Method using gas chromatographic method to measure purity of tri-n-octylamine

A gas chromatography and tri-n-octylamine technology, which is applied in the field of measuring the purity of tri-n-octylamine, can solve the problems of reducing processing effect, complicated operation steps, reducing extraction effect and the like, and achieves high accuracy and sensitivity, simple and rapid method, The effect of detecting a wide range

Inactive Publication Date: 2017-05-17
BLUESTAR LEHIGH ENG INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is no unified national standard for the determination of the purity of tri-n-octylamine products. Most manufacturers use chemical methods to determine the content of tertiary amine nitrogen in products. The content of tri-n-octylamine also includes other long-chain tertiary amines and short-carbon-chain tertiary amines, which lead to higher determination results than the actual purity of the product, which directly affects the user's use of tri-n-octylamine: for metal and When used as an extractant of organic acid, its extraction effect will be reduced, and its treatment effect will also be reduced when it is used for organic wastewater treatment
This has led to many users failing to obtain the theoretical effect when using the product according to the purity in the product delivery test report provided by the manufacturer of tri-n-octylamine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1, a kind of method adopting gas chromatography to measure the purity of tri-n-octylamine, described assay method comprises:

[0027] (1) The detector adopts hydrogen flame ionization detector FID;

[0028] (2) split injection, the split ratio is 50:1;

[0029] (3) The separation method adopts temperature programming. Set the initial temperature of the chromatographic column to 30°C, raise it to 250°C at 10°C / min, and stay for 2 minutes; set the temperature of the vaporization chamber to 250°C; set the temperature of the detector to 300°C;

[0030] (4) The quantitative method adopts the area normalization method.

[0031] The retention time is qualitative, and the qualitative reagent adopts chromatographically pure tri-n-octylamine;

[0032] The carrier gas is high-purity nitrogen, the combustion gas is high-purity hydrogen, and the supporting gas is high-purity air;

[0033] The separation column adopts a capillary chromatographic column;

[0034] The ga...

Embodiment 2

[0036] Embodiment 2, a kind of method adopting gas chromatography to measure the purity of tri-n-octylamine, described assay method comprises:

[0037] (1) The detector adopts hydrogen flame ionization detector FID;

[0038] (2) split injection, the split ratio is 100:1;

[0039] (3) The separation method adopts temperature programming. Set the initial temperature of the chromatographic column to 100°C, raise it to 300°C at 30°C / min, and stay for 10 minutes; set the temperature of the vaporization chamber to 300°C; set the temperature of the detector to 330°C;

[0040] (4) The quantitative method adopts the area normalization method.

Embodiment 3

[0041] Embodiment 3, a kind of method adopting gas chromatography to measure the purity of tri-n-octylamine, described assay method comprises:

[0042] (1) The detector adopts hydrogen flame ionization detector FID;

[0043] (2) split injection, the split ratio is 90:1;

[0044] (3) The separation method adopts temperature programming. Set the initial temperature of the chromatographic column to 50°C, raise it to 260°C at 20°C / min, and stay for 5 minutes; set the temperature of the vaporization chamber to 300°C; set the temperature of the detector to 330°C;

[0045] (4) The quantitative method adopts the area normalization method.

[0046] The retention time is qualitative, and the qualitative reagent adopts imported chromatographically pure tri-n-octylamine;

[0047] The carrier gas is high-purity nitrogen, the combustion gas is high-purity hydrogen, and the supporting gas is high-purity air; the purity of high-purity nitrogen, high-purity hydrogen, and high-purity air is p...

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Abstract

The invention relates to a method using a gas chromatographic method to measure the purity of tri-n-octylamine. The method is characterized in that a detector of the method is a flame ionization detector FID; split sampling is used, and the split ratio is (50:1)-(100:1); a separation method adopts programmed temperature rising, the initial temperature of a chromatographic column is set as 30-100 DEG C, the temperature is risen to 250-300 DEG C at the speed of 10-30 DEG C / minute, and the temperature is kept for 2-10 minutes; the temperature of a vaporizing chamber is set as 250-300 DEG C; the temperature of the detector is set as 300-330 DEG C; a quantitative method uses an area normalization method, and the purity of the tri-n-octylamine is determined. The method is simple, fast, wide in impurity detecting range, high in accuracy and sensitivity and good in reproducibility.

Description

technical field [0001] The invention relates to a method for measuring the purity of tri-n-octylamine by gas chromatography, which belongs to the technical field of chemical product quality detection. Background technique [0002] Tri-n-octylamine, also known as trioctylamine, is a colorless oily liquid, easily soluble in non-polar solvents, soluble in ethanol and ether. Insoluble in water. It is obtained by ammoniating n-octanol as raw material and alumina as catalyst. It is used as a metal extractant, which has good extraction performance for actinide elements such as uranium and thorium, and is also used for extraction and separation of non-ferrous metals such as rare earths and platinum groups, and metal anti-corrosion agents. Tri-n-octylamine can also be used in the extraction and recovery of organic acids and the treatment of organic wastewater. The purity of tri-n-octylamine directly affects the extraction effect of the extractant and the treatment effect of wastew...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 崔庆兰王开春董自斌刘娟徐军王克云郭涛陈添敏
Owner BLUESTAR LEHIGH ENG INST CO LTD
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