CN116539751A - Method for detecting acetochlor in water - Google Patents
Method for detecting acetochlor in water Download PDFInfo
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- CN116539751A CN116539751A CN202310495632.9A CN202310495632A CN116539751A CN 116539751 A CN116539751 A CN 116539751A CN 202310495632 A CN202310495632 A CN 202310495632A CN 116539751 A CN116539751 A CN 116539751A
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- Prior art keywords
- proportioning
- acetochlor
- liquid
- hole
- water
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- VTNQPKFIQCLBDU-UHFFFAOYSA-N Acetochlor Chemical compound CCOCN(C(=O)CCl)C1=C(C)C=CC=C1CC VTNQPKFIQCLBDU-UHFFFAOYSA-N 0.000 title claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 108
- 239000000243 solution Substances 0.000 claims abstract description 39
- 239000012086 standard solution Substances 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000012528 membrane Substances 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims description 40
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 33
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 12
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 235000010323 ascorbic acid Nutrition 0.000 claims description 6
- 229960005070 ascorbic acid Drugs 0.000 claims description 6
- 239000011668 ascorbic acid Substances 0.000 claims description 6
- 238000004807 desolvation Methods 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 238000001819 mass spectrum Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims 1
- 235000019253 formic acid Nutrition 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 8
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000004817 gas chromatography Methods 0.000 abstract 1
- 238000002372 labelling Methods 0.000 abstract 1
- 238000004885 tandem mass spectrometry Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 20
- 238000004949 mass spectrometry Methods 0.000 description 8
- 230000004308 accommodation Effects 0.000 description 5
- 230000000149 penetrating effect Effects 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- HQVFCQRVQFYGRJ-UHFFFAOYSA-N formic acid;hydrate Chemical compound O.OC=O HQVFCQRVQFYGRJ-UHFFFAOYSA-N 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 239000004009 herbicide Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000002384 drinking water standard Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 230000003054 hormonal effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Library & Information Science (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a method for detecting acetochlor in water, which comprises the following steps of; s1: preparing 0.10ug/L, 0.20ug/L, 0.50ug/L, 1.00ug/L, 2.00ug/L, 5.00ug/L and 10.0ug/L of acetochlor standard solution by a solution proportioning device; s2, respectively injecting 1ul of standard solution, measuring peak area by a liquid chromatograph-tandem quadrupole mass spectrometer, and drawing a corresponding standard curve; s3: weighing 500ml of water sample, and filtering the water sample by using a 0.45um water system filter membrane; according to the invention, the liquid chromatography tandem mass spectrometry (LC-MS-MS) is adopted to detect the content of acetochlor in water, and compared with the gas chromatography tandem mass spectrometry in the aspect of preliminary treatment, the method is simpler, more convenient and faster, less in material consumption, shorter in sample treatment time, shorter in detection time, higher in sensitivity, higher in precision and better in labeling recovery rate.
Description
Technical Field
The invention relates to the technical field of pesticide residue detection, in particular to a method for detecting acetochlor in water.
Background
The acetochlor is one of herbicides with the largest use amount in China at present, and has the advantages of wide herbicide controlling spectrum, prominent effect, low price, convenient application and the like. Researches show that the acetochlor has obvious environmental hormone effect and has a great threat to human health and environmental safety, so that the method has very important significance for detecting the acetochlor in water quality. The new living drinking water standard in China prescribes that the concentration of acetochlor in drinking water is not more than 0.02mg/L.
In the prior art, a gas chromatography-mass spectrometry (GC-MS) is mostly adopted for the method for detecting acetochlor in water, but the gas chromatography-mass spectrometry has the problems of complex pretreatment operation process, more material consumption, long detection time and the like.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a method for detecting acetochlor in water so as to solve the technical problems.
In order to achieve the above purpose, the present invention provides the following technical solutions: the method for detecting acetochlor in water comprises the following steps:
s1: preparing 0.10ug/L, 0.20ug/L, 0.50ug/L, 1.00ug/L, 2.00ug/L, 5.00ug/L and 10.0ug/L of acetochlor standard solution by a solution proportioning device;
s2, respectively injecting 1ul of standard solution, measuring peak area by a liquid chromatograph-tandem quadrupole mass spectrometer, and drawing a corresponding standard curve;
s3: weighing 500ml of water sample, and filtering the water sample by using a 0.45um water system filter membrane;
s4, adding an equal volume of methanol into a water sample, directly injecting the sample, separating the sample by a C18 chromatographic column, and then, entering a liquid chromatograph-tandem quadrupole mass spectrometer, and carrying out qualitative and quantitative determination by ion pairs;
s5: and (5) comparing the measurement result of the liquid chromatography-tandem quadrupole mass spectrometer with a standard curve to obtain the corresponding concentration.
