WO2022014665A1 - 検査装置 - Google Patents

検査装置 Download PDF

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Publication number
WO2022014665A1
WO2022014665A1 PCT/JP2021/026573 JP2021026573W WO2022014665A1 WO 2022014665 A1 WO2022014665 A1 WO 2022014665A1 JP 2021026573 W JP2021026573 W JP 2021026573W WO 2022014665 A1 WO2022014665 A1 WO 2022014665A1
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WO
WIPO (PCT)
Prior art keywords
column
unit
degassing
container
inspection device
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2021/026573
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English (en)
French (fr)
Japanese (ja)
Inventor
章雄 今井
孝一 霜鳥
明興 中森
紀幸 能登
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
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Shimadzu Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Priority to US18/016,202 priority Critical patent/US20230273169A1/en
Priority to JP2022536437A priority patent/JP7400978B2/ja
Priority to EP21843153.4A priority patent/EP4184163A4/en
Priority to CN202180061332.9A priority patent/CN116194769A/zh
Publication of WO2022014665A1 publication Critical patent/WO2022014665A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/30—Control of physical parameters of the fluid carrier of temperature
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/74—Optical detectors
    • 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
    • G01N31/005—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods investigating the presence of an element by oxidation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
    • B01D15/34—Size-selective separation, e.g. size-exclusion chromatography; Gel filtration; Permeation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/30—Control of physical parameters of the fluid carrier of temperature
    • G01N2030/3007—Control of physical parameters of the fluid carrier of temperature same temperature for whole column
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/30—Control of physical parameters of the fluid carrier of temperature
    • G01N2030/3084—Control of physical parameters of the fluid carrier of temperature ovens

Definitions

  • the present invention relates to an inspection device for inspecting an aqueous sample.
  • the amount of DOM Dissolved organic matter in water is inspected.
  • the amount of TOC Total Organic Carbon is used as one index of the inspection.
  • the amount of TOC is obtained by oxidizing an organic substance (organic carbon) to generate carbon dioxide and measuring the generated carbon dioxide using an NDIR (Nondispersive infrared) type sensor or the like.
  • Patent Document 1 As a method for oxidizing organic carbon, a method of burning using a catalyst, a method of using ultraviolet rays, a method of oxidizing in two steps, and the like are known (Patent Document 1).
  • Non-Patent Document 1 discloses an inspection device in which an SEC (Size-exclusion chromatography) and a TOC detector are combined in order to obtain a molecular weight distribution of DOM.
  • SEC Size-exclusion chromatography
  • Non-Patent Document 1 can detect organic carbon that cannot be detected by an ultraviolet-visible spectrophotometer or a fluorometer by combining an SEC and a TOC detector.
  • Non-Patent Document 1 measures the TOC amount by converting inorganic carbon into carbon dioxide and removing it, then oxidizing the organic carbon and detecting carbon dioxide derived from the organic carbon. At this time, if carbon dioxide derived from inorganic carbon remains, it causes a measurement error. Therefore, it is required to improve the efficiency of removing carbon dioxide derived from inorganic carbon.
  • the present invention has been made to solve such a problem, and one of the purposes thereof is to improve the efficiency of removing carbon dioxide derived from inorganic carbon.
  • the inspection device is an inspection device for inspecting the water quality of an aqueous sample.
  • the inspection device flows through a column that separates the substances contained in the aqueous sample according to the size, and a flow path connected to the outlet of the column in order to convert the inorganic carbon contained in each substance into carbon dioxide.
  • the degassing unit includes a container, a gas permeation tube arranged in the container and connected to the flow path, and a pressure adjusting unit that makes the pressure in the container negative with respect to the gas permeation tube.
  • the inspection device further includes a heat insulating part for maintaining the temperature of each of the column and the container.
  • the container in which the gas permeation tube is arranged is kept warm by the heat insulating part common to the heat insulating part that maintains the temperature of the column, the solubility of carbon dioxide can be lowered and the degassing efficiency of carbon dioxide can be improved. .. Further, since the heat insulating unit for maintaining the temperature of the column and the heat insulating unit for maintaining the temperature of the container in which the gas permeation tube is arranged can be shared, the device configuration of the inspection device can be simplified.
  • FIG. 1 is a diagram schematically showing the configuration of the inspection device 1 of the embodiment.
