CN214485727U - Pressure extraction device for replacing Soxhlet extractor in material analysis - Google Patents
Pressure extraction device for replacing Soxhlet extractor in material analysis Download PDFInfo
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- CN214485727U CN214485727U CN202120107022.3U CN202120107022U CN214485727U CN 214485727 U CN214485727 U CN 214485727U CN 202120107022 U CN202120107022 U CN 202120107022U CN 214485727 U CN214485727 U CN 214485727U
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Abstract
The utility model belongs to the technical field of the material test technique and specifically relates to a replace pressurization extraction device of soxhlet extractor in material analysis, including cross selector valve, syringe pump, purge valve, exhaust valve, control by temperature change and heating device, heat exchange assembly and coil pipe, sample cell, back pressure coil pipe, backward flow pond, extraction liquid bottle, washing liquid bottle and waste liquid bottle, the extraction liquid bottle with cross selector valve intercommunication, the washing liquid bottle with cross selector valve intercommunication, purge valve with heat exchange assembly and coil pipe intercommunication, control by temperature change and heating device with heat exchange assembly and coil pipe link, heat exchange assembly and coil pipe with sample cell intercommunication, sample cell with back pressure coil pipe intercommunication, back pressure coil pipe with the backward flow pond intercommunication, the backward flow pond with exhaust valve intercommunication, the device has the advantages of high extraction speed, small volume and capability of simultaneously operating a plurality of samples.
Description
Technical Field
The utility model relates to a material test technical field especially relates to a replace pressurization extraction device of soxhlet's extractor in material analysis.
Background
In the field of material testing, the leaching amount of a material soaked in a solvent is a necessary item for material physical and chemical testing in multiple national standards. The amount of elution can correspond to various properties of the material. Typical test methods for waterproofing rolls of construction as described in GB/T328.26-2007 part 26: soluble content (dip coating material content) of the asphalt waterproof roll; GB/T2412-2008 method for measuring isotactic index of polypropylene (PP) and propylene copolymer thermoplastic plastics.
The Soxhlet extractor was a laboratory instrument invented by Franzvon Soxhlet in 1879. If the compound to be extracted has a limited solubility in the solvent and the impurities are insoluble in this solvent, a Soxhlet extractor can be used.
Generally, the sample is placed in a cartridge made of very thick filter paper, and then the entire cartridge is placed in a cannula for soxhlet extraction. The Soxhlet extraction tube was placed in a flask containing the extraction solvent, and a reflux condenser tube was placed above the Soxhlet extraction tube.
The solvent will be heated to reflux and will travel up the vapor path and flow into the cannula, wetting out the solids. The condenser ensures that all solvent vapor is cooled back to the jacket to wet the solids.
The sleeve will gradually fill with hot solvent. Some of the substance to be purified gradually dissolves in the hot solvent. When the soxhlet tube is nearly full, the solvent will flow out along the siphon tube due to gravity and enter the flask again for distillation. This cycle can be performed many times, and can reach hours in most standard methods.
During each cycle a portion of the compound is dissolved in the solvent and after many cycles the compound is mainly concentrated in the flask. The advantage of this set of apparatus is that although there are many batches of solvent passing through the sample, only one batch needs to be recovered at the end of the experiment.
After extraction the solvent is removed and the insoluble solid matter remains in the extractor. In the testing method of the material, different from the application of the Soxhlet extraction device in the aspects of biology, medicine, chemistry and food, the residual solid residue after the Soxhlet extraction is taken as a target to be recovered, the weight of the residue is weighed after the residual solvent is removed (such as drying), and the physicochemical property of the material is verified by comparing the weight of the solid before the extraction.
The existing Soxhlet extraction device has the following disadvantages: 1. the system can not be pressurized, so that the normal pressure extraction speed is slow, the glass device interface is complex and fragile, and the device is large in size and high in energy consumption. 2. The pipetting and drainage cycles cannot be set or performed automatically. 3. In applications where the material to be collected is extraction residue, the extraction solvent on the residue cannot be removed automatically. And after extraction is finished, collecting residues, drying and weighing.
