WO2015011954A1 - Chromatographe en phase gazeuse - Google Patents

Chromatographe en phase gazeuse Download PDF

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Publication number
WO2015011954A1
WO2015011954A1 PCT/JP2014/059305 JP2014059305W WO2015011954A1 WO 2015011954 A1 WO2015011954 A1 WO 2015011954A1 JP 2014059305 W JP2014059305 W JP 2014059305W WO 2015011954 A1 WO2015011954 A1 WO 2015011954A1
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WO
WIPO (PCT)
Prior art keywords
gas
setting
display
electricity
functions
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PCT/JP2014/059305
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English (en)
Japanese (ja)
Inventor
真吾 増田
貴秀 横矢
雅史 山根
Original Assignee
株式会社島津製作所
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by 株式会社島津製作所 filed Critical 株式会社島津製作所
Priority to JP2015528166A priority Critical patent/JP6020726B2/ja
Priority to CN201480037662.4A priority patent/CN105358972B/zh
Publication of WO2015011954A1 publication Critical patent/WO2015011954A1/fr

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/86Signal analysis
    • G01N30/8658Optimising operation parameters
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier

Definitions

  • the present invention relates to a gas chromatograph that performs analysis by supplying a carrier gas into a column together with sample components.
  • a carrier gas is supplied into a column together with sample components, and each component is separated in the process of passing the carrier gas through the column.
  • the carrier gas is mixed with the sample components in the sample vaporization chamber and then supplied into the column from the column inlet.
  • the gas chromatograph is provided with a column oven.
  • the carrier gas can be supplied into the column while heating the column in the column oven.
  • a fan for stirring air, for example, is provided in the column oven.
  • the temperature distribution in the column oven can be kept uniform by driving the fan.
  • Japanese Patent Application Laid-Open No. H10-228688 proposes a configuration that can execute an energy saving mode for reducing the consumption of carrier gas and electricity.
  • the present invention has been made in view of the above circumstances, and an object thereof is to provide a gas chromatograph capable of easily and efficiently reducing the consumption of gas or electricity.
  • the gas chromatograph according to the present invention is a gas chromatograph that performs analysis by supplying a carrier gas together with a sample component into a column, and settings relating to a plurality of functions for reducing consumption of the gas containing the carrier gas
  • a gas reduction setting value storage unit for storing values, an electricity reduction setting value storage unit for storing setting values related to a plurality of functions for reducing electricity consumption in the gas chromatograph, gas consumption and electricity
  • a display processing unit for displaying a batch setting key selected to reduce at least one of the consumption amounts on a display unit; and the gas reduction setting value storage unit and the electric reduction setting value based on the selection of the batch setting key
  • Setting value change processing for reading setting values from at least one of the storage units and collectively changing setting values related to the plurality of types of functions Characterized by comprising and.
  • the setting values for a plurality of types of functions for reducing the amount of gas consumption, and the types of functions for reducing the amount of electricity consumed are changed at once. Therefore, for example, even a user who is unfamiliar with work can easily set the setting values for a plurality of types of functions to appropriate values, so that the consumption of gas or electricity can be reduced easily and efficiently. it can.
  • the display processing unit causes the display unit to separately display a batch setting key selected to reduce gas consumption and a batch setting key selected to reduce electricity consumption. Is preferred.
  • the setting values for gas often include parameter setting values that affect the analysis, so change the setting values more carefully than when changing the setting values for electricity.
  • the set values for gas and electricity can be set more appropriately.
  • the display processing unit collectively displays a set value related to a plurality of types of functions for reducing gas consumption, and a set value related to a plurality of types of functions for reducing electricity consumption. It is preferable to separately display an electrical batch display screen that displays the batches on the display unit.
  • the user can confirm the set values for gas and electricity in an easy-to-understand manner by using the gas batch display screen and the electrical batch display screen separately displayed on the display unit. Therefore, the setting operation can be performed smoothly and in a short time compared to the conventional configuration in which it is necessary to individually check the set values for a plurality of types of functions related to gas and electricity.
  • the display processing unit displays the fact on the display unit when the setting values related to the plurality of types of functions are collectively changed by the setting value change processing unit.
  • the user can easily confirm from the display on the display section that the set values for gas or electricity have been changed in a lump. Therefore, it is easy to understand that the consumption of gas or electricity is efficiently reduced, and it is easy to use.
