Water removal device and extraction instrument

Abstract

The utility model relates to a water removal device, which is used in an extraction instrument and comprises a water removal column provided with an inlet, an opposite outlet and an accommodating space between the inlet and the outlet; the cooling pipeline is connected between an extraction device of the extraction instrument and an inlet of the water removal column and used for enabling extraction liquid from the extraction device to directly enter the water removal column after being cooled by the cooling pipeline, and the water removal agent is arranged in the containing space of the water removal column and used for conducting online water removal on the extraction liquid. According to the water removal device, full-automatic extraction and water removal processes without manual intervention can be realized, external interference is prevented from being introduced, adverse effects on the environment or operators are reduced, and the operation efficiency and reliability are improved. In addition, the utility model further relates to an extraction instrument.

Description

TECHNICAL FIELD

[0001] The utility model relates to a kind of water removal devices. In addition, the utility model further relates to a kind of extraction instrument comprising such water removal device. BACKGROUND

[0002] According to market investigation, almost all of the samples (soil and sediment, silt, plant and animal tissues) to be tested of 70% of environmental users are wet samples, which contain a certain proportion of water. For example, soil samples contain 1-50% water, and vegetables contain 50-90% water. Current extraction process is usually to directly extract these wet solid samples, remove water manually, and then manually transfer the samples to the concentration instrument for evaporation to target volume. This manual water removal process is time-consuming and laborious, is easy to introduce external interference, and can cause leakage or loss of extraction liquid, which can adversely affect the environment or operator, and is difficult to realize one-stop automatic sample processing process, reducing operation efficiency and reliability.

[0003] In addition, the existing water removal operation still has other defects. For example, the cost of water removal agent is relatively high, and the water removal is not thorough enough, so that some water remains in the extraction liquid after water removal. In this way, the water contained in the extraction liquid precipitates from the final extraction liquid, causing evaporation constant volume failure.

[0004] In addition, the extraction process, especially the accelerated solvent extraction process, is usually carried out at relatively high pressure and temperature. For example, the working pressure of the extraction cell is usually in the range of 1,380 Kpa-11,800 KPa (i.e., about 200-1,700 psi), and the working temperature is usually 50-110℃. In this way, the temperature of the extraction liquid containing the sample is also relatively high, and such relatively high temperature extraction liquid is not suitable for direct water removal treatment. Therefore, before the extraction liquid is subjected to water removal treatment, how to carry out reliable, efficient and low-cost cooling or temperature reduction and pressure control also presents a challenge.

[0005] There is still a need to provide an improved water removal device that can overcome one or more shortcomings of the prior art. SUMMARY

[0006] The utility model aims at providing a kind of water removal devices, which allows to realize the full automation process of sample extraction, extraction liquid water removal and concentration constant volume.

[0007] According to the first aspect of the utility model, a kind of water removal device, the water removal device can be used in extraction instrument, the water removal device can include: water removal column, water removal column is provided with inlet, opposite outlet and the containing space between inlet and outlet;Cooling pipeline, cooling pipeline is connected between the extraction device of extraction instrument and the inlet of water removal column, for the extraction liquid from extraction device is directly entered into water removal column after cooling by cooling pipeline, and water removal agent, water removal agent is arranged in the containing space of water removal column, for carrying out online water removal to extraction liquid.

[0008] This water removal device enables to realize full-automatic extraction and water removal process without manual intervention, avoids introducing external interference, reduces adverse effects on environment or operating personnel, and improves operation efficiency and reliability.

[0009] According to the above aspect of the utility model, preferably, the water removal agent can include inorganic water removal agent and organic water removal agent, wherein the organic water removal agent can be arranged downstream of the inorganic water removal agent, and the weight ratio between the organic water removal agent and the inorganic water removal agent can be in the range of 1:99 to 49:51.

[0010] In this way, on the one hand, the water removal effect can be improved while reducing the cost of the water removal agent, and on the other hand, the gel formed by the inorganic filler after absorbing water can be effectively prevented from entering the extraction liquid, and the water not absorbed by the inorganic filler can also be further absorbed, thereby improving the water removal efficiency.

[0011] According to the above aspect of the utility model, preferably, the weight ratio between the organic water removal agent and the inorganic water removal agent is 1:20 or 5:20.

[0012] The inventors have found that, by such arrangement, there is substantially no water residue in the sample after water removal and concentration by the water removal device, leaving only uniform organic phase, and the success rate of liquid level detection and constant volume is high.

[0013] According to the above aspect of the utility model, in order to further improve the water absorption while keeping a low cost, preferably, the inorganic water removal agent can be selected from at least one of the following: anhydrous sodium sulfate, anhydrous magnesium sulfate; the organic water removal agent can be selected from at least one of the following: modified or unmodified polyacrylate copolymer, polyvinyl alcohol copolymer, vinyl acetate copolymer, polyurethane copolymer, polyethylene oxide copolymer, starch graft copolymer.

[0014] According to the above aspect of the utility model, in order to further improve the water removal / absorption effect, preferably, the organic water removal agent is arranged in the water removal column in a granular form, and the particles satisfy the following requirements: the particle size is in the range of 0.01-2000 μm, and the specific surface area of the particles is in the range of 0.05-500 m 2 / g.

