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N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]methyl carbamate content analysis method

A technology of methyl carbamate and trifluoromethoxy, applied in the field of analysis and determination, can solve the problem of not detecting N-chloroformyl trifluoromethoxy) phenyl] methyl carbamate, unavoidable inorganic salts and moisture It can avoid the interference of inorganic salts and moisture, the baseline is stable, and it is not easy to be lost.

Active Publication Date: 2013-04-10
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, in the production of methyl N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]carbamate, it is usually detected by liquid chromatography, however, N-chloroformyl- N-[4-(trifluoromethoxy) phenyl] methyl carbamate is very unstable and easily decomposes when meeting water; when using conventional gas chromatography to detect, it is inevitable that N-chloroformyl-N-[ Inorganic salt and moisture in the production of 4-(trifluoromethoxy) phenyl] methyl carbamate are brought into, but, FID detector has no response value to inorganic salt and moisture, therefore, conventional area percentage method cannot be true accurately reflect the content of methyl N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]carbamate (the measured value is larger than the real value)
At present, there is no fast and accurate method for detecting the content of N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]carbamate at home and abroad.

Method used

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  • N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]methyl carbamate content analysis method

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Agilent7890A gas chromatograph with hydrogen flame ionization detector is used, using capillary column, the column length is 15 meters, the column temperature is 140 ℃, the gasification chamber is 200 ℃, the detector is 200 ℃, high-purity helium is used as the carrier gas, and the flow rate 1.0ml / min, hydrogen flow rate 30ml / min, air flow rate 300ml / min, injection volume 1 microliter, theoretical plate number according to N-chloroformyl-N-[4-(trifluoromethoxy)phenyl] Methyl carbamate is counted as 2000.

[0025] Internal standard preparation

[0026] Accurately weigh 5.0500g of diethyl phthalate in a 500ml volumetric flask, dissolve in toluene, cool to room temperature, dilute to volume with toluene, shake well, and set aside.

[0027] Standard sample preparation

[0028] Accurately weigh 0.0509g N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]carbamate standard substance and place it in a 10ml volumetric flask, accurately transfer into 5ml internal standard solution, di...

Embodiment 2

[0036] Adopt Agilent7890A gas chromatograph with hydrogen flame ionization detector, internal standard and standard sample preparation, test and calculation method are the same as embodiment 1. A capillary chromatographic column is used, the column length is 30 meters, the inner diameter is 0.32 mm, and the film thickness is 0.24 microns. Use HP-5 as the stationary phase, the temperature of the column chamber is 150°C, the gasification chamber is 200°C, the detection chamber is 200°C, high-purity nitrogen is used as the carrier gas, the flow rate is 2.0ml / min, the flow rate of hydrogen is 30ml / min, and the flow rate of air is 300ml / min , with an injection volume of 1 μl. The number of theoretical plates is 3000 according to methyl N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]carbamate.

[0037] Sample preparation

[0038] Accurately weigh 6 samples containing 0.05g (accurate to 0.0002g) of methyl N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]carbamate, and place them in 10ml ...

Embodiment 3

[0045] Adopt Agilent7890A gas chromatograph with hydrogen flame ionization detector, internal standard and standard sample preparation, test and calculation method are the same as embodiment 1. A capillary column with a length of 20 meters, an inner diameter of 0.32 mm and a film thickness of 0.25 microns was used. Use HP-5 as the stationary phase, the temperature of the column chamber is 160°C, the gasification chamber is 200°C, the detection chamber is 200°C, high-purity nitrogen is used as the carrier gas, the flow rate is 1.5ml / min, the flow rate of hydrogen is 30ml / min, and the flow rate of air is 300ml / min , with an injection volume of 1 μl. The number of theoretical plates was 2500 based on methyl N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]carbamate.

[0046] Sample preparation

[0047] Accurately weigh a sample containing 0.0504g (accurate to 0.0002g) of methyl N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]carbamate, place it in a 10ml volumetric flask, and accurate...

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Abstract

The invention relates to an N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]methyl carbamate content analysis method which comprises the following steps: separating and determining N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]methyl carbamate in a sample by utilizing a gas chromatograph with a hydrogen flame ionization detector and a quartz capillary gas chromatographic column and taking diethyl phthalate as an internal standard substance; and through the comparison with the standard substance, calculating the N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]methyl carbamate content in the measured sample. The invention can effectively avoid the interference of inorganic salt and water, has the advantages of favorable precision, high recovery rate, high result accuracy and favorable reproducibility, and is especially applicable to the quality control on the pesticidal chemical intermediate product N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]methyl carbamate, thereby achieving important functions and practical meanings for ensuring the quality of the final product.

Description

technical field [0001] The invention belongs to the technical field of analysis and measurement, relates to chromatographic analysis technology, in particular to an analysis and testing technology for the content of methyl N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]carbamate. Background technique [0002] Methyl N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]carbamate is a key intermediate for the synthesis of indoxacarb, N-chloroformyl-N-[4-(trifluoroformyl Oxygen) phenyl] methyl carbamate content is low, directly affects the quality of follow-up product, yield, production cost. [0003] At present, in the production of methyl N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]carbamate, it is usually detected by liquid chromatography, however, N-chloroformyl- N-[4-(trifluoromethoxy) phenyl] methyl carbamate is very unstable and easily decomposes when meeting water; when using conventional gas chromatography to detect, it is inevitable that N-chloroformyl-N-[ Inorganic salt and...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/60
Inventor 杨得霞张建林门振史庆苓马韵升栾波高洪奎李太衬
Owner CHAMBROAD CHEM IND RES INST CO LTD
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