CN111257076A - Pretreatment method for extracting organochlorine pesticide in soil - Google Patents
Pretreatment method for extracting organochlorine pesticide in soil Download PDFInfo
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- CN111257076A CN111257076A CN202010112099.XA CN202010112099A CN111257076A CN 111257076 A CN111257076 A CN 111257076A CN 202010112099 A CN202010112099 A CN 202010112099A CN 111257076 A CN111257076 A CN 111257076A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention discloses a pretreatment method for extracting organochlorine pesticide in soil, which is used for treating soil to be detected before extracting organochlorine pesticide by adopting a solution extraction method, aims to refine and homogenize sample soil, is beneficial to extraction of organochlorine pesticide, and mainly comprises the following steps: s1: carrying out centralized low-temperature air drying on the sample soil; s2: grinding the air-dried sample soil, and continuously air-drying; s3: collecting ground sample soil, and horizontally oscillating; s4: filling the vibrated sample soil in bottles, putting an anhydrous dehydrating agent into the filling bottles, and covering the bottles; s5: placing the filling bottle with the sample soil in a turnover shaking machine for shaking; s6: changing bottles and filling soil samples, adding anhydrous dehydrating agents, and covering; s7: carrying out ultrasonic smashing on a soil sample; s8: and finishing the soil pretreatment. The invention has the advantages of high efficiency, convenient operation and accurate result.
Description
Technical Field
The invention relates to the technical field of soil detection, in particular to a pretreatment method for extracting organochlorine pesticides in soil.
Background
Soil environment detection refers to determination of environmental quality (or pollution degree) and change trend thereof by measuring representative values of factors affecting soil environment quality, and soil monitoring generally refers to soil environment monitoring, which generally includes technical contents such as distribution sampling, sample preparation, analysis method, result characterization, data statistics, quality evaluation and the like.
The detection of organochlorine pesticides in soil belongs to a common soil detection type, and the extraction modes of organochlorine pesticides in existing soil and sediments mainly comprise the following modes: the existing pretreatment method is low in treatment efficiency, the soil needs to be treated firstly when the operation is linear, the organic chlorine pesticide can be quickly separated, and the detection effect is reported.
Disclosure of Invention
To the deficiency of the prior art, the technical problem to be solved by the present patent application is: how to provide a pretreatment method for extracting organochlorine pesticide in soil, which has high efficiency, convenient operation and accurate result.
In order to achieve the purpose, the invention adopts the following technical scheme:
a pretreatment method for extracting organochlorine pesticides in soil is used for treating soil to be detected before extracting organochlorine pesticides by adopting a solution extraction method, aims to refine and homogenize sample soil, is beneficial to extraction of organochlorine pesticides, and mainly comprises the following steps:
s1: carrying out centralized low-temperature air drying on the sample soil;
s2: grinding the air-dried sample soil, and continuously air-drying;
s3: collecting ground sample soil, and horizontally oscillating;
s4: filling the vibrated sample soil in bottles, putting an anhydrous dehydrating agent into the filling bottles, and covering the bottles;
s5: placing the filling bottle with the sample soil in a turnover shaking machine for shaking;
s6: changing bottles and filling soil samples, adding anhydrous dehydrating agents, and covering;
s7: carrying out ultrasonic smashing on a soil sample;
s8: and finishing the soil pretreatment.
Preferably, the air drying in the steps S1 and S2 is performed by a direct blowing manner in which a fan is additionally provided with a refrigeration pipeline, and the output temperature of the refrigeration pipeline is controlled to be 15-20 ℃, wherein the refrigeration pipeline avoids direct blowing of the soil sample during grinding, and the grinding machine is cooled.
Preferably, when the soil sample is ground in the step S2, a grinder, which is a JX2G mini planetary soil grinder, is used.
Preferably, the main body of the soil grinder is provided with an air inlet and an air outlet, and the refrigeration pipeline is hermetically connected with the air inlet.