[0015] According to the above aspect of the present application, preferably, the inner diameter of the cooling line is in the range of 0.1-10mm, and / or the length of the cooling line is in the range of 1-500cm.

[0016] This arrangement enables the natural cooling of the high-temperature extracted extract to a predetermined temperature by means of the cooling line without the need for additional cooling devices, with low cost and high reliability.

[0017] According to the above aspect of the present application, in order to further improve the cooling function of the cooling line on the extract and save space, preferably, the cooling line can have a spiral portion that is at least partially wound to form a spring shape.

[0018] According to the above aspect of the present application, preferably, the water removal device further comprises an adjusting device, which enables the working temperature of the water removal column to be in the range of 4-50℃, and the working pressure to be less than 1380Kpa.

[0019] The inventors have found that the water removal device according to the present application can improve the water removal effect at this working temperature and pressure, and avoid the dissolution of polymers at high temperatures and the precipitation in the subsequent evaporation and concentration process.

[0020] According to the above aspect of the present application, preferably, the water removal device can further comprise a back pressure valve, which can be arranged along the cooling line between the extraction device of the extraction instrument and the inlet of the water removal column, and the back pressure valve is arranged to open when the pressure of the extract in the cooling line (i.e. the upstream pipeline portion of the back pressure valve) is higher than a threshold pressure.

[0021] With this arrangement, the back pressure valve can be used as a switch valve, and the degree of automation of the water removal device can be further improved.

[0022] According to the above aspect of the present application, in order to avoid the leakage of organic fillers and also prevent the particles precipitated or in the sample from entering the evaporation flask, preferably, a filter device can be arranged between the inlet and outlet of the water removal column and the water removal agent, respectively, for retaining the water removal agent in the containment space of the water removal column.

[0023] According to the above aspect of the present application, in order to obtain the desired filtering effect, preferably, the filter device can comprise a filter membrane and / or a filter screen plate with a pore size in the range of 0.2μm to 50μm.

[0024] According to the second aspect of the utility model, an extraction instrument is provided, which can include: an extraction device, which extracts a sample using an extraction solvent to form an extract; a water removal device, which removes water from the extract online and includes: a water removal column, which is provided with an inlet, an opposite outlet, and a containing space between the inlet and the outlet; a cooling pipeline, which is connected between the extraction device and the inlet of the water removal column of the extraction instrument, for allowing the extract from the extraction device to enter the water removal column directly after being cooled by the cooling pipeline, and a water removal agent, which is arranged in the containing space of the water removal column, for removing water from the extract online; and a collection device, which is arranged downstream of the water removal column, for receiving the water-removed extract from the water removal column and evaporating the extract.

[0025] The extraction instrument can realize fully automated extraction, water removal, and evaporation processes without manual intervention, improving operation efficiency.

[0026] According to the above aspect of the utility model, preferably, the collection device can receive the water-removed extract from the water removal column via a discharge pipeline, wherein the inlet and the outlet of the water removal column are provided with first connectors, and the outlet end of the cooling pipeline and the inlet end of the discharge pipeline are respectively provided with second connectors, the second connectors cooperate with the first connectors to seal and connect the cooling pipeline and the discharge pipeline to the water removal column respectively. This arrangement allows the operator to conveniently switch the water removal column (for example, conveniently manually switch), thereby reducing the downtime of the extraction instrument and being cost-effective.

[0027] According to the above aspect of the utility model, preferably, the extraction instrument can be provided with multiple water removal columns and a switching device carrying the multiple water removal columns, the switching device allowing at least one of the multiple water removal columns to be selectively connected between the extraction device and the collection device.

[0028] This arrangement allows automatic switching of the water removal column, further improving the degree of automation of extraction and water removal.

[0029] According to the above aspect of the utility model, preferably, the switching device can include a first switching device, which can include: a holder, which carries the multiple water removal columns and can be rotated to change the circumferential positions of the multiple water removal columns; an adapter, which is made of a flexible material and cooperates with the inlet of the water removal column to cover the inlet; and an insert, a first end of which is connected to the outlet end of the cooling pipeline, and an opposite second end of which is an open pointed end and can be inserted through the adapter to allow the extract to be fed into the water removal column.

[0030] The water removal column can be switched by rotating the holder, the replacement of the water removal column can be quickly and accurately realized, and the water removal device can be arranged in a sealed space, further avoiding the introduction of external interference and reducing the adverse effects on the environment or the operator.

[0031] According to the above aspect of the present application, preferably, the switching device can include a second switching device, the second switching device including: an inlet flow path selection valve for connecting at least one of the plurality of water removal columns to the extraction device; and an outlet flow path selection valve for connecting at least one of the plurality of water removal columns to the collection device.

[0032] Similarly, this arrangement can also achieve quick and automatic switching of the water removal column, avoid the introduction of external interference, and reduce the adverse effects on the environment or the operator.

