WO2022124260A1 - 蒸発濃縮機構、これを備えた分析装置、および、蒸発濃縮機構の制御方法 - Google Patents
蒸発濃縮機構、これを備えた分析装置、および、蒸発濃縮機構の制御方法 Download PDFInfo
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- WO2022124260A1 WO2022124260A1 PCT/JP2021/044695 JP2021044695W WO2022124260A1 WO 2022124260 A1 WO2022124260 A1 WO 2022124260A1 JP 2021044695 W JP2021044695 W JP 2021044695W WO 2022124260 A1 WO2022124260 A1 WO 2022124260A1
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- 230000007246 mechanism Effects 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims description 31
- 238000004458 analytical method Methods 0.000 title description 10
- 239000007788 liquid Substances 0.000 claims abstract description 120
- 238000010438 heat treatment Methods 0.000 claims abstract description 44
- 238000001704 evaporation Methods 0.000 claims description 91
- 230000008020 evaporation Effects 0.000 claims description 88
- 238000001816 cooling Methods 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- 230000008859 change Effects 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 8
- 230000007613 environmental effect Effects 0.000 abstract description 6
- 239000012141 concentrate Substances 0.000 abstract description 5
- 239000012488 sample solution Substances 0.000 abstract 7
- 238000001514 detection method Methods 0.000 description 9
- 238000010586 diagram Methods 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000003505 heat denaturation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000002285 radioactive effect Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 238000007630 basic procedure Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002901 radioactive waste Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N35/1009—Characterised by arrangements for controlling the aspiration or dispense of liquids
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4027—Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N2035/00346—Heating or cooling arrangements
- G01N2035/00356—Holding samples at elevated temperature (incubation)
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N35/1009—Characterised by arrangements for controlling the aspiration or dispense of liquids
- G01N2035/1025—Fluid level sensing
Definitions
- the present invention relates to an evaporative concentration device for evaporating and concentrating a sample liquid as a pre-measurement treatment of the analyzer.
- Patent Document 1 describes a storage rate detector that detects the storage rate of the condensed liquid generated from the gas drawn from the evaporation can, and a radioactive waste liquid so that the storage rate becomes a predetermined value.
- a solidifying device for a radioactive liquid liquid having a heating control device for controlling the heating of the radioactive liquid waste liquid is disclosed.
- an analyzer is required to analyze a small amount of a sample composed of various kinds of sample components and solvent compositions accurately in a short time.
- the evaporation rate varies depending on the solvent composition, ambient temperature, exhaust conditions, etc., and if the evaporation rate is too slow, the concentration of the component to be analyzed cannot be sufficiently increased within a predetermined time. Further, if the evaporation rate is too fast and the sample liquid is excessively concentrated, the amount of sample liquid required for analysis cannot be secured, and additional treatment such as adding a solvent and re-diluting is required.
- the present invention is configured as follows.
- the temperature of the container for accommodating the sample liquid, the heating unit for heating the container, the liquid level sensor for detecting the liquid level height of the sample liquid contained in the container, and the temperature of the heating unit are controlled.
- the control unit controls the temperature of the heating unit based on the liquid level of the sample liquid detected by the liquid level sensor.
- a small amount of sample liquid can be accurately evaporated and concentrated in a short time regardless of the composition of the sample liquid and the ambient environmental conditions.
- FIG. It is a schematic diagram which shows the whole structure of the analyzer which concerns on Example 1.
- FIG. It is a schematic diagram which shows the structure of the evaporation concentration mechanism of Example 1.
- It is a flowchart which shows the evaporation concentration procedure of Example 1.
- It is a graph which shows the transition of the liquid level at the time of carrying out the evaporation concentration procedure of Example 1.
- the analyzer 100 has a pretreatment unit 101 and an analysis unit 102, and the pretreatment unit 101 includes an evaporation concentration mechanism 103.
- the operator installs the sample container 1 containing the sample liquid containing the component to be analyzed in the pretreatment section 101, and the pretreatment section 101 performs analysis pretreatment such as adjustment and purification.
- the evaporation concentration mechanism 103 evaporates the solvent in the sample liquid to increase the concentration of the component to be analyzed.
- the sample liquid for which the pretreatment has been completed is automatically or manually supplied to the analysis unit 102, and when the analysis is completed, the analysis result is output from the analysis unit 102.
