WO2023112679A1 - 元素分析方法及び元素分析装置 - Google Patents
元素分析方法及び元素分析装置 Download PDFInfo
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- WO2023112679A1 WO2023112679A1 PCT/JP2022/044172 JP2022044172W WO2023112679A1 WO 2023112679 A1 WO2023112679 A1 WO 2023112679A1 JP 2022044172 W JP2022044172 W JP 2022044172W WO 2023112679 A1 WO2023112679 A1 WO 2023112679A1
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- Prior art keywords
- gas
- heating furnace
- sample
- heating
- elemental analysis
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- 238000000921 elemental analysis Methods 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000007789 gas Substances 0.000 claims abstract description 116
- 238000010438 heat treatment Methods 0.000 claims abstract description 110
- 239000011261 inert gas Substances 0.000 claims abstract description 55
- 239000012159 carrier gas Substances 0.000 claims abstract description 51
- DHNCFAWJNPJGHS-UHFFFAOYSA-J [C+4].[O-]C([O-])=O.[O-]C([O-])=O Chemical compound [C+4].[O-]C([O-])=O.[O-]C([O-])=O DHNCFAWJNPJGHS-UHFFFAOYSA-J 0.000 claims abstract description 19
- 238000004458 analytical method Methods 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 63
- 229910052799 carbon Inorganic materials 0.000 description 63
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 238000002485 combustion reaction Methods 0.000 description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- OUYCCCASQSFEME-QMMMGPOBSA-N L-tyrosine Chemical compound OC(=O)[C@@H](N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-QMMMGPOBSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- IUHFWCGCSVTMPG-UHFFFAOYSA-N [C].[C] Chemical compound [C].[C] IUHFWCGCSVTMPG-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000012024 dehydrating agents Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- -1 ferrous metals Chemical class 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 239000012494 Quartz wool Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001745 non-dispersive infrared spectroscopy Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing 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
-
- 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
Definitions
- the present invention relates to an elemental analysis method and an elemental analysis apparatus for analyzing elements such as carbon (C) and sulfur (S) contained in samples such as steel, non-ferrous metals and ceramics.
- this type of elemental analysis apparatus introduces a container (boat) containing a sample into a heating furnace, and analyzes the gas to be analyzed generated from the sample heated and burned in the heating furnace.
- This elemental analyzer is configured to supply a combustion-supporting gas such as oxygen gas into the heating furnace to accelerate the combustion of the sample.
- the present invention has been made in view of the above problems, and the main problem is to separate and detect the organic carbon component and the inorganic carbon component contained in the sample.
- the elemental analysis method according to the present invention is a method of elemental analysis in which a sample containing at least a carbonate carbon component is heated in a heating furnace, and an analysis target gas generated from the heated sample is analyzed with a gas analyzer, After starting to heat the sample in a state in which an inert gas is supplied as a carrier gas into the heating furnace, the carrier gas supplied into the heating furnace is switched from the inert gas to the combustion-supporting gas. do.
- the heating of the sample is started while an inert gas is supplied as a carrier gas into the heating furnace, so the sample burns and CO 2 derived from the inorganic carbon component is produced. Instead, only volatile organic carbon components are generated, which can be detected by gas analyzers. Thereafter, by switching the carrier gas supplied to the heating furnace to a combustion-supporting gas and starting the combustion of the sample, CO 2 derived from the inorganic carbon component is generated and can be detected by an analyzer. By switching the carrier gas supplied into the heating furnace from the non-volatile gas to the combustion-supporting gas while the sample is being heated, the organic carbon component and the inorganic carbon component are separated and removed from the sample. can be analyzed quantitatively.
- organic carbon component means carbon contained in organic substances such as hydrocarbons.
- inorganic carbon component means elemental carbon and crystalline carbon, and does not include carbonate carbon such as calcium carbonate.