  • the inspection device 1 is a device for inspecting the water-based sample 2.
  • the inspection device 1 includes a separation device 100 and a TOC device 200 (measurement unit).
  • the inspection device 1 separates the substances in the aqueous sample 2 according to the size by the separation device 100, oxidizes each substance eluted from the separation device 100 in the order according to the size, and the organic contained in each substance.
  • the amount of carbon (TOC amount) is measured by the TOC device 200.
  • the inspection device 1 measures the TOC amount for each dissolved organic substance in the aqueous sample 2 having different sizes.
  • the water-based sample 2 to be inspected using the inspection device 1 is not limited as long as it is a sample containing water as a main component, and is tap water, well water, river or lake water, and desalted. In addition to seawater and the like, it may contain artificial beverages, reagents and the like. Further, the inspection device 1 can be used not only for water quality inspection but also for inspection for the purpose of measuring organic carbon contained in the solution.
  • the separation device 100 separates the substance group contained in the water-based sample 2 to be measured according to the size.
  • the separation device 100 typically separates the substance group contained in the aqueous sample 2 by SEC according to the size.
  • the separation device 100 includes a sample injection unit 110 and a column 120.
  • the sample injection unit 110 injects the water-based sample 2 into the flow path F through which the eluent flows.
  • the eluent can typically be a phosphate buffer.
  • the eluent used is selected in consideration of the type of column 120 and its effect on the TOC apparatus 200 and TOC measurements.
  • the substances in the water-based sample 2 injected into the flow path F from the sample injection section 110 pass through the column 120, and each substance is separated according to the molecular size. More specifically, substances having a large molecular size (generally, a large molecular weight) are sequentially eluted from the column 120 and sent to the TOC device 200.
  • the TOC device 200 measures the amount of TOC contained in the eluate (mixture of the separated substance and the eluent) from the column 120.
  • the TOC device 200 measures the pretreatment unit 220 for removing the inorganic carbon contained in the separated substance and the total carbon amount (that is, the TOC amount) contained in the substance after the inorganic carbon is removed.
  • the measuring unit 240 is provided.
  • the pretreatment unit 220 acidifies the eluate from the column 120 to convert the inorganic carbon in the aqueous sample 2 (in each separated substance) into carbon dioxide and remove it.
  • the pretreatment section 220 includes an addition section 222 for adding a reagent for acidifying the eluate into the flow path, and a degassing section 224 for degassing carbon dioxide.
  • the addition unit 222 is provided at the entrance of the TOC device 200.
  • the reagent added by the addition unit 222 is, for example, phosphoric acid, sulfuric acid, or the like.
  • the addition unit 222 sends the reagent to the flow path F by the pump P.
  • the degassing section 224 is provided downstream of the adding section 222.
  • the degassing section 224 is typically a degasser, which degass carbon dioxide derived from the inorganic carbon generated by the addition of the reagent in the addition section 222.
  • the eluate (mixture of the aqueous sample 2 (separated substances) and the eluent) after being degassed by the degassing unit 224 is sent to the measuring unit 240.
  • the measuring unit 240 measures the TOC amount by oxidizing the organic carbon in the aqueous sample 2 (in each separated substance) after removing the inorganic carbon to carbon dioxide, and measuring the generated carbon dioxide.
  • the measuring unit 240 includes an oxidizing unit 242 that oxidizes the organic carbon in the aqueous sample 2 (in each separated substance) after removing the inorganic carbon, and carbon dioxide (gas) and a liquid generated by oxidizing the organic carbon. It is provided with a gas-liquid separation unit 244 for separating the carbon dioxide and a CO2 detector 246 for measuring the carbon dioxide obtained by the separation.
  • the oxidizing unit 242 oxidizes organic carbon by a wet UV oxidation method. More specifically, the oxidizing portion 242 adds an oxidizing agent to each substance (eluate) after removing the inorganic carbon, and then irradiates the organic carbon with ultraviolet rays to oxidize the organic carbon.
  • the configuration of the oxidized portion 242 will be described later with reference to FIG.
  • the oxidizing unit 242 does not need to add an oxidizing agent when the TOC amount is lower than the predetermined amount.
  • the gas-liquid separation unit 244 separates the liquid and the gas, discharges the liquid as a waste liquid to the outside, and sends the gas to the CO2 detector 246.
