WO2022071111A1 - 全有機炭素計及び燃焼反応ユニット - Google Patents
全有機炭素計及び燃焼反応ユニット Download PDFInfo
- Publication number
- WO2022071111A1 WO2022071111A1 PCT/JP2021/035070 JP2021035070W WO2022071111A1 WO 2022071111 A1 WO2022071111 A1 WO 2022071111A1 JP 2021035070 W JP2021035070 W JP 2021035070W WO 2022071111 A1 WO2022071111 A1 WO 2022071111A1
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- WIPO (PCT)
- Prior art keywords
- organic carbon
- furnace body
- unit
- combustion reaction
- total organic
- Prior art date
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- 238000002485 combustion reaction Methods 0.000 title claims abstract description 97
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 54
- 239000007788 liquid Substances 0.000 claims abstract description 84
- 230000008016 vaporization Effects 0.000 claims abstract description 67
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000003054 catalyst Substances 0.000 claims abstract description 38
- 230000007246 mechanism Effects 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 19
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 19
- 238000009834 vaporization Methods 0.000 claims description 26
- 238000005070 sampling Methods 0.000 claims description 21
- 230000002093 peripheral effect Effects 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000000919 ceramic Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 11
- 238000001514 detection method Methods 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 description 23
- 239000012159 carrier gas Substances 0.000 description 20
- 238000010586 diagram Methods 0.000 description 10
- 238000003745 diagnosis Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- 230000006870 function Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 238000009429 electrical wiring Methods 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000011144 upstream manufacturing Methods 0.000 description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000009530 blood pressure measurement Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000007791 dehumidification Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 230000010349 pulsation Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1826—Organic contamination in water
- G01N33/1846—Total carbon analysis
-
- 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
-
- 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
- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
-
- 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
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
Definitions
- the present invention relates to an all-organic carbon meter used for analysis of water quality and the like and a combustion reaction unit used therein.
- this type of total organic carbon meter guides a liquid sample to a combustion furnace made of ceramics to burn the total organic carbon contained in the liquid sample, and detects carbon dioxide generated thereby.
- a combustion furnace made of ceramics to burn the total organic carbon contained in the liquid sample, and detects carbon dioxide generated thereby.
- carbon dioxide generated thereby There is one configured in.
- the heating furnace of this all-organic carbon meter has a double-tube structure consisting of an outer cylinder and an inner cylinder provided inside the outer cylinder, and a vaporizing member is arranged below the inner cylinder.
- a catalyst is provided between the outer cylinder and the inner cylinder.
- the present invention has been made to solve the above-mentioned problems, and its main purpose is to allow the vaporizing member and the catalyst to be placed close to each other in a configuration in which a sample vaporized by the vaporizing member is passed through the catalyst. It is an issue.
- the total organic carbon meter according to the present invention is a total organic carbon meter that measures the total organic carbon contained in the liquid sample, and is a combustion reaction that burns the total organic carbon contained in the liquid sample to generate carbon dioxide. It has a unit and a carbon dioxide detection unit that detects carbon dioxide generated by the combustion reaction unit, and the combustion reaction unit includes a combustion furnace main body, a vaporization member housed inside the combustion furnace main body, and the above. It is characterized by having a heating mechanism for heating the vaporizing member and a catalyst arranged below the vaporizing member.
- the catalyst is arranged below the vaporizing member, it is not necessary to raise the sample vaporized by the vaporizing member toward the catalyst, and the vaporizing member and the catalyst can be used. Can be placed close to each other, the combustion efficiency of organic substances in the liquid sample can be improved, and the measurement accuracy can be improved.
- the catalyst is in contact with the vaporizing member inside the combustion furnace main body.
- the catalyst and the vaporizing member can be arranged without sandwiching the air layer between them, the above-mentioned improvement of combustion efficiency and the like becomes more effective.
- the vaporizing member and the catalyst may be made of different materials.
- the combustion furnace main body preferably has an inner furnace body into which the liquid sample is introduced and an outer furnace body surrounding the inner furnace body.
- the heating furnace body has an inner furnace body into which the liquid sample is introduced and an outer furnace body surrounding the inner furnace body, so that the inner furnace body expands the outer furnace body. It is possible to suppress cracking and the like.
- the outer furnace body is characterized in that the inner peripheral surface from one end opening to the other end opening forms a straight tubular shape having the same cross-sectional shape.
- the outer furnace body can be easily molded by, for example, drawing. It can also improve workability.
- the vaporization member is a granular material made of ceramics
- the heating mechanism has a heater that surrounds an axially central portion of the outer furnace body, and the granular body is placed in the combustion furnace inside the inner furnace body.
- a holding member for holding the main body is provided at the central portion in the axial direction. With such a configuration, the ceramic granules can be held in the vicinity of the heater by the holding member.
- the holding member has a passage passage through which the gas generated from the liquid sample passes.
- the inner furnace body, the vaporization member, and the holding member are unitized and are collectively detachable from the outer furnace body. With such a configuration, maintainability such as replacement work can be improved.
