Method for pretreating aqueous solution containing organic amine compounds and determination method

An aqueous solution and pretreatment technology, applied in the field of detection and analysis, can solve problems such as reducing the service life of expensive capillary columns, affecting the accuracy level of detection and analysis, and failing to solve problems such as sulfate, so as to reduce maintenance frequency, reduce clogging, and reduce solution alkalinity. Enhanced effect

Active Publication Date: 2012-07-18
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP +1
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Problems solved by technology

However, although the patent application discloses the use of alkaline reagents to eliminate the interference caused by metal ions and hydrogen ions, it not only does not solve the problem of the influence of inorganic salts such as sulfate, but also introduces a high concentration of Alkali metal ions such as sodium and potassium will instead lead to a substantial increase in the concentration of inorganic salts such as sodium sulfate in the prepared sample solution, which will lead to a large increase in the concentration of organic amines in the chromatographic analysis instruments such as GC or GC-MS. At high temperature, the organic components

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  • Method for pretreating aqueous solution containing organic amine compounds and determination method

Examples

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example 1

[0039] Pretreatment to prepare sample solution of organic amine desulfurizer solution

[0040] Measure 80mL of organic amine desulfurizer solution (hereinafter referred to as original sample 1) into a 250mL Erlenmeyer flask, add 10g of solid sodium hydroxide and cover with a stopper, shake to dissolve and adjust the pH of the solution to > 11; continue to shake the conical flask vigorously bottle for 3 minutes to promote a sufficient chemical reaction between sodium hydroxide and the interfering components in the desulfurizer, filter and separate the metal hydroxide precipitate, collect the filtrate in a 150mL volumetric flask, and wash the Erlenmeyer flask and metal hydride three times with 15mL of water The oxide precipitates, and the washing solution is collected in the original filtrate, diluted with water to volume, and shaken up.

[0041] The filtrate was transferred to a 250mL Erlenmeyer flask, placed in a refrigerator freezer, and kept frozen for 1.5 hours at a low t...

example 2

[0049] Measure 120mL of organic amine desulfurizer solution (hereinafter referred to as original sample 2), add 20g of sodium hydroxide to adjust the pH>11; shake for 5 minutes, filter the metal hydroxide precipitate and wash the Erlenmeyer flask and the precipitate with 20mL of water 5 times . The filtrate was frozen at 3°C ​​for 2.5 hours. Except for this, the rest were carried out in the same manner as Example 1 to prepare the sample solution to be tested, and sample solution 2 was obtained and determined by GC-MS.

example 3

[0051] Measure 100mL organic amine desulfurizer solution (hereinafter referred to as original sample 3), add 15g sodium hydroxide to adjust the pH>11; shake for 4 minutes, filter the metal hydroxide precipitate and wash the Erlenmeyer flask and the precipitate 4 times with 18mL water . The filtrate was frozen at 7°C for 2 hours. Except for this, the rest were carried out in the same manner as Example 1 to prepare the sample solution to be tested, and the sample solution 3 was obtained and determined by GC-MS.

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Abstract

The invention provides a method for pretreating an aqueous solution containing organic amine compounds and a determination method. The method for pretreating the aqueous solution containing the organic amine compounds comprises the following steps of: adding sodium hydroxide into the aqueous solution, and regulating the pH value of the aqueous solution to be more than 11 so as to ensure that metal ions in the aqueous solution are subjected to chemical reaction to obtain a metal hydroxide precipitate; dry-filtering to obtain a filtrate and the metal hydroxide precipitate, washing the metal hydroxide precipitate and a precipitation reaction container, and collecting a washing liquid into the filtrate; reducing the temperature of the filtrate to ensure that inorganic salts in the filtrate are crystallized and precipitated from the filtrate; and dry-filtering the filtrate which is subjected to temperature reduction to remove inorganic salt crystals and obtain a clear liquid, namely a sample solution. The determination method comprises the following step of: performing assay determination on the sample solution by one or more methods of gas chromatography-mass spectrometry, gas chromatography, liquid chromatography, and liquid chromatography-mass spectrometry to obtain the content of the organic amine compounds.

Description

technical field [0001] The invention relates to the detection and analysis of a solution containing organic amine compounds, in particular to a method capable of eliminating the influence of inorganic salts such as metal ions, hydrogen ions and sodium sulfate in the solution on the determination of organic amine compounds, thereby accurately A method for determining the content of organic amine compounds in a solution. Background technique [0002] In the prior art, organic amine compounds refer to organic compounds produced by the chemical reaction between organic substances and ammonia, and are generally divided into fatty amines, alcohol amines, amides, alicyclic amines, aromatic amines, naphthalene amines, and other amines. and other seven categories. For example, organic amine compounds include: methylamine, ethylamine, n-propylamine, tert-butylaminoethanol (TBE), tert-butylaminoethoxyethanol (TBEE), 2-pyridineethanol (PE), 2-amino-2-methanol 1-propanol (AMP), monoeth...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/14G01N30/02
Inventor 成勇黎建明杨平杨新能李光跃
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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