  • the display processing unit displays, on the display unit, a reduction rate of at least one of gas consumption and electricity consumption when setting values related to the plurality of types of functions are collectively changed by the setting value change processing unit. It is preferable to make it.
  • the present invention it is possible to easily set the setting values related to a plurality of types of functions to appropriate values, so that it is possible to easily and efficiently reduce the consumption of gas or electricity.
  • FIG. 1 is a schematic diagram showing a configuration example of a gas chromatograph according to an embodiment of the present invention.
  • This gas chromatograph is used for analysis by supplying a carrier gas together with sample components into the column 1, and includes a column oven 2, a gas introduction unit 3, a detector 4 and the like in addition to the column 1. Yes.
  • the column 1 is composed of, for example, a capillary column and is heated in the column oven 2 during analysis.
  • the carrier gas is supplied into the column 1 together with each sample component from the gas inlet 3 through the column inlet 5.
  • Each sample component is separated in the process of passing through the column 1 and detected by the detector 4.
  • the detector 4 can be composed of various detectors such as a flame ionization detector (FID).
  • a heater 21 and a fan 22 are provided in the column oven 2.
  • the heater 21 heats the column 1 by heating the air in the column oven 2.
  • the fan 22 is for stirring the air by being rotated by the motor M. By controlling the driving of the fan 22, the temperature distribution in the column oven 2 can be kept uniform.
  • the gas introduction unit 3 is for introducing a carrier gas into the column 1 from the column inlet 5, and for example, a sample vaporizing chamber (not shown) is formed therein.
  • a liquid sample is injected into the sample vaporizing chamber, and the sample components vaporized in the sample vaporizing chamber are introduced into the column 1 from the column inlet 5 together with the carrier gas.
  • a gas supply channel 6, a purge channel 7, a split channel 8, and the like communicate with the sample vaporizing chamber.
  • the gas supply channel 6 is a channel for supplying a carrier gas to the sample vaporization chamber of the gas introduction unit 3.
  • the purge flow path 7 is a flow path for discharging undesired components generated from a septum or the like to the outside.
  • the split flow path 8 is a flow path for discharging excess sample components together with the carrier gas when the carrier gas is introduced into the column 1 from the column inlet 5 by the split introduction method.
  • FIG. 2 is a block diagram showing an example of an electrical configuration in the gas chromatograph of FIG.
  • the operation of this gas chromatograph is controlled by a control unit 10 including a CPU (Central Processing Unit), for example.
  • An operation unit 20, a display unit 30, a storage unit 40, and the like are connected to the control unit 10.
  • the operation unit 20 includes, for example, a keyboard and a mouse, and the user can perform various setting operations by operating the operation unit 20.
  • the display part 30 is comprised, for example with the liquid crystal display, and can display the various information regarding operation
  • the storage unit 40 is composed of, for example, a ROM (Read Only Memory) and a RAM (Random Access Memory).
  • the control unit 10 functions as a display processing unit 11, a set value processing unit 12, and the like when the CPU executes a program.
  • the display processing unit 11 performs processing for display on the display unit 30 based on the operation of the operation unit 20.
  • the set value processing unit 12 performs processing for various set values related to the operation of the gas chromatograph, and includes, for example, a set value change processing unit 13 and a reduction rate calculation processing unit 14.
  • parameters related to gas such as the flow rate of the carrier gas and parameters related to electricity such as driving of the fan 22 can be set.
  • the set values of these parameters are stored in a set value storage unit 41 assigned to the storage unit 40.
  • the setting value change processing unit 13 changes the setting values stored in the setting value storage unit 41. Perform the process.
  • setting values gas reduction setting values related to a plurality of types of functions for reducing gas consumption and setting values (electricity reductions) related to a plurality of types of functions for reducing electricity consumption.
  • Set value is stored in the reduction set value storage unit 42 assigned to the storage unit 40. That is, the reduction setting value storage unit 42 includes a gas reduction setting value storage unit that stores gas reduction setting values related to a plurality of types of functions, and an electricity reduction setting value storage unit that stores electric reduction setting values related to a plurality of types of functions. It is composed.
  • the gas reduction setting value is a setting value determined in advance so that the gas consumption amount is smaller than the amount normally consumed during analysis for a plurality of types of functions related to gas.
  • the gas includes not only a carrier gas but also a gas other than the carrier gas.
