CN114441700A - Method for determining deltamethrin in water based on gas-mass linkage method - Google Patents
Method for determining deltamethrin in water based on gas-mass linkage method Download PDFInfo
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- CN114441700A CN114441700A CN202111601149.1A CN202111601149A CN114441700A CN 114441700 A CN114441700 A CN 114441700A CN 202111601149 A CN202111601149 A CN 202111601149A CN 114441700 A CN114441700 A CN 114441700A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000005892 Deltamethrin Substances 0.000 title claims abstract description 28
- 229960002483 decamethrin Drugs 0.000 title claims abstract description 28
- OWZREIFADZCYQD-NSHGMRRFSA-N deltamethrin Chemical compound CC1(C)[C@@H](C=C(Br)Br)[C@H]1C(=O)O[C@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 OWZREIFADZCYQD-NSHGMRRFSA-N 0.000 title claims abstract description 28
- 239000011521 glass Substances 0.000 claims abstract description 27
- 239000005416 organic matter Substances 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 230000018044 dehydration Effects 0.000 claims abstract description 7
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 230000001376 precipitating effect Effects 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 21
- 230000000087 stabilizing effect Effects 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000005096 rolling process Methods 0.000 claims description 5
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 3
- 239000013049 sediment Substances 0.000 claims description 3
- 244000309464 bull Species 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 6
- 238000001556 precipitation Methods 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 6
- 230000000712 assembly Effects 0.000 description 5
- 238000000429 assembly Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002728 pyrethroid Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- NYPJDWWKZLNGGM-UHFFFAOYSA-N fenvalerate Chemical compound C=1C=C(Cl)C=CC=1C(C(C)C)C(=O)OC(C#N)C(C=1)=CC=CC=1OC1=CC=CC=C1 NYPJDWWKZLNGGM-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- KAATUXNTWXVJKI-NSHGMRRFSA-N (1R)-cis-(alphaS)-cypermethrin Chemical compound CC1(C)[C@@H](C=C(Cl)Cl)[C@H]1C(=O)O[C@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 KAATUXNTWXVJKI-NSHGMRRFSA-N 0.000 description 1
- ZXQYGBMAQZUVMI-RDDWSQKMSA-N (1S)-cis-(alphaR)-cyhalothrin Chemical compound CC1(C)[C@H](\C=C(/Cl)C(F)(F)F)[C@@H]1C(=O)O[C@@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-RDDWSQKMSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 239000005884 Beta-Cyfluthrin Substances 0.000 description 1
- 239000005946 Cypermethrin Substances 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- VXSIXFKKSNGRRO-MXOVTSAMSA-N [(1s)-2-methyl-4-oxo-3-[(2z)-penta-2,4-dienyl]cyclopent-2-en-1-yl] (1r,3r)-2,2-dimethyl-3-(2-methylprop-1-enyl)cyclopropane-1-carboxylate;[(1s)-2-methyl-4-oxo-3-[(2z)-penta-2,4-dienyl]cyclopent-2-en-1-yl] (1r,3r)-3-[(e)-3-methoxy-2-methyl-3-oxoprop-1-enyl Chemical class CC1(C)[C@H](C=C(C)C)[C@H]1C(=O)O[C@@H]1C(C)=C(C\C=C/C=C)C(=O)C1.CC1(C)[C@H](/C=C(\C)C(=O)OC)[C@H]1C(=O)O[C@@H]1C(C)=C(C\C=C/C=C)C(=O)C1 VXSIXFKKSNGRRO-MXOVTSAMSA-N 0.000 description 1
- QQODLKZGRKWIFG-RUTXASTPSA-N [(R)-cyano-(4-fluoro-3-phenoxyphenyl)methyl] (1S)-3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropane-1-carboxylate Chemical compound CC1(C)C(C=C(Cl)Cl)[C@@H]1C(=O)O[C@@H](C#N)C1=CC=C(F)C(OC=2C=CC=CC=2)=C1 QQODLKZGRKWIFG-RUTXASTPSA-N 0.000 description 1
- 150000001448 anilines Chemical class 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- ZXQYGBMAQZUVMI-UNOMPAQXSA-N cyhalothrin Chemical compound CC1(C)C(\C=C(/Cl)C(F)(F)F)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-UNOMPAQXSA-N 0.000 description 1
- KAATUXNTWXVJKI-UHFFFAOYSA-N cypermethrin Chemical compound CC1(C)C(C=C(Cl)Cl)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 KAATUXNTWXVJKI-UHFFFAOYSA-N 0.000 description 1
- 229960005424 cypermethrin Drugs 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000005910 lambda-Cyhalothrin Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- HYJYGLGUBUDSLJ-UHFFFAOYSA-N pyrethrin Natural products CCC(=O)OC1CC(=C)C2CC3OC3(C)C2C2OC(=O)C(=C)C12 HYJYGLGUBUDSLJ-UHFFFAOYSA-N 0.000 description 1
- 229940070846 pyrethrins Drugs 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