The invention is further provided with: the mass spectrometry conditions of the liquid chromatograph-tandem quadrupole mass spectrometer are as follows: capilliary: 3.0KV; cone:60V; desolvation temp:350 ℃; desolvation gas flow (L/Hr): 400; cone gas flow (L/Hr): 50; collsion Gas Flow:0.12L/Hr; collision: 4eV; sourcemp: 150 ℃.
The invention is further provided with: the mass spectrometry conditions of the liquid chromatograph-tandem quadrupole mass spectrometer are as follows: the mobile phase A is formic acid water solution with the volume fraction of 0.1%, the mobile phase B is acetonitrile with the flow rate of 0.4mL/min, gradient elution is carried out, and the gradient elution program is as follows: in the initial state, the proportion of the mobile phase A is 50%, and the proportion of the mobile phase B is 50%; in 0-1.0min, the proportion of the mobile phase A gradually changes from 50% to 0%, and the proportion of the mobile phase B gradually changes from 50% to 100%; the proportion of the mobile phase A is maintained to be 0 percent and the proportion of the mobile phase B is maintained to be 100 percent within 1.0 to 2.5 minutes; the proportion of the mobile phase A is gradually changed from 0% to 50% and the proportion of the mobile phase B is gradually changed from 100% to 50% within 2.5-3.5 min.
The invention is further provided with: the acetochlor standard solution in s1 is obtained by diluting the acetochlor solution with methanol water.
The invention is further provided with: when the water sample contains residual chlorine, adding ascorbic acid to remove interference, wherein 0.1-0.15g of ascorbic acid is added to each liter of water sample.
The invention is further provided with: the solution proportioning device comprises a box body, a first liquid tank for storing acetochlor solution, a second liquid tank for storing methanol aqueous solution, a liquid mixing tank and a proportioning unit, wherein the first liquid tank and the second liquid tank are connected with the liquid mixing tank through pipelines, the proportioning unit is connected with each pipeline together and is used for quantitatively proportioning the solution flowing through each pipeline to the proportioning unit, and the liquid mixing tank is connected with the proportioning unit and is used for fully mixing the liquid after proportioning by the proportioning unit.
The invention is further provided with: the proportioning unit comprises a proportioning tank, a first proportioning cavity is arranged in the proportioning tank, a second proportioning cavity is arranged on one side of the first proportioning cavity in an extending mode, the other end of the second proportioning cavity is communicated with the outside of the proportioning tank, the first liquid tank is connected and communicated with the first proportioning cavity through a first liquid inlet pipe, the first proportioning cavity is also connected with a first liquid outlet pipe, the other end of the first liquid outlet pipe is connected and communicated with a liquid mixing tank, the second liquid tank is communicated with the second proportioning cavity through a second liquid inlet pipe, a second liquid outlet pipe is further arranged on the corresponding side of the second liquid inlet pipe, the other end of the second liquid outlet pipe is connected and communicated with the liquid mixing tank, a power piston is arranged in the second proportioning cavity in a sliding mode, the outer end of the power piston is connected with a driving rod, and a matching block matched with the first liquid outlet pipe is arranged in the first proportioning cavity in a sliding mode
The invention is further provided with: the through hole has been seted up at the cooperation piece middle part, the through hole deviates from second ratio chamber one side open end and has set firmly the screw thread cover, threaded connection has the locating screw in the screw thread cover, the locating screw outer end runs through and extends to the ratio jar outside and be connected with its pivoted power supply of control, the other open end of through-hole slides and is provided with the flexible piece that can stretch out or retract to in the through-hole, flexible piece inner has the first tooth post of rotating with the locating screw and being connected, the cooperation piece is close to second ratio chamber one side and is located the through-hole top and has seted up the accommodation hole, the outer open end of accommodation hole slides and is provided with the movable block, the movable block inner has the second tooth post, the cooperation piece is located and has seted up the through-hole between through-hole and the accommodation hole, the through-hole both ends are switched on with through-hole and accommodation hole respectively, the through-hole internal rotation is provided with first tooth post and second tooth post synchromesh's gear.
The invention is further provided with: the inside first collection that is provided with of liquid mixing tank mixes the storehouse, first collection is mixed the storehouse bottom and is provided with the second collection and mixes the storehouse, second collection is mixed the storehouse lower extreme and is run through and extend to liquid mixing tank below, first collection is mixed the storehouse lower bottom and is frustum column structure and outer wall equidistance and circumference are provided with two at least vibrating motor, second collection is mixed storehouse upper portion and is provided with U type pipe and U type pipe both ends and is connected with liquid mixing tank and switch on, second collection is mixed the storehouse and is located U type pipe lower part array and is provided with a plurality of ring pipes, second collection is mixed the storehouse lower part and is offered the discharge gate that switches on with the ring pipe.