- a metal introduction-side flange portion is connected to the end on the one-end opening side, and the introduction-side flange portion is made of resin for introducing the liquid sample into the combustion furnace main body. It is preferable that the sample introduction pipe is connected and a cooling mechanism for cooling the sample introduction pipe by cooling the introduction side flange portion is provided outside the introduction side flange portion. With such a configuration, since a resin-made sample introduction tube is used, a predetermined amount of liquid sample can be introduced into the combustion furnace body without remaining in the sample introduction tube, and the cooling mechanism can be used. The sample introduction tube can be cooled efficiently.
- a metal introduction side flange portion is detachably connected to the end portion on the one end opening side, and the metal introduction side flange portion is detachably connected to the end portion on the other end opening side.
- An embodiment in which the lead-out side flange portion is detachably connected can be mentioned.
- the upstream side or the downstream side of the combustion reaction unit is provided with a gas return mechanism for returning the gas flowing out from the combustion reaction unit to the combustion reaction unit.
- a sampling unit for sampling the liquid sample a combustion reaction unit having the combustion reaction unit, a dehumidifying unit having a dehumidifying unit for dehumidifying the gas flowing out from the combustion reaction unit, and a control unit for controlling the total organic carbon meter. It is preferable that the control unit is separated from the control unit. With such a configuration, since each function is unitized and separated, the degree of freedom in arranging each unit can be improved.
- any one of the units has a support having a substantially U-shaped cross section having a pair of side plates and a front plate connecting the pair of side plates.
- a support having a substantially U-shaped cross section having a pair of side plates and a front plate connecting the pair of side plates.
- the total organic carbon meter in the total organic carbon meter according to the present invention, various components such as a plurality of valves and a sample measuring unit are connected by a large number of pipes, for example, when a user assembles each unit, a certain component. May be mistakenly connected to a component other than the component to be connected. Then, problems such as inability to measure correctly occur, and measurement accuracy cannot be guaranteed. Therefore, a diagnostic function for diagnosing the connection point between the sampling unit and the combustion reaction unit is further provided, and the diagnostic function is normal with the actual pressure which is the pressure when gas is poured into the diagnosis area including the connection point. Occasionally, it is preferable to diagnose the connection point by comparing with a reference pressure which is the pressure when gas is poured into the diagnosis area. With such a configuration, it is possible to notify the user that there is a connection failure or incorrect connection at the time of assembly.
- the combustion reaction unit according to the present invention is used in an all-organic carbon meter that measures total organic carbon contained in a liquid sample, and is a combustion reaction that burns all organic carbon contained in the liquid sample to generate carbon dioxide.
- the unit is characterized by having a combustion furnace main body, a vaporizing member housed inside the combustion furnace main body, a heating mechanism for heating the vaporizing member, and a catalyst arranged below the vaporizing member. Is to be. According to the combustion reaction unit configured in this way, the same effect as that of the above-mentioned total organic carbon meter can be obtained.
- the vaporizing member and the catalyst can be arranged close to each other in the configuration in which the sample vaporized by the vaporizing member is passed through the catalyst.
- the total organic carbon total 100 indicates the total amount of organic matter contained in a liquid sample such as tap water or sewage by the amount of carbon contained in the organic matter, and is specifically shown in FIG.
- the apparatus main body 10 the sampling unit 20, the combustion reaction unit 30, the dehumidifying unit 40, and the control unit 50 are provided.
- the apparatus main body 10 includes a housing 11 for accommodating the above-mentioned units 20 to 50, and the units 20 to 50 are attached to the housing 11 by fasteners such as screws, for example. ..
- Each of these units 20 to 50 is removable from the housing 11 so that the user can customize the arrangement of each unit 20 to 50 within a certain degree of freedom.
- FIG. 1 shows an example of the arrangement.
- the control unit 50 is viewed from the front of the middle stage, and the sampling unit 20 is viewed from the front of the middle stage on the right side.
- the combustion reaction unit 30 is arranged on the left side, and the dehumidifying unit 40 is arranged on the lower side.
- the arrangement of each unit is not limited to this.
- each unit 20 to 50 or units 20 to 50 are connected to each other via, for example, electrical wiring or piping through which liquid or gas flows. More specifically, each unit 20 to 50 is connected to the device main body 10 or another unit 20 to 50 with one touch via a connector having a plurality of connection pins, for example, a 20-pin connector. It is configured.
- the sampling unit 20 supplies a sample container 21 for storing a liquid sample, a pretreatment unit having a valve 22 or the like for sending an acid such as hydrochloric acid to the sample container 21, and a carrier gas.
- the carrier gas supply unit 23 is provided, and the liquid sample is acidified and aerated to release the inorganic carbon contained in the liquid sample, and the liquid sample is sent to the combustion reaction unit 30 by the carrier gas. ..
- the sampling unit 20 has a support 24 having a substantially U-shaped cross section having a pair of side plates 241 and a front plate 242 connecting the pair of side plates 241.
- the support 24 is supported by various parts such as a sample container 21, a pump, an on-off valve, and a filter constituting the sampling unit 20.