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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)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to the technical field of pollutant measurement, in particular to a method for measuring deltamethrin in water based on a gas-mass linkage method, which comprises the steps of precipitating the water to be measured to obtain a precipitate and precipitated water; filtering the precipitated water to obtain filtered water; dropwise adding the filtered water on a watch glass for dehydration to obtain organic matter residues; dissolving organic matter residues on the watch glass by using an organic solvent, and then carrying out centrifugal separation to obtain a sample to be detected; the method has the advantages that the content of the deltamethrin in the sample to be detected is detected by using a gas-mass linkage method, and the water to be detected is subjected to double filtration treatment through precipitation and filtration, so that the residue of impurities is reduced, and the problem that the detection result of the content of the deltamethrin is influenced by the impurities in the sample in the conventional detection method is solved.
Description
Technical Field
The invention relates to the technical field of pollutant measurement, in particular to a method for measuring deltamethrin in water based on a gas-mass linkage method.
Background
With the rapid development of the industry in China, the discharge amount of organic wastewater is increasing day by day, and the types of organic pollutants are becoming more and more complex. The organic pollutants in the water body mainly comprise phenolic compounds, aniline compounds, total organic halides, polycyclic aromatic hydrocarbon compounds and the like. A variety of organic pollutants can accumulate in the environment for long periods of time, posing serious threats to the ecological environment and human health. Qualitative analysis of organic pollutants in water is an important prerequisite for quantitative analysis and risk evaluation. At present, the organic pollutants are qualitatively analyzed mainly by adopting an organic pollutant pretreatment-gas chromatography-mass spectrometer (GC-MS).
At present, the prior art (CN101650343A) discloses a method for rapidly detecting pyrethroid pesticides in water, and specifically, the method monitors the residue and digestion dynamics of pyrethroid pesticides in the environment by High Performance Liquid Chromatography (HPLC). The method simplifies the pretreatment of the sample, and can simultaneously determine the total residue of cyhalothrin, deltamethrin, fenvalerate, cypermethrin, beta-cypermethrin, lambda-cyhalothrin, beta-cyfluthrin and isomers of the above six pyrethrins in the water sample. The method has good repeatability and simple operation.
By adopting the mode, the detected sample is subjected to filtration treatment, and impurities contained in the sample can influence the detection result of the content of the deltamethrin.
Disclosure of Invention
The invention aims to provide a method for determining deltamethrin in water based on a gas-mass linkage method, and aims to solve the problem that impurities contained in a sample in the conventional determination method influence the detection result of the content of the deltamethrin.
In order to achieve the aim, the invention provides a method for determining deltamethrin in water based on a gas linkage method, which comprises the following steps:
precipitating the water to be detected to obtain a precipitate and precipitated water;
filtering the precipitated water to obtain filtered water;
dropwise adding the filtered water on a watch glass for dehydration to obtain organic matter residues;
dissolving the organic matter residue on the watch glass by using an organic solvent, and then carrying out centrifugal separation to obtain a sample to be detected;
and detecting the content of the deltamethrin in the sample to be detected by using a gas-mass linkage method.
The specific mode for dripping the filtered water on a watch glass for dehydration to obtain the organic matter residue is as follows:
dropwise adding the filtered water on a watch glass;
and (4) placing the watch glass in an oven for drying until the water in the filtered water is completely evaporated to obtain organic matter residues.
Wherein the drying temperature of the oven is 40-50 ℃.
