CN112578057A - Pretreatment method and device for semi-volatile organic compounds in underground water - Google Patents
Pretreatment method and device for semi-volatile organic compounds in underground water Download PDFInfo
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Abstract
The invention provides a pretreatment method and a pretreatment device for semi-volatile organic compounds in underground water, wherein the device adopted by the method at least comprises 3 layers of organic pretreatment devices with detachable operation tables for treatment, the top operation table is used for placing a separating funnel and a positive pressure filtering device, the middle operation table is used for placing a drying and purifying device and a concentrating cup, the bottom operation table is used for placing a sample bottle, and an extraction flow path formed on the basis of the device is used for performing combined extraction by using normal hexane and dichloromethane in sequence so as to pretreat organic chlorine pesticides, polycyclic aromatic hydrocarbons, nitrobenzene compounds, polychlorinated biphenyl total amount, organic phosphorus pesticides, chlorothalonil and atrazine 7 type to-be-detected substances in an underground water sample, so that the liquid-liquid extraction operation treatment efficiency and stability in the organic pretreatment process are greatly improved, and the detection precision and sensitivity are improved.
Description
Technical Field
The invention relates to the technical field of organic matter pretreatment, in particular to a pretreatment method and a pretreatment device for semi-volatile organic matters in underground water.
Background
In organic analysis, gas, liquid or solid samples are in most cases complex in composition and exist in the form of heterogeneous phases. Such as oil aerosol and floating dust contained in the atmosphere, emulsion, solid particles and suspended matters contained in the wastewater, water, microorganisms, stones and the like in the soil, so that a complex sample can be analyzed and determined only after pretreatment, and the specific purpose is to concentrate trace components to be detected, improve the sensitivity of the method and reduce the detection limit; removing matrix and other interfering substances in the sample; through derivatization and other reactions, the object to be detected is converted into a substance with higher detection sensitivity or a substance which can be separated from interfering components in the sample, so that the sensitivity and the selectivity of the method are improved; the quality and the volume of the sample are concentrated, so that the sample is convenient to transport and store, and the stability of the sample is improved, so that the sample is not influenced by air; the analytical instrument and the test system are protected from affecting performance and lifetime together.
The method mainly adopts a liquid-liquid extraction mode to the organic matter pretreatment process of organic chlorine pesticides, polycyclic aromatic hydrocarbons, nitrobenzene compounds, polychlorinated biphenyl total, organic phosphorus pesticides, chlorothalonil and atrazine 7 to-be-detected substances, and the liquid-liquid extraction process relates to a large number of operation steps and comprises the following steps: liquid separation, shaking, liquid transfer, drying, concentration, and the like, the operation process is complicated, and errors are likely to occur.
Disclosure of Invention
In view of this, the embodiment of the present invention provides a method and an apparatus for pre-treating semi-volatile organic compounds in groundwater, which can efficiently pre-treat organic compounds in a water sample by establishing a stable liquid-liquid extraction flow path, thereby improving the pre-treatment efficiency and reducing errors caused by manual operations.
The technical scheme of the invention is as follows:
on one hand, the invention provides a pretreatment method of semi-volatile organic compounds in underground water,
the method adopts an organic pretreatment device at least comprising 3 layers of detachable operation platforms for processing, wherein the top operation platform is used for placing a plurality of separating funnels and a plurality of positive pressure filtering devices, the middle operation platform is used for placing a plurality of drying and purifying devices and a plurality of concentration cups, the bottom operation platform is used for placing a plurality of sample bottles, and the separating funnels, the drying and purifying devices, the concentration cups and the sample bottles are aligned in the vertical direction to form an extraction path, and the method comprises the following steps:
quantitatively collecting a sample by using the sample bottle;
removing the middle operating platform, introducing a quantitative sample into the positive pressure filtering device from the sample bottle of the bottom operating platform, and introducing the sample into the separating funnel after filtering;
adding n-hexane with a first set amount into the separating funnel for multiple times, oscillating and standing after adding the n-hexane every time, wherein an liquid-liquid extraction oscillator is arranged on the top operating platform for oscillating;
introducing the first raffinate in the lower layer of the separating funnel into the original sample bottle along an extraction path;
removing the bottom layer operating platform, installing the middle layer operating platform, and placing the drying and purifying device and a concentration cup connected with the drying and purifying device on the middle layer operating platform;
drying the residual first extract liquid in the separating funnel by the drying and purifying device and then introducing the first extract liquid into the concentrating cup;
reintroducing the first raffinate stored in the sample bottle into the separating funnel, adding a second set amount of dichloromethane for multiple times, oscillating and standing after adding the dichloromethane for each time, wherein the top operation table is provided with a liquid-liquid extraction oscillator for oscillation;
leading the second extract liquid of the lower layer in the separating funnel into the concentration cup along an extraction path after being processed by the drying and purifying device;
and (3) heating the mixed solution in the concentration cup through a water bath, blowing nitrogen to concentrate the mixed solution to 1.0mL, and adding an internal standard substance mixed standard solution.