- the support 24 of the present embodiment is formed by bending one sheet metal, for example, and a replacement part to be removed at the time of maintenance or the like is attached to the front surface 24a of the front plate 242, such as piping and electrical wiring. Regular parts such as connectors are attached to the back surface 24b of the front plate 242.
- the combustion reaction unit 30 includes a sample measuring unit 31 that measures a predetermined amount of the liquid sample sampled by the sampling unit 20 described above, and a combustion reaction in which the measured predetermined amount of the liquid sample is injected. It is provided with a unit 32.
- the sample measuring unit 31 measures a predetermined amount of liquid sample by using, for example, a member having a known volume.
- a measuring container capable of measuring a predetermined amount of liquid sample is used, and a predetermined amount of liquid sample can be stored in this measuring container.
- the predetermined amount of liquid sample measured in this way is burned together with the carrier gas supplied by the carrier gas supply unit 23 described above by switching the three-way valve, which is an on-off valve connected to the downstream side of the sample measurement unit 31. It is injected into the reaction unit 32.
- a buffer tank T in which the carrier gas is stored is provided on the flow path of the carrier gas, and the carrier gas stored in the buffer tank T is poured at once.
- this buffer tank T is not always necessary.
- the weighed predetermined amount of the liquid sample is introduced into the combustion reaction section 32 from the sample introduction tube 311.
- the sample introduction tube 311 is made of highly heat-resistant ceramic.
- the liquid sample adheres to the inner surface and remains, and it may not be possible to inject all the measured predetermined amount of the liquid sample.
- the sample measuring section 31 of the present embodiment is connected to a sample introduction tube 311 made of a resin such as fluororesin, and the sample introduction tube 311 is connected to the sample introduction tube 311 in order to reduce the thermal influence of the combustion reaction section 32.
- a blower fan 312, which is a cooling mechanism for cooling the sample introduction tube 311, is provided.
- the sample introduction tube 311 does not necessarily have to be made of resin, and may be, for example, a tube made of ceramic or metal coated with water repellent.
- a predetermined amount of liquid sample is introduced from the sample introduction tube 311 and all organic carbon contained in this liquid sample is burned to generate carbon dioxide.
- the combustion reaction unit 32 includes a combustion furnace main body 33, a vaporization member 34 housed inside the combustion furnace main body 33, a holding member 35 for holding the vaporization member 34, and vaporization. It is provided with a heating mechanism 36 for heating the member 34.
- the combustion furnace main body 33 has a tubular shape in which a liquid sample is introduced through the opening at one end and carbon dioxide is derived from the opening at the other end.
- the inner furnace body 331 into which the liquid sample is introduced. It has a double pipe structure having an outer furnace body 332 surrounding the inner furnace body 331.
- the inner furnace body 331 is made of ceramics, for example, and is interposed between the outer furnace body 332 and the vaporizing member 34 to prevent cracking due to expansion of the outer furnace body 332.
- the inner peripheral surface 331a and the outer peripheral surface 331b form a straight tubular shape having the same cross-sectional shape from one end opening to the other end opening, and are molded by, for example, drawing. Is.
- the inner furnace body 331 may be one in which a part of the inner peripheral surface 331a or the outer peripheral surface 331b is cut out, and does not necessarily have to be a straight tubular one.
- the outer furnace body 332 is made of, for example, ceramics, and is provided with a gap between the outer peripheral surface 331b of the inner furnace body 331, and here, the central axis of the outer furnace body 332 and the inner furnace body 331. It is arranged so that it is coaxial with the central axis.
- the outer furnace body 332 of the present embodiment has an inner peripheral surface 332a forming a straight tubular shape having the same cross-sectional shape from one end opening to the other end opening, and is molded by, for example, drawing.
- the outer furnace body 332 may have a part of the inner peripheral surface 332a cut out, and may not necessarily have a straight tubular shape.
- a metal introduction side flange portion 37 is detachably connected to the outer furnace body 332 at one end on the opening side, and a metal lead-out side flange 38 is detachably connected to the end on the other end opening side. Can be connected.
- the introduction-side flange portion 37 has, for example, an annular shape, and here, a pair of annular elements 371 and 372 (hereinafter referred to as the first element 371 and the second element 372) facing each other and a bolt or the like for fastening them.
- the first element 371 is made of metal provided at the upper end of the outer furnace body 332 via the seal member S1, and here, the above-mentioned resin sample introduction pipe 311 is fixed. Specifically, the first element 371 is formed with a screw hole H1 communicating with the internal space of the outer furnace body 332, and the above-mentioned sample introduction pipe 311 is held by the bolt member B screwed into the screw hole H1. (See Fig. 4).
- the sample introduction pipe 311 is in a state along the pipe axis of the inner furnace body 331, for example. Will be connected to the introduction side flange portion 37.
- the second element 372 is made of metal whose inner diameter is slightly larger than the outer diameter of the outer furnace body 332 and is fixed to the first element 371 by using the fastener B1. More specifically, a downward step portion D1 is formed on one of the inner peripheral surface of the second element 372 and the outer peripheral surface 332b on the one end opening side of the outer furnace body 332, and the upward step portion D2 is formed on the other side. It is formed, and an upper intermediate member 373 is interposed between the downward step portion D1 and the upward step portion D2.
