Method for detecting weeding ether pesticide residues in soil

A technology for pesticide residues and detection methods, applied to measuring devices, instruments, scientific instruments, etc., to achieve the effects of convenient operation, high resolution, and high degree of automation

Pending Publication Date: 2022-06-24
浙江中一检测研究院股份有限公司
View PDF0 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a soil sample extraction operation convenient, strong qualitative anti-interference ability, high quantitative accuracy of the determination method of pesticide residues of bibenbicide in the soil, using pressure solvent extraction instrument to extract the bibenbow ether in the soil, the extract is concentrated, After purification and conversion of the solvent to n-hexane, it enters the gas chromatograph for separation and is detected by a mass spectrometer to solve the technical defects of existing detection methods in qualitative analysis, sample extraction, etc.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for detecting weeding ether pesticide residues in soil
  • Method for detecting weeding ether pesticide residues in soil
  • Method for detecting weeding ether pesticide residues in soil

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0041] (2) Preparation and extraction of samples: remove foreign bodies, sticks, leaves, stones, etc. in the soil samples, and mix the samples evenly; at the same time, weigh two soil samples of about 10g (accurate to 0.01g), and one is used for determination Dry matter content, one part is used for extraction with a pressure solvent extractor; the sample used for extraction is added with an appropriate amount of diatomaceous earth and ground to a quicksand-like shape and then loaded into the extraction cell, and the mixed solvent of dichloromethane and acetone (volume Ratio 1:1) pressure extraction of herbicides in soil samples.

[0042] (3) Condition settings of the pressure solvent extractor: carrier gas (nitrogen) pressure 1.0MPa, heating temperature 100°C, pressure 1700psi, preheating equilibrium 5min, static extraction time 5min, solvent rinsing volume 60% pool volume, extraction nitrogen blowing The sweep time was 70s, and the static extraction was performed twice.

[...

Embodiment 1

[0057] (1) The detection limit of the method: Dilute the standard solution of herbicide 10 times to become the standard solution of herbicide, refer to the "Technical Guidelines for the Development of Environmental Monitoring Analysis Methods" (HJ 168), and accurately pipette 20 μL with a micropipette In the extraction tank equipped with 10g quartz sand, the standard solution of herbicidal ether was extracted with dichloromethane:acetone (1:1) on the pressure solvent extractor according to the instrument conditions in step (3), and the extract was extracted according to the steps (6) Concentrate by nitrogen blowing to convert the solvent into n-hexane, quantitatively add 100 μL of the internal standard solution, and then use n-hexane to dilute to 1 mL, and send it to the gas chromatograph from the automatic sampler according to the instrument conditions in step (7). Separation and detection by mass spectrometry detector, determination of herbicidal ether content. Repeat the ab...

Embodiment 2

[0064] Method precision: Use a micropipette to accurately pipette different volumes of the standard solution of herbicide into the extraction cell containing 10g of soil matrix samples, and use dichloromethane:acetone (1:1) on a pressure solvent extractor to press In step (3), pressurized extraction is carried out under the conditions of the apparatus, and the extract is subjected to nitrogen blowing and concentration according to step (6) to convert the solvent into n-hexane, quantitatively add 100 μL of internal standard solution, and dilute to 1 mL with n-hexane, and press step (7). ) in the instrument condition is sent to the gas chromatograph by the automatic sampler for separation and detected by the mass spectrometer detector to determine the herbicide content in the soil matrix sample. The above operation was repeated 5 times in the whole process, and the precision was measured. The precision measurement data are shown in Table 1. When the herbicide content in the soil ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a method for detecting herbicidal ether pesticide residues in soil, which comprises the following steps of: pressurizing and extracting herbicidal ether in the soil on a pressure solvent extraction instrument by using a dichloromethane and acetone mixed solvent, concentrating, purifying and carrying out solvent conversion on extract liquor, separating by using a gas chromatograph, and detecting by using a mass spectrum detector. A matrix labeling experiment shows that when the content of the herbicidal ether in a soil matrix sample is 0.2 mg/kg-2. 0mg/kg, the relative standard deviation (n = 6) of a measurement result is 4.0%-5.3%; when the addition scalar amount of the herbicidal ether in the soil matrix sample is 2 [mu] g, 5 [mu] g and 10 [mu] g, the recovery rates of the six times of independent determination are 93.5%-106%, 94.2%-104% and 95.2%-106% respectively; when the soil sampling amount is 10 g and the constant volume of the extract is 1.0 mL, the method detection limit of the herbicidal ether in the soil is 0.04 mg/kg, and the determination lower limit is 0.16 mg/kg. The mass spectrometric detector is adopted for determining the nature, the resolution ratio is high, and the anti-interference capability is high; the pressure solvent extractor is used for extracting soil samples, operation is convenient, and the automation degree is high; soil pollution investigation, risk assessment and repair evaluation can be met.

Description

technical field [0001] The invention belongs to the technical field of environmental detection, and relates to a detection method for herbicide residues in soil. Background technique [0002] Herbicide, chemical name 2,4-dichlorophenyl-4-nitrophenyl ether, is a contact herbicide. In June 2002, the Ministry of Agriculture issued Announcement No. 199 that herbicide is a pesticide prohibited by the state. In October 2017, the International Agency for Research on Cancer of the World Health Organization announced the list of carcinogens, and herbicide was included in the list of Class 2B carcinogens. Herbicides were once one of the main varieties of herbicide pesticides, widely used in agriculture and forestry weeding. Because the molecular structure of pesticides is generally relatively stable and difficult to degrade naturally, they will not degrade and disappear in the natural environment soon after application, but accumulate in soil, groundwater, surface water and marine w...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/72G01N30/8634G01N2030/045
Inventor 肖学喜朱振宏杨锦辉孙晓欣施超宇杜芳叶飙孙阳洋
Owner 浙江中一检测研究院股份有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap