CN115219606A - Automatic water sample pretreatment device, treatment method and automatic water sample detection system - Google Patents
Automatic water sample pretreatment device, treatment method and automatic water sample detection system Download PDFInfo
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- 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
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
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- G01N30/08—Preparation using an enricher
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- G—PHYSICS
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- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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- G01N30/14—Preparation by elimination of some components
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- G—PHYSICS
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
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- G—PHYSICS
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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Abstract
The invention discloses an automatic water sample pretreatment device, a treatment method and an automatic water sample detection system. The automatic water sample pretreatment device comprises a rack, and a solid phase micro-extraction mechanism, a liquid sample introduction mechanism, a nitrogen blowing mechanism, a liner tube grabbing mechanism, a solvent supply mechanism, a vortex mixing mechanism, an automatic liner tube replacing mechanism, an incubation mechanism, an aging mechanism and a multi-azimuth movement mechanism which are arranged on the rack; the solid-phase micro-extraction mechanism is provided with a solid-phase micro-extraction head for adsorbing organic matters in the sample; the liquid sample injection mechanism is provided with a liquid sample injection needle for sucking and adding a liquid sample. The automatic pretreatment device for the water sample can automatically complete two pretreatment modes of headspace solid-phase microextraction and liquid-liquid extraction of the water sample, the treated water sample can be automatically injected into a chromatograph for detection and analysis, and the automatic pretreatment device is simple to operate, high in detection efficiency and friendly to the health of operators and the environment.
Description
Technical Field
The invention relates to the field of detection, in particular to an automatic water sample pretreatment device, a treatment method and an automatic water sample detection system.
Background
With the rapid development of industry, a large amount of various organic pollutants are discharged into the water environment along with the activities of human beings, and the organic pollutants have the characteristics of various types, low content, complex composition and great harm, thereby seriously threatening the safety of water resources. In order to understand the water pollution condition, the composition of organic matters in water needs to be detected by various technical means, so that the source of pollutants in the water environment is traced, and the source of the pollution source is controlled, so that the water quality condition of a target water body is improved.
The organic matters in the water body can be divided into volatile organic matters (VOCs), semi-volatile organic matters (SVOCs) and non-volatile organic matters according to physical properties. Wherein the volatile organic compounds are compounds with boiling point below 170 ℃, mainly comprising halogenated hydrocarbon, benzene series compounds and the like; the boiling point of the semi-volatile and nonvolatile organic compounds is above 170 ℃, and the main compounds comprise polycyclic aromatic hydrocarbon, organic pesticide, chlorobenzene, nitrobenzene, aniline and the like.
Volatile organic compounds in water are often detected and analyzed by a gas chromatograph after a target compound is extracted from water by a Headspace (HS) sampling method. The semi-volatile organic compounds and the non-volatile organic compounds are generally detected and analyzed by a gas chromatograph after extracting the target compounds from a water sample by a liquid-liquid extraction method. The two detection and analysis methods have the following defects: 1) Organic pollutants in water are usually mixed and polluted by organic matters of various different types, and in order to comprehensively know the source of the water pollutants, a headspace gas chromatography method and a liquid-liquid extraction gas chromatography method are generally combined for use, but in the prior art, two pretreatment modes of headspace sampling and liquid-liquid extraction can only be respectively and independently processed and then analyzed by a gas chromatograph, and equipment of various different types is required to be used. 2) In addition, headspace sampling generally only can extract part of gas (usually 1 mL) at the top of a headspace bottle to be injected into a chromatograph for analysis, and the sample utilization rate is low, so that part of trace components are difficult to detect. 3) The organic matter content in water is relatively low, a large amount of water samples (more than 250 mL) and dozens to hundreds of milliliters of organic solvents are required to be used for extraction in a separating funnel in a conventional liquid-liquid extraction method, then, an extracted organic phase is dried by anhydrous sodium sulfate and then concentrated and enriched by a rotary evaporator or a nitrogen blowing instrument to meet the requirement of detection sensitivity, and more samples and organic solvents are consumed in the whole process. In addition, the detection and analysis method in the prior art can only realize semi-automatic liquid-liquid extraction by using a manual mode or an extraction instrument, and the detection and analysis method needs to be manually transferred to a chromatograph for sample detection and analysis after the treatment is finished, so that the operation is complex, time-consuming and labor-consuming. In addition, a large amount of harmful organic solvent is needed in the whole liquid-liquid extraction process, and the prior art needs more manual operations, so that certain harm is caused to the health of operators and the environment.