- the upper intermediate member 373 is composed of, for example, a pair of half-split elements obtained by dividing the annulus plate in half, and its inner diameter is formed on the outer peripheral surface 332b on the one-end opening side of the outer furnace body 332. It is equal to the outer diameter of the downward step portion D1.
- connection method for connecting the introduction side flange portion 37 to the one end opening side of the outer furnace body 332 the following procedure can be mentioned.
- the second element 372 is passed through one end opening side of the outer furnace body 332, and each of the pair of halves is fitted onto the downward step portion D1 formed on the outer peripheral surface of the outer furnace body 332 on the one end opening side to form a circle.
- An annular upper intermediate member 373 is sandwiched between the downward step portion D1 and the upward step portion D2 of the second element 372, and the second element 372 is fixed to the first element 371 by the fastener B1.
- the blower fan 312 which is the cooling mechanism described above, is provided outside the introduction side flange portion 37 configured in this way. Then, the blower fan 312 cools the metal first element 371 and the bolt member B holding the sample introduction pipe 311 to cool the sample introduction pipe 311.
- the lead-out side flange portion 38 has, for example, an annular shape, and here, a pair of annular elements 381 and 382 facing each other (hereinafter referred to as a third element 381 and a fourth element 382) and a bolt or the like for fastening them.
- the third element 381 is made of metal provided at the lower end of the outer furnace body 332 via the seal member S2, and a gas outflow pipe (not shown here) is fixed to the third element 381.
- the third element 381 is formed with a screw hole H2 communicating with the internal space of the outer furnace body 332, and a gas outflow pipe is connected to the screw hole H2 via, for example, a joint or the like.
- the fourth element 382 is made of metal whose inner diameter is slightly larger than the outer diameter of the outer furnace body 332 and is fixed to the third element 381 by using the fastener B2. More specifically, a downward step portion D3 is formed on one of the inner peripheral surface of the fourth element 382 and the outer peripheral surface 332b on the other end opening side of the outer furnace body 332, and the upward step portion D4 is formed on the other side. Is formed, and a lower intermediate member 383 is interposed between the downward step portion D3 and the upward step portion D4.
- the lower intermediate member 383 is composed of, for example, a pair of half-split elements obtained by dividing the annular plate in half, and its inner diameter is formed on the outer peripheral surface 332b on the other end opening side of the outer furnace body 332. It is made equal to the outer diameter of the upward step portion D4.
- connection method for connecting the introduction side flange portion 37 to the other end opening side of the outer furnace body 332 the following procedure can be mentioned.
- the fourth element 382 is passed through the other end opening side of the outer furnace body 332, and each of the pair of half elements is externally fitted to the upward step portion D4 formed on the outer peripheral surface of the outer furnace body 332 on the other end opening side.
- the lower intermediate member 383 is an annular shape.
- the lower intermediate member 383 is sandwiched between the upward step portion D4 and the downward step portion D3 of the fourth element 382, and the fourth element 382 is fixed to the third element 381 by the fastener B2.
- the vaporization member 34 is provided inside the inner furnace body 331 and vaporizes the liquid sample.
- it is, for example, a granular body made of ceramics.
- the combustion reaction unit 32 of the present embodiment further includes a catalyst Z below the vaporization member 34.
- This catalyst Z is a layered material made of a material different from the vaporizing member 34 such as CeO2 (cerium oxide), CuO (copper oxide), Pt (platinum), Pd (palladium), and ZrO 2 (zirconia). Here, it is arranged in contact with the vaporization member 34. By providing such a catalyst, it is possible to improve the combustion efficiency of organic substances in the liquid sample, and it is possible to improve the measurement accuracy.
- another catalyst layer may be provided inside or above the vaporization member 34, or the catalyst may be mixed (added) in the whole or a part of the vaporization member 34.
- the holding member 35 is provided below the vaporization member 34 of the inner furnace body 331, and holds the granules in the axial center portion of the combustion furnace body 33.
- the holding member 35 is made of ceramics having a passage passage for passing a gas generated from a liquid sample, and specific examples thereof include a honeycomb plate having a plurality of passage passages.
- the above-mentioned inner furnace body 331, the vaporization member 34, and the holding member 35 are unitized, and are configured to be collectively detachable from the outer furnace body 332.
- the inner furnace body 331, the vaporization member 34, and the holding member 35 do not necessarily have to be unitized.
- the heating mechanism 36 has a heater that surrounds the central portion in the axial direction of the outer furnace body 332, and heats the vaporization member 34 to, for example, about 1000 ° C.
- the heating temperature may be lowered by using a catalyst.
- the dehumidifying unit 40 vaporizes the acid used for the above-mentioned pretreatment from the dehumidifier 41 in which the gas generated by the above-mentioned combustion reaction unit 30 is guided and the gas after passing through the dehumidifier 41. It is provided with an absorber 42 for removing the corrosive gas.
- the dehumidifying unit 40 has a support 43 having a substantially U-shaped cross section having a pair of side plates 431 and a front plate 432 connecting the pair of side plates 431.