In some embodiments, the sample comprises: raw water sample, laboratory blank sample standard and matrix standard.
In some embodiments, the mixture in the concentration cup is concentrated to 1ml by heating in a water bath and blowing nitrogen.
In some embodiments, before the mixture in the concentration cup is introduced into a parallel concentrator for concentration, the method further includes: the extract flow path was flushed with dichloromethane and introduced into the concentration cup.
In some embodiments, the sample vial has a capacity of 1L, the first set amount is 50ml, and the second set amount is 50 ml.
In some embodiments, the positive pressure filtration device employs a glass fiber filter membrane for filtration; and the drying and purifying device adopts anhydrous sodium sulfate for drying treatment.
On the other hand, the invention also provides a pretreatment device for semi-volatile organic compounds in underground water, which comprises:
the frame comprises a frame main body and at least three layers of detachable operation platforms, wherein the operation platforms are sequentially arranged on the frame main body along the vertical direction, and each operation platform is respectively provided with an operation window corresponding to the position; the bottom of the frame main body is provided with a roller; the operation table of the bottom layer consists of two adjacent sub-supporting layers, and the diameter of an operation window of the upper sub-supporting layer is larger than that of the operation window of the lower sub-supporting layer;
the positive pressure filtering device is fixed on the operating platform at the top layer;
the drying and purifying device is fixed on the operating table of the middle layer, and a glass wool and anhydrous sodium sulfate filling layer are arranged in the drying and purifying device;
the separating funnel is arranged in each operation window of the operation table at the top layer, and a liquid inlet of the separating funnel is detachably connected with the positive pressure filtering device;
the concentration cup is arranged on the operating platform in the middle layer, and the cup opening of the concentration cup is detachably connected with the drying and purifying device;
and the sample bottles are arranged in the operation windows of the operation table on the bottom layer.
In some embodiments, the positive pressure filtering device is fixed on the operating platform of the top layer through a triangular support, and an oscillator is further arranged on the operating platform of the top layer.
In some embodiments, an air pressure pump for supplying pressure and a glass fiber filter membrane for filtering are arranged in the positive pressure filtering device.
In some embodiments, the interval between two adjacent sub-support layers is 3cm, the diameter of the operation window of the upper sub-support layer is 6.6cm, and the diameter of the operation window of the lower sub-support layer is 1 cm.
The beneficial effects of the invention at least comprise:
according to the pretreatment method and the device for the semi-volatile organic compounds in the underground water, the stable liquid-liquid extraction flow path is established by configuring the multilayer operation tables, and the operation steps of liquid separation, oscillation, liquid transfer and the like are simplified, so that the liquid-liquid extraction operation treatment efficiency and stability in the organic pretreatment process are greatly improved, and the detection precision and sensitivity are improved.
Furthermore, each layer of operation platform of the device can be freely assembled and disassembled, so that the maneuverability is improved, the form can be randomly changed according to the operation steps, the detection purpose is achieved, the liquid transfer smoothness and stability are guaranteed, and the detection precision is improved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
It will be appreciated by those skilled in the art that the objects and advantages that can be achieved with the present invention are not limited to the specific details set forth above, and that these and other objects that can be achieved with the present invention will be more clearly understood from the detailed description that follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. The components in the figures are not necessarily to scale, emphasis instead being placed upon illustrating the principles of the invention. For purposes of illustrating and describing some portions of the present invention, corresponding parts of the drawings may be exaggerated, i.e., may be larger, relative to other components in an exemplary apparatus actually manufactured according to the present invention. In the drawings:
FIG. 1 is a diagram of a testing apparatus for a method of pre-treating semi-volatile organic compounds in groundwater according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart illustrating a method for pre-treating semi-volatile organic compounds in groundwater according to another embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a pretreatment device for semi-volatile organic compounds in groundwater according to an embodiment of the present invention;
fig. 4 is a schematic structural view of an operation table for removing an intermediate layer of the pretreatment device for semi-volatile organic compounds in groundwater according to an embodiment of the present invention.