Disclosure of Invention
In view of the above, it is necessary to provide an automatic water sample pretreatment apparatus, a treatment method, and an automatic water sample detection system. The automatic pretreatment device for the water sample can automatically complete two pretreatment modes of headspace solid-phase microextraction and liquid-liquid extraction of the water sample, the treated water sample can be automatically injected into a chromatograph for detection and analysis, and the automatic pretreatment device is simple to operate, high in detection efficiency and friendly to the health of operators and the environment.
An automatic water sample pretreatment device comprises a rack, and a solid phase micro-extraction mechanism, a liquid sample introduction mechanism, a nitrogen blowing mechanism, a liner tube grabbing mechanism, a solvent supply mechanism, a vortex mixing mechanism, an incubation mechanism, an aging mechanism and a multi-azimuth movement mechanism which are arranged on the rack; the solid-phase micro-extraction mechanism is provided with a solid-phase micro-extraction head for adsorbing organic matters in the sample; the liquid sample injection mechanism is provided with a liquid sample injection needle for sucking and adding a liquid sample; the nitrogen blowing mechanism is used for nitrogen blowing concentration of the sample; the liner gripping mechanism is used for gripping and moving the liner; the solvent supply mechanism is used for providing an extraction solvent; the vortex mixing mechanism is used for vortex mixing of samples; the hatching mechanism is used for hatching the sample; the aging mechanism is used for aging the solid phase micro-extraction head; the multi-azimuth movement mechanism can automatically acquire the solid phase micro-extraction mechanism, the liquid sampling mechanism, the nitrogen blowing mechanism or the liner tube grabbing mechanism and drive the liner tube grabbing mechanism to move.
In one embodiment, the automatic water sample pretreatment device further comprises a tool support, the tool support is arranged on a rack, and the liquid sampling mechanism, the nitrogen blowing mechanism and the liner tube grabbing mechanism are mounted on the tool support.
In one embodiment, the automatic water sample pretreatment device further comprises a liner rack for placing a liner.
In one embodiment, the automatic pretreatment device for the water sample further comprises a sample rack, wherein a plurality of placing positions for placing sample bottles are arranged on the sample rack, and each placing position is marked with a position serial number.
In one embodiment, the incubation mechanism comprises one or more of a heating component, an oscillating component, and an ultrasound component.
The utility model provides a water sample automated inspection system, include the chromatograph and the automatic preceding processing apparatus of water sample, the automatic preceding processing apparatus of water sample can with the introduction port cooperation of chromatograph, arrange the sample in nitrogen in the bushing pipe after the automatic preceding processing apparatus of water sample handles the sample and blow the concentration, again by the bushing pipe snatchs the mechanism and snatchs the bushing pipe and put into analytic introduction in the introduction port of chromatograph.
In one embodiment, the chromatograph includes, but is not limited to, a gas chromatograph-mass spectrometer, a gas chromatograph-triple quadrupole mass spectrometer, and an all two-dimensional gas chromatograph-time-of-flight mass spectrometer.
A water sample automatic pretreatment method using the water sample automatic pretreatment device comprises the following steps:
when the automatic headspace solid phase microextraction mode is carried out, the method comprises the following steps:
s1: adding a predetermined amount of water sample to be analyzed into the sample bottle;
s2: controlling a multi-directional movement mechanism to obtain a solid-phase micro-extraction mechanism, controlling the multi-directional movement mechanism to drive the solid-phase micro-extraction mechanism to move sample bottles to an incubation mechanism, and incubating the sample bottles in the incubation mechanism according to preset incubation conditions to volatilize volatile organic compounds in water sample water to be analyzed;
s3: controlling a multi-directional movement mechanism to drive a solid-phase micro-extraction mechanism to move to an aging mechanism, and placing an extraction head on the solid-phase micro-extraction mechanism into the aging mechanism for aging treatment to remove residual volatile organic compounds;
s4: after the sample incubation is finished, controlling a multi-azimuth motion mechanism to drive a solid phase micro-extraction mechanism to move to an incubation mechanism, placing an extraction head on the solid phase micro-extraction mechanism into a sample bottle, and extracting volatile organic compounds at the top in the sample bottle under a preset extraction condition;
s5: after extraction is finished, controlling the multi-azimuth motion mechanism to drive the solid phase micro-extraction mechanism to move to a chromatographic sample inlet of a chromatograph, and placing an extraction head into the chromatographic sample inlet to perform sample analysis so as to perform detection and analysis by the chromatograph;
when the automatic liquid-liquid extraction mode is carried out, the method comprises the following steps:
s1: adding a predetermined amount of water sample to be analyzed into the first sample bottle; adding a predetermined amount of desiccant to the second sample vial; taking a first liner tube for standby;