  • the gas separated by the gas-liquid separation unit 244 contains at least carbon dioxide generated by oxidizing organic carbon.
  • the CO2 detector 246 measures the carbon dioxide concentration in the gas sent from the gas-liquid separation unit 244.
  • the CO2 detector 246 is typically a non-dispersive infrared gas detector (NDIR detector).
  • NDIR detector non-dispersive infrared gas detector
  • the CO2 detector 246 is not limited to the NDIR detector, and may be another detector as long as it can measure the carbon dioxide concentration.
  • FIG. 2 is a diagram schematically showing the configurations of the separation device 100 and the pretreatment unit 220.
  • the eluent is produced by feeding pure water and a phosphate buffer solution by separate pumps and mixing them in the flow path F.
  • the separation device 100 includes a first solvent feeding section 130 for feeding water and a second solvent feeding section 140 for feeding a phosphoric acid buffer solution (phosphoric acid eluent).
  • the sample injection section 110 is provided downstream of the first solvent delivery section 130.
  • the second solvent feeding unit 140 is connected via the mixer M between the flow paths from the sample injection unit 110 to the column 120.
  • the first solvent feeding section 130 and the second solvent feeding section 140 are provided with a first degassing section 132 and a second degassing section 142 as pretreatment sections for degassing the gas dissolved in the solvent, respectively.
  • the degassing unit 224 for removing carbon dioxide derived from inorganic carbon includes a container 225, a tube 226 arranged in the container 225, and a pressure adjusting unit that makes the pressure in the container 225 negative with respect to the tube 226.
  • the vacuum pump 227 and the like are provided.
  • the tube 226 is connected to the flow path F through which the aqueous sample 2 flows.
  • the tube 226 is a gas permeable tube and is made of a material that is permeable to gas while impermeable to liquid.
  • the tube 226 is typically, but is not limited to, a gas permeable tube made of an amorphous Teflon (registered trademark) resin material, a hollow fiber membrane made of a polytetrafluoroethylene material, and the like.
  • the pressure inside the container 225 When the pressure inside the container 225 is reduced by the vacuum pump 227, the pressure inside the container 225 becomes a negative pressure with respect to the tube 226, the gas in the flow path F moves out of the tube 226, and carbon dioxide derived from inorganic carbon elutes. Removed from the liquid (mixture of each substance and eluent). It is only necessary that the pressure in the container 225 be a negative pressure with respect to the tube 226, and the method is not limited to the method using the vacuum pump 227.
  • the temperature of the container 225 in which the tube 226 is arranged can be maintained high, the solubility of carbon dioxide in the eluent can be lowered, so that the degassing efficiency of carbon dioxide can be improved. Therefore, it is preferable to provide a heat insulating portion for keeping the container 225 warm.
  • the inspection device 1 further includes a column oven 60.
  • the column oven 60 has a function of adjusting the temperature of the column 120.
  • the container 225 of the degassing unit 224 for removing carbon dioxide derived from inorganic carbon is housed in the column oven 60. That is, the column oven 60 contains the column 120 and the container 225. Thereby, the column oven 60 regulates and maintains the temperature of the column 120 and the container 225.
  • the column oven 60 not only regulates the temperature of the column 120, but also functions as a heat insulating unit for keeping the container 225 warm.
  • the column oven 60 for adjusting the temperature of the column 120 functions as a heat insulating unit for keeping the container 225 warm.
  • the heat insulating unit that keeps the container 225 warm may be configured to further function as a heat insulating unit for maintaining the temperature of the column 120.
  • the set temperature of the column oven 60 is preferably set to a temperature higher than the temperature outside the column oven 60 (room temperature). Further, the set temperature of the column oven 60 is set to the recommended operating temperature of the column 120. For example, the set temperature of the column oven 60 is above room temperature and below 30 degrees Celsius. If the set temperature of the column oven 60 is set high, the holding time of each substance in the column 120 tends to be short, so that the analysis time can be shortened.
  • the column oven 60 is usually used to maintain the temperature of the column 120 at a constant temperature.
  • the temperature in the container 225 can be maintained at room temperature or higher, so that carbon dioxide to the eluent can be maintained.
  • the solubility of carbon dioxide can be lowered, and the degassing efficiency of carbon dioxide can be improved.