SUMMERY OF THE UTILITY MODEL
The utility model aims at solving the defects existing in the prior art and providing a pressurized extraction device which replaces a Soxhlet extractor in material analysis.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
designing a pressurizing extraction device for replacing a Soxhlet extractor in material analysis, comprising a four-way selection valve, an injection pump, a purge valve, a waste discharge valve, a temperature control and heating device, a heat exchange assembly and a coil pipe, a sample tube, a pressure-prepared coil pipe, a reflux pool, an extraction liquid bottle, a flushing liquid bottle and a waste liquid bottle, wherein the extraction liquid bottle is communicated with the four-way selection valve, the flushing liquid bottle is communicated with the four-way selection valve, the purge valve is communicated with the heat exchange assembly and the coil pipe, the temperature control and heating device is connected with the heat exchange assembly and the coil pipe, the heat exchange assembly and the coil pipe are communicated with the sample tube, the sample tube is communicated with the pressure-prepared coil pipe, the pressure-prepared coil pipe is communicated with the reflux pool, the reflux pool is communicated with the waste discharge valve, and the waste discharge valve is communicated with the four-way selection valve, the waste discharge valve is communicated with the waste liquid bottle, and the output end of the injection pump is communicated with the four-way selector valve.
Preferably, the waste liquid bottle is a borosilicate glass bottle.
Preferably, the sample tube is a 304 stainless steel hollow column.
The utility model provides a pair of replace pressurization extraction device of soxhlet extractor in material analysis, beneficial effect lies in: the pressurized extraction device system replacing the Soxhlet extractor in the material analysis can perform pressurized extraction, and the extraction speed is high. The device is small in size and can run a plurality of samples simultaneously. The heating is in the interior, the energy waste is less, and the condensed water is not consumed. Can cyclically extract samples and set automatic liquid suction and liquid discharge circulation. In the application that the material that needs to collect is the extraction residue, this device can blow dry the extraction solvent on the residue automatically. And after extraction is finished, directly weighing the sample tube, and subtracting the empty weight of the sample tube to obtain the weight of the residue.
Drawings
Fig. 1 is a schematic structural diagram of a pressure extraction device for replacing a soxhlet extractor in material analysis according to the present invention.
In the figure: the device comprises a four-way selector valve 1, an injection pump 2, a purge valve 3, a waste discharge valve 4, a temperature control and heating device 5, a heat exchange assembly and coil 6, a sample tube 7, a pressure preparation coil 8, a reflux pool 9, an extract liquid bottle 10, a flushing liquid bottle 11, a waste liquid bottle 12 and a nitrogen gas source 13.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments.
Referring to fig. 1, a pressurized extraction device for replacing a soxhlet extractor in material analysis comprises the following components: the device comprises a four-way selector valve 1, an injection pump 2, a purge valve 3, a waste discharge valve 4, a temperature control and heating device 5, a heat exchange assembly and coil 6, a sample tube 7, a pressure preparation coil 8, a reflux pool 9, an extract liquid bottle 10, a washing liquid bottle 11, a waste liquid bottle 12, and a middle connecting joint and a pipeline.
The four-way selector valve 1 provides solvent and flow path selection functions. The switching of the valve is driven by a motor and controlled by a circuit part. The valve head has 5 ports, which are respectively marked as a public end (marked as C in the figure) and five ports 1-4. The four-way selector valve 1 can only select one switching position at the same time, and the public end can only be communicated with the currently selected port and disconnected with other three unselected ports. The four digital ports are not communicated pairwise.
The injection pump 2 is composed of a stepping motor and a driver thereof, a screw rod, a bracket, an injector and the like, and the pushing and the sucking of liquid are realized by pushing and extracting the piston of the injector. The injection pump 2 is connected to the common end of the four-way selector valve 1 through a pipeline. In the application example of the present application, the syringe pump 2 having a 100mL glass syringe mounted thereon is used to construct a system, and the specification of the syringe may be adjusted as necessary.
The rinsing liquid bottle 11 and the extraction liquid bottle 10 are respectively connected to the No. 1 and No. 2 positions of the four-way selector valve 1 through pipelines. In the application example in this application, use 1000mL or 2000mL borosilicate glass bottle as reagent stock solution bottle, can replace other suitable specifications and materials as required.