- the support 43 is supported by various parts such as a dehumidifier 41 and an absorber accommodating portion 44 that constitute the dehumidifying unit 40.
- the support 43 of the present embodiment is formed by bending one sheet metal, for example, and replacement parts to be removed at the time of maintenance or the like are attached to the front surface 43a of the front plate 432, such as piping and electrical wiring. Regular parts such as connectors are attached to the back surface 43b of the front plate 432.
- the gas that has passed through the dehumidifying unit 40 passes through the filter and is guided to the carbon dioxide detection unit X.
- the carbon dioxide detector X here is provided with a detector for detecting carbon dioxide contained in the combustion gas by, for example, NDIR (non-dispersion infrared absorption method), and is provided in the vicinity of the control unit 50 here. Has been done.
- NDIR non-dispersion infrared absorption method
- Control unit 50 is physically a dedicated or general-purpose computer equipped with a CPU, a memory, an AD converter, an input / output means, and the like, and functionally operates according to an analysis program stored in a predetermined area of the memory. By doing so, at least the function of calculating the amount and concentration of total organic carbon contained in the liquid sample based on the light intensity signal detected by the above-mentioned detection unit is exhibited.
- the catalyst Z is arranged below the vaporizing member 34, it is not necessary to raise the sample vaporized by the vaporizing member 34 toward the catalyst, and the vaporizing member 34 And the catalyst Z can be arranged close to each other, the combustion efficiency of the organic substance in the liquid sample can be improved, and the measurement accuracy can be improved.
- the catalyst Z is arranged in contact with the vaporization member 34, the catalyst Z and the vaporization member 34 can be arranged without sandwiching an air layer between them, so that the above-mentioned improvement in combustion efficiency and the like can be further improved. It will be effective.
- the heating furnace body has an inner furnace body 331 into which the liquid sample is introduced and an outer furnace body 332 surrounding the inner furnace body 331, the inner furnace body 331 cracks the outer furnace body 332 due to expansion. Etc. can be suppressed.
- the inner peripheral surface 332a of the outer furnace body 332 forms a straight tube having the same cross-sectional shape from the opening at one end to the opening at the other end, the outer furnace body 332 can be easily molded by, for example, drawing. You can also improve your sex.
- the inner furnace body 331, the vaporization member 34, and the holding member 35 are unitized and are configured to be detachably attached to the outer furnace body 332 at once, for example, replacement work of the vaporization member 34 It is possible to improve maintainability such as.
- sample introduction pipe 311 is made of resin, a predetermined amount of liquid sample can be introduced into the combustion furnace main body 33 without remaining in the sample introduction pipe 311, and the sample introduction pipe is provided by the cooling mechanism. Since the 311 is cooled, it is possible to prevent thermal damage to the sample introduction tube 311.
- the sampling unit 20, the combustion reaction unit 30, the dehumidifying unit 40, and the control unit 50 are separated, the degree of freedom in arranging each unit can be improved.
- the present invention is not limited to the above embodiment.
- a gas return mechanism 39 may be provided on the upstream side of the combustion reaction unit 32 to return the gas flowing out from the combustion reaction unit 32 to the combustion reaction unit 32.
- the gas return mechanism 39 may be provided on the downstream side of the combustion reaction unit 32.
- this gas return mechanism 39 As an example of this gas return mechanism 39, as shown in FIG. 8, the gas vaporized in the combustion reaction unit 32 is made to flow back into the sample introduction pipe 311 and then returned to the combustion reaction unit 32 via the sample introduction pipe 311 again. Aspects are mentioned. As a specific configuration in this case, a configuration including a backflow flow path 39L communicating with the sample introduction pipe 311 and a pump P provided in the backflow flow path 39L can be mentioned.
- the gas return mechanism 39 there is an embodiment in which the gas derived from the combustion reaction unit 32 is returned to the combustion reaction unit 32 again without flowing to the dehumidification unit 40.
- a configuration including a circulation flow path and a switching valve for selectively flowing the gas to either the circulation flow path or the dehumidification unit 40 can be mentioned.
- the combustion reaction unit 32 may be provided with a position adjusting mechanism for adjusting the position of the sample introduction pipe 311 with respect to the heating furnace main body.
- a position adjusting mechanism for example, a mechanism using a moving stage or the like can be mentioned, and the sample introduction pipe 311 is provided so that the pipe axis of the sample introduction pipe 311 is located on the central axis of the inner furnace body 331. It can be mentioned that the position is adjustable.
- combustion reaction unit 30 may be provided, for example, with a mounting table provided at the lower part of the heating furnace body and on which the used vaporizing member 34 can be temporarily placed when the vaporizing member 34 is replaced.
- the supports 24 and 43 constituting the sampling unit 20 and the dehumidifying unit 40 have been described as having a substantially U-shaped cross section, but the shapes of the supports 24 and 43 are not limited to this, and for example, the cross section is roughly outlined. It may be L-shaped.
- the vaporization member 34 of the above embodiment has been described as a granular body made of ceramics, the shape and material of the vaporization member 34 may be appropriately changed, for example, a flat plate-shaped vaporization member made of ceramics may be used.