  • the electricity reduction setting value is a setting value determined in advance so that the consumption amount of electricity for each of a plurality of types of functions related to electricity is smaller than the amount normally consumed during analysis.
  • the setting value change processing unit 13 reads the gas reduction setting value or the electricity reduction setting value stored in the reduction setting value storage unit 42 and performs a process of changing the setting value stored in the setting value storage unit 41. be able to. Further, the reduction rate calculation processing unit 14 calculates a reduction rate of gas consumption or electricity consumption based on the gas reduction setting value or the electricity reduction setting value stored in the reduction setting value storage unit 42. Can do. The result of the processing by the set value change processing unit 13 can be displayed on the display unit 30 by the display processing unit 11.
  • FIG. 3 to 6 are diagrams showing specific examples of the display screen of the display unit 30.
  • FIG. 3 shows an eco setting screen 31
  • FIG. 4 shows a gas collective display screen 32
  • FIG. 5 shows an electric collective display screen 33
  • FIG. 6 shows a gas charge display screen 34, respectively.
  • a gas selection key 311 for displaying the gas collective display screen 32 of FIG. 4 and an electric collective display screen 33 of FIG. 5 are displayed by the processing of the display processing unit 11.
  • An electrical selection key 312 is displayed. The user can select either the gas selection key 311 or the electricity selection key 312 by operating the operation unit 20.
  • a gas saver setting key 321, a carrier gas type setting key 322, a CRG operation start temperature setting key 323, an AFC leak check function setting key 324, and batch setting are performed by the processing of the display processing unit 11.
  • a key 325, an eco state display 326, a gas reduction rate display 327, and the like are displayed.
  • the gas batch display screen 32 is a screen that collectively displays setting values relating to a plurality of types of functions for reducing gas consumption.
  • the gas saver setting key 321 is selected by the operation unit 20 when setting a function (gas saver) for reducing carrier gas consumption.
  • a transition is made to the gas saver setting screen, and each setting value of the save function split ratio, start time, gas saver AOC interlocking and gas saver automatic on time, which are parameters of the function concerned. Can be set.
  • the gas saver setting key 321 is selected and set, as shown in FIG. 4, the characters “ON” are displayed on the side of the gas saver setting key 321 and the side of each parameter is set. The set value is displayed on.
  • the split ratio during saving is the ratio of the flow rate of the carrier gas discharged from the split flow path 8 to the flow rate of the carrier gas introduced into the column 1 (split ratio).
  • the start time is a time for changing the split ratio to a set value, and it can be set how many minutes after the start of the analysis the split ratio is changed to the set value.
  • the split ratio is automatically set in conjunction with the operation of the autosampler (AOC). This function returns the value and can be set to ON or OFF.
  • the gas saver auto-on time is a time from when the analysis is completed until the gas saver is started after entering the standby state.
  • the carrier gas type setting key 322 is selected by the operation unit 20 when setting the type of carrier gas.
  • the carrier gas helium gas, nitrogen gas, hydrogen gas, or the like can be used.
  • the carrier gas type setting key 322 is selected and set, the type of the selected carrier gas is displayed on the side of the carrier gas type setting key 322 as shown in FIG.
  • the CRG operation start temperature setting key 323 is used to determine the temperature at which the temperature of the column 1 is supplied when the temperature of the column 1 is rapidly cooled by the liquefied carbon dioxide gas using a low temperature addition device (CRG). Is selected by the operation unit 20.
  • CRG operation start temperature setting key 323 is selected and set, the temperature (CRG operation start temperature) set to the side of the CRG operation start temperature setting key 323 is displayed as shown in FIG. Is done.
  • This CRG operation start temperature is normally set to about 50 ° C.
  • the AFC leak check function setting key 324 controls the carrier gas flow rate with an electronic flow controller (AFC), and sets a function for checking whether the carrier gas is leaking in the sample vaporization chamber or other piping. At this time, it is selected by the operation unit 20. This function can be set to ON or OFF, and the contents set on the side of the AFC leak check function setting key 324 are displayed.
  • AFC electronic flow controller
  • the collective setting key 325 is selected by the operation unit 20 to collectively reduce gas consumption for a plurality of types of functions related to gas displayed on the gas collective display screen 32.
  • the collective setting key 325 includes an ON key and an OFF key. By selecting the ON key, the gas consumption can be reduced collectively.
  • the set value change processing unit 13 reads out the gas reduction set values stored in the reduction set value storage unit 42, and the plurality of the above-described plural values. Setting values for various types of functions are changed at once.
  • the save split ratio is “5”
  • the start time is “1”
  • the gas saver AOC interlock is “ON”