s2: controlling the multi-directional movement mechanism to obtain the liquid sampling mechanism, and controlling the multi-directional movement mechanism to drive the liquid sampling mechanism to move into the solvent supply mechanism to extract a predetermined amount of extraction solvent and inject the extraction solvent into the first sample bottle;
s3: controlling a multi-directional movement mechanism to drive a liquid sampling mechanism to move a first sample bottle to move into a vortex oscillation mechanism for vortex mixing, and standing for a preset time to extract organic matters in a water sample to be analyzed;
s4: controlling a multi-directional movement mechanism to drive a liquid sampling mechanism to absorb the supernatant liquid after layering in the first sample bottle and transfer the supernatant liquid into a second sample bottle, and controlling the multi-directional movement mechanism to drive the liquid sampling mechanism to move the second sample bottle into a vortex oscillation mechanism for vortex mixing so as to dry and remove water;
s5: controlling the multi-directional movement mechanism to drive the liquid sampling mechanism to extract a predetermined amount of liquid in the second sample bottle and add the liquid into the first liner tube;
s6: controlling the multi-directional movement mechanism to release the liquid sampling mechanism and obtain the nitrogen blowing mechanism, controlling the multi-directional movement mechanism to drive the nitrogen blowing mechanism to move into the first liner tube and blowing nitrogen to the liquid in the first liner tube to remove the solvent, and realizing concentration and enrichment of the sample;
s7: and controlling the multidirectional movement mechanism to release the nitrogen blowing mechanism and obtain the liner tube grabbing mechanism, controlling the multidirectional movement mechanism to drive the liner tube grabbing mechanism to move to the chromatographic sample inlet of the chromatograph, and controlling the multidirectional movement mechanism to drive the liner tube grabbing mechanism to move the first liner tube to the chromatographic sample inlet so as to carry out detection and analysis on the chromatograph.
In one embodiment, the first liner is prepared for loading with a predetermined amount of filler material, which may comprise glass wool or an adsorbent.
In one embodiment, when the automatic headspace solid phase microextraction mode is performed, a predetermined amount of sodium chloride is simultaneously added when a predetermined amount of water sample to be analyzed is added into the sample bottle;
and/or, when the automatic liquid-liquid extraction mode is carried out, adding a predetermined amount of demulsifier into the first sample bottle when a predetermined amount of water sample to be analyzed is added.
In one embodiment, the automatic top-air solid-phase micro-extraction mode and the automatic liquid-liquid extraction mode are controlled to be automatically switched to automatically perform different pretreatment modes on a water sample to realize the detection of different types of targets, and the automatic switching process comprises the following steps:
saving the step of performing the automatic headspace solid-phase microextraction mode as a first method file, and saving the automatic liquid-liquid extraction mode as a second method file;
and setting an operation sequence table in the automatic water sample pretreatment device, filling the operation sequence table with the position serial numbers of the sample racks of the sample bottles and the first method files or the second method files corresponding to the sample bottles, and sequentially loading the first method files or the second method files corresponding to the samples by the automatic water sample pretreatment device according to the operation sequence table to treat the samples in the sample bottles at the corresponding positions.
The automatic pretreatment device for the water sample can automatically complete two pretreatment modes of headspace solid-phase microextraction and liquid-liquid extraction of the water sample, the treated water sample can be automatically injected into a chromatograph for detection and analysis, and the device is simple to operate, high in detection efficiency, healthy for operators and environment-friendly.
Compared with the traditional pretreatment method, the automatic pretreatment device for the water sample has the following beneficial effects:
(1) Compared with the traditional water sample liquid-liquid extraction mode, hundreds of milliliters of samples and dozens of milliliters of organic solvents are usually consumed, but the invention only needs to use about ten milliliters of samples and dozens of milliliters of organic solvents for sample extraction, thereby obviously reducing the sample loading amount and the solvent consumption amount.
(2) Compared with the conventional method that after liquid-liquid extraction is finished, the extraction solvent is transferred into a flask, the sample is concentrated and enriched to about 200 mu L by using a nitrogen blowing or rotary evaporation mode, and then 1 mu L of the sample is injected into a chromatograph for analysis by using a micro-injector, so that the sample utilization rate is low; the invention carries out nitrogen blowing concentration in the liner tube, and all the concentrated samples are injected into a chromatograph for analysis, thereby effectively improving the utilization rate of the samples.
(3) The liquid-liquid extraction can be automatically carried out, so that the manual participation is reduced, the accuracy is improved, and meanwhile, the artificial pollution caused in the operation process is reduced.
(4) The invention combines automatic liquid-liquid extraction and solid-phase microextraction, and the two modes can be automatically switched, thereby realizing full-automatic pretreatment of different types of organic matters in a water sample to be analyzed.
(5) The invention can realize that the pretreated sample is automatically injected into the chromatograph for analysis and realize the full-automatic detection of the organic matters in the water.
(6) The automatic water sample pretreatment device has wide application range, and the device used for sample detection is a chromatograph, including but not limited to the following types: gas Chromatograph (GC), gas chromatograph-mass spectrometer (GCMS), gas chromatograph-triple quadrupole mass spectrometer (GC-MSMS), and two-dimensional gas chromatograph-time of flight mass spectrometer (GC × GC-TOFMS).
(7) The automatic water sample pretreatment device has wide applicable treatment objects, including but not limited to surface water, underground water, drinking water and seawater.
Drawings
Fig. 1 is a schematic view of an automatic preprocessing apparatus according to an embodiment of the present invention.
Description of the reference numerals
10. An automatic pre-treatment device; 100. a frame; 200. a solid phase micro-extraction mechanism; 300. a liquid sample introduction mechanism; 400. a nitrogen blowing mechanism; 500. a tool holder; 600. a solvent supply mechanism; 700. a vortex mixing mechanism; 800. a hatching mechanism; 900. an aging mechanism; 1000. a multi-directional movement mechanism; 1100. a sample holder; 1200. a liner support.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, as those skilled in the art will recognize without departing from the spirit and scope of the present invention.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of the feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "above," and "over" a second feature may be directly on or obliquely above the second feature, or simply mean that the first feature is at a higher level than the second feature. A first feature "under," "beneath," and "under" a second feature may be directly under or obliquely under the second feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. As used herein, the terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like are for purposes of illustration only and do not denote a single embodiment.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, an embodiment of the invention provides an automatic water sample pretreatment apparatus 10.
An automatic water sample pretreatment device 10 comprises a rack 100, and a solid phase micro-extraction mechanism 200, a liquid sample introduction mechanism 300, a nitrogen blowing mechanism 400, a liner tube grabbing mechanism, a solvent supply mechanism 600, a vortex mixing mechanism 700, an incubation mechanism 800, an aging mechanism 900 and a multi-azimuth movement mechanism 1000 which are arranged on the rack 100.
The solid-phase micro-extraction mechanism 200 has a solid-phase micro-extraction head for adsorbing organic matter in a sample.
The liquid sample injection mechanism 300 has a liquid sample injection needle for sucking and adding a liquid sample.
The nitrogen blowing mechanism 400 is used for nitrogen-blowing concentration of the sample.
The liner gripping mechanism is used to grip and move the liner. The liner gripping mechanism is not shown in the drawings. The liner gripping mechanism may be a motorized gripper.
The solvent supply mechanism 600 is used to supply an extraction solvent.
The vortex mixing mechanism 700 is used for vortex mixing of the sample.
The incubation mechanism 800 is used to incubate the sample.
The aging mechanism 900 is used for aging the solid phase micro-extraction head.
Referring to fig. 1, the multi-directional movement mechanism 1000 can automatically capture and drive the solid phase micro-extraction mechanism 200, the liquid sample injection mechanism 300, the nitrogen blowing mechanism 400, or the liner tube grasping mechanism to move. The multi-directional movement mechanism 1000 can move along the X, Y, Z directions.
Preferably, in one embodiment, the multi-directional movement mechanism 1000 may be a robotic arm.
In one embodiment, referring to fig. 1, the automatic water sample pretreatment device 10 further comprises a tool holder 500. The tool holder 500 is disposed on the rack 100, and the liquid sampling mechanism 300, the nitrogen blowing mechanism 400, and the liner grasping mechanism are mounted on the tool holder 500. The tool holder 500 is provided with three stations for placing the liquid sampling mechanism 300, the nitrogen blowing mechanism 400 and the liner tube grabbing mechanism respectively.
The liquid sampling mechanism 300, the nitrogen blowing mechanism 400 and the liner tube grabbing mechanism can be respectively and independently arranged, one or more of the liquid sampling mechanism, the nitrogen blowing mechanism and the liner tube grabbing mechanism can be integrated into a whole, and the integrated mode is set, namely, one mechanism can simultaneously display the sampling, nitrogen blowing and grabbing functions.
In one embodiment, referring to fig. 1, the automatic water sample pretreatment apparatus 10 further comprises a liner frame 1200. The liner frame 1200 is mounted to the frame 100. Liner holder 1200 is used to place liners.
In one embodiment, referring to fig. 1, the automatic water sample pretreatment device 10 further includes a sample rack 1100. The sample holder 1100 is mounted on the rack 100. The sample rack 1100 is provided with a plurality of placing positions for placing sample bottles, and each placing position is marked with a position serial number.