110: a frame main body; 111: a slot; 120: a top layer operation platform;
130: an intermediate layer operating table; 140: a bottom layer operation table; 1401: an upper sub-support layer;
1402: a lower sub-support layer; 150: operating a window; 160: a separating funnel;
170: a sample bottle; 180: and a roller.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following embodiments and accompanying drawings. The exemplary embodiments and descriptions of the present invention are provided to explain the present invention, but not to limit the present invention.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme according to the present invention are shown in the drawings, and other details not so relevant to the present invention are omitted.
It should be emphasized that the term "comprises/comprising" when used herein, is taken to specify the presence of stated features, elements, steps or components, but does not preclude the presence or addition of one or more other features, elements, steps or components.
It is also noted herein that the term "coupled," if not specifically stated, may refer herein to not only a direct connection, but also an indirect connection in which an intermediate is present.
Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings. In the drawings, the same reference numerals denote the same or similar parts, or the same or similar steps.
49 organic matter indexes in the groundwater quality standard (GB/T14848-2017) comprise: 22 volatile organic compounds, 5 organochlorine pesticides, 5 polycyclic aromatic hydrocarbons, 2 nitrobenzene compounds, the total amount of polychlorinated biphenyl, 5 organophosphorus pesticides, chlorothalonil, atrazine, di (2-ethylhexyl) phthalate, 2 phenol compounds, 2,4-D, 2 carbamate pesticides and glyphosate. The volatile organic compounds are measured by adopting a sweeping trapping-gas chromatography-mass spectrometry method, 2,4-D, 2 carbamate pesticides and glyphosate are measured by adopting a liquid chromatography-mass spectrometry method, the related pretreatment process is simple, and the discussion is omitted. The rest 23 semi-volatile organic compounds are divided into 9 major classes according to chemical properties, the boiling point is within the range of 219-475 ℃, and for 7 classes of the 9 classes, organic chlorine pesticides, polycyclic aromatic hydrocarbons, nitrobenzene compounds, polychlorinated biphenyl total amount, organic phosphorus pesticides, chlorothalonil and atrazine, a liquid-liquid extraction flow is selected to complete pretreatment, so that the sampling amount is reduced, the pretreatment efficiency is improved, but the applicability of the pretreatment process is wide, and 7 classes of compounds can be effectively recovered. But the liquid-liquid extraction pretreatment process has more operation steps and large workload, and the application integrates semi-automatic operation tools and modes in order to reduce the workload of operation and human errors.
Therefore, the present application provides an organic pretreatment method based on a novel organic pretreatment device, as shown in fig. 1, the method for pretreating semi-volatile organic compounds in groundwater adopts an organic pretreatment device including at least 3 layers of detachable operation platforms, the top operation platform 120 is used for placing a plurality of separating funnels 160 and a plurality of positive pressure filtering devices, the middle operation platform 130 is used for placing a plurality of drying and purifying devices (not shown in the figure) and a plurality of concentration cups (not shown in the figure), the bottom operation platform 140 is used for placing a plurality of sample bottles 170, and the separating funnels 160, the drying and purifying devices, the concentration cups and the sample bottles 170 are aligned in a vertical direction to form an extraction path, as shown in fig. 2, the method includes steps S101 to S108:
step S101: the sample is quantitatively collected using a sample bottle 170.
Step S102: the middle stage 130 is removed and a fixed amount of sample is introduced from the sample bottle 170 of the bottom stage 140 into the positive pressure filtration device, filtered and introduced into the separatory funnel 160.
Step S103: a first set amount of n-hexane was added to the separatory funnel 160 in several portions, shaken and allowed to stand after each addition of the n-hexane, wherein shaking was performed by setting a liquid-liquid extraction shaker (not shown) on the top stage 120.