- inert gas means a gas having an inert gas component concentration of 99% or more, and the term “combustion-supporting gas” means that the oxygen concentration in the gas is It means a gas whose concentration is equal to or higher than that of oxygen.
- the heating furnace it is preferable to raise the temperature of the heating furnace while supplying an inert gas as a carrier gas into the heating furnace.
- an inert gas as a carrier gas into the heating furnace.
- the signal strength of the gas to be analyzed detected by the analyzer rises and reaches an initial peak value, and then the heating of the heating furnace is started. is preferred.
- the temperature of the heating furnace is raised after the analyzer detects the organic carbon component, so if the sample contains a carbonate carbon component, the organic carbon component and the carbonate carbon component can be separated. can be detected by
- the carrier gas supplied to the heating furnace is preferably switched from an inert gas to a combustion-supporting gas. In this way, the carbonate carbon component and the inorganic carbon component contained in the sample can be more reliably separated and detected.
- a front chamber communicating with the heating furnace is provided in the front stage of the heating furnace, the sample is placed in the front chamber, and after the front chamber is filled with an inert gas, the It is preferable to start heating the sample by putting the sample into the heating furnace from the front chamber. In this way, carbon dioxide in the atmosphere can be prevented from entering the heating furnace when the sample is put into the heating furnace, so that the organic carbon component can be analyzed with high accuracy.
- the elemental analysis method of the present invention is a method of elemental analysis in which a sample is heated in a heating furnace and a gas to be analyzed generated from the heated sample is analyzed by a gas analyzer, and an undesired carrier gas is present in the heating furnace.
- the heating of the sample is started while the active gas is being supplied, the temperature of the heating furnace is raised in this state, and then the carrier gas supplied into the heating furnace is switched from the inert gas to the combustion-supporting gas. You may do so. Even with such an elemental analysis method, the same effects as those of the above-described elemental analysis method can be obtained.
- the elemental analysis apparatus of the present invention comprises a heating furnace for heating a sample, and an analyzer for analyzing an analysis target gas generated from the sample heated and burned in the heating furnace, wherein The heating of the sample is started in a state in which an inert gas is supplied as a carrier gas, and after the temperature of the heating furnace is raised in this state, the carrier gas to be supplied is switched from the inert gas to a combustion-supporting gas. It is characterized by: With such an elemental analysis apparatus, the same effects as those of the above-described elemental analysis method can be achieved.
- the organic carbon component and the inorganic carbon component contained in the sample can be separated and detected.
- FIG. 4 is a diagram showing an example of temporal changes in the type of carrier gas to be supplied, the temperature of the heating furnace, and the signal intensity of the gas analyzer in the elemental analysis method of the embodiment.
- the flow chart of the elemental-analysis apparatus used by the experiment example. 4 is a graph showing changes over time in signal intensity detected by a gas analyzer in an experimental example; A table showing the results of quantification of each carbon component in an experimental example.
- the elemental analysis apparatus 100 of the present embodiment heats and burns a powdery or bulk solid sample S, and extracts carbon (C), sulfur (S), etc. contained in the sample S from the gas generated thereby.
- samples include those containing inorganic materials such as steel and non-ferrous metals, those containing organic materials such as coal, and those containing both inorganic and organic materials.
- this elemental analysis apparatus 100 includes a heating furnace 1 in which a container V containing a sample S is arranged, and a gas (analysis gas) generated from the sample S heated and burned in the heating furnace 1
- a gas analyzer 2 for analyzing a target gas) and a carrier gas supply mechanism 3 for supplying a carrier gas into the heating furnace 1 are provided.
- the container V accommodates, for example, a powdery sample S inside.
- the container V of this embodiment has an elongated shape with an opening at the top, and is specifically a porcelain combustion boat, a ceramic board, a quartz board, or the like.
- the shape of the container V is not limited to this, and various shapes can be used.
- the heating furnace 1 is a tubular furnace having therein a heating space 1 s into which the container V is taken in and out. By heating the container V, the sample S is heated and gas is generated.