Wherein, the organic solvent is used for dissolving the organic substance residue on the watch glass and then the centrifugal separation is carried out, and the concrete mode of obtaining the sample to be measured is as follows:
dropwise adding an organic solvent onto the organic residue on the watch glass, and crushing the organic residue by an ultrasonic instrument to obtain a first mixture;
transferring the first mixture in the watch glass to a centrifuge tube, and oscillating the first mixture in the centrifuge tube through an oscillator to obtain a second mixture;
and placing the centrifugal tube on a centrifugal machine, and carrying out centrifugal separation on the second mixture to obtain a sample to be detected and sediment.
The centrifugal machine comprises a box body, a power mechanism, a clamping mechanism, a driving mechanism and a stabilizing mechanism;
the power mechanism comprises a first motor, a rotating rod and a rotating disc, the first motor is fixedly connected with the box body and is located in the box body, the rotating rod is fixedly connected with the output end of the first motor, the rotating disc is fixedly connected with the rotating rod and is rotationally connected with the box body and is located on the inner side wall of the box body, the clamping mechanism is arranged on one side of the rotating disc, the driving mechanism is arranged on one side, close to the clamping mechanism, of the rotating disc, and the stabilizing mechanism is arranged on one side of the driving mechanism.
The driving mechanism comprises a second motor, a gear, two sliding grooves, two sliding blocks, two racks and a push rod, the second motor is fixedly connected with the rotating disc and is located on one side of the rotating rod, the gear is fixedly connected with the output end of the second motor, the two sliding grooves are fixedly connected with the rotating disc and are respectively located on two sides of the second motor, the two sliding blocks are respectively connected with the two sliding grooves in a sliding mode and are located on the inner side wall of the sliding groove, the two racks are respectively fixedly connected with the two sliding blocks and are located on one side of the sliding groove, the two push rods are respectively fixedly connected with the racks and are located on the other side of the push rod and are fixedly connected with the clamping mechanism and located between the racks and the clamping mechanism.
The clamping mechanism comprises two abutting plates, a plurality of first fitting blocks and a plurality of second fitting blocks, the two abutting plates are fixedly connected with the two push rods respectively, the first fitting blocks are connected with the two abutting plates in a sliding mode and located on one side far away from the push rods respectively, and the second fitting blocks are fixedly connected with the rotating disc respectively and located on one side close to the first fitting blocks.
The invention relates to a method for determining deltamethrin in water based on a gas-mass linkage method, which comprises the steps of precipitating water to be determined to obtain a precipitate and precipitated water; filtering the precipitated water to obtain filtered water; dropwise adding the filtered water on a watch glass for dehydration to obtain organic matter residues; dissolving the organic matter residue on the watch glass by using an organic solvent, and then carrying out centrifugal separation to obtain a sample to be detected; the method comprises the steps of detecting the content of the deltamethrin in the sample to be detected by using a gas-mass linkage method, and performing double filtration treatment on water to be detected by precipitation and filtration, so that the residue of impurities is reduced, and the problem that the detection result of the content of the deltamethrin is influenced by the impurities in the sample in the conventional detection method is solved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a method for determining deltamethrin in water based on a gas-mass linkage method provided by the invention.
Fig. 2 is a flow chart of obtaining a sample to be measured by performing centrifugal separation after dissolving the organic matter residue on the watch glass by using an organic solvent.
FIG. 3 is a schematic diagram of the structure of the centrifuge.
Fig. 4 is a cross-sectional view of the centrifuge in the direction of the cushioning spring.
Fig. 5 is a cross-sectional view of the guide assembly and the buffer spring.
1-centrifuge, 2-box, 3-power mechanism, 4-clamping mechanism, 5-driving mechanism, 6-stabilizing mechanism, 7-first motor, 8-rotating rod, 9-rotating disk, 10-second motor, 11-gear, 12-sliding chute, 13-sliding block, 14-rack, 15-push rod, 16-abutting plate, 17-first engaging block, 18-second engaging block, 19-side plate, 20-guiding component, 21-buffer spring, 22-fixed cylinder, 23-guiding cylinder and 24-limiting block.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are merely for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1 to 5, the present invention provides a method for determining deltamethrin in water based on a gas-mass linkage method, including the following steps:
s1, precipitating the water to be detected to obtain a precipitate and precipitated water;
and preliminarily removing suspended impurities in the water to be detected through precipitation.