Step S104: the lower first raffinate from the separatory funnel 160 is directed along the extraction path to the raw sample bottle 170.
Step S105: the bottom stage 140 is removed, the middle stage 130 is installed, and the dry-cleaning device and the thickening cup connected to the dry-cleaning device are placed on the middle stage 130.
Step S106: the remaining first extract from the separatory funnel 160 is dried by a drying and purifying apparatus and then introduced into a concentrating cup.
Step S107: the first raffinate retained in the sample bottle 170 was reintroduced into the separatory funnel 160, and a second set amount of dichloromethane was added in multiple portions, and after the additional addition of dichloromethane, the two portions were shaken and left to stand, wherein the shaking was performed by installing a liquid-liquid extraction shaker on the top stage 120.
Step S108: the lower layer of the second extract in the separating funnel 160 is processed by the drying and purifying device and then introduced into the concentrating cup along the extraction path.
Step S109: and heating the mixed solution in the concentration cup through a water bath, blowing nitrogen for concentration, and adding an internal standard substance mixed standard solution.
The method utilizes the n-hexane and the dichloromethane for combined extraction, carries out organic pretreatment on 7 types of organic matters to be detected, including organochlorine pesticide, polycyclic aromatic hydrocarbon, nitrobenzene compounds, total amount of polychlorinated biphenyl, organophosphorus pesticide, chlorothalonil and atrazine, respectively utilizes the n-hexane and the dichloromethane for alternate extraction, combines and concentrates raffinate obtained twice, and is used for subsequent detection, thereby further improving the detection precision.
In step S101, a sample of groundwater is collected through the sample bottle 170, and a specific sample bottle 170 is selected according to the nature of the reagent to be added and the analysis item. Most organic targets must be collected with glass, while inorganic targets can be collected with plastics or fluoropolymers in addition to glass. In particular, the detection items need to adopt brown bottles to prevent the influence of illumination. The capacity of the sample vial 170 may be set with reference to experimental requirements. The sample bottle may have a capacity of 1L.
In some embodiments, the sample comprises: raw water sample, laboratory blank sample standard and matrix standard.
For more accurate studies, accurate qualitative and quantitative analysis results, control tests are required. Wherein the raw water sample is groundwater raw water; the laboratory blank was a pure water sample; the laboratory blank adding standard sample refers to adding a known amount of standard substance into pure water; the sample is a matrix except the object to be detected, and the matrix and the standard sample are obtained by adding a known amount of standard substances into the matrix.
In step S102, the organic pretreatment apparatus having a multilayer structure allows the separatory funnel 160, the sample bottle 170, and the concentration bottle to be arranged vertically, and a stable liquid-liquid extraction flow path is formed without moving equipment manually. The sample bottle 170 is disposed on the bottom stage 140, and is directly introduced into the separating funnel 160 disposed on the top stage 120 after being filtered by the positive pressure filtering device, and the sample bottle 170 is controlled to further retain the raffinate generated by the first extraction. The positive pressure filtering device is used for filtering suspended matters or sediments in water.
In step S103, n-hexane is used for the first extraction, and is a straight-chain saturated aliphatic hydrocarbon, and has strong solubility to organochlorine pesticides, polycyclic aromatic hydrocarbons, nitrobenzene compounds, polychlorinated biphenyl, organophosphorus pesticides, chlorothalonil and atrazine, almost insoluble in water, has a boiling point of 68 ℃, and is easy to volatilize. During extraction, the separatory funnel 160 needs to be shaken well and a sufficient time for separation is ensured in order to transfer more of the compound to be measured to the extractant. The first set amount of n-hexane added may be 50ml based on a 1L capacity of a sampling bottle. Further, in this example, the oscillation time was 10min, and the standing time was 10 min.
Further, n-hexane is added for multiple times, and oscillation and standing are carried out after each addition so as to fully improve the extraction effect. The oscillation operation is performed using a liquid-liquid extraction oscillator, which is disposed on the top stage 120, directly fixes the separatory funnel, and can complete all operations without moving the separatory funnel.
In step S104, when n-hexane is used for extraction, the layered extract is on the upper layer of the raffinate, that is, the n-hexane solution is on the upper layer of the groundwater sample solution, because the density of n-hexane is low. The lower, first raffinate is directed to the original sample bottle 170 using a separatory funnel 160 and is retained for further extraction. The introduction of the raw sample bottle 170 can wash the residual liquid in the raw sample bottle 170 to improve the detection accuracy.