[0033] Therefore, the water removal device of the present application can meet the use requirements, overcome the shortcomings of the prior art and achieve the predetermined purpose. BRIEF DESCRIPTION OF DRAWINGS

[0034] In order to further clearly describe the water removal device according to the present application, the present application will be described in detail below in combination with the drawings and specific embodiments, in which:

[0035] Figure 1 A schematic working process of an extraction instrument of the prior art is shown;

[0036] Figure 2 A schematic working process of an extraction instrument according to a non-limiting embodiment of the present application is shown;

[0037] Figure 3 A schematic diagram of an extraction instrument according to a first non-limiting embodiment of the present application is shown;

[0038] Figure 4 A schematic diagram of Figure 3 a part of the extraction instrument shown;

[0039] Figure 5 A schematic diagram of Figure 3 another part of the extraction instrument shown;

[0040] Figure 6 A schematic diagram of a water removal column of a water removal device according to a non-limiting embodiment of the present application is shown;

[0041] Figure 7 Another schematic diagram of a water removal column of a water removal device according to a non-limiting embodiment of the present application is shown;

[0042] Figure 8A comparison diagram of water removal effect of the water removal column according to the utility model and the prior art is shown.

[0043] Figure 9 A schematic diagram of an extractor according to the second non-limiting embodiment of the utility model is shown.

[0044] Figure 10 A schematic diagram of an extractor according to the second non-limiting embodiment of the utility model is shown. Figure 9 A schematic diagram of an extractor according to the second non-limiting embodiment of the utility model is shown.

[0045] Figure 11 A schematic diagram of an extractor according to the second non-limiting embodiment of the utility model is shown. Figure 9 A schematic diagram of an extractor according to the second non-limiting embodiment of the utility model is shown.

[0046] Figure 12 A schematic diagram of an extractor according to the second non-limiting embodiment of the utility model is shown.

[0047] The above-mentioned drawings are merely schematic and are not drawn strictly to scale.

[0048] The reference numerals in the drawings are listed in the drawings and embodiments:

[0049] 1000 - extractor, comprising:

[0050] 100 - water removal device, comprising:

[0051] 10 - water removal column, comprising:

[0052] 11 - inlet;

[0053] 12 - outlet;

[0054] 13 - containing space;

[0055] 20 - cooling line, comprising:

[0056] 20A - spiral portion;

[0057] 201 - outlet end;

[0058] 202 - inlet end;

[0059] 30 - water removal agent, comprising:

[0060] 31 - inorganic water removal agent;

[0061] 32 - organic water removal agent;

[0062] 40 - adjusting device;

[0063] 50 - back pressure valve;

[0064] 60 - filtering device, comprising:

[0065] 61 - filter membrane;

[0066] 62 - filter screen;

[0067] 200 - extraction device, comprising:

[0068] 210 - extraction pump;

[0069] 220 - extraction cell;

[0070] 300 - collection device, comprising:

[0071] 310 - discharge line, comprising:

[0072] 310A - inlet end;

[0073] 320 - evaporation flask;

[0074] 330 - vacuum system, comprising:

[0075] 330A - vacuum pump;

[0076] 330B - hydrazine;

[0077] 400 - first switching device, comprising:

[0078] 401 - holder;

[0079] 402 - adapter;

[0080] 403 - insert;

[0081] 404 - cradle;

[0082] 500 - second switching device, comprising:

[0083] 501 - inlet flow path selection valve;

[0084] 502 - outlet flow path selection valve;

[0085] 600 - level sensor;

[0086] S - sample. DETAILED DESCRIPTION

[0087] It should be understood that the present application can employ various alternative orientations and step sequences, except where expressly specified to the contrary. It is also to be understood that the specific devices illustrated in the attached drawings, and described in the following specification, are simply exemplary embodiments of the inventive concepts disclosed and defined herein. Hence, specific orientations, direction or sequence of steps are not to be understood as limiting, unless expressly so defined.

[0088] Figure 1A schematic working process of the prior art extractor 1000 is shown. As shown, the prior art working process generally extracts a sample S, such as a wet solid sample, in the extractor 1000. Manual water removal is then performed. As shown in Figure 1 the manual water removal requires the use of multiple instruments and containers, and requires the transfer of the sample or extract between various containers. The water-removed sample then needs to be manually transferred to a concentrator for evaporation to a target volume. As can be seen, this manual water removal process is time-consuming and labor-intensive, is prone to the introduction of external interference, and can cause the leakage or loss of the extract, which can adversely affect the environment or the operator.

[0089] Figure 2 A schematic working process of the extractor 1000 according to the non-limiting embodiments of the present application is shown. According to the inventive concept of the present application and as shown, this extractor 1000 allows a one-stop automated sample processing flow, such that manual transfer of the sample S or extract between various containers or instruments is not required. The extractor 1000 according to the present application will be further described below in conjunction with the accompanying drawings.

[0090] Figure 3 A schematic view of the extractor 1000 according to the first non-limiting embodiment of the present application is shown.

[0091] As shown and as a non-limiting example, the extractor 1000 can mainly include a water removal device 100, an extraction device 200, and a collection device 300, etc.

[0092] The extraction device 200 can be arranged upstream of the water removal device 100. The extraction device 200 can use an extraction solvent to extract a sample to form an extract, and supply the extract to the water removal device 100 for water removal.

