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Methylation treatment gas phase detection and analysis method

A technology of gas phase detection and analysis method, which is applied in the direction of analyzing materials, measuring devices, and material separation. It can solve problems such as long-term preservation, difficult control of ultrasonic conditions, and high toxicity. It achieves simple operation, fast derivation speed, and high sensitivity. Effect

Active Publication Date: 2019-06-04
HANGZHOU PROCESS DETECTION TECH CO LTD
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  • Abstract
  • Description
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Problems solved by technology

[0011] In view of the above problems, the present invention proposes a gas-phase detection and analysis method for methylation treatment, which solves the problem that the diazomethane reagent used in the gas-phase detection and analysis method for methylation treatment has a very short validity period and cannot be stored for a long time. High toxicity; the use of iodomethane method has the disadvantages of cumbersome operation and difficult control of ultrasonic conditions

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  • Methylation treatment gas phase detection and analysis method
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  • Methylation treatment gas phase detection and analysis method

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Embodiment 1

[0057] Embodiment 1: The present invention discloses a gas-phase detection and analysis method for methylation treatment,

[0058] 1) Water sample pretreatment: first measure 200mL of water sample and place it in a 500mL separating funnel, add 50mL of ethyl acetate to extract the water sample for a total of three times, a total of 150mL was combined in a 200mL beaker, and nitrogen was blown in a water bath at 45°C. When there is 4-5 mL of ethyl acetate left, transfer it to the derivation tube, rinse the beaker with 2 mL of ethyl acetate, combine them into the derivation tube, and continue drying in a water bath with nitrogen.

[0059] 2) Methylation reaction: Take the sample solution in the organic phase (that is, obtained by extraction) and transfer it to the derivatization test tube, blow dry with nitrogen, and add 200 μL of N,N-dimethylformamide dimethyl acetal after drying and 1.0 mL of isooctane, capped and sealed, vortexed for 1 min, and placed in an oven at 80°C for met...

Embodiment 2

[0065] 1) Water sample pretreatment: first measure 200mL of water sample and place it in a 500mL separating funnel, add 50mL of ethyl acetate to extract the water sample for a total of three times, a total of 150mL was combined in a 200mL beaker, and nitrogen was blown in a water bath at 45°C. When there is 4-5 mL of ethyl acetate left, transfer it to the derivation tube, rinse the beaker with 2 mL of ethyl acetate, combine them into the derivation tube, and continue drying in a water bath with nitrogen.

[0066] 2) Methylation reaction: take the sample solution in the organic phase and transfer it into a container, blow dry with nitrogen gas, and add 500 μL of N,N-dimethylformamide dimethylformamide after drying Base acetal and 1.0mL isooctane, cover and seal, vortex for 5min, put in an oven at 180°C for methylation reaction for 3h.

[0067] 3) Extraction of the solution to be tested: after completion, take it out to return to room temperature, add 1.5mL of saturated sodium c...

Embodiment 3

[0071] 1) Water sample pretreatment: first measure 200mL of water sample and place it in a 500mL separating funnel, add 50mL of ethyl acetate to extract the water sample for a total of three times, a total of 150mL was combined in a 200mL beaker, and nitrogen was blown in a water bath at 45°C. When there is 4-5 mL of ethyl acetate left, transfer it to the derivation tube, rinse the beaker with 2 mL of ethyl acetate, combine them into the derivation tube, and continue drying in a water bath with nitrogen.

[0072] 2) Methylation reaction: take the sample solution in the organic phase and transfer it into a container, blow dry with nitrogen, add 400 μL of N,N-dimethylformamide dimethyl Base acetal and 1.0mL isooctane, cover and seal, vortex for 5min, put into an oven at 160°C for methylation reaction for 1h.

[0073] 3) Extraction of the solution to be tested: after completion, take it out to return to room temperature, add 1.5mL of saturated sodium chloride aqueous solution, co...

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Abstract

The invention discloses a methylation treatment and gaseous phase detection analysis method used for analyzing bentazone or 2,4-D. The method comprises the following steps: 1) carrying out a methylation reaction, namely transferring a sample solution obtained by extraction into a container, drying by gases, adding N,N-dimethylformamide dimethyl acetal, and carrying out the methylation reaction at the temperature of 80-180 DEG C; 2) extracting a to-be-detected solution, namely adding an aqueous solution of chloride or water into the reactants, mixing, standing and separating, taking the upper organic phase solution for later detection; and 3) performing gaseous phase detection, namely detecting the previous to-be-detected solution on a gas chromatograph. According to the method disclosed by the invention, the bentazone and 2,4-D are methylated by adopting the N,N-dimethylformamide dimethyl acetal, and detection is performed by using the gas chromatograph. The method is high in derivation speed, high in sensitivity and simple in operation.

Description

technical field [0001] The invention relates to the mechanical field of a gas-phase detection and analysis method for methylation treatment, in particular to a gas-phase detection and analysis method for methylation treatment. Background technique [0002] At present, the existing bentazone (3-isopropyl-(1H)-benzo-2,1,3-thiadiazin-4-one-2,2-dioxide) and 2,4-D ( 2,4-dichlorophenoxyacetic acid), the chemical structural formula is as follows: [0003] [0004] Both are widely used herbicides with low or moderate toxicity. In GB5749-2006 "Drinking Water Hygienic Standards", the limit of bentazone in drinking water is 0.3mg / L, and the limit of 2,4-D is 0.03mg / L. The detection methods of the two residues in water include gas chromatography, gas chromatography-mass spectrometry, high performance liquid chromatography, liquid chromatography-tandem mass spectrometry, ion chromatography and other methods reported in national standards and literature. [0005] In the National Dri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/02G01N30/70
CPCG01N30/02G01N30/06G01N30/70G01N2030/062G01N2030/067
Inventor 安建华韦红映
Owner HANGZHOU PROCESS DETECTION TECH CO LTD
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