- one end is connected to the sample container 21 and the other end is the sample measuring unit 31 as shown in FIG.
- the liquid sample line L1 connected to the liquid sample line L1, the pump P such as a tubing pump provided in the liquid sample line L1, the three-way valve V0 provided in the liquid sample line L1, and the liquid sample line via the three-way valve V0.
- An embodiment provided with an introduction line L2 connected to L1 and guiding the weighed liquid sample to the combustion reaction unit 32 can be mentioned.
- the liquid sample stored in the sample container 21 is pressurized by the pump P and sent to the sample measuring unit 31, so that the liquid sample is located in the pipe T from the three-way valve V0 to the sample measuring unit 31 in the liquid sample line L1. A fixed amount of liquid sample remains. Then, by switching the three-way valve V0, this predetermined amount of liquid sample can be guided to the combustion reaction unit 32 via the introduction line L2.
- the liquid sample may or may not be filled up to the tip of the pipe T connected to the sample measuring unit 31 due to the pulsation of the pump P, so that the amount of liquid filled in the pipe T, that is, The amount of liquid after weighing varies.
- droplets may adhere to the tip of the pipe T, and the liquid amount further varies due to the droplets.
- the total organic carbon meter 100 may be configured to feed the liquid sample to the sample measuring unit 31 by the carrier gas.
- the branch line L4 branched from the carrier gas line L3 that supplies the carrier gas to the sample measuring unit 31 and connected to the sample container 21 and the liquid sample line L1 described above are connected by the connection line L5. It is connected.
- the branch line L4 is a line for removing inorganic carbon from the liquid sample stored in the sample container 21 by sending the carrier gas to the sample container 21.
- one end of the connection line L5 does not necessarily have to be connected to the branch line L4, and may be connected to the carrier gas line L3.
- connection line L5 and the branch line L4 are connected via the first three-way valve V1
- connection line L5 and the liquid sample line L1 are connected via the second three-way valve V2.
- An on-off valve V3 such as a solenoid valve is provided on the upstream side or the downstream side of the second three-way valve V2 in the liquid sample line L1.
- the liquid sample stored in the sample container 21 is sent to the sample measuring unit 31 by the pump P.
- the pump P is stopped and the first three-way valve V1 and the second three-way valve V2 are switched to send the carrier gas to the liquid sample line L1 via the connection line L5.
- the on-off valve V3 is in the open state.
- the liquid sample is pushed out to the sample measuring unit 31 by the carrier gas flowing through the liquid sample line L1.
- the carrier gas is poured into the sample measuring unit 31 via the carrier gas line L3 to pressurize the inside of the sample measuring unit 31.
- the liquid sample is pushed out to the sample measuring unit 31 by the carrier gas, and since there is no pulsation in the flow velocity of the carrier gas, the liquid sample can be sent to the sample measuring unit 31 at a constant speed. .. Further, since the on-off valve V3 is closed while the liquid sample is being pushed out to the sample measuring unit 31, it is possible to prevent droplets from remaining at the tip of the pipe T described above. As a result, a predetermined amount of liquid sample can be left in the pipe T with good reproducibility, and the liquid sample can be accurately weighed.
- the total organic carbon total 100 according to the present invention may be configured so that the connection of each unit 20 to 50 can be confirmed after assembling each unit 20 to 50, and here, particularly the sampling unit 20 and combustion.
- the configuration is such that the correctness of the connection with the reaction unit 30 can be confirmed.
- gas is poured into a diagnostic area including one or a plurality of connection points (specifically, piping members) connecting the sampling unit 20 and the combustion reaction unit 30, and the diagnostic area is closed. Then, a method of measuring the pressure in the diagnostic area can be mentioned.
- the pressure sensor mounted on the detection unit X may be used for pressure measurement, or a pressure sensor for pressure measurement in the diagnostic area may be separately provided.
- the connection point connecting the sampling unit 20 and the combustion reaction unit 30 is a pipe connecting the component of the sampling unit 20 and the component of the combustion reaction unit 30.
- the combustion reaction unit Examples thereof include a pipe connecting the 32 and the three-way valve V0, a pipe connecting the second three-way valve V2 and the on-off valve V3, and a pipe connected to the sample measuring unit 31 and introducing a liquid sample or a carrier gas.
- the actual pressure which is the pressure in the diagnosis area at the time of diagnosis
- the reference pressure which is the pressure of the air rear to be diagnosed acquired in advance in the normal state
- the difference or ratio between the reference pressure and the measured pressure is a predetermined threshold value. If it exceeds, it is determined that there is a defect or error in the piping connection included in the diagnosis area. It should be noted that this determination may be performed by an operator, or for example, the control unit 50 or the like may be provided with this diagnostic function to enable automatic diagnosis.
- the diagnosis area can be changed by switching the opening and closing of various valves V0 to V3, and by advancing the above-mentioned diagnosis for each diagnosis area, it is possible to narrow down defects and incorrect connection points. ..
- the valve for switching the opening and closing is not limited to the valves V0 to V3 shown in FIG. 10, and valves provided at various locations (not shown) may be switched.
