42 is increased to maintain the degassing action, and the internal pressure of the heating furnace 1 is increased by the boosting action due to the flow path resistance.
- the reason why the purge can be performed in a short time during the above-described high-speed degassing operation is that the heating furnace 1 is at atmospheric pressure.
- the present inventors have found that even if the flow rate is the same, the closer the heating furnace is to the atmospheric pressure, the higher the degassing effect.
- the experimental data are shown in FIG. In the graph of FIG. 7, the more the peak is located on the left, the greater the degassing effect. is leaning to the left. This tendency was the same for nitrogen gas.
- the flow rate of the purge gas is made smaller than in the conventional art, thereby reducing the amount of consumption and shortening the purge time.
- the purge gas flow rate control mechanism 43 may be provided with two or more capillaries in parallel so that the flow rate of the purge gas can be switched in three or more stages, or a variable valve may be used in the resistance flow path.
- the resistance may be changed continuously, and the flow rate of the purge gas may be adjusted steplessly and continuously. In this case, the flow rate of the purge gas is reduced at the end of degassing, and the heating furnace 1 is brought into a constant pressurized state at the end of degassing.
- the resistance flow path is not limited to a capillary, and may be an orifice or the like.
- the discharge channel 42 is connected directly to the heating furnace 1 at its beginning, or the carrier gas introduction channel 31 and the pumping channel 41 are provided separately, so that the channel system of the carrier gas used during analysis and the degassing It may be separated from the passage system of the purge gas which is sometimes used. In that case, different gases may be used for the carrier gas and the purge gas.
- Various on-off valves, switching valves, and piping configurations related thereto may be changed by using other types of valves, etc., as long as they have equivalent functions.
- the purge gas flow rate limiting mechanism 44 is not necessarily required.
- the resistance channel is not limited to a capillary, and may be configured by an orifice or the like.