  • the device for maintaining the temperature of the container 225 at room temperature or higher since the temperature inside the container 225 can be maintained at room temperature or higher by the column oven 60 normally used when the column 120 is used, the device for maintaining the temperature of the container 225 at room temperature or higher. There is no need to prepare a new one.
  • FIG. 3 is a diagram schematically showing the configuration of the oxidized portion 242.
  • the oxidizing unit 242 includes an adding unit 422 and an irradiation unit 424.
  • the addition unit 422 is provided at the entrance of the oxidation unit 242.
  • the irradiation unit 424 is provided downstream of the addition unit 422.
  • Addition unit 422 adds an oxidizing agent to the aqueous sample 2 (eluent) after removing the inorganic carbon.
  • the oxidizing agent is, for example, sodium persulfate.
  • the addition unit 422 sends the oxidant to the flow path F by the pump P.
  • the irradiation unit 424 includes a UV lamp 426 that irradiates the aqueous sample 2 (eluate) flowing through the flow path F with ultraviolet rays.
  • the configuration of the irradiation unit 424 includes a cylindrical UV lamp and a spiral flow path that receives ultraviolet rays from the UV lamp.
  • An inflow section 500 is provided in the flow path F between the addition section 422 and the irradiation section 424.
  • the inflow unit 500 controls the flow rate of the gas to flow into the flow path F.
  • the gas to be introduced is a gas that does not contain a carbon-based compound that may be oxidized to generate carbon dioxide, and is, for example, nitrogen, helium, oxygen, or the like.
  • the carbon-free gas is nitrogen.
  • the inflow unit 500 includes a nitrogen supply source 520 and a mass flow controller 540. Nitrogen gas is supplied to the flow path F from the nitrogen supply source 520. The mass flow controller 540 controls the flow rate of the nitrogen gas supplied to the flow path F.
  • the mass flow controller 540 controls the flow rate of nitrogen gas so that the flow rate of nitrogen gas supplied from the nitrogen supply source 520 to the flow path F becomes constant.
  • the liquid and the gas are separated by the gas-liquid separation unit 244, and only the gas is sent to the CO2 detector 246, and the carbon dioxide concentration generated by oxidizing the organic carbon. Is measured by the CO2 detector 246.
  • FIG. 4 is a diagram schematically showing the configuration of the inspection device 1a according to the modified example.
  • the inspection device 1 includes only the TOC device 200 as a measuring device.
  • the inspection device 1 may include another measuring device in addition to the TOC device 200.
  • the inspection device 1a according to the modified example is different from the inspection device 1 shown in the above embodiment in that it further includes an ultraviolet-visible spectrophotometer 12 and a fluorescence photometer 14 in addition to the TOC device 200.
  • the ultraviolet-visible spectrophotometer 12 and the fluorescence photometer 14 are provided on the flow path F between the separation device 100 and the TOC device 200. More specifically, the ultraviolet-visible spectrophotometer 12 and the fluorometer 14 are provided between the path from the column 120 to the addition section 222.
  • the amount of TOC is measured by measuring carbon dioxide derived from organic carbon by applying a chemical treatment to an aqueous sample.
  • the ultraviolet-visible spectrophotometer 12 and the fluorescence photometer 14 water-based samples are measured without physically or chemically treating each separated substance and without changing the composition, shape, or function of the substance. can do.
  • each measuring device can be arranged on one flow path, and the eluents eluted from the separation device 100 can be arranged. There is no need to branch to the measuring device. Therefore, it is not necessary to reduce the liquid volume of the water-based sample used in each measuring device, and the measurement accuracy can be maintained.
  • the inspection device 1a includes an ultraviolet-visible spectrophotometer 12 and a fluorescence photometer 14.
  • the inspection device may be configured to include one of the ultraviolet-visible spectrophotometer 12 and the fluorescence photometer 14 in addition to the TOC device 200.
  • the inspection device is an inspection device for inspecting an aqueous sample, and is included in each substance and a column that separates a group of substances contained in the aqueous sample according to the size.
  • an addition part that adds a reagent that acidifies the aqueous sample flowing through the flow path connected to the outlet of the column into the flow path and a carbon dioxide downstream part are provided downstream of the addition part. It is provided with a degassing unit for degassing and a measuring unit for oxidizing each substance after removing carbon dioxide in the degassing unit and measuring the organic carbon contained in each substance.