The invention is further provided with: a fixed seat is fixedly arranged on one side of the proportioning unit in the box body, a rotating seat is fixedly arranged in the middle of the right side of the fixed seat, a swinging rod is arranged on the rotating seat in a rotating mode, the lower end of the swinging rod is connected with a driving rod through a linkage rod, a power motor is fixedly arranged above the fixed seat in the box body, a power shaft of the power motor is eccentrically connected with a driving turntable, an annular groove which is coaxially arranged with the driving turntable is concavely arranged on the front side of the driving turntable, and a sliding part which is in sliding fit with the annular groove is arranged on the upper end of the swinging rod.
In summary, the invention has the following beneficial effects: according to the invention, the liquid chromatography tandem mass spectrometry (LC-MS-MS) is adopted to detect the content of acetochlor in water, a solution proportioning device is used for proportioning a plurality of acetochlor standard solutions with different concentrations in the early treatment, 1ul of the sample is respectively injected and the peak area is measured by a liquid chromatography-tandem quadrupole mass spectrometer, a corresponding standard curve is drawn, then a water sample is measured, the water sample is filtered and added with equal volume of methanol and then is directly injected, and the corresponding concentration is obtained by comparing the measurement result of the liquid chromatography-tandem quadrupole mass spectrometer with the standard curve, so that the detection can be completed. And the acetochlor standard solution with the required concentration can be rapidly proportioned by the proportioning device.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a standard graph of acetochlor measured by liquid phase mass spectrometry according to the present invention;
FIG. 2 is a regression equation for measuring acetochlor by liquid phase mass spectrometry according to the present invention;
FIG. 3 is a graph showing the precision test data of acetochlor measured by the liquid phase mass spectrometry of the present invention;
FIG. 4 is a graph showing the labeled recovery of acetochlor measured by liquid phase mass spectrometry according to the present invention;
FIG. 5 shows the precision and accuracy of the acetochlor detection method of the present invention;
FIG. 6 is a schematic diagram of the overall structure of the proportioning device of the present invention;
FIG. 7 is a schematic structural diagram of a proportioning unit of the present invention;
FIG. 8 is an enlarged schematic view of a partial structure at A in FIG. 2;
FIG. 9 is a schematic view of the internal structure of the liquid mixing tank of the present invention;
fig. 10 is a schematic operation of the swing lever of the present invention.
Reference numerals: 1. a case; 100. a first liquid tank; 101. a second liquid tank; 2. a liquid mixing tank; 200. a first collection mixing bin; 201. a second mixing bin; 202. a vibration motor; 203. a U-shaped tube; 204. an annular tube; 205. a discharge port; 3. a proportioning unit; 300. a proportioning tank; 4. a first proportioning cavity; 400. a first liquid inlet pipe; 401. a first liquid outlet pipe; 402. a mating block; 403. a through hole; 404. a thread sleeve; 405. positioning a screw; 406. a telescopic block; 407. a first tooth post; 408. an accommodation hole; 409. a movable block; 410. a second tooth post; 411. a through hole; 412. a gear; 413. a slide bar; 414. a return spring; 416. sealing sleeve; 417. adjusting a turntable; 5. a second proportioning cavity; 500. a second liquid inlet pipe; 501. a second liquid outlet pipe; 502. a one-way valve; 6. a power piston; 600. a driving rod; 601. a fixing seat; 602. a rotating seat; 603. a swinging rod; 604. a linkage rod; 605. a power motor; 606. driving a turntable; 607. an annular groove; 608. a sliding part; 609. a vertical plate; 610. an auxiliary rod.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-2, the invention discloses a method for detecting acetochlor in water, which comprises the following steps:
s1: preparing 0.10ug/L, 0.20ug/L, 0.50ug/L, 1.00ug/L, 2.00ug/L, 5.00ug/L and 10.0ug/L of acetochlor standard solution by a solution proportioning device;
s2, respectively injecting 1ul of standard solution, measuring peak area by a liquid chromatograph-tandem quadrupole mass spectrometer, and drawing a corresponding standard curve;
s3: weighing 500ml of water sample, and filtering the water sample by using a 0.45um water system filter membrane;
s4, adding an equal volume of methanol into the water sample, directly injecting the sample, separating the sample by a C18 chromatographic column, and then, entering a liquid chromatograph-tandem quadrupole mass spectrometer, and carrying out qualitative and quantitative determination by ion pairs.