[0093] As a simplified example, the extraction device 200 can be provided with an extraction pump 210 and an extraction cell 220. The extraction pump 210 can be used to deliver solvent from a solvent storage tank into the extraction cell 220. The sample S can be placed in the extraction cell 220 for extraction. The extraction cell 220 can generally be made of stainless steel and designed to withstand high pressure / high temperature. For example, the working pressure range of the extraction cell 220 is 1,378.95 KPa-11,721 kPa (i.e., 200-1700 psi), while the working temperature is a relatively high temperature, such as a stable range of 50-110°C. An example of the extraction solvent is a mixed solution of acetone: dichloromethane at 1:1, and the extraction temperature is, for example, 100°C.

[0094] Figure 4 and 5 different schematic views of a portion of the extractor 1000 are shown. Figure 3 different schematic views of a portion of the extractor 1000 are shown.

[0095] In combination Figures 3-5 And as an example, the water removal device 100 can mainly comprise a water removal column 10, a cooling pipeline 20 and a water removal agent 30, etc.

[0096] Figure 6 And 7 Different schematic views of the water removal column 10 of the water removal device 100 according to non-limiting embodiments of the present application are shown respectively.

[0097] As shown, the water removal column 10 can be a generally columnar structure and can be provided with an inlet 11, an opposite outlet 12 and a containing space 13 between the inlet and the outlet.

[0098] In Figure 3 , 6 And in the embodiments shown in Figs. 6 and 7, both the inlet 11 and the outlet 12 of the water removal column 10 can be provided with a first joint, which can be shown as a threaded joint with internal threads.

[0099] The cooling pipeline 20 can be connected between the extraction device 200 of the extraction instrument 1000 and the inlet 11 of the water removal column 10, for allowing the extraction liquid from the extraction device 200 to enter the water removal column 10 directly after being cooled by the cooling pipeline 20.

[0100] The cooling pipeline 20 can have an outlet end 201 connected to the inlet 11 of the water removal column 10 and an inlet end 202 connected to the extraction device 200. For example, the inlet end 202 can be fixedly connected to the outlet of the extraction cell 220 of the extraction device 200, while the outlet end 201 can be detachably connected with the inlet 11 of the water removal column 10, and the outlet end 201 is provided with a second joint. The second joint can cooperate with the first joint for sealingly connecting the cooling pipeline 20 to the water removal column 10

[0101] In the embodiments where the first joint is a threaded joint with internal threads, the second joint can be a threaded joint with external threads, as shown schematically in Figure 3 Fig. 5.

[0102] Also as shown in Figure 3 Fig. 6, the outlet 12 of the water removal column 10 can also be connected to the inlet end 310A of the discharge pipeline 310 via a joint such as a threaded joint, for sealingly connecting the discharge pipeline 310 to the water removal column 10.

[0103] As a non-limiting example, the inner diameter of the cooling pipeline 20 can be in the range of 0.1-10 mm, and / or the length of the cooling pipeline 20 can be in the range of 1-500 cm. As Figure 4 And 5As schematically shown, the cooling line 20 has a spiral portion 20A which is at least partially wound to form a spring shape.

[0104] As a preferred embodiment, the cooling line 20 and the discharge line 310 can be pipes of 1.5875 mm (i.e. 1 / 16 inch) gauge, and have threaded joints at the ends. At this time, the inlet 11 and the outlet 12 of the water removal column 10 can also be threaded joints of 1.5875 mm (i.e. 1 / 16 inch) gauge, for sealingly connecting the extraction cell 220 and the evaporation bottle 320 (e.g. a generally large bottle of 2 ml small bottle) to the inlet 11 and the outlet 12 of the water removal column 10, respectively, in the manner of a hand-tight joint.

[0105] Continuing to refer to Figures 6-7 wherein an example arrangement of the water removal agent 30 is also shown. As can be seen, the water removal agent 30 can be provided in the accommodation space 13 of the water removal column 10, particularly in a layered arrangement therein.

[0106] As an example, the water removal agent 30 can include an inorganic water removal agent 31 (schematically shown in a triangular pattern) arranged in the upper layer. The inorganic water removal agent 31 is selected from at least one of: anhydrous sodium sulfate or anhydrous magnesium sulfate, etc.

[0107] The water removal agent 30 can also include an organic water removal agent 32 (schematically shown in a circular pattern) arranged in the lower layer. The organic water removal agent 32 can be a superabsorbent resin and can be selected from at least one of: a modified or unmodified polyacrylate-based copolymer, a polyvinyl alcohol-based copolymer, a vinyl acetate copolymer, a polyurethane-based copolymer, a polyethylene oxide-based copolymer, a starch graft copolymer, etc.

[0108] Preferably, the organic water removal agent 32 can be provided in the water removal column 10 in a granular form, and the granules can satisfy the following requirements: the granule size is in the range of 0.01 - 2000 pm, and the specific surface area of the granules is in the range of 0.05 - 500 m 2 / g.

[0109] As an example, the weight ratio between the organic water removal agent 32 and the inorganic water removal agent 31 can be in the range of 1:99 to 49:51.

[0110] Compared with the existing in-cell purification water removal, the water removal agent or water removal filler in the water removal column 10 is able to stably fix or hold all absorbed water, has high water removal efficiency, and thus can be applied to direct extraction, water removal and concentration evaporation of a wet sample which is not dried and has a water content of 1-90%.