- the heating furnace 1 as shown in FIG. , and a power supply circuit (not shown) that supplies electric power to the electric resistor 12 to generate heat.
- the heating furnace 1 is configured such that the temperature of the furnace body 11 (furnace temperature) can be arbitrarily set, and the current value of the furnace temperature can be measured by a temperature sensor such as a thermocouple.
- the furnace main body 11 is a tubular (straight) ceramic molded body, and has an opening (sample inlet/outlet) 1p for inserting a container V into the heating space 1s at one end along the tube axis direction. is formed. At the other end of the furnace body 11, a gas outlet 1q is formed for leading the gas generated from the sample S to the gas analyzer 2. As shown in FIG.
- the furnace body 11 may be heated by passing an electric current through an electric resistance furnace to perform resistance heating (Joule heating).
- the furnace body 11 is made of a conductive metal.
- a method of induction-heating the container V or the sample S accommodated in the furnace main body 11 may be used.
- An open/close lid 13 is provided at the opening 1p of the furnace body 11.
- the open/close lid 13 moves between a closed position for closing the opening 1p and an open position for opening the opening 1p, and is driven by an actuator such as an air cylinder.
- a front chamber 4 s is provided in the front stage of the heating furnace 1 to accommodate the container V before being put into the heating furnace 1 .
- the front chamber 4 s is formed by the inner space of the box-shaped housing 4 and is configured to communicate with the opening 1 p of the heating furnace 1 through the opening/closing lid 13 .
- An inert gas filling channel L5 through which an inert gas such as nitrogen gas flows and an exhaust channel (not shown) are connected to the front chamber 4s, so that the air in the front chamber 4s can be replaced with the inert gas. It's like
- the gas analyzer 2 analyzes the gas generated in the heating furnace 1 and obtains the content of each component contained in the sample S.
- analysis is performed using a non-dispersive infrared absorption method (NDIR method).
- this gas analyzer 2 has a non-dispersive infrared detector (not shown), and detects CO 2 , CO, SO 2 and the like contained in the gas led out from the gas outlet 1q of the heating furnace 1. By doing so, the contents of carbon (C), sulfur (S), etc. contained in the sample S are obtained.
- NDIR method non-dispersive infrared absorption method
- the gas analyzer 2 is provided on a gas lead-out passage L1 connected to the gas outlet 1q of the heating furnace 1, and a dust filter 5 and a A dehydrating agent 6 and the like are provided.
- the carrier gas supply mechanism 3 supplies different types of carrier gas (specifically, a combustion-supporting gas and an inert gas) into the heating furnace 1 in a switchable manner.
- the carrier gas supply mechanism 3 includes a combustion-supporting gas supply source 31, an inert gas supply source 32, a carrier gas supply passage L2 for supplying the carrier gas into the heating furnace 1, and a combustion-supporting gas a combustion-supporting gas introduction passage L3 connecting the supply source 31 and the carrier gas supply passage L2, an inert gas introduction passage L4 connecting the inert gas supply source 32 and the carrier gas supply passage L2;
- a switching mechanism 33 is provided for switching the connection destination of the carrier gas supply flow path L2 between the combustion-supporting gas introduction flow path L3 and the inert gas introduction flow path L4.
- the combustion-supporting gas supply source 31 is for sending the combustion-supporting gas to the combustion-supporting gas introduction path L3. It includes a regulator and the like. This combustion-supporting gas promotes the combustion of the sample in the heating furnace 1, and is specifically O 2 (oxygen) gas.
- the inert gas supply source 32 is for feeding the inert gas to the inert gas introduction path L4, and specifically includes a gas cylinder filled with the inert gas, a regulator attached to the gas cylinder, and the like. It is a thing. Specifically, this inert gas is N 2 (nitrogen) gas, Ar (argon gas) gas, He (helium) gas, or the like.