The purge valve 3 and the waste discharge valve 4 are two-position three-way electromagnetic valves. The two-position three-way electromagnetic valve is controlled by double coils, one coil is powered on instantly, the power supply is closed, the valve is opened, and the other coil is powered on instantly, the power supply is closed, and the valve is closed. The mode is one-inlet two-outlet, when the solenoid valve coil is electrified, the NC end is connected with the common end, and the NO end is disconnected; when the solenoid valve coil is powered off, the NO end is connected with the common end, and the NC end is disconnected. In the application example of the present application, the above electromagnetic valve is controlled by using 24V power supply.
The pipeline led out from the No. 3 position of the four-way selector valve 1 is defined as a liquid inlet pipe, is connected to the NO end of the purge valve 3 and the NC end of the purge valve 3, and is connected to a nitrogen gas source 13 by using the pipeline for purging the solvent. In the application example of the present application, the input pressure of the connected nitrogen gas source 13 is 0.2 MPa.
The main component of the temperature control and heating device 5 is a cylindrical metal bath block with a spiral groove, and an electric heating device is arranged in the metal bath block and used for heating the metal bath block. In the application example of the present application, an electric heating plate with 24V power supply is used as the heating device. The heating device is controlled by a temperature control device, in the application example of the application, the temperature control device is controlled by PID, wherein PT-100 is used for measuring temperature, 24V is used for supplying power. The temperature control range is room temperature plus 5-100 ℃.
The cylindrical metal bath block with the spiral groove is coiled with a metal coil to form a heat exchange assembly. The liquid in the tube exchanges heat with the metal bath block, so that the liquid (extraction liquid) conveyed inside is heated. In the example of use in this application, the coils in the heat exchange assembly were stainless steel tubing of 0.5mm inside diameter, 1/16 inches outside diameter, and 1.5m length. The inlet end of the heat exchange assembly is connected to the common end of the purge valve 3.
The sample tube 7 is a cylindrical metal container and has a main body-screw cap structure which can be unscrewed, and a powdery or flaky solid sample can be contained in the sample tube after being unscrewed. The inlet and outlet of the sample tube 7 are provided with filter sieve plates to prevent the sample inside from flowing out of the sample tube 7. The device supports a plurality of sample tubes 7 to be connected in series in front and back. In the application example of the present application, a 304 stainless steel hollow column with a capacity of 10mL is used as the sample tube 7, and 5 sample tubes 7 are used in series at the same time as an example. The inlet ends of a plurality of sample tubes 7 in series are connected to the outlet end of the heat exchange assembly.
The pressure preparation coil 8 is a metal pipe with a diameter smaller than that of the heat exchange coil and a length longer than that of the heat exchange coil, when liquid is pushed to a pipeline automatically, a large back pressure is generated, meanwhile, the section of coil is placed in a normal-temperature environment to exchange heat with an external environment, and the temperature of a solvent is reduced to be close to the room temperature. The inlet end of the pressure preparation coil pipe 8 is connected to the outlet end of the last stage of the serial sample pipe 7. In the application example of the present application, the coil 8 was prepared using a stainless steel line of 0.25mm inside diameter, 1/16 inches outside diameter, 2m length.
The outlet end of the pressure preparation coil 8 is connected to the reflux pool 9. The reflux pool 9 is a pointed vessel with a volume greater than the syringe stroke of the syringe pump 2. The liquid discharged from the syringe eventually enters the reflux pool 9. In the application example of the present application, the reflux cell 9 is a 304 stainless steel conical container with a capacity of 200 mL. The pointed bottom of the reflux pool 9 is provided with a liquid outlet hole for connecting an outlet pipeline.
The common end of the waste discharge valve 4 is connected with the outlet of the reflux pool 9. The NO end of the waste valve 4 is connected to the No. 4 position of the four-way selector valve 1, and the pipeline is called a return pipe. The NC end of the waste discharge valve 4 is connected to a waste liquid bottle 12. In the application example of the present application, a borosilicate glass bottle of 2000mL was used as the waste liquid bottle 12.