Preferably, the anhydrous dehydrating agent is anhydrous sodium sulfate, and the anhydrous sodium sulfate is added to the mixture without agglomeration.
Preferably, the filling bottles in the steps S4 and S6 are cylindrical, and the bottom and the side walls are coated with teflon.
Preferably, in step S3, a horizontal oscillator is used for horizontal oscillation, and the horizontal oscillator is a JRY-S08 full-automatic horizontal oscillator.
Preferably, the upset in step S5 vibrates the drum that the machine includes the axis level setting, the drum includes the lower fixed half section of thick bamboo that the articulated setting of each other and the half section of thick bamboo that overturns on, coaxial arrangement has the pivot in the drum, pivot and leg joint, the pivot is connected with the driving motor transmission, axial fixedly connected with branch in the pivot, the branch tip rotates installs the installation section of thick bamboo, the installation section of thick bamboo in the installation fill bottle, the axis of installation section of thick bamboo with the axis of drum is parallel, the installation section of thick bamboo still is provided with the cover, the cover with installation section of thick bamboo bottom is just being provided with clamping spring, the outside fixed driving lever that is provided with in bottom of the lateral wall of installation section of thick bamboo, the driving lever is in with the setting the spout sliding connection of drum inside wall, the spout is in the drum for the wave setting.
Preferably, the rotating speed of the driving motor is 40r/min-60 rmin.
Preferably, in step S7, ultrasonic crushing is performed by using an ultrasonic instrument, and the service time is 2 hours.
Has the advantages that:
(1): the method can provide a complete set of soil pretreatment mode, and can fully refine the soil form after multistage oscillation and ultrasonic smashing, so that the maximum separation of organochlorine pesticide extraction is realized during subsequent solution extraction;
(2): the interference of water and liquid in the soil is effectively reduced, the adhesion of the wet soil to equipment during grinding, oscillation and ultrasonic treatment is reduced, and the loss is reduced;
(3): the input cost is low, batch processing can be realized without adopting larger equipment, and the processing efficiency is greatly improved.
Description of the drawings:
FIG. 1 is a schematic structural diagram of a pretreatment method for extracting organochlorine pesticides from soil disclosed by the invention.
Fig. 2 is a schematic structural diagram of the turnover shaker involved in the method.
Fig. 3 is a schematic view of the internal structure of fig. 2.
Fig. 4 is a schematic view of the internal structure of the expanded view of the cylinder according to the present invention.
FIG. 5 is a schematic view of the inner structure of the mounting barrel
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1-5, a pretreatment method for extracting organochlorine pesticides from soil, which is used for treating soil to be detected before extracting organochlorine pesticides by a solution extraction method, aims to refine and homogenize sample soil, and is beneficial to extraction of organochlorine pesticides, and is characterized by mainly comprising the following steps:
s1: carrying out centralized low-temperature air drying on the sample soil;
s2: grinding the air-dried sample soil, and continuously air-drying;
s3: collecting ground sample soil, and horizontally oscillating;
s4: filling the vibrated sample soil in bottles, putting an anhydrous dehydrating agent into the filling bottles, and covering the bottles;
s5: placing the filling bottle with the sample soil in a turnover shaking machine for shaking;
s6: changing bottles and filling soil samples, adding anhydrous dehydrating agents, and covering;
s7: carrying out ultrasonic smashing on a soil sample;
s8: and finishing the soil pretreatment.
Further, the air drying in the steps S1 and S2 is carried out in a direct blowing mode by adding a fan to a refrigeration pipeline, the output temperature of the refrigeration pipeline is controlled to be 15-20 ℃, the refrigeration pipeline avoids direct blowing of a soil sample during grinding, and the grinding machine is cooled.
Like this, the activity of organochlorine pesticide can be inhibited to the low temperature, avoids it to break away from in the sample soil, and then influences the efficiency and the accuracy that later stage detected, can air-dry when each form to sample soil simultaneously, avoids the too big interference that causes follow-up processing and detection of moisture.