S5: obtaining corresponding concentration by comparing the measurement result of the liquid chromatograph-tandem quadrupole mass spectrometer with a standard curve;
when the method is used, the liquid chromatography tandem mass spectrometry (LC-MS-MS) is adopted to detect the content of the acetochlor in water, 1ul of acetochlor standard solutions with various concentrations are respectively sampled by a solution proportioning device in the early treatment, the peak area is measured by the liquid chromatography-tandem quadrupole mass spectrometer, a corresponding standard curve is drawn, then a water sample is measured, the water sample is filtered and is directly sampled after the equal volume of methanol is added, and the corresponding concentration is obtained by comparing the measuring result of the liquid chromatography-tandem quadrupole mass spectrometer with the standard curve, so that the detection can be completed. And the acetochlor standard solution with the required concentration can be rapidly proportioned by the proportioning device.
The mass spectrometry conditions of the liquid chromatograph-tandem quadrupole mass spectrometer are as follows: capilliary: 3.0KV; cone:60V; desolvation Temp:350 ℃; desolvation gas flow (L/Hr): 400; cone gas flow (L/Hr): 50; collsion Gas Flow:0.12L/Hr; collision: 4eV; sourcemp: 150 ℃; the mass spectrometry conditions of the liquid chromatograph-tandem quadrupole mass spectrometer are as follows: the mobile phase A is formic acid water solution with the volume fraction of 0.1%, the mobile phase B is acetonitrile with the flow rate of 0.4mL/min, gradient elution is carried out, and the gradient elution program is as follows: in the initial state, the proportion of the mobile phase A is 50%, and the proportion of the mobile phase B is 50%; in 0-1.0min, the proportion of the mobile phase A gradually changes from 50% to 0%, and the proportion of the mobile phase B gradually changes from 50% to 100%; the proportion of the mobile phase A is maintained to be 0 percent and the proportion of the mobile phase B is maintained to be 100 percent within 1.0 to 2.5 minutes; 2.5-3.5min, the proportion of the mobile phase A is gradually changed from 0% to 50%, and the proportion of the mobile phase B is gradually changed from 100% to 50%; s1, the acetochlor standard solution is obtained by diluting the acetochlor solution with methanol water; when the water sample contains residual chlorine, adding ascorbic acid to remove interference, wherein 0.1-0.15g of ascorbic acid is added to each liter of water sample.
When in use, the detection precision and sensitivity are effectively improved by adopting the mass spectrum conditions.
The solution proportioning device comprises a box body 1, a first liquid tank 100 for storing acetochlor solution, a second liquid tank 101 for storing methanol aqueous solution, a liquid mixing tank 2 and a proportioning unit 3, wherein the first liquid tank 100 and the second liquid tank 101 are connected with the liquid mixing tank 2 through pipelines, the proportioning unit 3 is connected with each pipeline together and is used for quantitatively proportioning the solution flowing through each pipeline to the proportioning unit 3, and the liquid mixing tank 2 is connected with the proportioning unit 3 and is used for fully mixing the liquid after proportioning of the proportioning unit 3.
When the water-saving type water-saving device is used, when the standard acetochlor solution with the required concentration is required to be mixed, the proportioning unit 3 guides methanol water in the second liquid tank 101 into the liquid-mixing tank 2, the required acetochlor is guided into the liquid-mixing tank 2 by the proportioning unit 3, the acetochlor solution and the methanol water solution are fully mixed through the liquid-mixing tank 2, and the fully mixed standard solution is discharged out of the liquid-mixing tank 2 and is collected; wherein, box 1 one side is provided with radiator fan, and then guarantees the heat dispersion of box 1.