[0111] The inventors found that when the weight ratio between the organic water scavenger 32 and the inorganic water scavenger 31 is 1:20 or 5:20, the sample S after water removal and concentration by the water removal device 100 has substantially no water residue, leaving only a uniform organic phase, and the liquid level detection and constant volume success rate is high. Although the filler of such a ratio can improve the constant volume success rate, the system pressure required during water removal in the water removal column 10 is higher when the weight ratio between the organic water scavenger 32 and the inorganic water scavenger 31 is 5:20.

[0112] For example, the extraction liquid after water removal by the water removal device 100 has no water residue or has water residue of <20 mg, thereby avoiding the water and organic phase separation when the aqueous extraction liquid is evaporated to 0.3-1 ml, thereby ensuring accurate and automatic constant volume.

[0113] The effect comparison between water removal by the water removal column 10 according to the present application (right side) and the in-pool water removal of the prior art (left side) is shown in Figure 8 . It can be seen that after water removal and concentration of the extraction liquid by the water removal column 10 according to the present application, there is substantially no water residue, leaving only a uniform organic phase, and the liquid level detection and constant volume are successful. In contrast, the in-pool water removal method of the prior art dissolves the organic water scavenger filler at high temperature, and the water removal is incomplete, and after solution cooling and concentration, water and organic water scavenger filler are separated and layered, resulting in failure of liquid level constant volume.

[0114] In addition, such a water scavenger 30 including the inorganic water scavenger 31 and the organic water scavenger 32 can significantly reduce the cost. As an example, the cost of such a water scavenger 30 is about 1 / 20 of the cost of pure organic filler, significantly reducing the cost of consumables required by the user for corresponding tests. In addition, the water removal effect of such a water scavenger 30 is also better than that of pure organic water scavenger, and the problem of blocking the pipeline after water absorption of pure organic water scavenger is also avoided.

[0115] According to an embodiment of the present application and as shown in Figure 6 and 7 , a filter device 60 can be provided between the inlet 11 and the outlet 12 of the water removal column 10 and the water scavenger 30, respectively.

[0116] In the example shown in Figure 6 , a filter screen 62 can be provided between the inlet 11 of the water removal column 10 and the inorganic water scavenger 31, and a filter screen 62 can also be provided between the organic water scavenger 32 and the outlet 12 of the water removal column 10.

[0117] In the example shown in Figure 7In the example shown, a filter membrane 61 can additionally be provided between the organic water scavenger 32 and the filter screen 62. In addition, although not shown in the drawings, a filter membrane 61 or a filter screen 62 can also be provided between the organic water scavenger 32 and the inorganic water scavenger 31 as needed by those skilled in the art.

[0118] As an example, the pore size of the filter membrane 61 and the filter screen 62 can both be in the range of 0.2 μιη to 50 μιη.

[0119] In this way, the organic water scavenger 32 can be provided downstream of the inorganic water scavenger 31, thereby forming at least a two-stage water scavenging arrangement. When the sample S flows from the inlet 11 at the top of the water scavenging column 10 into the water scavenging column 10, the liquid first passes through the filter screen 62, and then flows from top to bottom through the portion containing the inorganic water scavenger 31 and then through the portion containing the organic water scavenger 32, whereas the solution passing through the organic water scavenger 32 flows out after passing through the filter screen 62. The organic water scavenger 32 can not only effectively prevent the gel formed after the inorganic water scavenger 31 absorbs water from entering the extract solution, but also further absorb the water not absorbed by the inorganic water scavenger 31, thereby improving the efficiency of water scavenging.

[0120] In this way, the water scavenging device 100 according to the present application can be used for online water scavenging of the extract solution. As used herein, the description "online water scavenging" refers to a water scavenging mode without manual transfer of the sample, so that the extract solution flowing out of the extraction tank 220 directly enters the water scavenging column 10 via the cooling pipeline 20, and after water scavenging by the water scavenging column 10, the extract solution also directly goes to the collection device 300 via the discharge pipeline 310.

[0121] As an example, the inert gas or the solvent pump or the extraction pump 210 in the front section of the extraction tank can be used to push the extract solution in the water scavenging column 10 to flow out, be collected in the evaporating flask 320, and then be online evaporated and concentrated to a target volume. For example, the extract solution can be continuously evaporated and concentrated to a set volume, for example, online evaporated and concentrated to approximately 1 ml, under conditions such as nitrogen, vacuum, or heating.

[0122] While the extract solution flows out of the high-temperature extraction tank 220 and the extract solution cooled by the cooling pipeline 20 is online water scavenged, the solution that has flowed from the water scavenging column 10 to the evaporating flask 320 can be simultaneously online evaporated, or alternatively, the evaporation can be started after all the extract solution is collected. In this way, the extraction instrument 1000 according to the present application can realize a one-stop process of online extraction, online water scavenging, and online concentration.

[0123] Continuing to refer to Figure 4 and 5 , the water scavenging device 100 can further include a regulating device 40 and a switching valve, which can be, for example, a back pressure valve 50.

[0124] The regulating device 40 makes the working temperature of the water removal column 10 in the range of 4-50℃, and the working pressure less than 1380KPa. As an example, the regulating device 40 can include a corresponding temperature sensor and / or pressure sensor, etc., and can include a corresponding heat exchange device or pump, etc. to achieve the desired stabilization and pressure regulation functions.