  • the gas saver automatic on time is “2”
  • the CRG operation is performed.
  • the start temperature is set to “25” ° C. and the AFC leak check function is set to “ON” at once.
  • the type of carrier gas is a very important parameter for the analysis, and it is preferable that the user selects and sets the carrier gas type setting key 322 one by one instead of the batch setting. Even if the ON key 325 is selected, it is not changed.
  • the setting values before the change are temporarily stored in the storage unit 40. Then, when the OFF key of the collective setting key 325 is selected thereafter, the setting value before the change is read from the storage unit 40 and changed to the setting value, thereby setting values relating to a plurality of types of functions. Are returned to the original values in a batch.
  • setting values related to a plurality of types of functions for reducing gas consumption can be changed at a time. Even so, the setting values for a plurality of types of functions can be easily set to appropriate values. Therefore, gas consumption can be easily and efficiently reduced.
  • the eco status display 326 is displayed when the set values related to a plurality of types of functions for gas are changed in a batch by selecting the ON key of the batch setting key 325. As a result, the user can easily confirm from the display on the display unit 30 that the set values for the gas have been changed in a batch. Therefore, it is easy to understand that the gas consumption is efficiently reduced, and it is easy to use.
  • the gas consumption reduction rate is displayed. For example, when a set value related to a plurality of functions for gas is changed in a batch by selecting the ON key of the batch setting key 325, the gas consumption in each state and each set value are initialized.
  • the reduction rate of the gas consumption is calculated by the reduction rate calculation processing unit 14 based on the difference from the gas consumption in the state set to the value (the gas saver function is in the off state), and the reduction rate is the gas It is displayed as a reduction rate display 327.
  • the reduction rate calculation processing unit 14 may calculate a reduction rate of gas consumption, and the reduction rate may be displayed as the gas reduction rate display 327.
  • a setting key 336, an eco state display 337, an electricity reduction rate display 338, and the like are displayed.
  • This electricity collective display screen 33 is a screen that collectively displays setting values relating to a plurality of types of functions for reducing electricity consumption.
  • the LCD backlight lighting time key 331 is selected by the operation unit 20 when setting the number of minutes after the backlight provided in the display unit 30 is turned off after the gas chromatograph is not operated.
  • the backlight intensity key 332 is selected by the operation unit 20 when setting the intensity (light quantity) of the backlight provided in the display unit 30.
  • the intensity of the backlight can be set in three stages, for example, strong, medium, and weak.
  • the intensity of the selected backlight is displayed on the side of the backlight intensity key 332 as shown in FIG.
  • the buzzer key 333 is selected by the operation unit 20 when setting the buzzer sound output when an error occurs or a key is operated.
  • the buzzer sound can be set in four stages, for example, large, medium, small, and OFF.
  • the magnitude of the selected buzzer sound is displayed on the side of the buzzer key 333 as shown in FIG.
  • the round indicator key 334 is selected by the operation unit 20 when setting whether or not to turn on the circular decorative light provided on the opening / closing door of the column oven 2.
  • the function can be set to ON or OFF, and as shown in FIG. 5, the contents set to the side of the round indicator key 334 are displayed.
  • the non-analysis oven fan key 335 is selected by the operation unit 20 when setting whether or not to drive the fan 22 when analysis is not being performed.
  • the function can be set in three stages of strong, weak, and OFF. As shown in FIG. 5, the contents set on the side of the fan key 335 in the oven outside the analysis time are displayed.
  • the collective setting key 336 is selected by the operation unit 20 in order to collectively reduce the amount of electricity consumed for a plurality of types of functions related to electricity displayed on the electricity collective display screen 33.
  • the collective setting key 336 includes an ON key and an OFF key. By selecting the ON key, it is possible to reduce electricity consumption in a batch.
  • the setting value change processing unit 13 reads out the electricity reduction setting value stored in the reduction setting value storage unit 42, and the plurality of the above-described plural values. Setting values for various types of functions are changed at once.
  • the LED backlight lighting time is “2”
  • the backlight intensity is “weak”
  • the buzzer is “OFF”
  • the round indicator is “OFF”
  • the fan in the oven outside the analysis time is “OFF” is set all at once.
  • the setting values before the change are temporarily stored in the storage unit 40. Then, when the OFF key of the collective setting key 336 is selected thereafter, the setting value before the change is read from the storage unit 40 and changed to the setting value, thereby setting values relating to a plurality of types of functions. Are returned to the original values in a batch.