The proportioning unit 3 comprises a proportioning tank 300, a first proportioning cavity 4 is arranged in the proportioning tank 300, a second proportioning cavity 5 is extended from one side of the first proportioning cavity 4, the other end of the second proportioning cavity 5 is communicated with the outside of the proportioning tank 300, the first liquid tank 100 is connected and communicated with the first proportioning cavity 4 through a first liquid inlet pipe 400, the first proportioning cavity 4 is also connected with a first liquid outlet pipe 401, the other end of the first liquid outlet pipe 401 is connected and communicated with a liquid mixing tank 2, the second liquid tank 101 is communicated with the second proportioning cavity 5 through a second liquid inlet pipe 500, a second liquid outlet pipe 501 is further arranged on the corresponding side of the second liquid inlet pipe 500, the other end of the second liquid outlet pipe 501 is connected and communicated with the liquid mixing tank 2, a power piston 6 is slidably arranged in the second proportioning cavity 5, the outer end of the power piston 6 is connected with a driving rod 600, and a matching block 402 matched with the first liquid proportioning cavity 4 is slidably arranged in the first proportioning cavity 4; the middle part of the matching block 402 is provided with a through hole 403, one side opening end of the through hole 403, which is away from the second proportioning cavity 5, is fixedly provided with a threaded sleeve 404, the internal thread of the threaded sleeve 404 is connected with a positioning screw 405, the outer end of the positioning screw 405 extends out of the proportioning tank 300 in a penetrating way and is connected with a power source for controlling the rotation of the positioning screw, the other opening end of the through hole 403 is slidably provided with a telescopic block 406 which can extend out of or retract into the through hole 403, the inner end of the telescopic block 406 is provided with a first tooth post 407 rotationally connected with the positioning screw 405, the matching block 402 is close to one side of the second proportioning cavity 5 and is positioned above the through hole 403, the outer opening end of the accommodating hole 408 is slidably provided with a movable block 409, the inner end of the movable block 409 is provided with a second tooth post 410, a through hole 411 is arranged between the through hole 403 and the accommodating hole 408, two ends of the through hole 411 are respectively communicated with the through hole 403 and the accommodating hole 408, and a gear 412 which is synchronously meshed with the first tooth post 407 and the second tooth post 410 is rotationally arranged in the through hole 411.
When the proportioning unit 3 of the invention is used, the driving rod 600 drives the power piston 6 to reciprocate along the second proportioning cavity 5 (the driving rod 600 is connected with an external power source, the power source can control the driving rod 600 to drive the piston rod to reciprocate, which belongs to the prior art and is not described in detail herein), the power piston 6 reciprocates to further enable the second proportioning cavity 5 to generate negative pressure, the negative pressure generated by the second proportioning cavity 5 drives methanol water in the second liquid tank 101 to enter the second proportioning cavity 5 through the second liquid inlet pipe 500, methanol water solution entering the second proportioning cavity 5 is guided into the liquid mixing tank 2 through the second liquid outlet pipe 501, and the amount of the methanol water solution fed into the liquid mixing tank 2 by each movement of the driving piston is a fixed value;
wherein, two slide bars 413 are correspondingly arranged in the second proportioning cavity 5, the matching block 402 and the two slide bars 413 are in sliding fit, a reset spring 414 is arranged between the outer ring of the two slide bars 413 and the matching block 402 and the inner wall of the proportioning cavity, and the reset performance of the matching block 402 is effectively improved by arranging the reset spring 414;
further, one end of the positioning screw 405 of the invention extends out of the proportioning tank 300 in a penetrating way and is connected with a power source for controlling the rotation of the positioning screw, a sealing sleeve 416 is arranged at the penetrating position of the screw and the proportioning tank 300, the sliding fit of the screw and the proportioning tank 300 is ensured, the leakage of liquid at the penetrating position is avoided, the positioning screw is preferably connected with an adjusting rotary table 417 at the penetrating end of the positioning screw, and the adjusting rotary table 417 is manually rotated by a worker to provide power for the rotation of the screw; in operation, the adjusting turntable 417 is rotated to drive the screw rod, the screw rod comprises a threaded section matched with the threaded sleeve 404 and a smooth section matched with the proportioning tank 300 in a sliding manner, when the screw rod rotates, the screw rod is driven to axially move towards one side in the through hole 403 through the matching between the threaded section and the threaded sleeve 404, the screw rod moves and is connected with the first tooth post 407 in a rotating manner, the sliding matching between the telescopic block 406 and the through hole 403 drives the first tooth post 407 and the telescopic block 406 to radially move and enables the other end of the telescopic block 406 to extend out of the through hole 403, the telescopic block 406 extends out of the through hole 403 and enters a reciprocating motion path of the power piston 6, at the moment, when the power piston 6 reciprocates, the telescopic block 406 is contacted and drives the matching block 402 to synchronously move through the telescopic block 406, and simultaneously enables the first proportioning cavity 4 to generate negative pressure, the negative pressure generated by the first proportioning cavity 4 enables the acetochlor solution in the first liquid tank 100 to enter the first proportioning cavity 4 through the first liquid inlet pipe 400, and the acetochlor solution entering the first proportioning cavity 4 is guided into the liquid mixing tank 2 through the first liquid outlet pipe 401 and is mixed with the water solution discharged from the second proportioning cavity 5 to obtain a required standard solution;
the aqueous solution of methanol discharged from the second proportioning chamber 5 is fixed each time, so that when the concentration of acetochlor in the standard solution to be proportioned needs to be changed, only the screw rod is required to be rotated forward or backward and the extension amount of the extension block 406 extending out of the through hole 403 is required to be changed, for example, when the standard solution with higher proportioning concentration is required, the screw rod is rotated to drive the extension block 406 to extend out a distance, at this time, the movement of the power piston 6 can drive the matching block 402 to move more greatly due to the extension of the extension block 406, when the movement amplitude of the matching block 402 in the first proportioning chamber 4 is increased, the amount of acetochlor solution guided to the liquid mixing tank 2 through the first proportioning chamber 4 is increased, when the standard solution with lower proportioning concentration is required, the operation is performed correspondingly, and when the amount of the acetochlor solution discharged each time is fixed, the concentration of acetochlor in the prepared standard solution is changed; and the outer ring of the connection section of the screw and the rotating adjusting turntable 417 is provided with scale marks, so that a worker can more intuitively know the concentration of the corresponding acetochlor of the standard solution obtained by the current extending amount of the screw according to the scale marks, and the worker can conveniently and quickly adjust the screw to a required position.