[0125] As an example, the back pressure valve 50 can be arranged along the cooling line 20 between the extraction device 200 of the extractor 1000 and the inlet 11 of the water removal column 10, and the back pressure valve 50 can be arranged to open when the pressure of the extraction liquid in the cooling line 20 is higher than a threshold pressure. For example, the back pressure valve 50 can open when the pressure in its upstream line is higher than a threshold pressure.

[0126] In the embodiment shown in Figure 4 , the back pressure valve 50 is arranged downstream of the spiral portion 20A of the cooling line 20, while in the embodiment shown in Figure 5 , the back pressure valve 50 is arranged upstream of the spiral portion 20A of the cooling line 20.

[0127] Figure 9 A schematic view of an extractor 1000 according to a second non-limiting embodiment of the present application is shown.

[0128] The second embodiment of the extractor 1000 is similar to the first embodiment of the extractor 1000 shown in Figure 3 , except for the differences described below, wherein identical or similar elements are generally indicated with identical or similar reference numerals herein and can not be reintroduced hereinafter.

[0129] In the embodiment shown in Figure 9 , the extractor 1000 is provided with a plurality of water removal columns 10 and with a switching device carrying the plurality of water removal columns 10, the switching device making at least one of the plurality of water removal columns 10 selectively connectable between the extraction device 200 and the collection device 300.

[0130] The switching device can be a first switching device 400 and can include a holder 401, an adapter 402 and an insert 403, etc.

[0131] The holder 401 can be used to carry the plurality of water removal columns 10 and can be rotatable to change the circumferential position of the plurality of water removal columns 10. As an example, the holder 401 can be designed as a substantially disc-shaped support and can be driven in rotation by a drive mechanism not shown. Preferably, 4 / 5 of the circumferential portion of the holder 401 can be a carrying portion, which can be provided with corresponding cradles 404, for example Figure 9The receptacle-shaped holder 401 is shown schematically to load a single or multiple water removal column 10 for in-line water removal. The remaining 1 / 5 of the circumferential portion of the holder 401 can be a notch position or an empty position for direct connection of the extraction cell 220 to the evaporative flask 320 for the next step of in-line evaporation.

[0132] As shown, in this embodiment, the holder 401 can be provided with 12 or 16 cradles 404, and 4 water removal columns 10 can be simultaneously rotated into position between the extraction cell 220 and the evaporative flask 320 to enable flow communication of the accelerated solvent extraction and evaporation module (e.g., including the extraction fluid collection flask and evaporation heating device, etc.).

[0133] Figure 10 and 11 are shown, respectively, Figure 9 are shown, respectively.

[0134] As shown, the adapter 402 can mate with the inlet 11 of the water removal column 10 to cap the inlet 11, e.g., removably cap the inlet 11. As an example, the adapter 402 can be made of a flexible material and elastically deforms upon insertion mating to the inlet 11 to form a sealed engagement. For example, the sealed engagement between the adapter 402 and the inlet 11 of the water removal column 10 can be less than 3,447 kpa (i.e., less than 500 psi).

[0135] Continuing with reference to Figure 9 , the insert 403 can be an elongated member, such as a fluid passageway bearing steel needle, etc. The first end (upper end in the figures) of the insert 403 can be connected to the outlet end 201 of the cooling line 20, while the opposite second end (lower end in the figures) of the insert 403 is an open tip and is capable of being inserted through the adapter 402 to allow feeding of the extraction fluid into the water removal column 10.

[0136] The liquid flowing out of the outlet 12 of the water removal column 10 flows directly into the evaporative flask 320 (or collection flask). Likewise, the connection between the outlet 12 and the evaporative flask 320 can also be achieved via another adapter and insert, and for brevity, the description is not repeated herein.

[0137] After the extraction and extraction fluid collection is completed, the insert 403 can be automatically removed from the water removal column 10 and the adapter 402, such that the water removal column 10 is disconnected from the extraction and evaporation flow path. At this time, the water removal column 10 is automatically moved away by rotating the holder 401 loaded with the water removal column 10.

[0138] Figure 12 A schematic view of an extractor according to a third non-limiting embodiment of the present utility model is shown.

[0139] The third embodiment of the extractor 1000 can be similar to the second embodiment of the extractor 1000 shown above, except for the differences described below, wherein the same or similar elements are generally indicated with the same or similar reference numerals herein and can not be reintroduced below. Figure 9 The second embodiment of the extractor 1000 shown above, wherein the same or similar elements are generally indicated with the same or similar reference numerals herein and can not be reintroduced below.

[0140] In the embodiment shown above, the extractor 1000 can be provided with a second switching device 500. The second switching device 500 can be a device switched by a valve, and can include an inlet flow path selection valve 501 and an outlet flow path selection valve 502, and corresponding connecting pipelines, etc. Figure 12 The inlet flow path selection valve 501 can be used to connect at least one of the plurality of water removal columns 10 to the extraction device 200, and the outlet flow path selection valve 502 can be used to connect at least one of the plurality of water removal columns 10 to the collection device 300.

[0141] As shown and as a non-limiting example, the inlet flow path selection valve 501 and the outlet flow path selection valve 502 can be 4-position 16-port valves, respectively, and can achieve simultaneous online water removal of 4 samples S in 4 extraction channels, and switching of the four valve positions can be performed to achieve automatic continuous processing of 4 groups of samples (4*4=16 samples S).