- the carrier gas supply flow path L2 has a starting end connected to the combustion-supporting gas introduction flow path L3 and the inert gas introduction flow path L4, a terminal end connected to the furnace main body 11 of the heating furnace 1, and communicated with the heating space 1s. ing.
- the switching mechanism 33 is provided at a connection point between the carrier gas supply channel L2 and the combustion-supporting gas introduction channel L3 and the inert gas introduction channel L4.
- the switching mechanism 33 is a three-way valve or the like that selectively opens and closes the combustion-supporting gas introduction passage L3 and the inert gas introduction passage L4.
- the sample S accommodated in the container V is placed in the front chamber 4s, and an inert gas (such as N 2 gas) is introduced into the front chamber 4s from the inert gas filling channel L5. is supplied to replace the air in the front chamber 4s with an inert gas (step S1).
- an inert gas such as N 2 gas
- the opening/closing lid 13 is in the closed position.
- the heating furnace 1 is operated using the operation panel or the like to set the set temperature of the furnace main body 11 to a predetermined first set temperature, thereby heating the inside of the furnace main body 11 (step S2).
- the first set temperature is preferably 100° C. or higher and 700° C. or lower, more preferably 200° C. or higher and 500° C. or lower.
- an inert gas eg, N2 gas
- the supply flow rate of the inert gas from the carrier gas supply flow path L2 is, for example, 1 L/min or more and 5 L/min or less, but is not limited thereto.
- the order of steps S1 to S3 may be changed.
- the opening/closing lid 13 is moved to the open position to open the furnace, as shown in FIG. 3(c).
- the sample entrance 1p of the main body 11 is opened, and a metal rod or the like is used to push out the container V containing the sample S from the front chamber 4s into the heating space 1s (step S4).
- a metal rod or the like is used to push out the container V containing the sample S from the front chamber 4s into the heating space 1s (step S4).
- the opening/closing lid 13 is moved to the closed position to close the sample inlet/outlet 1p of the furnace body 11 as shown in FIG. 3(d).
- the organic carbon component volatilizes from the heated sample S, and an intensity signal derived from the organic carbon component is detected in the gas analyzer 2 as shown in FIG.
- the sample inlet/outlet 1p is closed, until the peak value of the intensity signal derived from the organic carbon component (the “initial peak value” in the claims) is detected in the gas analyzer 2, preferably the organic It is preferable to keep the set temperature of the furnace body 11 constant until the peak value of the intensity signal derived from the carbon component is no longer detected.
- the carrier gas supplied to the furnace body 11 only the inert gas continues to flow without flowing the combustion-supporting gas.
- the heating furnace 1 is operated using the operation panel or the like to change the set temperature of the furnace main body 11 to a second set temperature higher than the first set temperature, thereby increasing the temperature inside the furnace main body 11 (step S5).
- the change from the first set temperature to the second set temperature is preferably performed at least after the gas analyzer 2 detects the peak value of the signal intensity derived from the organic carbon component, and the gas analyzer 2 detects the organic carbon component. More preferably after no signal strength is detected.
- the second set temperature may be a temperature at which the inorganic carbon component contained in the sample is combusted, and is preferably 800° C. or higher and 1500° C. or lower, more preferably 1000° C. or higher and 1200° C. or lower.
- the carbon salt carbon component contained in the sample can be extracted separately from the organic carbon component and the inorganic carbon component.
- the heating rate is not particularly limited, it is preferably 0.1° C./second or more and 1° C./second or less, and the lower the temperature rising rate, the better, in order to easily resolve the peak of the signal intensity.
- the carbonate carbon component contained in the sample S is thermally decomposed to generate CO 2 .
- the gas analyzer 2 detects an intensity signal derived from the carbonate carbon component.