The screw rod is driven to axially move towards one side in the through hole 403 by the cooperation between the thread section and the thread sleeve 404 when rotating, the screw rod moves and is connected with the first tooth post 407 in a rotating way, and the sliding cooperation between the telescopic block 406 and the through hole 403 drives the first tooth post 407 and the telescopic block 406 to radially move and drives the other end of the telescopic block 406 to extend out of the through hole 403, the telescopic block 406 drives the gear 412 to anticlockwise rotate by the cooperation between the first tooth post 407 and the gear 412, the gear 412 anticlockwise rotates and drives the second tooth post 410 and the first tooth post 407 to synchronously and reversely move by the meshing cooperation between the gear 412 and the second tooth post 410, so that the cooperation block 402 and the telescopic block 406 are driven to synchronously and reversely move, namely, when the telescopic block 406 extends outwards, the movable block 409 synchronously contracts inwards, so that the extension of the telescopic block 406 is prevented from being influenced by the filling of liquid in the second proportioning cavity 5; the telescopic block 406 and the movable block 409 are respectively provided with a guide block in an extending way, the through hole 403 and the accommodating hole 408 are respectively provided with a guide groove matched with the guide block, and the telescopic block 406 and the movable block 409 are respectively in sliding fit with the through hole 403 and the accommodating hole 408 through the fit between the guide block and the guide groove;
the first liquid inlet pipe 400, the second liquid inlet pipe 500, the first liquid outlet pipe 401 and the second liquid outlet pipe 501 are all provided with one-way valves 502.
The inside first collection that is provided with of mixed liquid jar 2 mixes storehouse 200, first collection is mixed storehouse 200 bottom and is provided with second collection and mixes storehouse 201, second collection is mixed storehouse 201 lower extreme and is run through and extend to mixed liquid jar 2 below, first collection is mixed storehouse 200 lower bottom and is frustum-shaped structure and outer wall equidistance and circumference and be provided with two at least vibrating motor 202, second collection is mixed storehouse 201 upper portion and is provided with U type pipe 203 and U type pipe 203 both ends all are connected with mixed liquid jar 2 and switch on, second collection is mixed storehouse 201 and is located U type pipe 203 lower part array and is provided with a plurality of ring pipes 204, second collection is mixed storehouse 201 lower part and has been offered the discharge gate 205 that switches on with ring pipe 204.
When in use, the corresponding amount of acetochlor solution and methanol aqueous solution after being proportioned by the proportioning tank 300 is sent into the first mixing bin 200 of the liquid mixing tank 2 by the first liquid outlet pipe 401 and the second liquid outlet pipe 501, and the two solutions are mixed into the first mixing bin 200 and are subjected to high-speed and high-frequency vibration by the vibration motor 202, so that the two solutions are primarily mixed in the first mixing bin 200; and then the mixed liquid which is positioned in the first mixing bin 200 and is subjected to preliminary mixing is guided into the annular pipes 204 of the array through the two liquid inlet ends of the U-shaped pipe 203 under the action of high-speed and high-frequency vibration, two solutions are subjected to opposite flushing at the junction of each adjacent annular pipe 204, and the annular pipes 204 are arranged in a plurality of arrays, so that the solution can realize multiple opposite flushing in the second mixing bin, the efficient mixing of acetochlor solution and methanol aqueous solution is ensured, a more accurate standard curve can be obtained when standard solution sample injection detection is ensured, and the subsequent measurement and comparison are convenient.