Further, when the soil sample is ground in step S2, a grinder, which is a JX2G mini planetary soil grinder, is used.
Like this, equipment input is little, and is with low costs, and vibrate effectually, detect to play favorable effect to the small batch.
Furthermore, an air inlet and an air outlet are carried on the main body of the soil grinder, and the refrigeration pipeline is hermetically connected with the air inlet.
Thus, the grinding and air drying can be carried out simultaneously, the stability of the organochlorine pesticide is not damaged, and the detection accuracy is prevented from being damaged.
Further, the anhydrous dehydrating agent is anhydrous sodium sulfate, and the anhydrous sodium sulfate is added into the mixture and does not cake.
Therefore, the moisture in the sample soil can be further wife to achieve the maximum drying effect, and the subsequent treatment is positively performed.
Further, the filling bottles in the steps S4 and S6 are cylindrical, and the bottom and the side walls are coated with teflon.
Has effects of reducing sample soil adhesion and reducing loss
Further, in step S3, a horizontal oscillator is adopted during horizontal oscillation, and the horizontal oscillator is a JRY-S08 full-automatic horizontal oscillator.
Like this, this horizontal oscillator can realize the batched vibration, and the vibration effect is obvious, the sample soil that refines that can be further.
Further, the turnover oscillating machine in the step S5 includes a cylinder 1 with a horizontal axis, the cylinder 1 includes a lower fixed half cylinder and an upper turnover half cylinder hinged to each other, a rotating shaft 11 is coaxially installed in the cylinder 1, the rotating shaft 11 is connected to a bracket 12, the rotating shaft 11 is in transmission connection with a driving motor 13, a supporting rod 14 is axially and fixedly connected to the rotating shaft 11, an installation cylinder 15 is rotatably installed at an end of the supporting rod 14, the installation cylinder 15 is used for installing the filling bottle, an axis of the installation cylinder 15 is parallel to an axis of the cylinder 1, the installation cylinder 15 is further provided with a cylinder cover 16, the cylinder cover 16 and the bottom of the installation cylinder 15 are just provided with a clamping spring 17, a shift lever 18 is outwards fixedly installed at the bottom of the outer side wall of the installation cylinder 15, the shift lever 18 is in sliding connection with a sliding groove 19 formed in the inner side wall of the cylinder 1, the sliding grooves 19 are arranged in the cylinder 1 in a wave shape.
Like this, when providing a centrifugal oscillation for sample soil, the cooperation of driving lever and spout drives the installation section of thick bamboo and fills the bottle and realize the swing, increases the abundant refinement of inside sample soil.
Further, the rotating speed of the driving motor is 40r/min-60 rmin.
Further, in step S7, ultrasonic crushing is performed with an ultrasonic instrument for a use time of 2 hours.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A pretreatment method for extracting organochlorine pesticides in soil is used for treating soil to be detected before extracting organochlorine pesticides by adopting a solution extraction method, aims to refine and homogenize sample soil, and is beneficial to extraction of organochlorine pesticides, and is characterized by mainly comprising the following steps of:
s1: carrying out centralized low-temperature air drying on the sample soil;
s2: grinding the air-dried sample soil, and continuously air-drying;
s3: collecting ground sample soil, and horizontally oscillating;
s4: filling the vibrated sample soil in bottles, putting an anhydrous dehydrating agent into the filling bottles, and covering the bottles;
s5: placing the filling bottle with the sample soil in a turnover shaking machine for shaking;
s6: changing bottles and filling soil samples, adding anhydrous dehydrating agents, and covering;
s7: carrying out ultrasonic smashing on a soil sample;
s8: and finishing the soil pretreatment.
2. The pretreatment method for extracting organochlorine pesticides from soil according to claim 1, wherein the air drying in steps S1 and S2 is performed by directly blowing with a fan and a refrigeration pipeline, the output temperature of the refrigeration pipeline is controlled to be 15-20 ℃, the refrigeration pipeline avoids directly blowing the soil sample during grinding, and the grinding machine is cooled.