  • setting values related to a plurality of types of functions for reducing electricity consumption can be changed in a lump. Even so, the setting values for a plurality of types of functions can be easily set to appropriate values. Therefore, it is possible to easily and efficiently reduce electricity consumption.
  • the eco status display 337 is displayed when the setting values related to a plurality of types of functions for electricity are changed in a batch by selecting the ON key of the batch setting key 336. As a result, the user can easily confirm from the display on the display unit 30 that the set value for electricity has been changed in a lump. Therefore, it is easy to understand that the consumption of electricity is efficiently reduced, and it is easy to use.
  • the eco state display 326 for gas as shown in FIG. 4 and the eco state display 337 for electricity as shown in FIG. 5 may be displayed at the same position on the display screen of the display unit 30. In this case, only the set value for gas is changed in a batch, only the set value for electricity is changed in a batch, and the set value for gas and electricity is both changed in a batch. Thus, the eco status display 326, 337 may have different colors.
  • the electricity reduction rate display 338 displays the electricity consumption reduction rate. For example, when the set value for a plurality of types of functions for electricity is changed in a batch by selecting the ON key of the collective setting key 336, the electricity consumption and each set value in that state are initialized. Based on the difference from the electricity consumption in the state set to the value, the reduction rate calculation processing unit 14 calculates the electricity consumption reduction rate, and the reduction rate is displayed as the electricity reduction rate display 338.
  • the reduction rate calculation processing unit 14 may calculate a reduction rate of electricity consumption, and the reduction rate may be displayed as the electricity reduction rate display 338.
  • the gas and electricity consumption can be reduced separately by selecting the collective setting keys 325 and 336 for gas and electricity displayed on the display unit 30 separately.
  • the setting values for gas often include parameter setting values that affect the analysis, so change the setting values more carefully than when changing the setting values for electricity. There is a need. Therefore, it is possible to set the setting values for gas and electricity more appropriately by adopting a configuration in which the collective setting keys 325 and 336 for gas and electricity can be selected separately.
  • the gas batch display screen 32 and the electrical batch display screen 33 that are separately displayed on the display unit 30 allow the user to check the set values for gas and electricity in an easy-to-understand manner. . Therefore, the setting operation can be performed smoothly and in a short time compared to the conventional configuration in which it is necessary to individually check the set values for a plurality of types of functions related to gas and electricity.
  • the current gas charge 341 is a gas charge for a predetermined period at the current set value for gas.
  • the eco-recommended setting gas charge 342 is the gas charge for the predetermined period when the collective setting key 325 is selected and the set value for gas is changed to the recommended value collectively.
  • the eco-free gas charge 343 is a gas charge for the predetermined period when each set value for gas is set to an initial value (the function of the gas saver is off).
  • the predetermined period is the past month in this example, but is not limited thereto.
  • the gas charge display screen 34 displayed when the gas reduction rate display 327 in FIG. 4 is selected by the operation unit 20 has been described.
  • the electricity reduction rate display 338 in FIG. 5 is selected by the operation unit 20.
  • an electricity charge display screen may be displayed, and the current electricity charge, the eco-recommended setting electricity charge, and the eco-unused electricity charge may be displayed in a mutually comparable state.
  • the calculation of the gas charge or the electricity charge as described above can be performed by the control unit 10.
  • the unit price setting screen for inputting the unit price of the gas rate or the electricity rate may be displayed on the display unit 30 by the display processing unit 11, and the gas rate or the electricity rate may be calculated using the input unit price.
  • the control unit 10 functions as a charge calculation processing unit for calculating a gas charge or an electricity charge.
  • setting values related to a plurality of types of functions for reducing the consumption of gas and setting values related to a plurality of types of functions for reducing the consumption of electricity are set as separate collective setting keys 325.
  • a configuration that can be collectively changed by H.336 has been described.
  • the present invention is not limited to such a configuration, and a set value related to a plurality of types of functions for reducing gas consumption and a set value related to a plurality of types of functions for reducing electricity consumption are collected in one batch.
  • a configuration that can be collectively changed by a setting key may be used.
  • the plurality of types of functions for reducing gas consumption and the plurality of types of functions for reducing electricity consumption are not limited to the functions illustrated in the above embodiment, but other functions. It may be.