Further, because separating funnel 160, dry purifier, concentration cup and sample bottle 170 align along vertical direction, the process of shifting out first extraction liquid only need open separating funnel 160's top plug and piston, and first extraction liquid becomes the extraction route that can predetermine and flows to former sample bottle 170, and the position is accurate, does not need mobile device, has greatly reduced the error that moves liquid and produce.
In step S105, the bottom stage 140 of the apparatus is removed and the middle stage 130 is installed in preparation for combining the extraction solutions. The drying and purifying device can adopt anhydrous sodium sulfate or other drying agents. The drying and purifying device and the concentrating cup are arranged at the lower side of the separating funnel 160 and communicated with each other for receiving the extract.
In step S106, the first extraction liquid (n-hexane solution) remaining in the separatory funnel 160 during the first extraction process is discharged, and introduced into a concentration cup through a drying and purifying apparatus for temporary storage.
In step S107, the first raffinate held in the raw sample bottle 170 is reintroduced into the separatory funnel 160 to be subjected to the second extraction. The second extraction is carried out by adopting dichloromethane which is colorless transparent liquid, is slightly soluble in water, has irritant odor similar to ether, has boiling point of 39.8 ℃, is volatile and can be dissolved with normal hexane. The second set amount of methylene chloride added may be 50ml based on a sample bottle having a capacity of 1L. Further, in this example, the oscillation time was 10min, and the standing time was 10 min.
Further, dichloromethane is added in multiple times, and oscillation and standing are carried out after each addition, so that the extraction effect is fully improved. The oscillation operation is performed using a liquid-liquid extraction oscillator, which is disposed on the top stage 120, directly fixes the separatory funnel, and can complete all operations without moving the separatory funnel.
In step S108, the dichloromethane used in the second extraction is layered and located at the lower layer, i.e., the extract is at the lower layer and the raffinate is at the upper layer. And (4) treating the second extraction liquid at the lower layer in the paging funnel by a drying and purifying device, then introducing the second extraction liquid into a concentration cup, and combining the second extraction liquid with the first extraction liquid in the step (S106) to obtain a mixed liquid serving as a final extraction liquid. The remaining sample in the separatory funnel 160 is discarded and washed.
Furthermore, the process of removing the second extraction liquid only needs to open the top plug and the piston of the separating funnel 160, the second extraction liquid becomes a preset extraction path and flows into the concentration cup, the position is accurate, equipment does not need to be moved, and errors caused by liquid transfer are greatly reduced.
In step S109, the mixture of the first extract and the second extract obtained by the two extractions is concentrated, and the next detection is performed. In some embodiments, an internal standard may be added to mix with the standard solution for subsequent quantitative analysis. The third extract was concentrated to 1ml in some embodiments by a parallel concentrator using a water bath heated nitrogen-blown concentration. The subsequent drying and concentrating process can be saved, and the time consumption is greatly reduced.
In some embodiments, before step S109, before the step of introducing the third extraction liquid in the concentrating cup into the parallel concentrator for concentrating, the method further includes: the extract flow path was rinsed with dichloromethane and introduced into a concentration cup.
In this embodiment, in order to prevent the analyte from remaining in the extraction liquid flow path, the extraction liquid is washed by the extraction agent to improve the accuracy of the test.
In some embodiments, the positive pressure filtration device utilizes a glass fiber membrane filter for filtration.
The glass fiber filter membrane is made of high-purity alkali-free superfine glass fiber, is chemically inert, is a deep filter membrane made of no adhesive and is formed by pressing pure fiber. Has the advantages of small resistance and high filtering efficiency, and can bear the high temperature of 550 ℃. High porosity, high flux, high flow-intercepting capacity and high corrosion resistance.