- the carrier gas is supplied into the furnace main body 11 at least until the peak value of the intensity signal derived from the carbonate carbon component is no longer detected in the gas analyzer 2 after at least the temperature rise of the furnace main body 11 is started. , only the inert gas continues to flow without flowing the combustion-supporting gas.
- step S6 This carrier gas switching is preferably performed at least after the gas analyzer 2 no longer detects the signal intensity derived from the carbon salt carbon component, and more preferably after the temperature in the furnace body 11 reaches 1000° C. or higher.
- the carrier gas is switched to the combustion-supporting gas, the sample S is soon combusted to generate CO 2 , and an intensity signal derived from the inorganic carbon component is detected in the gas analyzer 2 as shown in FIG. 4 .
- the set temperature of the furnace body 11 may be maintained at the second set temperature, or may be raised.
- the supply flow rate of the combustion-supporting gas from the carrier gas supply flow path L2 may be the same as or different from the supply amount of the inert gas in the previous step.
- the supply flow rate of the combustion-supporting gas is, for example, 1 L/min or more and 5 L/min or less, but is not limited thereto.
- the heating of the sample S is started while the inert gas is being supplied as the carrier gas into the heating furnace 11. is combusted to generate only volatile organic carbon components without generating CO 2 derived from inorganic carbon components, which can be detected by the gas analyzer 2 . Then, after the signal intensity of the gas to be analyzed detected by the gas analyzer 2 rises and reaches the first peak value (that is, after the organic carbon component is detected by the gas analyzer 2), Since the temperature of the heating furnace 1 is raised while the inert gas is flowing, the carbonate carbon component contained in the sample S can be detected separately from the organic carbon component and the inorganic carbon component.
- the carrier gas supplied to the heating furnace 1 is switched to a combustion-supporting gas to start the combustion of the sample S, thereby generating CO 2 derived from the inorganic carbon component, which is detected by the gas analyzer 2. can be done.
- the organic carbon component, the carbonate carbon component, and the inorganic carbon component can be separated from the sample S, detected by the gas analyzer 2, and quantitatively analyzed.
- the present invention is not limited to the above embodiments.
- the elemental analysis apparatus 100 of the above-described embodiment is provided with the front chamber 4 in the front stage of the heating furnace 1, but the present invention is not limited to this.
- the front chamber 4 may not be provided, and the sample S stored in the container V may be put into the furnace main body 11 from the state of being placed in an air atmosphere. .
- the inert gas supplied to the furnace body 11 as a carrier gas may have a concentration of inert gas components of 99% or more, and is not limited to a single component gas such as N 2 gas, but a plurality of inert gas components. (O 2 etc.) may be mixed. In this case, if the O 2 concentration contained is high, the sample will not be steamed and will be oxidized, so the O 2 concentration is preferably 100 ppm or less.
- the combustion-supporting gas supplied to the furnace body 11 as a carrier gas may have an O 2 concentration equal to or higher than the O 2 concentration in the air.
- a gas in which a plurality of components (for example, CO 2 etc.) are mixed may be used instead of a single component gas.
- the CO 2 concentration in the combustion-supporting gas is low, and specifically, the CO 2 concentration is preferably 100 ppm or less.
- the combustion-supporting gas may contain an inert gas component.
- the temperature is raised while supplying the inert gas as the carrier gas, but the present invention is not limited to this.
- the carrier gas to be supplied is switched from an inert gas to a combustion-supporting gas, and then the temperature is raised. good too. Also in this way, the organic carbon component and the carbonate carbon component can be separated and detected.
- the organic carbon component is detected separately from the carbonate carbon component and the inorganic carbon component by lowering the first set temperature, but the present invention is not limited to this.
- at least the organic carbon component and the inorganic carbon component can be separated and detected by the gas analyzer 2. For example, by increasing the first set temperature, the organic carbon component and the carbonate carbon component overlap. It is also possible to detect only the inorganic carbon component alone by detecting it with the gas analyzer 2 .