A fixed seat 601 is fixedly arranged on one side of the proportioning unit 3 in the box body 1, a rotating seat 602 is fixedly arranged in the middle of the right side of the fixed seat 601, a swinging rod 603 is rotatably arranged on the rotating seat 602, the lower end of the swinging rod 603 is connected with a driving rod 600 through a linkage rod 604, a power motor 605 is fixedly arranged above the fixed seat 601 in the box body 1, a power shaft of the power motor 605 is eccentrically connected with a driving turntable 606, an annular groove 607 which is coaxially arranged with the driving turntable 606 is concavely arranged in front of the driving turntable 606, and a sliding part 608 which is in sliding fit with the annular groove 607 is arranged at the upper end of the swinging rod 603.
When the power piston driving device is used, the power motor 605 is started and drives the driving turntable 606 to eccentrically rotate, the driving turntable 606 eccentrically rotates and drives the swinging rod 603 to swing by taking the rotating seat 602 as the axis through sliding fit between the sliding part 608 and the annular groove 607, and the swinging rod 603 swings and drives the driving rod 600 to reciprocate through the linkage rod 604 at the lower end of the swinging rod 603 so as to drive the power piston 6 to reciprocate;
the upper portion of the front side of the fixing base 601 is fixedly provided with a vertical plate 609, the vertical plate 609 is rotatably provided with an auxiliary rod 610, the other end of the auxiliary rod 610 is rotatably connected with the sliding part 608 of the swinging rod 603, and the stability of the swinging rod 603 during swinging is improved through the arrangement of the auxiliary rod 610.
The electrical components are all connected with an external main controller and 220V mains supply, and the main controller can be conventional known equipment for controlling a computer and the like.
Also, the terms pointed out by the present invention are as follows: the directional or positional relationships indicated by the terms "front", "rear", "vertical", "horizontal", etc., are based on the directional or positional relationships shown in the drawings, are merely for convenience in describing the invention and to simplify the description, and are not indicative or implying that the apparatus or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed to limit the scope of the invention.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (10)
1. A method for detecting acetochlor in water is characterized by comprising the following steps: comprises the following steps:
s1: preparing 0.10ug/L, 0.20ug/L, 0.50ug/L, 1.00ug/L, 2.00ug/L, 5.00ug/L and 10.0ug/L of acetochlor standard solution by a solution proportioning device;
s2, respectively injecting 1ul of standard solution, measuring peak area by a liquid chromatograph-tandem quadrupole mass spectrometer, and drawing a corresponding standard curve;
s3: weighing 500ml of water sample, and filtering the water sample by using a 0.45um water system filter membrane;
s4, adding an equal volume of methanol into a water sample, directly injecting the sample, separating the sample by a C18 chromatographic column, and then, entering a liquid chromatograph-tandem quadrupole mass spectrometer, and carrying out qualitative and quantitative determination by ion pairs;
s5: and (5) comparing the measurement result of the liquid chromatography-tandem quadrupole mass spectrometer with a standard curve to obtain the corresponding concentration.
2. The method for detecting acetochlor in water according to claim 1, wherein the method comprises the following steps: the mass spectrum conditions of the liquid chromatography-tandem quadrupole mass spectrometer are as follows: capilliary: 3.0KV; cone:60V; desolvation Temp:350 ℃; desolvangASflow (L/Hr): 400; conegasflow (L/Hr): 50; collsionGasFlow:0.12L/Hr; collision: 4eV; sourcemp: 150 ℃.
3. The method for detecting acetochlor in water according to claim 1, wherein the method comprises the following steps: the mass spectrum conditions of the liquid chromatography-tandem quadrupole mass spectrometer are as follows: the mobile phase A is formic acid aqueous solution with the volume fraction of 0.1%, the mobile phase B is acetonitrile with the flow rate of 0.4mL/min, gradient elution is carried out, and the gradient elution program is as follows:
in the initial state, the proportion of the mobile phase A is 50%, and the proportion of the mobile phase B is 50%;
in 0-1.0min, the proportion of the mobile phase A gradually changes from 50% to 0%, and the proportion of the mobile phase B gradually changes from 50% to 100%;
the proportion of the mobile phase A is maintained to be 0 percent and the proportion of the mobile phase B is maintained to be 100 percent within 1.0 to 2.5 minutes;
the proportion of the mobile phase A is gradually changed from 0% to 50% and the proportion of the mobile phase B is gradually changed from 100% to 50% within 2.5-3.5 min.
4. The method for detecting acetochlor in water according to claim 1, wherein the method comprises the following steps: the acetochlor standard solution in s1 is obtained by diluting acetochlor solution with methanol water.
5. The method for detecting acetochlor in water according to claim 1, wherein the method comprises the following steps: when the water sample contains residual chlorine, adding ascorbic acid to remove interference, wherein 0.1-0.15g of ascorbic acid is added to each liter of water sample.