- the present invention is not limited to the above embodiments, and can be modified in various ways without departing from the scope of the invention.
- a heating furnace for heating a sample to generate a sample gas
- an analysis unit for analyzing elements contained in the sample based on the sample gas
- a purge gas circulating in the heating furnace
- the time required for degassing can be shortened without sacrificing analysis accuracy.
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Abstract
Description
さらに、エジェクターポンプで無制限に吸引するため、脱ガス時にパージガスを大量に消費する恐れもある。
本発明は、以上の課題に鑑み、分析精度を犠牲にすることなく脱ガスにかかる時間を短縮でき、さらにその際のパージガスの消費量も適度なものにすることができる元素分析装置を提供すべく図ったものである。
したがって、本発明によれば、分析精度を維持しつつ脱ガスにかかる時間を短縮でき、しかもさらにその際のパージガスの消費量も適度なものにすることができる。
種々の状態に対応できるようにするためには、前記パージガス流路制限機構を、流量制限動作を行う動作状態と流量制限を行わない非動作状態とに切り替え可能に構成しておくことが好ましい。
また、本発明は、前記パージガスの排出時において、前記パージガス流量調節機構を操作して、前記排出流路の流路抵抗が小さい状態を一定期間保った後、該流路抵抗を大きい状態に変化させる機能をコンピュータに発揮させることを特徴とする元素分析装置の動作プログラムでもよい。
1・・・加熱炉
2・・・分析部
4・・・脱ガス機構
41・・・圧送流路
42・・・排出流路
421・・・第1排気路
422・・・第2排気路
43・・・パージガス流量調節機構
V1・・・開閉弁
(2)前記加熱炉1で発生した試料ガスを分析する分析部2。
(3)HeやAr等の不活性ガスであるキャリアガスを前記加熱炉1に導入し、このキャリアガスとともに前記試料ガスを分析部2に送り込む試料ガス送出機構3。
前記加熱炉1は、例えば前記試料が入れられた黒鉛るつぼ11を加熱することにより試料を加熱するものである。この加熱炉1は、上下に分かれるように開成し、この開成状態で前記黒鉛るつぼ11を内部に挿入できるように構成されている。また、前記黒鉛るつぼ11は、一対の電極により挟持されており、これら電極から当該るつぼ11に電流を流して該るつぼ11を加熱するように構成されている。
該脱ガス動作においては、加熱炉1を加圧する初期加圧動作、該加熱炉の圧力を抜く圧抜き動作、加圧炉1を低圧(ここでは大気圧)に保ちながらパージガスを流す高速脱ガス動作、及び加熱炉1を分析に必要な高圧にしながらパージガスを流す分析前脱ガス動作がこの順で分析前に行われる。
なお、この一連の脱ガス動作において、各弁の制御は前記指令装置からの指令信号により自動的に行われる。
まず、脱ガス動作が始まる前に、加熱炉1内に空の黒鉛るつぼ11がセットされる。
次に、初期加圧動作が短時間(例えば2秒)行われる。
この圧抜き動作時には、図3に示すように、前記パージガス流量制限機構44及び前記抵抗付加機構7は、その開閉弁V3、V2がそれぞれ閉じられて、いずれも動作状態となる。他方、前記パージガス流量調節機構43は、その開閉弁V1が開かれて、キャピラリC1の流路抵抗の影響を受けない状態、すなわち排気流路42の流路抵抗が低い状態とされる。
この高速脱ガス動作時には、図4に示すように、前記抵抗付加機構7の開閉弁V2が開かれてこれが非動作状態となる。
このことにより、圧送流路41側は、パージガス流量制限機構44のキャピラリC3による流路抵抗が生じる一方、排気流路42側はほとんど流路抵抗がない状態なので、加圧炉1は、圧抜き動作時と同様に大気圧に維持される。パージガス流量は、キャピラリC3の流路抵抗により定まるが、この流路抵抗は、キャピラリC1の流路抵抗よりも大きく設定してあるので、パージガス流量は、初期加圧動作時よりも少なく、圧抜き動作時よりも多くなる。
この分析前脱ガス動作時には、図5に示すように、パージガス流量制限機構44の開閉弁V3が開かれてこれが非動作状態となるとともに、前記パージガス流量調節機構43の開閉弁V1が閉じられて、キャピラリC1のみにパージガスが流れる状態、すなわち排気流路42の流路抵抗が大きい状態とされる。この状態は前記初期加圧動作時と同じ状態である。
このことにより、前記初期加圧動作時と同様、加圧炉1は、圧送流路41の根元にある調圧弁(図示しない)に基づく高い圧力(例えば80kPa)になる。また、パージガス流量は、記初期加圧動作時と同じである。
また、前記各動作の所定時間は、オペレータ等が分析の都度、前記指令装置に入力するなどして変えられるようにしてもかまわない。