- FIG. 6 shows a flow diagram of the elemental analyzer used in this experimental example.
- the carrier gas supply mechanism was configured to manually switch between nitrogen gas (inert gas) and oxygen gas (combustion-supporting gas) by means of a three-way valve.
- the front chamber in the front stage of the heating furnace was filled with nitrogen gas to prevent contact between the sample and the atmosphere during measurement standby.
- a quartz tube was used for the furnace body of the heating furnace, and the temperature inside the furnace could be set up to 1000°C.
- a converter was installed in the rear stage of the heating furnace to promote oxidation of the generated gas. Copper oxide (600° C.) was used as the converter.
- a dust filter (quartz wool) and a dehydrating agent (potassium hydroxide) were installed in the rear stage of the heating furnace to remove dust and water generated during combustion.
- a non-dispersive infrared detector is used as the detector, and it is constructed so that only the gas to be analyzed can be selectively detected by an optical filter.
- sample and measurement A simulated sample (total 12.5 mg) prepared by mixing tyrosine (2.4 mg) and calcium carbonate (10.1 mg) was weighed in a quartz boat, and after weighing, the quartz boat was placed in the front chamber. Then, using an insertion rod, the quartz boat was inserted into a heating furnace set at 400°C. Here, the organic matter is thermally decomposed at around 400° C. to generate CHx, CO, etc., but is converted to CO 2 by the subsequent converter. After inserting the sample, the furnace temperature was raised to 1000° C. at a rate of about 0.5° C./second, and after reaching 1000° C., the carrier gas to be supplied was switched from nitrogen to oxygen and held for 100 seconds.
- FIG. 7 shows the results of the analysis.
- a signal intensity peak of organic carbon (derived from tyrosine) was detected shortly after the start of measurement. After 600 seconds from the start of measurement, the signal intensity gradually began to be detected due to thermal decomposition of calcium carbonate. Immediately after switching the carrier gas from nitrogen to oxygen, the signal intensity peak of inorganic carbon was detected. The measurement was completed at 1500 seconds, and after the measurement was completed, the integrated value of each peak was obtained and the concentration was calculated.
- FIG. 8 shows the calculated quantitative values of each component. As can be seen from FIGS. 7 and 8, it was confirmed that the organic carbon, carbonate carbon, and inorganic carbon in the sample could be separated and quantified.
- the present invention it becomes possible to separate and detect the organic carbon component and the inorganic carbon component contained in the sample.
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Citations (15)
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JPS5661458U (enrdf_load_stackoverflow) * | 1979-10-16 | 1981-05-25 | ||
US4409336A (en) * | 1981-02-17 | 1983-10-11 | Standard Oil Company (Indiana) | Method of analysis for determining very low sulfur levels in volatilizable samples |
JPS5983054A (ja) * | 1982-11-04 | 1984-05-14 | Horiba Ltd | 金属中の元素分析装置 |
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JP2015137906A (ja) * | 2014-01-22 | 2015-07-30 | 株式会社島津製作所 | 炭素測定装置 |
JP2020064001A (ja) * | 2018-10-18 | 2020-04-23 | 株式会社島津製作所 | 炭素測定方法及び全有機体炭素測定装置 |
WO2020115946A1 (ja) * | 2018-12-04 | 2020-06-11 | 株式会社堀場製作所 | 分析装置及び分析方法 |
JP2020101416A (ja) * | 2018-12-20 | 2020-07-02 | 株式会社堀場製作所 | 試料前処理装置及び分析システム |
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- 2022-11-30 JP JP2023567672A patent/JPWO2023112679A1/ja active Pending
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JPS5983054A (ja) * | 1982-11-04 | 1984-05-14 | Horiba Ltd | 金属中の元素分析装置 |
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JP2002148250A (ja) * | 2000-03-29 | 2002-05-22 | Horiba Ltd | エンジン排ガス中の粒子状物質の分析方法および装置 |
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