- the evaporative concentration mechanism 103 includes a sample container 1 for accommodating the sample liquid and a container holding portion 2, and by heating these with the heating means 3, the solvent in the sample liquid is evaporated and the sample liquid is concentrated.
- the heating means 3 is a heat generating element capable of controlling the amount of heat generated, and examples thereof include a heater and a Pelche element.
- the control unit 5 measures the temperature of the container holding unit by a temperature sensor 4 attached to the container holding unit 2, and controls the heating means 3 so that this coincides with a predetermined heating temperature Th.
- a liquid level sensor 6 having detection positions at two points, an upper detection point hu and a lower detection point hd.
- An example of a liquid level sensor is a photodiode.
- the liquid level sensor 6 detects transmitted light emitted from the opposite light source 7 and passing through the light source side slit 8, the sample container 1, and the liquid level sensor side slit 9.
- the material of the sample container 1 is light transmissive, and the transmitted light intensity changes depending on the presence or absence of the sample liquid on the optical path. From this change, the control unit 5 detects that the sample liquid level has passed the upper detection point hu or the lower detection point hd.
- liquid level detecting means is an optical sensor in this embodiment, the same effect can be realized by substituting the liquid level detecting means such as an ultrasonic sensor or a weight sensor. These alternative means do not require a slit and simplify the structure of the container holding portion 2. Further, a material having no light transmission can be used for the sample container 1.
- the exhaust means 10 may be provided in order to increase the evaporation efficiency.
- An example of an exhaust means is a vacuum pump.
- the evaporative gas is discharged to the outside by the exhaust means 10 through the exhaust pipe 11.
- the control unit 5 controls the exhaust by switching the opening and closing of the exhaust valve 12 on the exhaust pipe 11.
- FIG. 3 is a flowchart showing the procedure for evaporation and concentration
- FIGS. 4A and 4B are graphs showing changes in the liquid level and the temperature of the container holding portion during evaporation and concentration.
- the operator sets the heating temperature Th and the target liquid level he in the control unit 5 as evaporation concentration conditions (S101). These parameters are determined in consideration of the boiling point of the solvent species, the heat denaturation temperature of the component to be analyzed, the target evaporation rate, the target concentration rate, and the like.
- the sample container 1 containing the sample liquid is installed in the container holding unit 2 (S102), and the control unit 5 is instructed to start evaporation concentration (S103).
- the control unit 5 starts heating by the heating means 3, opens the exhaust valve 12, and starts evaporation concentration.
- the liquid level drops and passes through the upper detection point hu and the lower detection point hd in sequence (S104, S105).
- the control unit 5 obtains the evaporation rate from the time when the liquid level passes each detection point, and calculates the expected time te to reach the target liquid level he (S106). At time te, the control unit 5 stops heating, closes the exhaust valve 12, and ends evaporation concentration (S107).
- FIG. 5 is a schematic view showing the configuration of the evaporation concentration mechanism 103 according to the second embodiment.
- the overall configuration of the analyzer 100 in the second embodiment is the same as that of the first embodiment, the illustration and description will be omitted. Further, the configuration of the evaporation concentration mechanism 103 is the same as that of the first embodiment, and the same reference numerals in FIGS. 2 and 5 indicate the same parts, and thus the description thereof will be omitted again.
- the difference from the first embodiment is that the liquid level sensor 6, the light source 7, the light source side slit 8, and the liquid level sensor side slit 9 have a width in the height direction, and the transmitted light intensity pattern can be measured in this range.
- An example of such a liquid level sensor 6 is a CCD image sensor.
- the control unit 5 can continuously measure the sample liquid level and perform more precise control than in the first embodiment.
- FIG. 6 is a flowchart showing the procedure for evaporation and concentration
- FIGS. 7A and 7B are graphs showing changes in the liquid level and the temperature of the container holding portion during evaporation and concentration.
- Example 2 The basic procedure of Example 2 is the same as that of Example 1, but as shown in the liquid level graph of FIG. 7A, first evaporating and concentrating at the rapid evaporation rate vf until the liquid level is close to the target (hsd). When it goes down, it switches to the slow evaporation rate vsd. Further, as shown in the container holding portion temperature graph of FIG. 7B, the heating temperature Th is adjusted within the range of the heating temperature upper limit Thorium and the environmental temperature ta, and feedback control is performed so that the evaporation rate matches the target value (vf or vsd). I do.
