A kind of content determination method of n-(2-methoxycyclohexyl)-1,3-propanediamine

A methoxycyclohexyl, determination method technology, applied in the field of content determination of advanced amines, to achieve the effects of high detection sensitivity, good reproducibility, and accurate content value precision

Active Publication Date: 2022-05-10
ZHEJIANG XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the content determination method of N-(2-methoxycyclohexyl)-1,3-propanediamine is not available in the literature at present.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] A method for determining the content of N-(2-methoxycyclohexyl)-1,3-propanediamine, using a thermal conductivity detector for detection, the detection conditions are: the carrier gas is hydrogen, and the chromatographic column adopts a quartz capillary as the material The chromatographic column, the column flow rate is 3ml / min, the initial column temperature is 80°C, keep it for 1 minute, use the temperature program to raise the temperature at a rate of 10°C / min, the final temperature is 250°C, keep it for 18 minutes, the detection temperature is 280°C, the injection temperature 280°C, when testing the sample, mix an equal volume of absolute ethanol and the sample evenly, and the injection volume is 1ul.

[0014] Adopt gas chromatography to measure the content of N-(2-methoxycyclohexyl)-1,3-propanediamine, through 10 parallel determination results, sample 1 # X average = 99.28%, relative standard deviation RSD = 0.04%, sample 2 # X average=99.30% relative standard devi...

Embodiment 2

[0016] A method for determining the content of N-(2-methoxycyclohexyl)-1,3-propanediamine, using a thermal conductivity detector for detection, the detection conditions are: the carrier gas is hydrogen, and the chromatographic column adopts a quartz capillary as the material The chromatographic column, the column flow rate is 3ml / min, the initial column temperature is 60°C, keep for 1 minute, use the temperature program to raise the temperature at a rate of 10°C / min, the final temperature is 255°C, keep for 18 minutes, the detection temperature is 260°C, the injection temperature 260°C, when testing the sample, mix an equal volume of absolute ethanol and the sample evenly, and the injection volume is 1ul.

Embodiment 3

[0018] A method for determining the content of N-(2-methoxycyclohexyl)-1,3-propanediamine, using a thermal conductivity detector for detection, the detection conditions are: the carrier gas is hydrogen, and the chromatographic column adopts a quartz capillary as the material The chromatographic column, the column flow rate is 3ml / min, the initial column temperature is 60°C, keep for 1 minute, use the temperature program to raise the temperature at a rate of 10°C / min, the final temperature is 260°C, keep for 18 minutes, the detection temperature is 270°C, the injection temperature 270°C, when testing the sample, mix an equal volume of absolute ethanol and the sample evenly, and the injection volume is 1ul.

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Abstract

The invention provides a method for determining the content of N-(2-methoxycyclohexyl)-1,3-propylenediamine, which is detected by a thermal conductivity detector, and the detection conditions are: the carrier gas is hydrogen, and the chromatographic column adopts The chromatographic column DB-1301 made of quartz capillary has a length of 60 meters, a diameter of 0.32mm, and a film thickness of 1.05um. The column flow rate is 3ml / min, the initial column temperature is 60-80°C, and the temperature is programmed to rise at a rate of 10°C / min. The final temperature is 250-270°C and kept for 18 minutes. The detection temperature is 260-280°C, and the injection temperature is 260- 280°C, when testing the sample, mix an equal volume of absolute ethanol and the sample evenly, and the injection volume is 1ul. The advantage of the present invention is to adopt gas chromatography to carry out content determination to the product by groping for specific measuring conditions, select specific chromatographic column to make N-(2-methoxycyclohexyl)-1,3-propylenediamine and solvent And other organic impurities can be better separated, the method has high accuracy and good reproducibility, which makes the determination method more scientific, advanced, applicable and economical.

Description

technical field [0001] The invention relates to a method for determining the content of higher amines, in particular to a method for determining the content of N-(2-methoxycyclohexyl)-1,3-propanediamine. Background technique [0002] Propylenediamine referred to in the present invention is a kind of N-(2-methoxycyclohexyl)-1,3-propanediamine, N-(2-methoxycyclohexyl)-1,3-propanediamine Amine properties, N-(2-methoxycyclohexyl)-1,3-propanediamine, English name N-(2-methoxycyclohexl)-1,3-Propanediamine, molecular formula C10H 22 N 2 O, molecular weight 186.29, is a colorless transparent liquid, miscible with water, soluble in most organic solvents such as ethanol. Slight ammonia odor. It is strongly alkaline. Relative density (d20) 0.95±0.1. Low viscosity, boiling point 288.2±30°C. The freezing point is below -18°C. Refractive index (n20D) 1.478. The flash point (closed cup) is 93°C and no flash is found. combustible. Low toxicity, median lethal dose (rat): oral LD50:...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 段小刚兰昭洪方胜军涂利根黎晓华
Owner ZHEJIANG XINHUA CHEM
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