[0142] As shown and as a non-limiting example, the inlet flow path selection valve 501 and the outlet flow path selection valve 502 can be 4-position 16-port valves, respectively, and can achieve simultaneous online water removal of 4 samples S in 4 extraction channels, and switching of the four valve positions can be performed to achieve automatic continuous processing of 4 groups of samples (4*4=16 samples S).

[0143] As shown and as a non-limiting example, the inlet flow path selection valve 501 and the outlet flow path selection valve 502 can be 4-position 16-port valves, respectively, and can achieve simultaneous online water removal of 4 samples S in 4 extraction channels, and switching of the four valve positions can be performed to achieve automatic continuous processing of 4 groups of samples (4*4=16 samples S). Figure 12 As shown and as a non-limiting example, the inlet flow path selection valve 501 and the outlet flow path selection valve 502 can be 4-position 16-port valves, respectively, and can achieve simultaneous online water removal of 4 samples S in 4 extraction channels, and switching of the four valve positions can be performed to achieve automatic continuous processing of 4 groups of samples (4*4=16 samples S).

[0144] In addition, when the inlet flow path selection valve 501 and the outlet flow path selection valve 502 are both switched or rotated to the B1, B2, B3, B4 positions, the corresponding flow paths will be in communication with the B group water removal columns 10 numbered B1, B2, B3, B4, and the B group of 4 samples S will be subjected to online water removal. By analogy, similar operations can be performed on the samples of the C group and the D group.

[0145] Therefore, the extractor 1000 can support continuous uninterrupted online water removal of 4 groups of samples S, each group of 4 samples S. In addition, single channel to multi-channel parallel sample processing, and continuous uninterrupted pretreatment process of single group to multiple groups of samples can be achieved by increasing or decreasing the design of valve ports.

[0146] In addition, Figure 12 An example is shown in more detail in which the collection device 300 can include a discharge line 310, an evaporating flask 320, and a vacuum system 330. The vacuum system 330 can include a vacuum pump 330A and hydrazine 330B to achieve online evaporation of the sample S-containing solution contained in the evaporating flask 320, achieving automatic constant volume. During this process, the liquid level or volume of the solution can be detected in real time via the liquid level sensor 600 to evaporate the solution to the desired liquid level or volume, for example, 1 ml.

[0147] It should be understood that Figure 9 and 12 The first switching device 400 and the second switching device 500 shown in Figs. 4 and 5 can be arranged inside or outside the extractor 1000 without limitation, so as to facilitate, expedite and reliably achieve switching of the pretreatment column flow path of multiple groups of samples.

[0148] The extractor 1000 according to the present application can automatically and continuously process wet samples in parallel on an accelerated solvent extraction system. The water-containing sample S is directly subjected to accelerated solvent extraction, and the extractant can be subjected to online automatic water removal after pipeline cooling, and can be directly introduced into an evaporation device for simultaneous online evaporation. The extractor 1000 can achieve a full-automatic sample processing process of continuous extraction, water removal and concentration, and can support multi-channel parallel sample processing and continuous operation of multiple groups of samples.

[0149] The terms "upper side" or "lower side" as used herein to indicate an orientation or an orientation, and the terms "first", "second", and the like used to indicate an order, are merely for the purpose of better understanding the concept of the present application shown in the preferred embodiment by the person skilled in the art, and are not used to limit the present application. Unless otherwise specified, all orders, orientations or orientations are only for the purpose of distinguishing one element / component / structure from another element / component / structure, and unless otherwise specified, do not indicate any particular order, sequence of operations, direction or orientation. For example, in alternative embodiments, the "first switching device" can be the "second switching device", and the "upper side" can alternatively refer to the "lower side".

[0150] As used herein, unless otherwise indicated, the terms "approximately" and "about" are interpreted to mean plus or minus five percent of the numerical value or numerical range, or to mean that the shape and / or position has a deviation of plus or minus five percent. In addition, it should be understood that the various numerical ranges described herein include the values at the endpoints.

[0151] In summary, the water removal device 100 and the extraction instrument 1000 according to the embodiments of the present application overcome the shortcomings in the prior art, and achieve the intended utility model purposes.

[0152] Although the water removal column and the extraction instrument of the present application have been described above in conjunction with the preferred embodiments, it should be appreciated by those skilled in the art that the above examples are only used for illustration, and cannot be regarded as a limitation on the present application. Therefore, various modifications and variations can be made to the present application within the scope of the essential spirit of the claims, and these modifications and variations will all fall within the scope of the claims required by the present application.

Claims

1. A water removal device (100) for use in an extractor (1000), characterized in that, The water removal device (100) comprises: a water removal column (10) provided with an inlet (11), an opposite outlet (12), and a containing space (13) between the inlet and the outlet; a cooling pipeline (20) connected between an extraction device (200) of the extraction instrument (1000) and the inlet (11) of the water removal column (10), for directly entering the extraction liquid from the extraction device (200) into the water removal column (10) after cooling through the cooling pipeline (20), and a water removal agent (30) arranged in the containing space (13) of the water removal column (10), for online water removal of the extraction liquid.