On the other hand, the invention also provides a pretreatment device for semi-volatile organic compounds in groundwater, as shown in fig. 3, comprising:
the frame comprises a frame main body 110 and at least three layers of detachable operation tables, wherein the operation tables are sequentially arranged on the frame main body 110 along the vertical direction, and each operation table is respectively provided with an operation window 150 corresponding to the position; the bottom of the frame body 110 is provided with a roller 180; the operation table at the bottom layer consists of two adjacent sub-support layers, and the diameter of the operation window 150 of the upper sub-support layer 1401 is larger than that of the operation window 150 of the lower sub-support layer 1402;
a positive pressure filter (not shown) fixed to the top stage;
a drying and purifying device (not shown in the figure) fixed on the operation table of the middle layer, wherein a glass wool and anhydrous sodium sulfate filling layer are arranged in the drying and purifying device;
a separating funnel 160 arranged in each operation window 150 of the operation table 120 at the top layer, wherein a liquid inlet of the separating funnel 160 is detachably connected with a positive pressure filtering device;
a concentration cup (not shown in the figure) which is arranged on the operation table of the middle layer, and the cup mouth of the concentration cup can be detachably arranged on the drying and purifying device;
and a sample bottle 170 disposed in each of the manipulation windows 150 of the lower stage 140.
In this embodiment, the pretreatment device for semi-volatile organic compounds in groundwater is used for extracting solutes to be detected in a sample, and the carriage body 110 may have a rectangular frame structure or other shapes. To prevent corrosion or corrosion by chemical agents, the frame body 110 may be made of stainless steel material or sprayed with a corrosion-resistant coating, such as epoxy corrosion-resistant paint.
The table top of the operation table is horizontally arranged for placing processing equipment, and the operation tables are sequentially aligned in the vertical direction and used for constructing an extraction channel flowing by gravity. The operation panel is detachable for the corresponding relation between each operation panel of configuration according to the experiment needs. Referring to fig. 4, the console and the frame body 110 may be connected by a slot 111 and a latch, or may be connected by a latch or other means.
The operation table is provided with an operation window 150 for communicating the operation table surfaces of all layers, so that the extraction equipment can be communicated in the vertical direction. The shape of the operating window 150 is a circular through hole, and can be configured to a corresponding shape according to the needs of a specific equipment container.
The bottom of the frame body 110 is provided with a roller 180, the roller 180 can be a universal caster or an omni-directional wheel, and the roller 180 can be further provided with a lock catch to fix the frame body 110 in a working state to prevent sliding.
The operation panel of bottom is generally used for placing sample bottle 170, sampling bottle etc. for the guarantee stability, and the operation panel of bottom comprises adjacent two sub-supporting layers, and the operation window 150 diameter of upper sub-supporting layer 1401 is greater than lower sub-supporting layer 1402, and sampling bottle or sample bottle 170 is held by lower sub-supporting layer 1402, is fixed by upper sub-supporting layer 1401, prevents the slippage.
In some embodiments, the adjacent two sub-support layers are spaced 3cm apart, the operating window 150 of the upper sub-support layer 1401 is 6.6cm in diameter, and the operating window 150 of the lower sub-support layer 1402 is 1cm in diameter.
The positive pressure filtering device is fixed on the operating platform of the top layer through a triangular support, and the operating platform of the top layer is also provided with an oscillator.
Positive pressure filtration devices, also known as compact mechanical filters, are manufactured from stainless steel and are used for filtering liquids, clarification and sterilization. The positive pressure filter is filled with different filter media, has different purposes and functions, can specifically adopt multi-media filtration, activated carbon filtration and membrane filtration, and the equipment is often used jointly but also can be used independently in water treatment engineering.
In some embodiments, a pneumatic pump for supplying pressure and a glass fiber filter membrane for filtering are arranged in the positive pressure filtering device.
The drying and purifying device is used for removing residual water in the extraction liquid so as to improve the detection precision.
In some embodiments, the pretreatment method of the semi-volatile organic compounds in the groundwater mainly comprises the following steps:
1) water sample filtration: when suspended matters or precipitates exist in a water sample, glass microfiber filter paper is required to be used for filtering;
2) water sample extraction: adding a substitute use solution into a water sample, a laboratory blank labeling sample and a matrix labeling sample, adding a standard use solution containing a detection component into the laboratory blank labeling sample and the matrix labeling sample, adding 50mL of n-hexane as an extraction solvent, oscillating for 10min, standing for 10min, and taking an upper organic solvent; then 50mL of dichloromethane is added as an extraction solvent, the mixture is shaken for 10min and kept stand for 10min, and then the organic solvent of the lower layer is taken out. The two extraction solvents were combined.