このことにより、脱ガス動作は終了し、図6に示すように、キャリアガスが加熱炉を通って分析部2に導入される分析可能状態となる。この後、加熱炉1内の黒鉛るつぼ11に試料が投入されると分析動作が始まる。
したがって、分析精度を維持しつつ、脱ガス時間を従来よりも短縮できるようになる。また、脱ガス時間を従来と同じにすれば、パージガスの消費量を従来よりも低減させることができるようになる。
この実施形態では、キャピラリC3の流路抵抗値を調整することにより、パージガス流量を、従来よりも小さくしてその消費量を低減しながら、パージ時間の短時間化をも実現している。
例えば、パージガス流量調節機構43は、キャピラリを並列に2以上設けるなどして、パージガスの流量を3段階以上に切り替えることができるようにしてもよいし、抵抗流路に可変バルブを用いるなどしてその抵抗を連続的に変えられるようにし、パージガスの流量を無段階連続的に調節できるようにしてもよい。その場合、脱ガス終期には、パージガスの流量を絞り、脱ガス終了時には、加熱炉1を一定の加圧状態にする。
抵抗流路はキャピラリに限られずオリフィスなどでもよい。
各種開閉弁や切替弁、あるいはそれに係る配管構成などは、同等の機能を奏するのであれば、他種の弁を用いるなどして変更して構わない。
前記パージガス流量制限機構44は、必ずしも必要ない。
抵抗流路はキャピラリに限られず、オリフィスなどで構成してもよい。
その他、本発明は前記実施形態に限られず、その趣旨を逸脱しない範囲において種々変形可能である。
Claims (9)
- 試料を加熱して試料ガスを発生させる加熱炉と、前記試料ガスに基づいて当該試料に含まれる元素を分析する分析部と、パージガスを流通させて前記加熱炉内の残存ガスを排出する脱ガス機構とを備えた元素分析装置であって、
前記脱ガス機構が、
前記加熱炉にパージガスを圧送する圧送流路と、
前記加熱炉と外気とを連通させ、該加熱炉内に圧送されたパージガスを外気に排出する排出流路と、
前記排出流路の流路抵抗を複数段階又は連続的に変化させてパージガスの流量を調節するパージガス流量調節機構とを備えていることを特徴とする元素分析装置。 - 前記排出流路が、互いに並行に設けられた第1排気路及び第2排気路を有したものであり、
前記パージガス流量調節機構が、前記第2排気路を開閉することにより、前記排出流路の流路抵抗を2段階に変化させる開閉弁を備えたものであることを特徴とする請求項1記載の元素分析装置。 - 前記第1排気路が抵抗流路を備えており、該第1排気路の流路抵抗が前記第2排気路の流路抵抗よりも高くなるように構成されていることを特徴とする請求項2記載の元素分析装置。
- 前記第2排気路が配管部材のみによって構成されていることを特徴とする請求項3記載の元素分析装置。
- 前記パージガス流量調節機構は、前記排出流路の流路抵抗が小さい状態を一定期間保った後、該流路抵抗を大きい状態に変化させることを特徴とする請求項1乃至4いずれか記載の元素分析装置。
- 前記圧送流路に設けられてパージガスの最大流量を制限するパージガス流量制限機構をさらに備えており、
該パージガス流路制限機構が、流量制限動作を行う動作状態と流量制限を行わない非動作状態とに切り替え可能に構成されていることを特徴とする請求項1乃至5いずれか記載の元素分析装置。 - 前記排出流路が、互いに並行に設けられた第1排気路及び第2排気路を有したものであり、前記パージガス流量調節機構が、前記第2排気路を開閉することにより、前記排出流路の流路抵抗を2段階に変化させる開閉弁を備えているものであって、
前記第2排気路が開状態においては前記パージガス流路制限機構が動作状態となり、前記第2排気路が閉状態においては前記パージガス流路制限機構が非動作状態となることを特徴とする請求項6記載の元素分析装置。 - 試料を加熱して試料ガスを発生させる加熱炉と、前記試料ガスを検出して当該試料に含まれる元素を分析する分析部と、パージガスを流通させて前記加熱炉内の残存ガスを排出する脱ガス機構とを備え、
前記脱ガス機構が、前記加熱炉にパージガスを圧送する圧送流路と、前記加熱炉と外気とを連通させ、該加熱炉内に圧送された前記パージガスを外気に排出する排出流路と、前記排出流路の流路抵抗を複数段階又は連続的に変化させるパージガス流量調節機構とを備えている元素分析装置の操作方法であって、
前記パージガスの排出時において、前記パージガス流量調節機構を操作して、前記排出流路の流路抵抗が小さい状態を一定期間保った後、該流路抵抗を大きい状態に変化させることを特徴とする元素分析装置の操作方法。 - 試料を加熱して試料ガスを発生させる加熱炉と、前記試料ガスを検出して当該試料に含まれる元素を分析する分析部と、パージガスを流通させて前記加熱炉内の残存ガスを排出する脱ガス機構とを備え、
前記脱ガス機構が、前記加熱炉にパージガスを圧送する圧送流路と、前記加熱炉と外気とを連通させ、該加熱炉内に圧送された前記パージガスを外気に排出する排出流路と、前記排出流路の流路抵抗を複数段階又は連続的に変化させるパージガス流量調節機構とを備えている元素分析装置の動作プログラムであって、
前記パージガスの排出時において、前記パージガス流量調節機構を操作して、前記排出流路の流路抵抗が小さい状態を一定期間保った後、該流路抵抗を大きい状態に変化させる機能をコンピュータに発揮させることを特徴とする元素分析装置の動作プログラム。
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