- the vaporizing member and the catalyst can be arranged close to each other in a configuration in which a sample vaporized by the vaporizing member is passed through the catalyst.
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Abstract
Description
これならば、触媒と気化部材とをこれらの間に空気層を挟まず配置することができるので、上述した燃焼効率の向上等がより効果的なものとなる。
このように構成であれば、加熱炉本体が、液体試料が導入される内側炉体と、内側炉体を取り囲む外側炉体とを有しているので、内側炉体によって外側炉体の膨張による割れ等を抑制することができる。
そこで、前記外側炉体は、一端開口から他端開口に至るまで内側周面が同断面形状の直管状をなすものであることを特徴とする。
このような構成であれば、セラミックス製の粒状体を保持部材によりヒータ近傍に保持することができる。
このような構成であれば、交換作業等のメンテナンス性の向上を図れる。
このような構成であれば、試料導入管として樹脂製のものを用いているので、所定量の液体試料を試料導入管に残存させることなく燃焼炉本体に導入させることができ、しかも冷却機構によって試料導入管を効率良く冷却することができる。
このような構成であれば、燃焼反応部における燃焼効率の向上を図れる。
このような構成であれば、各機能をユニット化して分離させているので、各ユニットの配置の自由度を向上させることができる。
そこで、前記サンプリングユニットと前記燃焼反応ユニットとの接続箇所の診断する診断機能をさらに備え、前記診断機能が、前記接続箇所を含む診断エリアにガスを流し込んだ際の圧力である実圧力と、正常時に当該診断エリアにガスを流し込んだ際の圧力である基準圧力とを比較して、前記接続箇所を診断することが好ましい。
このような構成であれば、組立時の接続の不具合や誤った接続があることをユーザに知らせることができる。
このように構成された燃焼反応ユニットによれば、上述した全有機炭素計と同様の作用効果を奏し得る。
10 ・・・装置本体
20 ・・・サンプリングユニット
30 ・・・燃焼反応ユニット
40 ・・・除湿ユニット
50 ・・・制御ユニット
31 ・・・試料計量部
311・・・試料導入管
312・・・送風ファン
32 ・・・燃焼反応部
33 ・・・燃焼炉本体
331・・・内側炉体
332・・・外側炉体
34 ・・・気化部材
35 ・・・保持部材
装置本体10は、図1に示すように、上述した各ユニット20~50を収容する筺体11を備えており、この筺体11に各ユニット20~50が例えばネジ等の締結具により取り付けられている。なお、これらの各ユニット20~50は、筺体11に対して着脱可能であり、ユーザが各ユニット20~50の配置をある程度の自由度の範囲内でカスタマイズできるようにしてある。図1にはその配置の一例を示してあり、上中下段に区切られた筺体11のうち、上段に制御ユニット50が、中段の前方から視て右側にサンプリングユニット20が、中段の前方から視て左側に燃焼反応ユニット30が、下段に除湿ユニット40が配置されている。ただし、各ユニットの配置はこれに限られるものではない。
サンプリングユニット20は、図2に示すように、液体試料が貯留される試料容器21と、この試料容器21に塩酸等の酸を送り込むためのバルブ22等を有する前処理部と、キャリアガスを供給するキャリアガス供給部23とを備え、液体試料を酸性にして通気処理を行うことにより、液体試料に含まれる無機炭素を遊離し、その液体試料をキャリアガスによって燃焼反応ユニット30に送り込むものである。
燃焼反応ユニット30は、図2に示すように、上述したサンプリングユニット20によりサンプリングされた液体試料の所定量を計量する試料計量部31と、計量された所定量の液体試料が注入される燃焼反応部32とを備えるものである。
なお、試料導入管311としては、必ずしも樹脂製のものを用いる必要はなく、例えばセラミックや金属からなるチューブの内周面に撥水コートするなどしたものであっても良い。
ただし、内側炉体331、気化部材34、及び保持部材35は、必ずしもユニット化されている必要はない。
除湿ユニット40は、図2に示すように、上述した燃焼反応ユニット30により発生した気体が導かれる除湿器41と、除湿器41を通過した後の気体から上述した前処理に用いた酸が気化した腐食性ガスを除去するアブソーバ42とを備えている。
制御ユニット50は、物理的には、CPU、メモリ、ADコンバータ、入出力手段等を備えた専用乃至汎用のコンピュータであり、機能的には、前記メモリの所定領域に格納された分析プログラムに従って動作することにより、上述した検出ユニットにより検出された光強度信号に基づいて、液体試料に含まれる全有機炭素の量や濃度を演算する機能を少なくとも発揮するものである。
しかも、外側炉体332が一端開口から他端開口に至るまで内側周面332aが同断面形状の直管状をなすので、外側炉体332を例えば引き抜き加工等により簡単に成型することができ、加工性の向上をも図れる。