  • the degassing unit includes a container, a gas permeation tube arranged in the container and connected to the flow path, and a pressure adjusting unit (227) for making the pressure in the container negative with respect to the gas permeation tube.
  • the inspection device further includes a heat insulating unit for maintaining the temperature of each of the column and the container.
  • the solubility of carbon dioxide can be lowered.
  • the degassing efficiency of carbon dioxide can be increased.
  • the heat insulating unit for maintaining the temperature of the column and the heat insulating unit for maintaining the temperature of the container in which the gas permeation tube is arranged can be shared, the device configuration of the inspection device can be simplified.
  • the heat insulating unit has a function of adjusting the temperature of each of the column and the container.
  • the temperature can be adjusted according to the measurement conditions.
  • the inspection device according to paragraph 1 or 2 further includes a heat insulating unit and a column oven for accommodating a container.
  • the inspection device according to any one of the items 1 to 3 is provided upstream from the inlet of the column and has a pretreatment unit for degassing the gas dissolved in the eluent. Further prepare.
  • the temperature of the container in which the gas permeation tube is arranged can be maintained, so that the degassing efficiency of carbon dioxide can be improved. Further, since the heat insulating unit for maintaining the temperature of the column and the heat insulating unit for maintaining the temperature of the container in which the gas permeation tube is arranged can be shared, the device configuration of the inspection device can be simplified.
  • the inspection apparatus has at least one of an ultraviolet-visible spectrophotometer and a fluorescence photometer between the column and the path to the addition part. Further prepare.
  • the measurement can be performed by each measuring device without branching each substance eluted from the column to each measuring device. Since it is not necessary to branch each substance eluted from the column to each measuring device, the amount of each substance used in each measuring device can be maintained, and as a result, the measurement accuracy can be maintained.
  • 1,1a inspection device 2 water-based sample, 12 ultraviolet visible spectrophotometer, 14 fluorescence photometer, 60 column oven, 100 separation device, 110 sample injection section, 120 column, 130 first solvent delivery section, 132 first removal Air part, 140 second solvent feeding part, 142 second degassing part, 200 TOC device, 220 pretreatment part, 222,422 addition part, 224 degassing part, 225 container, 226 tube, 227 vacuum pump, 240 measurement 242 Oxidation section, 244 Gas-liquid separation section, 246 CO2 detector, 424 irradiation section, 426 UV lamp, 500 inflow section, 520 nitrogen supply source, 540 mass flow controller, F flow path, M mixer, P pump.

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PCT/JP2021/026573 2020-07-17 2021-07-15 検査装置 Ceased WO2022014665A1 (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US18/016,202 US20230273169A1 (en) 2020-07-17 2021-07-15 Inspection apparatus
JP2022536437A JP7400978B2 (ja) 2020-07-17 2021-07-15 検査装置
EP21843153.4A EP4184163A4 (en) 2020-07-17 2021-07-15 Inspection device
CN202180061332.9A CN116194769A (zh) 2020-07-17 2021-07-15 检查装置

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JP2020122725 2020-07-17
JP2020-122725 2020-07-17

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US (1) US20230273169A1 (https=)
EP (1) EP4184163A4 (https=)
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WO (1) WO2022014665A1 (https=)

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Title
KAWASAKI, NOBUYUKI: "Examination of molecular weight distribution of DOC in Kasumigaura using size exclusion chromatography with TOC detector", PROCEEDINGS OF 72ND GENERAL ASSEMBLY OF THE JAPANESE SOCIETY OF LIMNOLOGY, vol. 72, 1 September 2007 (2007-09-01), JP, pages 3C5, XP009533429, DOI: 10.14903/jslim.72.0.80.0 *
NOBUYUKI KAWASAKIKAZUO MATSUSHIGEAKIO IMAIKAZUHIRO KOMATSUFUMIKAZU OGISHIMASATO YAHATAHIROHISA MIKAMITAKESHI GOTO: "72nd Meeting, a collection of abstracts of lectures, Session ID: 3C5", September 2007, THE JAPANESE SOCIETY OF LIMNOLOGY, article "Consideration for molecular weight distribution of DOC in Kasumigaura using size-exclusion chromatography equipped with TOC detector"
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