6. The method for detecting acetochlor in water according to claim 1, wherein the method comprises the following steps: the solution proportioning device comprises a box body (1), a first liquid tank (100) for storing acetochlor solution, a second liquid tank (101) for storing methanol aqueous solution, a liquid mixing tank (2) and a proportioning unit (3), wherein the first liquid tank (100) and the second liquid tank (101) are connected with the liquid mixing tank (2) through pipelines together, the proportioning unit (3) is connected with each pipeline together and is used for quantitatively proportioning the solution flowing through each pipeline to the proportioning unit (3), and the liquid mixing tank (2) is connected with the proportioning unit (3) and is used for fully mixing the liquid after proportioning of the proportioning unit (3).
7. The method for detecting acetochlor in water according to claim 6, wherein the method comprises the following steps: the proportioning unit (3) comprises a proportioning tank (300), be equipped with first proportioning chamber (4) in proportioning tank (300), first proportioning chamber (4) one side extends there is second proportioning chamber (5), second proportioning chamber (5) other end and proportioning tank (300) outside switch on, first fluid reservoir (100) are connected with first proportioning chamber (4) through first feed liquor pipe (400), first proportioning chamber (4) still are connected with first drain pipe (401) and first drain pipe (401) other end and are connected with and switch on with mixed fluid reservoir (2), second fluid reservoir (101) are connected with second proportioning chamber (5) through second feed liquor pipe (500), second proportioning chamber (5) are located the corresponding side of second feed liquor pipe (500) and still are provided with second drain pipe (501), the second drain pipe (501) other end is connected with mixed fluid reservoir (2) and is switched on, second proportioning chamber (5) inner slide is provided with power piston (6) and first proportioning piston (6) outer end (600) are connected with power piston (600), first proportioning rod (600) are connected with and are suitable for the cooperation.
8. The method for detecting acetochlor in water according to claim 7, wherein the method comprises the following steps: the middle part of the matching block (402) is provided with a through hole (403), one side opening end of the through hole (403) deviating from the second matching cavity (5) is fixedly provided with a thread bushing (404), a positioning screw (405) is connected in the thread bushing (404) in a threaded manner, the outer end of the positioning screw (405) penetrates through and extends out of the matching tank (300) and is connected with a power source for controlling the rotation of the positioning screw, the other opening end of the through hole (403) is slidably provided with a telescopic block (406) which can extend out of or retract into the through hole (403), the inner end of the telescopic block (406) is provided with a first tooth column (407) rotationally connected with the positioning screw (405), the matching block (402) is close to one side of the second proportioning cavity (5) and is located above the through hole (403) and provided with a containing hole (408), an outer opening end of the containing hole (408) is slidably provided with a movable block (409), the inner end of the movable block (409) is provided with a second tooth column (410), the matching block (402) is located between the through hole (403) and the containing hole (408) and provided with a through hole (411), two ends of the through hole (411) are respectively communicated with the through hole (403) and the containing hole (408), and gears (412) which are synchronously meshed with the first tooth column (407) and the second tooth column (410) are rotationally arranged in the through hole (411).
9. The method for detecting acetochlor in water according to claim 6, wherein the method comprises the following steps: the utility model discloses a liquid mixing tank, including mixed liquid tank (2), first collection storehouse (200), second collection storehouse (201) are mixed to first collection storehouse (200) bottom, second collection storehouse (201) lower extreme runs through and extends to mixed liquid tank (2) below, first collection storehouse (200) lower bottom is frustum column structure and outer wall equidistance and circumference are provided with two at least vibrating motor (202), second collection storehouse (201) upper portion is provided with U type pipe (203) and U type pipe (203) both ends all are connected with mixed liquid tank (2) and are switched on, second collection storehouse (201) are located U type pipe (203) lower part array and are provided with a plurality of ring pipes (204), second collection storehouse (201) lower part offered discharge gate (205) that switch on with ring pipe (204).
10. The method for detecting acetochlor in water according to claim 1, wherein the method comprises the following steps: fixing base (601) has been set firmly in case (1) in proportioning unit (3) one side, fixing base (601) right side middle part has set firmly rotation seat (602), rotate on rotation seat (602) and be provided with swinging arms (603), swinging arms (603) lower extreme is connected with actuating lever (600) through gangbar (604), be located fixing base (601) top in case (1) and set firmly power motor (605), the power shaft eccentric connection of power motor (605) has driving turntable (606), driving turntable (606) front side concave be equipped with rather than coaxial ring channel (607), swinging arms (603) upper end have with this ring channel (607) be sliding fit's sliding part (608).
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Application publication date: 20230804 |