In one particular example, the incubation mechanism 800 includes one or more of a heating component, an oscillating component, and an ultrasonic component. For example, in one embodiment, the incubation mechanism 800 includes a heating component, in another embodiment, the incubation mechanism 800 includes an oscillating component, and in another embodiment, the incubation mechanism 800 includes an ultrasonic component. Further, the incubation mechanism 800 may also include a heating component, an oscillating component, and an ultrasonic component.
In one embodiment, the liquid sampling mechanism 300, the nitrogen blowing mechanism 400 and the liner grasping mechanism of the automatic water sample pretreatment device 10 can be made into a two-in-one or three-in-one tool.
In one particular example, the solid phase microextraction mechanism 200 can be replaced with a headspace sampling tool, a dynamic headspace sampling tool.
The automatic pretreatment device 10 for the water sample can automatically complete two pretreatment modes of headspace solid-phase microextraction and liquid-liquid extraction of the water sample, the treated water sample can be automatically injected into a chromatograph for detection and analysis, the operation is simple, the detection efficiency is high, and the device is healthy for operators and environment-friendly.
The embodiment of the invention also provides an automatic water sample detection system.
The utility model provides a water sample automated inspection system, includes chromatograph and foretell water sample automatic pretreatment device 10, water sample automatic pretreatment device 10 can with the introduction port cooperation of chromatograph, arrange the sample in nitrogen blow concentration in the bushing pipe after water sample automatic pretreatment device 10 handles the sample, snatch the mechanism by the bushing pipe again and snatch the analytic introduction in the introduction port that the bushing pipe put into the chromatograph.
In one specific example, chromatographs include, but are not limited to, gas Chromatographs (GCs), gas chromatographs-mass spectrometers (GCMS), gas chromatographs-triple quadrupole mass spectrometers (GC-MSMS), and two-dimensional gas chromatographs-time-of-flight mass spectrometers (GC x GC-TOFMS).
The embodiment of the invention also provides an automatic pretreatment method of the water sample.
The automatic water sample pretreatment method using the automatic water sample pretreatment device comprises the following steps:
when the automatic headspace solid phase microextraction mode is carried out, the method comprises the following steps:
s1: referring to fig. 1, a predetermined amount of water sample to be analyzed is added to a sample bottle, and the sample bottle is placed on a sample holder 1100 after a bottle cap is tightened.
S2: and controlling the multidirectional movement mechanism 1000 to obtain the solid-phase micro-extraction mechanism 200, controlling the multidirectional movement mechanism 1000 to drive the solid-phase micro-extraction mechanism 200 to move the sample bottles to the incubation mechanism 800, and incubating the sample bottles in the incubation mechanism 800 according to a preset incubation condition to volatilize volatile organic compounds in the water sample water to be analyzed.
S3: and controlling the multi-azimuth movement mechanism 1000 to drive the solid phase micro-extraction mechanism 200 to move to the aging mechanism 900, and placing the extraction head on the solid phase micro-extraction mechanism 200 into the aging mechanism 900 for aging treatment to remove residual volatile organic compounds.
S4: after the sample incubation is completed, the multi-directional movement mechanism 1000 is controlled to drive the solid phase micro-extraction mechanism 200 to move to the incubation mechanism 800, an extraction head on the solid phase micro-extraction mechanism 200 is placed into a sample bottle, and volatile organic compounds at the top in the sample bottle are extracted under the preset extraction condition.
S5: after extraction is completed, the multi-azimuth movement mechanism 1000 is controlled to drive the solid phase micro-extraction mechanism 200 to move to the chromatographic sample inlet of the chromatograph, and the extraction head is placed in the chromatographic sample inlet to perform sample analysis so as to perform detection and analysis by the chromatograph.
When the automatic liquid-liquid extraction mode is carried out, the method comprises the following steps:
s1: referring to fig. 1, a predetermined amount of water sample to be analyzed is added to a first sample bottle on a sample bottle rack, and a bottle cap is screwed; adding a predetermined amount of drying agent into a second sample bottle on the sample bottle rack, and screwing down the bottle cap; placing a first liner tube on the liner tube frame 1200 for later use; the desiccant can be anhydrous sodium sulfate, but it is understood that the desiccant can also be other substances, such as calcium oxide, calcium sulfate, potassium carbonate, anhydrous copper sulfate, potassium hydroxide, and the like.
s2: and controlling the multi-directional movement mechanism 1000 to acquire the liquid sampling mechanism 300, and controlling the multi-directional movement mechanism 1000 to drive the liquid sampling mechanism 300 to move into the solvent supply mechanism 600 to extract a predetermined amount of the extraction solvent and inject the extraction solvent into the first sample bottle.