3) Drying and purifying: the extract was dried over anhydrous sodium sulfate and placed in a concentration cup.
4) Concentrating the extract liquor: heating in water bath, blowing nitrogen to concentrate to 1.0mL, adding internal standard substance mixed standard solution, and waiting for analysis.
Further, adopt the semi-volatile organic compounds pretreatment tool bogie in the groundwater:
all materials of the tool bogie are stainless steel, the tool bogie comprises three layers of operation tables, can be pulled, has 10 openings on each layer, corresponds to one layer, can process 10 samples simultaneously, is a positive pressure filtering device on the 1 st layer, has the capacity of 1.0L, is more than or equal to 0.3MPa in pressure resistance, supplies pressure to an air pressure pump, has a replaceable filter membrane at an outlet, is fixed by a triangular support, and corresponds to the upper opening of a separating funnel on the 1 st layer.
A separating funnel is placed on the operation table of the layer 1, and the inner diameter of an opening is 14.5 cm; a drying and purifying device is arranged on the operation table of the layer 2, the inner diameter of an opening is 2.5cm, and glass wool and anhydrous sodium sulfate are filled in the device; the layer 3 operation platform is used for placing a concentration cup and/or a sample bottle and is divided into two small layers, wherein the distance between the two small layers is 3cm, the inner diameter of an opening of the upper layer is 6.6cm, and the inner diameter of an opening of the lower layer is 1 cm.
Aiming at 7 types of organic matters to be detected, namely organic chlorine pesticide, polycyclic aromatic hydrocarbon, nitrobenzene compounds, polychlorinated biphenyl, organic phosphorus pesticide, chlorothalonil and atrazine, the groundwater pretreatment method comprises the following steps: introducing a sample into a filtering device from a sample bottle, filtering by positive pressure and a glass fiber filter membrane, directly entering a separating funnel, adding n-hexane, oscillating for 10min by an oscillator, and standing for 10min on a tool car; at the moment, the layer 2 is drawn out, referring to fig. 4, a 1L sample bottle (the height of the sample bottle is 25cm, the outer diameter is 9.5cm) is placed on the layer 3, a water sample enters the original sample bottle from the lower opening of the separating funnel, and the sample bottle is taken away; installing the layer 2, placing a drying and purifying device, placing a concentrating cup on the layer 2, and drying and purifying the extract liquor in the separating funnel to enter the concentrating cup; adding the water sample into the separating funnel again, adding dichloromethane, oscillating for 10min by using an oscillator, and standing for 10min by using a tool car; the dichloromethane is discharged from a separating funnel at the lower layer, enters a concentration cup through a drying and purifying device, and a small amount of dichloromethane is used for washing an extract liquid flow path; the extract was concentrated by a parallel concentrator and the separatory funnel samples were discarded for cleaning.
In summary, the pretreatment method and device for semi-volatile organic compounds in underground water establish a stable liquid-liquid extraction flow path by configuring a plurality of layers of operation platforms, simplify operation steps such as liquid separation, oscillation and liquid transfer, and enable the whole pretreatment process of liquid-liquid extraction to be connected in series, thereby realizing semi-automation of the pretreatment process, greatly reducing workload, greatly improving treatment efficiency and stability of liquid-liquid extraction operation in the organic pretreatment process, reducing transfer times in the processes of collecting extract, purifying and drying, improving recovery rate of samples, and simultaneously improving detection precision and sensitivity.
Furthermore, each layer of operation platform of the device can be freely assembled and disassembled, so that the maneuverability is improved, the form can be randomly changed according to the operation steps, the detection purpose is achieved, the liquid transfer smoothness and stability are guaranteed, and the detection precision is improved.
It should also be noted that the exemplary embodiments mentioned in this patent describe some methods or systems based on a series of steps or devices. However, the present invention is not limited to the order of the above-described steps, that is, the steps may be performed in the order mentioned in the embodiments, may be performed in an order different from the order in the embodiments, or may be performed simultaneously.
Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments and/or in combination with or instead of the features of the other embodiments in the present invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made to the embodiment of the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The pretreatment method for semi-volatile organic compounds in underground water is characterized by comprising the following steps of treating by adopting an organic pretreatment device at least comprising 3 layers of detachable operation platforms, wherein the top operation platform is used for placing a plurality of separating funnels and a plurality of positive pressure filtering devices, the middle operation platform is used for placing a plurality of drying and purifying devices and a plurality of concentration cups, the bottom operation platform is used for placing a plurality of sample bottles, and the separating funnels, the drying and purifying devices, the concentration cups and the sample bottles are aligned in the vertical direction to form an extraction path, and the method comprises the following steps:
quantitatively collecting a sample by using the sample bottle;
removing the middle operating platform, introducing a quantitative sample into the positive pressure filtering device from the sample bottle of the bottom operating platform, and introducing the sample into the separating funnel after filtering;
adding n-hexane with a first set amount into the separating funnel for multiple times, oscillating and standing after adding the n-hexane every time, wherein an liquid-liquid extraction oscillator is arranged on the top operating platform for oscillating;
introducing the first raffinate in the lower layer of the separating funnel into the original sample bottle along an extraction path;
removing the bottom layer operating platform, installing the middle layer operating platform, and placing the drying and purifying device and a concentration cup connected with the drying and purifying device on the middle layer operating platform;
drying the residual first extract liquid in the separating funnel by the drying and purifying device and then introducing the first extract liquid into the concentrating cup;
reintroducing the first raffinate stored in the sample bottle into the separating funnel, adding a second set amount of dichloromethane for multiple times, oscillating and standing after adding the dichloromethane for each time, wherein the top operation table is provided with a liquid-liquid extraction oscillator for oscillation;
leading the second extract liquid of the lower layer in the separating funnel into the concentration cup along an extraction path after being processed by the drying and purifying device;
and heating the mixed solution in the concentration cup through a water bath, blowing nitrogen for concentration, and adding an internal standard substance mixed standard solution.
2. The method of claim 1, wherein the sample comprises: raw water sample, laboratory blank sample standard and matrix standard.
3. The pretreatment method for semi-volatile organic compounds in groundwater according to claim 1, wherein the mixed solution in the concentration cup is concentrated to 1ml by heating in water bath and blowing nitrogen.
4. The method for pre-treating semi-volatile organic compounds in groundwater according to claim 1, wherein before introducing the mixed solution in the concentration cup into a parallel concentration apparatus for concentration, the method further comprises: the extract flow path was flushed with dichloromethane and introduced into the concentration cup.
5. The method of claim 1, wherein the sample bottle has a capacity of 1L, the first set amount is 50ml, and the second set amount is 50 ml.
6. The pretreatment method for semi-volatile organic compounds in groundwater according to claim 1, wherein the positive pressure filtration device is used for filtration with a glass fiber membrane; and the drying and purifying device adopts anhydrous sodium sulfate for drying treatment.
7. A semi-volatile organic compounds pretreatment device in groundwater is characterized by comprising:
the frame comprises a frame main body and at least three layers of detachable operation platforms, wherein the operation platforms are sequentially arranged on the frame main body along the vertical direction, and each operation platform is respectively provided with an operation window corresponding to the position; the bottom of the frame main body is provided with a roller; the operation table of the bottom layer consists of two adjacent sub-supporting layers, and the diameter of an operation window of the upper sub-supporting layer is larger than that of the operation window of the lower sub-supporting layer;
the positive pressure filtering device is fixed on the operating platform at the top layer;
the drying and purifying device is fixed on the operating table of the middle layer, and a glass wool and anhydrous sodium sulfate filling layer are arranged in the drying and purifying device;
the separating funnel is arranged in each operation window of the operation table at the top layer, and a liquid inlet of the separating funnel is detachably connected with the positive pressure filtering device;
the concentration cup is arranged on the operating platform in the middle layer, and the cup opening of the concentration cup is detachably connected with the drying and purifying device;
and the sample bottles are arranged in the operation windows of the operation table on the bottom layer.
8. The apparatus of claim 7, wherein the positive pressure filter device is fixed on the top stage by a triangular bracket, and an oscillator is further provided on the top stage.
9. The apparatus of claim 7, wherein the positive pressure filtration device is provided with an air pressure pump for supplying pressure and a glass fiber filter membrane for filtration.
10. The device of claim 7, wherein the interval between two adjacent sub-support layers is 3cm, the diameter of the operation window of the upper sub-support layer is 6.6cm, and the diameter of the operation window of the lower sub-support layer is 1 cm.
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