S2, filtering the precipitated water to obtain filtered water;
and filtering the precipitated water by using a 0.45-micron microporous filter membrane.
S3, dropwise adding the filtered water on a watch glass for dehydration to obtain organic matter residues;
specifically, the filtered water is dripped on a watch glass; and (3) placing the watch glass in an oven for drying until the water in the filtered water is completely evaporated to obtain organic residue, wherein the drying temperature of the oven is 40-50 ℃, and the drying time is 10 hours.
S4, dissolving the organic matter residue on the watch glass by using an organic solvent, and then performing centrifugal separation to obtain a sample to be detected;
the concrete mode is as follows: s41, dropwise adding an organic solvent onto the organic matter residue on the watch glass, and crushing the organic matter residue through an ultrasonic instrument to obtain a first mixture;
the organic solvent is any one of acetonitrile, methanol, ethanol, isopropanol, pyridine, acetone, ethyl acetate, dichloromethane or chloroform, and the ultrasonic instrument performs ultrasonic treatment on the organic residue for 10 minutes to break the organic residue, and better mix the organic residue with the organic solvent.
S42, transferring the first mixture in the watch glass to a centrifuge tube, and oscillating the first mixture in the centrifuge tube through an oscillator to obtain a second mixture;
the shaking time of the first mixture by the shaker was 10 minutes.
And S43, placing the centrifuge tube on a centrifuge 1, and carrying out centrifugal separation on the second mixture to obtain a sample to be detected and sediment.
The speed of the centrifuge 1 is 10000 rpm and the time is 5 minutes.
And S5, detecting the content of deltamethrin in the sample to be detected by using a gas-mass linkage method.
The gas phase separation of the gas chromatography-mass spectrometry analyzer comprises a DB-5 capillary column and an MSD mass spectrometry detector, wherein the DB-5 capillary column and the capillary column have the length of 30mm, the inner diameter of 320 mu m and the film thickness of 0.5 mu m, the MSD mass spectrometry detector adopts an EI ionization source of 70eV, the ion source temperature is 230 ℃, the carrier gas He flow rate is 1.0mL/min, the sample injection amount is 1 mu L, the sample injection port temperature is 250 ℃, and the sample to be detected adopts a non-shunting mode; the chromatographic column adopts the following temperature-raising program: keeping the temperature at 40 ℃ for 2min, then heating to 150 ℃ at the speed of 10 ℃/min, keeping the temperature for 2min, then heating to 200 ℃ at the speed of 8 ℃/min, and keeping the temperature for 5min to obtain the result of the content of the deltamethrin.
Further, the centrifuge 1 comprises a box body 2, a power mechanism 3, a clamping mechanism 4, a driving mechanism 5 and a stabilizing mechanism 6;
the power mechanism 3 comprises a first motor 7, a rotating rod 8 and a rotating disc 9, the first motor 7 is fixedly connected with the box body 2 and is positioned in the box body 2, the rotating rod 8 is fixedly connected with the output end of the first motor 7, the rotating disc 9 is fixedly connected with the rotating rod 8 and is rotatably connected with the box body 2 and is positioned on the inner side wall of the box body 2, the clamping mechanism 4 is arranged on one side of the rotating disc 9, the driving mechanism 5 is arranged on one side of the rotating disc 9, which is close to the clamping mechanism 4, and the stabilizing mechanism 6 is arranged on one side of the driving mechanism 5.
In this embodiment, it is right when the second mixture carries out centrifugal separation, at first will be equipped with the second mixture the centrifuging tube place in power unit 3 on the rolling disc 9, 5 drives of actuating mechanism 4 will the centrifuging tube centre gripping is in on the rolling disc 9, first motor 7 is with 10000 commentaries on classics/minute drive bull stick 8 drives the rolling disc 9 rotates on the box 2, to in the centrifuging tube the second mixture carries out centrifugal separation, stabilizing mean 6 increases clamping mechanism 4 is right the stability of centrifuging tube centre gripping.