- the operator sets the heating temperature upper limit Tlim, the rapid evaporation rate vf, the low-speed evaporation rate vsd, the deceleration liquid level hsd, and the target liquid level he as the evaporation concentration conditions in the control unit 5 (S201). Similar to Example 1, these parameters are determined in consideration of the boiling point of the solvent species, the heat denaturation temperature of the component to be analyzed, the target evaporation rate, the target concentration rate, and the like.
- the sample container 1 containing the sample liquid is installed in the container holding unit 2 (S202), and the control unit 5 is instructed to start evaporation concentration (S203).
- control unit 5 starts heating by the heating means 3 with the evaporation rate target value as vf, opens the exhaust valve 12, and starts evaporation concentration (S204).
- the evaporation rate target value is switched to vsd (S205).
- the heating means 3 is stopped, the exhaust valve 12 is closed, and evaporation concentration is completed (S206).
- Example 2 the same method is effective in Example 2 as a countermeasure when the sample container 1 shown in Example 1 has a non-constant cross-sectional area and a countermeasure for an evaporation amount error due to a cooling delay after the completion of evaporation concentration.
- the second embodiment of the present invention has the following advantages in addition to obtaining the same effects as those of the first embodiment. -By switching the evaporation rate, it is possible to achieve both high-speed evaporation and concentration and precise control of the amount of evaporation near the target liquid level. -Since the evaporation rate is continuously controlled by feedback control, it is not easily affected by changes in conditions during evaporation and concentration (changes in ambient temperature and exhaust conditions, changes in solvent composition when a mixed solvent is used).
- the evaporation concentration mechanism is shown as a part of the pretreatment unit for the sake of explanation, but the evaporation concentration mechanism according to the present invention may be incorporated into a sample pretreatment device independent of the analyzer. However, it may be mounted as an evaporation concentrator independent of the pretreatment section.
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Abstract
Description
まず、図1および図2を用いて、実施例1の構成を説明する。
・試料容器1と排気バルブ12間の排気配管11内の容積を極力小さくする。
・試料液を冷却する図示しない冷却手段13をさらに備え、蒸発濃縮終了直後に試料液を速やかに冷却する。加熱手段3をペルチェ素子とすれば、冷却手段13を兼ねることができる。
(実施例2)
つづいて、図5を用いて実施例2の構成を説明する。
・蒸発速度を切り替えることにより、蒸発濃縮の高速化と目標液位付近での精密な蒸発量制御を両立できる。
・フィードバック制御により連続的に蒸発速度を制御するため、蒸発濃縮中の条件変化(周囲温度や排気条件の変化、混合溶媒使用時の溶媒組成変化)の影響を受けにくい。
Claims (15)
- 試料液を収容する容器と、
前記容器を加熱する加熱部と、
前記容器に収容された試料液の液面高さを検知する液位センサと、
前記加熱部の温度を制御する制御部と、を備え、
前記制御部が、前記液面センサにより検知した前記試料液の液位に基づいて、前記加熱部の温度を制御する蒸発濃縮機構。 - 請求項1に記載の蒸発濃縮機構であって、
前記制御部が、前記容器に収容された前記試料液の液位が所定の高さまで減衰したことを検知した時、前記加熱部による加熱を停止することで蒸発量を制御する蒸発濃縮機構。 - 請求項1に記載の蒸発濃縮機構であって、