s3: and controlling the multi-azimuth movement mechanism 1000 to drive the liquid sampling mechanism 300 to move the first sample bottle to move into the vortex oscillation mechanism for vortex mixing, and standing for a preset time to extract organic matters in the water sample to be analyzed.
s4: and controlling the multi-azimuth movement mechanism 1000 to drive the liquid sampling mechanism 300 to absorb the supernatant liquid after layering in the first sample bottle and transfer the supernatant liquid to the second sample bottle, and controlling the multi-azimuth movement mechanism 1000 to drive the liquid sampling mechanism 300 to move the second sample bottle to the vortex oscillation mechanism for vortex mixing so as to dry and remove water.
s5: the multi-azimuth movement mechanism 1000 is controlled to drive the liquid sampling mechanism 300 to extract a predetermined amount of liquid in the second sample bottle and add the liquid into the first liner.
s6: and controlling the multi-azimuth movement mechanism 1000 to release the liquid sampling mechanism 300 and obtain the nitrogen blowing mechanism 400, and controlling the multi-azimuth movement mechanism 1000 to drive the nitrogen blowing mechanism 400 to move into the first liner and carry out nitrogen blowing on the liquid in the first liner to remove the solvent, thereby realizing the concentration and enrichment of the sample.
s7: and controlling the multi-azimuth movement mechanism 1000 to release the nitrogen blowing mechanism 400 and obtain the liner tube grabbing mechanism, and controlling the multi-azimuth movement mechanism 1000 to drive the liner tube grabbing mechanism to grab an empty second liner tube detected in the previous detection procedure from a chromatographic sample inlet of the chromatograph and place the empty second liner tube on the liner tube frame 1000. And controlling the multidirectional movement mechanism 1000 to drive the liner tube grabbing mechanism to move to a chromatographic sample inlet of the chromatograph, and controlling the multidirectional movement mechanism 1000 to drive the liner tube grabbing mechanism to move the first liner tube to the chromatographic sample inlet so as to perform detection and analysis on the chromatograph.
In one specific example, the first liner is ready for use with a predetermined amount of filler material, which may include glass wool or an adsorbent.
In one particular example, when performing the automatic headspace solid phase microextraction mode, a predetermined amount of sodium chloride is also added simultaneously with the addition of a predetermined amount of water sample to be analyzed to the sample vial. In the automatic headspace solid-phase extraction, a certain amount of sodium chloride is added into a sample bottle, the salting-out effect is utilized to be beneficial to the volatilization of organic matters to improve the sensitivity, and other salts can be selected to replace the sodium chloride or not be added.
In one particular example, when performing the automatic liquid-liquid extraction mode, a predetermined amount of a demulsifier, which includes sodium chloride, is also added simultaneously to the addition of a predetermined amount of the water sample to be analyzed to the first sample bottle. During liquid-liquid extraction, a certain amount of sodium chloride is added into the first sample bottle to serve as a demulsifier, so that the organic phase and the water phase can be separated. If the clean water sample to be analyzed is not seriously emulsified, sodium chloride can be not added, or other compounds can be used as a demulsifier, or other methods such as an ultrasonic oscillation method can be used for demulsifying.
In one particular example, when performing an automatic headspace solid phase microextraction mode, the extraction head can be aged using the aging mechanism 900, as well as the chromatography sample inlet.
In one embodiment, the automatic switching between the automatic headspace solid-phase microextraction mode and the automatic liquid-liquid extraction mode is controlled to automatically perform different pretreatment modes on a water sample to realize the detection of different types of targets, and the automatic switching process comprises the following steps:
saving the step of performing the automatic headspace solid-phase microextraction mode as a first method file, and saving the automatic liquid-liquid extraction mode as a second method file;
setting an operation sequence table in the automatic water sample pretreatment device 10, filling the operation sequence table with the position number of the sample rack where each sample bottle is located and the first method file or the second method file corresponding to the sample bottle, and sequentially loading the first method file or the second method file corresponding to each sample by the automatic water sample pretreatment device according to the operation sequence table to treat the samples in the sample bottles at the corresponding positions.
Compared with the traditional pretreatment method, the automatic pretreatment device 10 for the water sample has the following beneficial effects:
(1) Compared with the traditional water sample liquid-liquid extraction mode, hundreds of milliliters of samples and dozens of milliliters of organic solvents are usually consumed, but the invention only needs to use about ten milliliters of samples and dozens of milliliters of organic solvents for sample extraction, thereby obviously reducing the sample loading amount and the solvent consumption amount.