3. The pretreatment method for extracting organochlorine pesticides from soil according to claim 2, wherein a grinder is used for grinding the soil sample in step S2, and the grinder is a JX2G small planetary soil grinder.
4. The pretreatment method for extracting organochlorine pesticides from soil according to claim 3, wherein an air inlet and an air outlet are mounted on a main body of the soil grinder, and a refrigeration pipeline is hermetically connected with the air inlet.
5. The method for pretreating organic chloride pesticides in soil for extraction according to claim 4, wherein the anhydrous dehydrating agent is anhydrous sodium sulfate, and the anhydrous sodium sulfate is added to the mixture without agglomeration.
6. The method as claimed in claim 5, wherein the filling bottles of steps S4 and S6 are cylindrical and have polytetrafluoroethylene coatings on the bottom and the side walls.
7. The pretreatment method for extracting organochlorine pesticides in soil according to claim 6, wherein in the step S3, a horizontal oscillator is adopted during horizontal oscillation, and the horizontal oscillator is a JRY-S08 full-automatic horizontal oscillator.
8. The method as claimed in claim 7, wherein the tumbling shaker of step S5 includes a cylinder with a horizontal axis, the cylinder includes a lower fixed half cylinder and an upper tumbling half cylinder hinged to each other, a rotating shaft is coaxially installed in the cylinder, the rotating shaft is connected to a bracket, the rotating shaft is in transmission connection with a driving motor, a supporting rod is axially and fixedly connected to the rotating shaft, an installation cylinder is rotatably installed at an end of the supporting rod, the installation cylinder is used for installing the filling bottle, an axis of the installation cylinder is parallel to an axis of the cylinder, the installation cylinder is further provided with a cylinder cover, a clamping spring is oppositely arranged at a bottom of the installation cylinder, a driving lever is fixedly arranged at a bottom of an outer side wall of the installation cylinder, and the driving lever is slidably connected to a sliding groove arranged at an inner side wall of the cylinder, the sliding groove is arranged in the cylinder in a wave shape.
9. The pretreatment method for extracting organochlorine pesticides from soil according to claim 8, wherein the rotation speed of the driving motor is 40r/min-60 rmin.
10. The pretreatment method for extracting organochlorine pesticides in soil according to claim 8, wherein in step S7, the organochlorine pesticides are ultrasonically crushed for 2 hours by using an ultrasonic instrument.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010112099.XA CN111257076A (en) | 2020-02-24 | 2020-02-24 | Pretreatment method for extracting organochlorine pesticide in soil |
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| CN202010112099.XA CN111257076A (en) | 2020-02-24 | 2020-02-24 | Pretreatment method for extracting organochlorine pesticide in soil |
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| CN202010112099.XA Pending CN111257076A (en) | 2020-02-24 | 2020-02-24 | Pretreatment method for extracting organochlorine pesticide in soil |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113720835A (en) * | 2021-08-31 | 2021-11-30 | 辽宁通正检测有限公司 | Soil pesticide residue detection method |
| CN114047179A (en) * | 2021-09-26 | 2022-02-15 | 浙江亚凯检测科技有限公司 | Method and device for detecting soil organic matters in suspected contaminated area |
| CN114047179B (en) * | 2021-09-26 | 2024-06-04 | 江苏格林勒斯检测科技有限公司 | Suspected contaminated area soil organic matter detection method and detection device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114047179A (en) * | 2021-09-26 | 2022-02-15 | 浙江亚凯检测科技有限公司 | Method and device for detecting soil organic matters in suspected contaminated area |
| CN114047179B (en) * | 2021-09-26 | 2024-06-04 | 江苏格林勒斯检测科技有限公司 | Suspected contaminated area soil organic matter detection method and detection device |
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Application publication date: 20200609 |