具体的に位置調整機構としては、例えば移動ステージなどを利用したものを挙げることができ、内側炉体331の中心軸上に試料導入管311の管軸が位置するように、試料導入管311の位置を調整可能に構成されたもの挙げることができる。
より具体的に説明すると、試料計量部31にキャリアガスを供給するキャリアガスラインL3から分岐して試料容器21に接続された分岐ラインL4と、上述した液体試料ラインL1とが、接続ラインL5により接続されている。なお、この分岐ラインL4は、キャリアガスを試料容器21に送り込むことで、試料容器21に貯留された液体試料から無機炭素を抜くためのラインである。また、接続ラインL5の一端は、必ずしも分岐ラインL4に接続されている必要はなく、キャリアガスラインL3に接続されていても良い。
そして、液体試料ラインL1における第2の三方弁V2の上流側又は下流側には電磁弁等の開閉弁V3が設けられている。
また、液体試料を試料計量部31に押し出している最中に開閉弁V3を閉じるので、上述した配管Tの先端に液滴が残ることも防ぐことができる。
その結果、この配管Tに再現性良く所定量の液体試料を残存させることができ、液体試料を精度良く計量することが可能となる。
Claims (15)
- 液体試料に含まれる全有機炭素を測定する全有機炭素計であって、
前記液体試料に含まれる全有機炭素を燃焼させて二酸化炭素を発生させる燃焼反応部と、
前記燃焼反応部により発生した二酸化炭素を検出する二酸化炭素検出部とを有し、
前記燃焼反応部は、
燃焼炉本体と、
前記燃焼炉本体の内部に収容された気化部材と、
前記気化部材を加熱する加熱機構と、
前記気化部材の下方に配置された触媒とを有する、全有機炭素計。 - 前記触媒が、前記燃焼炉本体の内部において前記気化部材と接触している、請求項1記載の有機炭素計。
- 前記気化部材と前記触媒とは、互いに異なる材質からなる、請求項1又は2記載の有機炭素計。
- 前記燃焼炉本体は、
前記液体試料が導入される内側炉体と、
前記内側炉体を取り囲む外側炉体とを有する、請求項1乃至3のうち何れか一項に記載の全有機炭素計。 - 前記外側炉体は、一端開口から他端開口に至るまで内側周面が同断面形状の直管状をなすものである、請求項4に記載の全有機炭素計。
- 前記気化部材は、セラミックス製の粒状体であり、
前記加熱機構は、前記外側炉体の軸方向中央部を取り囲むヒータを有し、
前記内側炉体の内部には、前記粒状体を前記燃焼炉本体の軸方向中央部に保持する保持部材が設けられている、請求項4又は5に記載の全有機炭素計。 - 前記保持部材は、前記液体試料から発生する気体を通過させる通過流路を有している、請求項6に記載の全有機炭素計。
- 前記内側炉体と、前記気化部材と、前記保持部材とがユニット化されており、前記外側炉体に対して一括して着脱可能に構成されている、請求項7に記載の全有機炭素計。
- 前記外側炉体は、前記一端開口側の端部に金属製の導入側フランジ部が接続されており、
前記導入側フランジ部には、前記液体試料を前記燃焼炉本体内に導入する樹脂製の試料導入管が接続されており、
前記導入側フランジ部の外部には、前記導入側フランジ部を冷却することにより前記試料導入管を冷却する冷却機構が設けられている、請求項5乃至8の何れか一項に記載の全有機炭素計。 - 前記外側炉体は、前記一端開口側の端部に金属製の導入側フランジ部が着脱可能に接続されており、前記他端開口側の端部に金属製の導出側フランジ部が着脱可能に接続されている、請求項5乃至8の何れか一項に記載の全有機炭素計。
- 前記燃焼反応部の下流側には、前記燃焼反応部から流出するガスを前記燃焼反応部に戻すガス戻し機構が設けられている、請求項1乃至10の何れか一項に記載の全有機炭素計。
- 前記液体試料をサンプリングするサンプリングユニットと、
前記燃焼反応部を有する燃焼反応ユニットと、
前記燃焼反応部から流出するガスを除湿する除湿部を有する除湿ユニットと、
前記全有機炭素計を制御する制御部を有する制御ユニットとに分離されている、請求項1乃至11の何れか一項に記載の全有機炭素計。 - 前記ユニットの何れか1つは、一対の側板及びそれら一対の側板を繋げる前板を有する断面概略コの字状の支持体を有し、当該支持体に前記ユニットを構成する部品が支持されている、請求項12に記載の全有機炭素計。
- 前記サンプリングユニットと前記燃焼反応ユニットとの接続箇所の診断する診断機能をさらに備え、
前記診断機能が、前記接続箇所を含む診断エリアにガスを流し込んだ際の圧力である実圧力と、正常時に当該診断エリアにガスを流し込んだ際の圧力である基準圧力とを比較して、前記接続箇所を診断する、請求項12又は13に記載の全有機炭素計。 - 液体試料に含まれる全有機炭素を測定する全有機炭素計に用いられ、前記液体試料に含まれる全有機炭素を燃焼させて二酸化炭素を発生させる燃焼反応ユニットであって、
燃焼炉本体と、
前記燃焼炉本体の内部に収容された気化部材と、
前記気化部材を加熱する加熱機構と、
前記気化部材の下方に配置された触媒とを有する、燃焼反応ユニット。
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CN116420073A (zh) | 2023-07-11 |
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