2. The water removal device (100) according to claim 1, characterized in that The water removal agent (30) comprises an inorganic water removal agent (31) and an organic water removal agent (32), wherein the organic water removal agent (32) is arranged downstream of the inorganic water removal agent (31) and the weight ratio between the organic water removal agent (32) and the inorganic water removal agent (31) is in the range of 1:99 to 49:

51.

3. The water removal device (100) according to claim 2, characterized in that The weight ratio between the organic water removal agent (32) and the inorganic water removal agent (31) is 1:20 or 5:

20.

4. The water removal device (100) according to claim 2, wherein The inorganic water removal agent (31) is selected from at least one of the following: anhydrous sodium sulfate, anhydrous magnesium sulfate; The organic water removal agent (32) is selected from at least one of the following: modified or unmodified polyacrylate copolymer, polyvinyl alcohol copolymer, vinyl acetate copolymer, polyurethane copolymer, polyethylene oxide copolymer, starch graft copolymer.

5. The water removal device (100) as claimed in claim 2, wherein, The organic water removing agent (32) is provided in the water removing column (10) in a granular form, and the granules satisfy the following requirements: the particle size is in the range of 0.01 - 2000 μm, and the specific surface area of the granules is in the range of 0.05 - 500 m 2 / g.

6. The water removal device (100) as claimed in claim 1, wherein, The inner diameter of the cooling pipeline (20) is in the range of 0.1-10mm, and / or the length of the cooling pipeline (20) is in the range of 1-500cm.

7. The water removal device (100) as claimed in claim 1, wherein, The cooling pipeline (20) has a spiral portion (20A) wound at least partially to form a spring shape.

8. The water removal device (100) as claimed in claim 1, wherein, The water removal device (100) further comprises an adjusting device (40) for allowing the working temperature of the water removal column (10) to be in the range of 4-50℃ and the working pressure to be less than 1380Kpa.

9. The water removal device (100) according to any one of claims 1 to 8, characterized in that The water removal device (100) further comprises a back pressure valve (50) arranged along the cooling pipeline (20) between the extraction device (200) of the extraction instrument (1000) and the inlet (11) of the water removal column (10), and the back pressure valve (50) is arranged to open when the pressure of the extraction liquid in the cooling pipeline (20) is higher than a threshold pressure.

10. The water removal device (100) according to any one of claims 1 to 8, characterized in that A filtering device (60) is arranged between the inlet (11) and the outlet (12) of the water removal column (10) and the water removal agent (30) respectively, for keeping the water removal agent (30) in the containing space (13) of the water removal column (10).

11. The water removal device (100) according to claim 10, characterized in that The filtering device (60) comprises a filtering membrane (61) and / or a filtering sieve plate (62) with a pore size in the range of 0.2μm to 50μm.

12. An extractor (1000) characterized by, The extraction instrument (1000) comprises: an extraction device (200) for extracting a sample with an extraction solvent to form an extract; a water removal device (100) for removing water from the extract on-line, and comprising: a water removal column (10) provided with an inlet (11), an opposite outlet (12), and a containing space (13) between the inlet and the outlet; a cooling line (20) connected between the extraction device (200) of the extraction instrument (1000) and the inlet (11) of the water removal column (10) for directly feeding the extract from the extraction device (200) into the water removal column (10) after cooling the extract in the cooling line (20), and a water removal agent (30) provided in the containing space (13) of the water removal column (10) for removing water from the extract on-line; and a collection device (300) provided downstream of the water removal column (10) for receiving the water-removed extract from the water removal column (10) and evaporating the extract.

13. The extractor (1000) according to claim 12, characterized in that The collection device (300) receives the water-removed extract from the water removal column (10) via a discharge line (310), wherein the inlet (11) and the outlet (12) of the water removal column (10) are respectively provided with a first joint, and the outlet end (201) of the cooling line (20) and the inlet end (310A) of the discharge line (310) are respectively provided with a second joint, the second joint cooperating with the first joint for sealingly connecting the cooling line (20) and the discharge line (310) to the water removal column (10) respectively.

14. The extractor (1000) according to claim 12, characterized in that, The extraction instrument is provided with a plurality of water removal columns (10) and a switching device carrying the plurality of water removal columns (10), the switching device allowing at least one of the plurality of water removal columns (10) to be selectively connected between the extraction device (200) and the collection device (300).

15. The extractor (1000) according to claim 14, characterized in that The switching device comprises a first switching device (400) comprising: a holder (401) carrying the plurality of water removal columns (10) and being rotatable to change the circumferential position of the plurality of water removal columns (10); an adapter (402) made of flexible material and cooperating with the inlet (11) of the water removal column (10) to cover the inlet (11); and an insert (403) having a first end connected to the outlet end (201) of the cooling line (20) and an opposite second end being an open tip and being insertable through the adapter (402) to allow the extract to be fed into the water removal column (10).

16. The extractor (1000) according to claim 14, characterized in that The switching device comprises a second switching device (500) comprising: an inlet flow path selection valve (501) for connecting at least one of the plurality of water removal columns (10) to the extraction device (200); and an outlet flow path selection valve (502) for connecting at least one of the plurality of water removal columns (10) to the collection device (300). An outlet flow path selection valve (502) for connecting the at least one of the plurality of water removal columns (10) to the collection device (300).

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