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Abstract

La présente invention concerne un chromatographe en phase gazeuse qui permet de réduire facilement et efficacement la consommation de gaz ou d'électricité. Un chromatographe en phase gazeuse est conçu de manière qu'il soit possible de modifier collectivement des réglages relatifs à une pluralité de fonctions destinées à réduire la consommation de gaz, des réglages relatifs à une pluralité de fonctions destinées à réduire la consommation d'électricité ou les deux à la fois par sélection d'une clé (325) de réglage collective. Par conséquent, par exemple, même un utilisateur qui n'est pas habitué à travailler avec un chromatographe peut facilement effectuer des réglages relatifs à une pluralité de fonctions à des valeurs appropriées. Ainsi, il est possible de réduire facilement et efficacement la consommation de gaz ou d'électricité.
PCT/JP2014/059305 2013-07-23 2014-03-28 Chromatographe en phase gazeuse WO2015011954A1 (fr)

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JP2015528166A JP6020726B2 (ja) 2013-07-23 2014-03-28 ガスクロマトグラフ
CN201480037662.4A CN105358972B (zh) 2013-07-23 2014-03-28 气相色谱仪

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JP2013152316 2013-07-23
JP2013-152316 2013-07-23

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JP2007040810A (ja) * 2005-08-03 2007-02-15 Hitachi High-Technologies Corp 液体クロマトグラフ装置
JP2008173815A (ja) * 2007-01-17 2008-07-31 Seiko Epson Corp 印刷データ生成装置、テープ印刷装置およびプログラム
JP2011017606A (ja) * 2009-07-08 2011-01-27 Shimadzu Corp ガスクロマトグラフ分析装置用設計・分析支援プログラム
JP2011095072A (ja) * 2009-10-29 2011-05-12 Shimadzu Corp ガスクロマトグラフ装置
JP2011220909A (ja) * 2010-04-13 2011-11-04 Shimadzu Corp ガスクロマトグラフ
JP2012052860A (ja) * 2010-08-31 2012-03-15 Shimadzu Corp ガスクロマトグラフ
JP2012145595A (ja) * 2012-05-07 2012-08-02 Ajinomoto Co Inc 液体クロマトグラフ装置

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