前記制御部が、前記容器に収容された前記試料液の液位変化速度から、前記試料液の液位が所定の高さまで減衰するのにかかる時間を予測し、この時間が経過した時に、前記加熱部による加熱を停止することで蒸発量を制御する蒸発濃縮機構。 - 請求項1に記載の蒸発濃縮機構であって、
前記制御部が、前記容器に収容された前記試料液の蒸発速度が所定の値になるように、前記加熱部の温度を制御する蒸発濃縮機構。 - 請求項1に記載の蒸発濃縮機構であって、
前記制御部が、前記試料液に含まれる分析対象成分または溶媒の特性に応じて、前記加熱部の温度を制御する蒸発濃縮機構。 - 請求項1に記載の蒸発濃縮機構であって、
蒸発した気体を排気する排気部をさらに備え、前記制御部が、前記液位センサにより検知した前記試料液の液位に基づいて、前記排気部の排気量を制御する蒸発濃縮機構。 - 請求項1に記載の蒸発濃縮機構であって、
前記試料液を冷却する冷却部をさらに備え、前記制御部が、前記液位センサにより検知した前記試料液の液位に基づいて、前記冷却部の温度を制御する蒸発濃縮機構。 - 請求項1乃至7のいずれか一項に記載の蒸発濃縮機構を備えた分析装置。
- 試料液を収容する容器と、
前記容器を加熱する加熱部と、
前記容器に収容された試料液の液面高さを検知する液位センサと、
を備えた蒸発濃縮機構の制御方法であって、
前記液面センサにより検知した前記試料液の液位に基づいて、前記加熱部の温度を制御する蒸発濃縮機構の制御方法。 - 請求項9に記載の蒸発濃縮機構の制御方法であって、
前記容器に収容された前記試料液の液位が所定の高さまで減衰したことを検知した時、前記加熱部による加熱を停止することで蒸発量を制御する蒸発濃縮機構の制御方法。 - 請求項9に記載の蒸発濃縮機構の制御方法であって、
前記容器に収容された前記試料液の液位変化速度から、前記試料液の液位が所定の高さまで減衰するのにかかる時間を予測し、この時間が経過した時に、前記加熱部による加熱を停止することで蒸発量を制御する蒸発濃縮機構の制御方法。 - 請求項9に記載の蒸発濃縮機構の制御方法であって、
前記容器に収容された前記試料液の蒸発速度が所定の値になるように、前記加熱部の温度を制御する蒸発濃縮機構の制御方法。 - 請求項9に記載の蒸発濃縮機構の制御方法であって、
前記試料液に含まれる分析対象成分または溶媒の特性に応じて、前記加熱部の温度を制御する蒸発濃縮機構の制御方法。 - 請求項9に記載の蒸発濃縮機構の制御方法であって、
蒸発した気体を排気する排気部をさらに備え、前記液位センサにより検知した前記試料液の液位に基づいて、前記排気部の排気量を制御する蒸発濃縮機構の制御方法。 - 請求項9に記載の蒸発濃縮機構の制御方法であって、
前記試料液を冷却する冷却部をさらに備え、前記液位センサにより検知した前記試料液の液位に基づいて、前記冷却部の温度を制御する蒸発濃縮機構の制御方法。
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CN202180076683.7A CN116547517A (zh) | 2020-12-07 | 2021-12-06 | 蒸发浓缩机构、具备该蒸发浓缩机构的分析装置以及蒸发浓缩机构的控制方法 |
EP21903361.0A EP4257949A1 (en) | 2020-12-07 | 2021-12-06 | Evaporative concentration mechanism, analysis device provided with same, and control method for evaporative concentration mechanism |
US18/036,920 US20240019347A1 (en) | 2020-12-07 | 2021-12-06 | Evaporative concentration mechanism, analyzer including the same, and method of controlling evaporative concentration mechanism |
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- 2021-12-06 US US18/036,920 patent/US20240019347A1/en active Pending
- 2021-12-06 CN CN202180076683.7A patent/CN116547517A/zh active Pending
- 2021-12-06 WO PCT/JP2021/044695 patent/WO2022124260A1/ja active Application Filing
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JP2001305031A (ja) * | 2000-04-20 | 2001-10-31 | Japan Organo Co Ltd | 加熱濃縮装置 |
JP2008203170A (ja) * | 2007-02-22 | 2008-09-04 | Jasco Corp | 旋光度測定方法及びその装置 |
JP2008246369A (ja) * | 2007-03-30 | 2008-10-16 | Daisho Seiki Kk | 液体濃縮装置 |
JP2012181092A (ja) * | 2011-03-01 | 2012-09-20 | Taiyo Nippon Sanso Corp | 加熱濃縮装置、及び加熱濃縮方法 |
CN203618746U (zh) * | 2013-12-24 | 2014-06-04 | 云南乍甸乳业有限责任公司 | 一种具有状态监视控制功能的食品浆料浓缩装置 |
WO2020017070A1 (ja) * | 2018-07-18 | 2020-01-23 | リファインホールディングス株式会社 | 溶液処理装置および溶液処理方法 |
CN210448119U (zh) * | 2019-08-15 | 2020-05-05 | 中触媒新材料股份有限公司 | 一种季铵碱水溶液连续浓缩装置 |
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JP7456004B2 (ja) | 2024-03-26 |
EP4257949A1 (en) | 2023-10-11 |
US20240019347A1 (en) | 2024-01-18 |
CN116547517A (zh) | 2023-08-04 |
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