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Method for determining the content of N, N-dihydroxyethyl glycine in alcohol amine solution

A bishydroxyethylglycine and alcohol amine solution technology, applied in the field of chemical detection, can solve the problems of difficult quantitative operation, weak ionization tendency, and impossibility, and achieve the effect of accurate measurement

Active Publication Date: 2019-01-04
PETROCHINA CO LTD
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Problems solved by technology

Therefore, the acid-base titration method cannot realize the accurate determination of the content of N,N-dihydroxyethylglycine in the alcohol amine solution.
When the colorimetric analysis method is used, if the alcohol amine solution contains primary amines, the primary amines will also develop color with ninhydrin and other display agents, seriously interfering with the determination of N,N-dihydroxyethylglycine, and the colorimetric analysis method What is important is the total content of various amino acids, so the colorimetric analysis method cannot realize the accurate determination of the content of N,N-bishydroxyethylglycine in the alcohol amine solution
When using high-performance liquid chromatography, only the method of high-sensitivity detectors such as post-column derivatization and fluorescence can detect trace amounts of N,N-dihydroxyethylglycine in the alcohol amine solution sample, which is complicated to operate and requires the use of toxic reagents. And when the alcohol amine mass fraction exceeds 32%, it will interfere with the determination of N,N-bishydroxyethylglycine, so high performance liquid chromatography cannot realize the accurate determination of N,N-bishydroxyethylglycine content in the alcohol amine solution
When capillary electrophoresis is used, the ionization tendency of N,N-dihydroxyethylglycine is weak, and it is difficult to separate from other weakly polar organic impurities in the alcohol amine solution; The content of these components is changed, and the electroosmotic flow will change due to the change of the content of these components in the alcohol amine solution sample, making the quantitative operation very difficult; in addition, when this method is applied to the analysis of the alcohol amine solution sample, there is also the problem of poor repeatability. Therefore, the capillary electrophoresis method cannot realize the accurate determination of the content of N,N-dihydroxyethylglycine in the alcohol amine solution.
[0004] In summary, due to the different physical and chemical properties of N,N-bishydroxyethylglycine and glycine and the influence of other components such as alcohol amine in the alcohol amine solution, the determination method of glycine content provided by the prior art cannot detect alcohol. Accurate Determination of N,N-Dihydroxyethylglycine Content in Amine Solution

Method used

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  • Method for determining the content of N, N-dihydroxyethyl glycine in alcohol amine solution
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  • Method for determining the content of N, N-dihydroxyethyl glycine in alcohol amine solution

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Embodiment 1

[0087] This embodiment provides a method for determining the content of N,N-dihydroxyethylglycine in an alcohol amine solution, the method comprising the following steps:

[0088] Glass wool is placed at the bottom of the ion exchange resin column tube, and 50 g of cation exchange resin is added.

[0089] Adopt 100mL deionized water to rinse this cation exchange resin, then add mass concentration and be 3% hydrochloric acid solution 100mL, make hydrochloric acid solution with 4hr -1 Slowly flow through the cation exchange resin. After the hydrochloric acid solution is exhausted, the cation exchange resin is rinsed with deionized water until the effluent is neutral.

[0090] Add 4 g of alcohol amine solution sample (accurate to 0.01 mg) to the resin column by decrement method. Then, 20 g of ethyl acetate was added to the resin column.

[0091] Accurately weigh a clean, dry, empty beaker and place it directly under the ion exchange resin column. Slowly open the bottom plug o...

Embodiment 2

[0116] The operation steps of this embodiment are the same as those of Embodiment 1. The difference is: the alcohol amine solution sample used in this embodiment is different from that of Example 1 (that is, the content of N,N-bishydroxyethylglycine in it is different);

[0117] The alcohol amine solution sample quality that adds in the ion exchange resin column is 3g, after adding the alcohol amine solution sample, the ethyl acetate that adds in the ion exchange resin column is 23g;

[0118] The gas chromatograph model is Agilent 7890A;

[0119] The column model is DB-1;

[0120] The column temperature is constant at 160°C;

[0121] Column flow (nitrogen) is 1.6mL / min;

[0122] Detector: The detector temperature is 280°C, the gas (hydrogen) flow rate is 1.4mL / min, and the assisted gas (air) flow rate is 14mL / min.

[0123] Measurement result:

[0124] Measure the mass fraction of N,N-bicine in the effluent for 5 times, obtain the content of N,N-bicine in the alcohol amin...

Embodiment 3

[0134] The operation steps of this embodiment are the same as those of Embodiment 1. The difference is: the alcohol amine solution sample used in this embodiment is different from that of Example 1 (that is, the content of N,N-bishydroxyethylglycine in it is different);

[0135] The type of cation exchange resin used is D113;

[0136] The alcohol amine solution sample quality that adds in the ion exchange resin column is 2g, after adding the alcohol amine solution sample, the ethyl acetate that adds in the ion exchange resin column is 23g;

[0137] The speed at which the effluent drips into the beaker is 3hr -1 ;

[0138] The column model is PH-5;

[0139] The gasification chamber temperature is 300°C;

[0140] The column temperature is programmed temperature rise (initial temperature 150°C, rising to 230°C at 10°C / min);

[0141] The column flow rate (nitrogen) was changed from 1.5mL / min to 1.8mL / min;

[0142] Detector: gas (hydrogen) flow rate is 1.8mL / min, assisted gas...

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Abstract

The invention discloses a method for determining the content of N, N-dihydroxyethyl glycine in alcohol amine solution, which belongs to the field of chemical detection. The method includes: adding a predetermined amount of alcohol amine solution sample to an ion exchange resin column filled with cation exchange resin, wherein the alcohol amine solution sample flows through the cation exchange resin, the alcohol amine is adsorbed on the cation exchange resin, N, N-dihydroxyethyl glycine is discharged from the outlet of the ion exchange resin column along with the effluent; determining the massfraction of N, N-dihydroxyethyl glycine in the effluent to obtain the content of N, N-dihydroxyethyl glycine in the alcohol solution. The method for determining the content of N, N-dihydroxyethyl glycine in alcohol amine solution is very accurate in measurement.

Description

technical field [0001] The invention relates to the field of chemical detection, in particular to a method for determining the content of N,N-dihydroxyethylglycine in an alcohol amine solution. Background technique [0002] The alcohol amine method is usually used to desulfurize and decarbonize natural gas, refinery gas and other industrial gases to achieve the purpose of gas purification. In the above gas purification process, the alcohol amine solution used is polluted by its own disproportionation, oxidation and raw material gas And generate N, N-bishydroxyethyl glycine and heat stable salt. N, N-bishydroxyethylglycine and heat-stable salts are highly corrosive, which will cause safety problems such as corrosion and perforation in the gas purification device used. In order to ensure the safe and stable operation of the gas purification device, the content of N,N-bishydroxyethylglycine and heat-stable salt in the alcohol amine solution must be strictly controlled. Among ...

Claims

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Application Information

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IPC IPC(8): G01N30/96G01N5/04
CPCG01N5/04G01N30/96
Inventor 颜晓琴常宏岗涂陈媛陈庆梅高立新熊钢吴明鸥
Owner PETROCHINA CO LTD
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