Further, the driving mechanism 5 includes a second motor 10, a gear 11, two sliding grooves 12, two sliding blocks 13, two racks 14 and a push rod 15, the second motor 10 is fixedly connected with the rotating disc 9 and is located at one side far away from the rotating rod 8, the gear 11 is fixedly connected with an output end of the second motor 10, the two sliding grooves 12 are respectively fixedly connected with the rotating disc 9 and are respectively located at two sides of the second motor 10, the two sliding blocks 13 are respectively slidably connected with the two sliding grooves 12 and are both located at an inner side wall of the sliding grooves 12, the two racks 14 are respectively fixedly connected with the two sliding blocks 13 and are located at one side far away from the sliding grooves 12, one sides of the two push rods 15 are respectively fixedly connected with the two racks 14, and the other sides of the two push rods 15 are respectively fixedly connected with the clamping mechanism 4, and is located between the rack 14 and the clamping mechanism 4; the clamping mechanism 4 comprises two abutting plates 16, a plurality of first fitting blocks 17 and a plurality of second fitting blocks 18, the two abutting plates 16 are respectively and fixedly connected with the two push rods 15, the plurality of first fitting blocks 17 are respectively and slidably connected with the two abutting plates 16 and are both positioned on one side far away from the push rods 15, and the plurality of second fitting blocks 18 are respectively and fixedly connected with the rotating disc 9 and are both positioned on one side close to the first fitting blocks 17.
In this embodiment, the centrifugal tube is placed between the second engaging block 18 and the first engaging block 17, the second motor 10 of the driving mechanism 5 drives the gear 11 to rotate, so that the gear 11 drives the two racks 14 to slide on the sliding chute 12 through the sliding block 13, and thus the push rod 15 pushes the first engaging block 17 on the abutting plate 16 to be close to the rotating disk 9, so as to be close to the second engaging block 18, and clamp the centrifugal tube, since the distance between the first engaging block 17 and the second engaging block 18 can be adjusted, the centrifugal tube with different tube orifice diameters can be clamped, and the first engaging block 17 and the centrifugal tube can be adjusted to slide on the abutting plate 16 according to the distance between the second engaging blocks 18.
Further, the stabilizing mechanism 6 includes two side plates 19, two guide assemblies 20 and two buffer springs 21, the two side plates 19 are respectively and fixedly connected with the two sliding chutes 12 and are located on the inner side walls of the sliding chutes 12, one sides of the two guide assemblies 20 are respectively and fixedly connected with the two side plates 19, the other sides of the two guide assemblies 20 are respectively and fixedly connected with the two sliding blocks 13 and are located between the side plates 19 and the sliding blocks 13, and the two buffer springs 21 are respectively and fixedly connected with the two guide assemblies 20 and are located in the guide assemblies 20; the direction subassembly 20 includes solid fixed cylinder 22, a guide cylinder 23 and stopper 24, gu fixed cylinder 22 with curb plate 19 fixed connection, and be located and be close to one side of slider 13, buffer spring 21 with gu fixed cylinder 22 fixed connection, and be located gu fixed cylinder 22, one side of guide cylinder 23 with buffer spring 21 fixed connection, the opposite side of guide cylinder 23 with slider 13 fixed connection, and run through gu fixed cylinder 22, stopper 24 with guide cylinder 23 fixed connection, and be located gu fixed cylinder 22.
In this embodiment, when the sliding block 13 slides, the guide cylinder 23 of the guide assembly 20 moves away from the side plate 19, the sliding groove 12 is formed in the fixed cylinder 22, and the buffer spring 21 is pulled, the buffer spring 21 can buffer the vibration transmitted to the sliding block 13 by the push rod 15 during the centrifugal separation of the second mixture in the rotating process of the rotating disc 9, so that the stability of the push rod 15 and the abutting plate 16 is increased, the stability of the clamping of the centrifugal tube is further increased, the guide cylinder 23 slides in the fixed cylinder 22 to guide the buffer spring 21, the buffer spring 21 is prevented from being bent due to external force, the buffering effect on the vibration is further influenced, the diameter of the limit block 24 is greater than the caliber of the fixed cylinder 22, and the guide cylinder 23 can be prevented from sliding out and breaking away from the fixed cylinder 22 under the driving of the sliding block 13, when the stopper 24 with during the export contact of fixed section of thick bamboo 22, for support hold board 16 with the maximum value that slider 13 removed avoids slider 13 excessively pulls buffer spring 21 still avoids support hold on the board 16 first agreeing with piece 17 excessively extrude with between the second agreeing with piece 18 the centrifuging tube is right the centrifuging tube causes the damage.