The using method of the device comprises the following steps:
1. the method comprises the steps of (1) cyclic pressurization and heating solvent extraction of a solid sample, (2) flushing of sample residues, and (3) nitrogen blow-drying of the sample residues. When the solid sample is applied to material analysis, a solid sample is crushed and filled into a sample tube similar to a national standard method, and after the weight of the solid sample is measured together with a shell of the sample tube, the empty weight of the sample tube is reduced to obtain a sampling amount. After the steps of 1, 2 and 3 (such as GB/T2412-2008) or 1 and 3(GB/T328.26-2007), the weight of the sample tube with the solid residue is directly measured, and the weight of the residue can be obtained by deducting the empty weight of the sample tube. The weight percentage of residue or weight loss was calculated according to the process requirements.
The operation of the apparatus in steps 1, 2 and 3 will be illustrated in steps below.
Step 1: cyclic pressurized heated solvent extraction of solid samples
1.1 extraction solvent inhalation:
the four-way selector valve 1 is switched to the No. 2 position, and the injection pump 2 sucks the extraction liquid quantitatively.
1.2 circulating solvent extraction:
and in the liquid pushing stroke, the four-way selector valve 1 is switched to the No. 3 position, and the injection pump 2 pushes the extraction liquid to the liquid inlet pipe until all the solvent in the extraction liquid is completely pushed out. The purge valve 3NO port is opened to introduce solvent into the heat exchange assembly. The heating temperature is suitably selected depending on the solvent and is generally set to the boiling point at atmospheric pressure of the solvent because the system is pressurized and thus the volume is not vaporized. The solvent is heated in the coil of the heat exchange assembly and enters the sample tube 7.
Because the liquid suction of the syringe pump 2 is larger than the total volume of the sample tube 7, the excess solvent will pass through the pressure-preparation coil 8 and be pressed into the reflux pool 9. Because of the small inner diameter and the large enough length of the backup pressure coil 8, the back pressure of 0.3-0.6MPa is generated by matching the liquid pushing speed. Under the condition that the liquid paths are communicated everywhere, in the sample tube 7, the extract liquid is simultaneously at the high temperature close to the boiling point of the solvent under the normal pressure and under the pressure of 0.3-0.6MPa, so that the solid sample is heated, pressurized and quickly extracted.
Meanwhile, because the pressure preparation coil 8 is in a room temperature environment, the extract passes through the stainless steel pipe, is subjected to heat exchange with the outside to be cooled, enters the solvent of the reflux pool 9, and is cooled to a temperature slightly higher than the room temperature.
In the suction stroke, the four-way selector valve 1 is switched to position 4, and the syringe pump 2 is pulled back from the fully pushed state until the suction amount is the same as the pushed amount in phase a. The syringe pump 2 will now suck liquid from the return line. The NO port of the waste valve 4 is opened so that the liquid in the solvent reflux sump 9 is sucked into the syringe pump 2.
Considering that the extract in the reflux pool 9 is cooled by the pressure-preparation coil 8, the injection pump 2 and the four-way selector valve 1 do not need special heat resistance.
The liquid pushing and liquid absorbing strokes are repeated, and each liquid pushing is a pressurizing and extracting process of the solid sample in the sample tube 7.
1.3 discharge of waste liquid.
The push stroke and the suction stroke are repeated several times (typically 5-10 times, each stroke cycle is 3-5 minutes; generally, the number of previous extraction cycles can be small), the soluble substances in the solvent reach the dissolving equilibrium, and the solvent needs to be discharged and replaced by new solvent for extraction.
During liquid drainage, the four-way selector valve 1 is switched to the No. 3 position, and the injection pump 2 pushes the extraction liquid to the liquid inlet pipe until all the solvent in the extraction liquid is completely pushed out. The purge valve 3NO port is opened to introduce solvent into the heat exchange assembly. The excess solvent flows through the sample tube 7 and passes through the pressure-preparation coil 8 and is pressed into the reflux pool 9. The NC port of the waste valve 4 is opened, and the solvent is poured into the waste bottle 12.