(2) Compared with the conventional method that after liquid-liquid extraction is finished, the extraction solvent is transferred into a flask, the sample is concentrated and enriched to about 200 mu L by using a nitrogen blowing or rotary evaporation mode, and then 1 mu L of the sample is injected into a chromatograph for analysis by using a micro-injector, so that the sample utilization rate is low; the invention carries out nitrogen-blowing concentration in the liner tube, and the concentrated sample is completely injected into the chromatograph for analysis, thereby effectively improving the utilization rate of the sample.
(3) The liquid-liquid extraction can be carried out automatically, so that the manual participation is reduced, the accuracy is improved, and meanwhile, the manual pollution caused in the operation process is reduced.
(4) The invention combines automatic liquid-liquid extraction and solid-phase microextraction, and the two modes can be automatically switched, thereby realizing full-automatic pretreatment of different types of organic matters in a water sample to be analyzed.
(5) The invention can realize that the pretreated sample is automatically injected into the chromatograph for analysis, and realize the full-automatic detection of the organic matters in the water.
(6) The automatic water sample pretreatment device 10 has a wide application range, and the device used for sample detection is a chromatograph, including but not limited to the following types: gas Chromatograph (GC), gas chromatograph-mass spectrometer (GCMS), gas chromatograph-triple quadrupole mass spectrometer (GC-MSMS), and two-dimensional gas chromatograph-time-of-flight mass spectrometer (GC × GC-TOFMS).
(7) The automatic water sample pretreatment apparatus 10 of the present invention is applicable to a wide range of treatment targets including, but not limited to, surface water, ground water, drinking water, and seawater.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (11)
1. An automatic water sample pretreatment device is characterized by comprising a rack, and a solid phase micro-extraction mechanism, a liquid sample introduction mechanism, a nitrogen blowing mechanism, a liner tube grabbing mechanism, a solvent supply mechanism, a vortex mixing mechanism, an incubation mechanism, an aging mechanism and a multi-azimuth movement mechanism which are arranged on the rack; the solid-phase micro-extraction mechanism is provided with a solid-phase micro-extraction head for adsorbing organic matters in a sample; the liquid sampling mechanism is provided with a liquid sampling needle for sucking and adding a liquid sample; the nitrogen blowing mechanism is used for nitrogen blowing concentration of the sample; the liner gripping mechanism is used for gripping and moving the liner; the solvent supply mechanism is used for providing an extraction solvent; the vortex mixing mechanism is used for vortex mixing of samples; the hatching mechanism is used for hatching the sample; the aging mechanism is used for aging the solid phase micro-extraction head; the multi-azimuth movement mechanism can automatically acquire the solid phase micro-extraction mechanism, the liquid sampling mechanism, the nitrogen blowing mechanism or the liner tube grabbing mechanism and drive the liner tube grabbing mechanism to move.
2. The automatic water sample pretreatment device according to claim 1, further comprising a tool holder, wherein the tool holder is disposed on the frame, and the liquid sampling mechanism, the nitrogen blowing mechanism and the liner tube grasping mechanism are mounted on the tool holder.
3. The automatic water sample pretreatment device according to claim 1, further comprising a liner rack for placing a liner.
4. The automatic pretreatment device for the water sample according to claim 1, further comprising a sample rack, wherein the sample rack is provided with a plurality of placing positions for placing sample bottles, and each placing position is marked with a position serial number.
5. The automatic pretreatment device for water samples according to any one of claims 1 to 4, wherein the incubation mechanism comprises one or more of a heating component, an oscillation component and an ultrasonic component.
6. An automatic water sample detection system, which comprises a chromatograph and the automatic water sample pretreatment device of any one of claims 1 to 5, wherein the automatic water sample pretreatment device can be matched with a sample inlet of the chromatograph, the automatic water sample pretreatment device treats a sample and then arranges the sample in a liner tube for nitrogen blowing concentration, and then the liner tube is grabbed by the liner tube grabbing mechanism and placed in the sample inlet of the chromatograph for analytic sample introduction.
7. The automatic water sample detection system of claim 6, wherein the chromatograph includes, but is not limited to, a gas chromatograph-mass spectrometer, a gas chromatograph-triple quadrupole mass spectrometer, and an all-two-dimensional gas chromatograph-time-of-flight mass spectrometer.