Although the above disclosure is only a preferred embodiment of the method for measuring deltamethrin in water based on the gas-mass linkage method, it is needless to say that the scope of the present invention is not limited thereby, and those skilled in the art can understand that all or part of the procedures of the above embodiment can be implemented and equivalent variations made according to the claims of the present invention are still within the scope of the present invention.
Claims (7)
1. A method for determining deltamethrin in water based on a gas linkage method is characterized by comprising the following steps:
precipitating the water to be detected to obtain a precipitate and precipitated water;
filtering the precipitated water to obtain filtered water;
dropwise adding the filtered water on a watch glass for dehydration to obtain organic matter residues;
dissolving the organic matter residue on the watch glass by using an organic solvent, and then carrying out centrifugal separation to obtain a sample to be detected;
and detecting the content of the deltamethrin in the sample to be detected by using a gas-mass linkage method.
2. The method for determining deltamethrin in water based on air-mass linkage method as claimed in claim 1,
the specific mode of dripping the filtered water on a watch glass for dehydration to obtain organic residue is as follows:
dropping the filtered water on a watch glass;
and (4) placing the watch glass in an oven for drying until the water in the filtered water is completely evaporated to obtain organic matter residues.
3. The method for measuring deltamethrin in water based on the air-mass linkage method as claimed in claim 2,
the drying temperature of the oven is 40-50 ℃.
4. The method for determining deltamethrin in water based on gas chromatography-mass spectrometry as claimed in claim 1,
the organic matter residue on the watch glass is dissolved by using an organic solvent and then is subjected to centrifugal separation, and the concrete mode of obtaining the sample to be detected is as follows:
dropwise adding an organic solvent onto the organic residue on the watch glass, and crushing the organic residue by an ultrasonic instrument to obtain a first mixture;
transferring the first mixture in the watch glass to a centrifuge tube, and oscillating the first mixture in the centrifuge tube through an oscillator to obtain a second mixture;
and placing the centrifugal tube on a centrifugal machine, and carrying out centrifugal separation on the second mixture to obtain a sample to be detected and sediment.
5. The method for determining deltamethrin in water based on air-mass linkage method as claimed in claim 4,
the centrifugal machine comprises a box body, a power mechanism, a clamping mechanism, a driving mechanism and a stabilizing mechanism;
the power mechanism comprises a first motor, a rotating rod and a rotating disc, the first motor is fixedly connected with the box body and is located in the box body, the rotating rod is fixedly connected with the output end of the first motor, the rotating disc is fixedly connected with the rotating rod and is rotationally connected with the box body and is located on the inner side wall of the box body, the clamping mechanism is arranged on one side of the rotating disc, the driving mechanism is arranged on one side, close to the clamping mechanism, of the rotating disc, and the stabilizing mechanism is arranged on one side of the driving mechanism.
6. The method for determining deltamethrin in water based on air-mass linkage method as claimed in claim 5,
actuating mechanism includes second motor, gear, two spouts, two sliders, two racks and push rod, the second motor with rolling disc fixed connection to be located and keep away from one side of bull stick, the gear with second motor output end fixed connection, two the spout respectively with rolling disc fixed connection, be located respectively the both sides of second motor, two the slider respectively with two spout sliding connection all is located the spout inside wall, two the rack respectively with two slider fixed connection, and be located and keep away from one side of spout, two one side of push rod respectively with two rack fixed connection, two the opposite side of push rod respectively with fixture fixed connection, and be located the rack with between the fixture.
7. The method for determining deltamethrin in water based on air-mass linkage method as claimed in claim 6,
the clamping mechanism comprises two abutting plates, a plurality of first fitting blocks and a plurality of second fitting blocks, the two abutting plates are fixedly connected with the two push rods respectively, the first fitting blocks are connected with the two abutting plates in a sliding mode and located on one side far away from the push rods respectively, and the second fitting blocks are fixedly connected with the rotating disc respectively and located on one side close to the first fitting blocks.
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