After the syringe pump 2 has pushed all the solvent out, the purge valve 3 is switched to the NC port, nitrogen is passed through the purge valve 3 into the liquid path and blows all the remaining solvent in the coil, sample tube 7 and reflux cell 9 into the waste bottle 12.
The steps 1.1, 1.2 and 1.3 are circulated for 3-5 times, and the soluble part in the solid sample can be completely extracted into the extraction liquid. At this point the weight of the solid fraction has reached equilibrium and the subsequent steps can be carried out.
Step 2: washing of extraction residues of solid samples
Some standards require the sample residue to be washed with a different solvent than the extract, for example GB/T2412-2008 requires the sample residue to be washed with acetone after n-heptane extraction.
2.1 flush solvent inhalation:
the four-way selector valve 1 is switched to the No. 1 position, and the injection pump 2 sucks washing liquid quantitatively.
2.2 flushing and flushing solvent discharge
The four-way selector valve 1 is switched to No. 3, and the injection pump 2 pushes the flushing liquid to the direction of the liquid inlet pipe until the internal flushing solvent is completely pushed out. The purge valve 3NO port is opened to introduce solvent into the heat exchange assembly. The excess solvent flows through the sample tube 7 and passes through the pressure-preparation coil 8 and is pressed into the reflux pool 9. The NC port of the waste valve 4 is opened, and the solvent is poured into the waste bottle 12.
After the syringe pump 2 has pushed all the solvent out, the purge valve 3 is switched to the NC port and nitrogen from the nitrogen source 13 is passed through the purge valve 3 into the liquid path and blows all the remaining solvent in the coil, sample tube 7 and reflux cell 9 into the waste bottle 12.
The steps 2.1 and 2.2 are circulated for 1-3 times, and the extraction solvent can be completely washed away for subsequent steps.
And step 3: blow drying of solid sample residue
In the final state of step 2.2, a nitrogen purge is continued. Until the nitrogen gas completely dried the solid sample residue in the sample tube 7. Through this step, the sample tube 7 can be directly weighed without being dried by other devices.
The above, only be the concrete implementation of the preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art is in the technical scope of the present invention, according to the technical solution of the present invention and the utility model, the concept of which is equivalent to replace or change, should be covered within the protection scope of the present invention.
Claims (2)
1. A pressurizing extraction device for replacing a Soxhlet extractor in material analysis is characterized by comprising a four-way selection valve (1), an injection pump (2), a purge valve (3), a waste discharge valve (4), a temperature control and heating device (5), a heat exchange assembly and a coil pipe (6), a sample pipe (7), a pressure preparation coil pipe (8), a backflow pool (9), an extract liquid bottle (10), a flushing liquid bottle (11) and a waste liquid bottle (12), wherein the extract liquid bottle (10) is communicated with the four-way selection valve (1), the flushing liquid bottle (11) is communicated with the four-way selection valve (1), the purge valve (3) is communicated with the heat exchange assembly and the coil pipe (6), the temperature control and heating device (5) is connected with the heat exchange assembly and the coil pipe (6), and the heat exchange assembly and the coil pipe (6) are communicated with the sample pipe (7), sample cell (7) with prepare pressure coil pipe (8) intercommunication, prepare pressure coil pipe (8) with backward flow pond (9) intercommunication, backward flow pond (9) with waste discharge valve (4) intercommunication, waste discharge valve (4) with four-way selector valve (1) intercommunication, waste discharge valve (4) with waste liquid bottle (12) intercommunication, the output of syringe pump (2) with four-way selector valve (1) intercommunication.
2. The pressurized extraction device for replacing the Soxhlet extractor in material analysis according to claim 1, wherein the sample tube (7) is a 304 stainless steel hollow column.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114210092A (en) * | 2021-11-30 | 2022-03-22 | 中科优术(黑龙江)科技产业有限公司 | Low-temperature negative-pressure type extraction integrated device and extraction method |
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2021
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114210092A (en) * | 2021-11-30 | 2022-03-22 | 中科优术(黑龙江)科技产业有限公司 | Low-temperature negative-pressure type extraction integrated device and extraction method |
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