8. An automatic water sample pretreatment method using the automatic water sample pretreatment apparatus according to any one of claims 1 to 5, comprising the steps of:
when the automatic headspace solid phase microextraction mode is carried out, the method comprises the following steps:
s1: adding a predetermined amount of water sample to be analyzed into the sample bottle;
s2: controlling a multi-azimuth motion mechanism to obtain a solid phase micro-extraction mechanism, controlling the multi-azimuth motion mechanism to drive the solid phase micro-extraction mechanism to move a sample bottle to an incubation mechanism, and incubating the sample bottle in the incubation mechanism according to a preset incubation condition to volatilize volatile organic compounds in water sample water to be analyzed;
s3: controlling a multi-azimuth motion mechanism to drive a solid phase micro-extraction mechanism to move to an ageing mechanism, and placing an extraction head on the solid phase micro-extraction mechanism into the ageing mechanism for ageing treatment to remove residual volatile organic compounds;
s4: after the sample incubation is finished, controlling a multi-directional movement mechanism to drive a solid-phase micro-extraction mechanism to move to an incubation mechanism, placing an extraction head on the solid-phase micro-extraction mechanism into a sample bottle, and extracting volatile organic compounds at the top in the sample bottle under a preset extraction condition;
s5: after extraction is finished, controlling the multi-azimuth motion mechanism to drive the solid phase micro-extraction mechanism to move to a chromatographic sample inlet of a chromatograph, and placing an extraction head into the chromatographic sample inlet to perform sample analysis so as to perform detection and analysis by the chromatograph;
when the automatic liquid-liquid extraction mode is carried out, the method comprises the following steps:
s1: adding a predetermined amount of water sample to be analyzed into the first sample bottle; adding a predetermined amount of desiccant to the second sample vial; taking a first liner tube for standby;
s2: controlling the multi-directional movement mechanism to obtain the liquid sampling mechanism, and controlling the multi-directional movement mechanism to drive the liquid sampling mechanism to move into the solvent supply mechanism to extract a predetermined amount of extraction solvent and inject the extraction solvent into the first sample bottle;
s3: controlling a multi-directional movement mechanism to drive a liquid sampling mechanism to move a first sample bottle to move into a vortex oscillation mechanism for vortex mixing, and standing for a preset time to extract organic matters in a water sample to be analyzed;
s4: controlling a multi-directional movement mechanism to drive a liquid sampling mechanism to absorb the supernatant liquid after layering in the first sample bottle and transfer the supernatant liquid into a second sample bottle, and controlling the multi-directional movement mechanism to drive the liquid sampling mechanism to move the second sample bottle into a vortex oscillation mechanism for vortex mixing so as to dry and remove water;
s5: controlling the multi-directional movement mechanism to drive the liquid sampling mechanism to extract a predetermined amount of liquid in the second sample bottle and add the liquid into the first liner tube;
s6: controlling the multi-azimuth movement mechanism to release the liquid sampling mechanism and obtain the nitrogen blowing mechanism, controlling the multi-azimuth movement mechanism to drive the nitrogen blowing mechanism to move into the first lining pipe and performing nitrogen blowing on the liquid in the first lining pipe to remove the solvent, and realizing concentration and enrichment of the sample;
s7: and controlling the multidirectional movement mechanism to release the nitrogen blowing mechanism and obtain the liner tube grabbing mechanism, controlling the multidirectional movement mechanism to drive the liner tube grabbing mechanism to move to the chromatographic sample inlet of the chromatograph, and controlling the multidirectional movement mechanism to drive the liner tube grabbing mechanism to move the first liner tube to the chromatographic sample inlet so as to carry out detection and analysis on the chromatograph.
9. The automatic pretreatment method for water samples according to claim 8, wherein a predetermined amount of filler is added into the first spare liner, and the filler comprises glass wool or adsorbent.
10. A method for automatic pre-treatment of water samples according to claim 8 or 9, wherein when the automatic headspace solid phase micro-extraction mode is performed, a predetermined amount of sodium chloride is added simultaneously with a predetermined amount of water sample to be analyzed being added to the sample bottle;
and/or, when the automatic liquid-liquid extraction mode is carried out, adding a predetermined amount of demulsifier into the first sample bottle when a predetermined amount of water sample to be analyzed is added.
11. The automatic water sample pretreatment method according to claim 8 or 9, wherein the automatic switching between the automatic headspace solid-phase microextraction mode and the automatic liquid-liquid extraction mode is controlled to automatically perform pretreatment of water samples in different modes to detect different types of targets, and the automatic switching process comprises the following steps:
saving the step of performing the automatic headspace solid-phase microextraction mode as a first method file, and saving the automatic liquid-liquid extraction mode as a second method file;
and setting an operation sequence table in the automatic water sample pretreatment device, filling the operation sequence table with the position serial numbers of the sample racks of the sample bottles and the first method files or the second method files corresponding to the sample bottles, and sequentially loading the first method files or the second method files corresponding to the samples by the automatic water sample pretreatment device according to the operation sequence table to treat the samples in the sample bottles at the corresponding positions.
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