Triethylamine content determination method

Abstract

The invention relates to the field of wastewater treatment, and discloses a triethylamine content determination method, which comprises: (1) preparing more than two different standard samples containing an internal standard substance and triethylamine and having different components, wherein the standard samples are used for determining a relative correction factor f1 and a calibration curve; (2)adding the internal standard substance to a triethylamine solution to be determined to obtain a sample to be determined; and (3) determining the internal standard substance peak areas and the triethylamine peak areas in the standard samples, the sample to be determined, and the triethylamine solution to be determined through chromatography, wherein f1, r, and the triethylamine content are calculated according to the following formulas defined in the specification. According to the present invention, the method has the simple operation, is especially suitable for the determination of the triethylamine content in the wastewater with large difference in the triethylamine content, can accurately calculate the relative correction factor f1 and the linear correlation coefficient r, can eliminatethe interference on the determination result due to the internal standard substance possibly existing in the wastewater, and can effectively improve the accuracy of the determination result.

Description

technical field

[0001] The invention relates to the field of wastewater treatment, in particular to a method for determining the content of triethylamine. Background technique

[0002] Triethylamine is an important chemical raw material, mainly used as medicine, polymerization inhibitor, preservative, insecticide and industrial solvent. In the production of molecular sieves such as SAPO-5, SAPO-34, and ZSM-12, triethylamine as a template is one of the main components of raw material costs. During the production and use of triethylamine, if it is discharged into the ground or water, it will cause great harm to the water quality environment and human health.

[0003] In the synthesis reaction of molecular sieves, triethylamine as a template is not consumed, and the research on its post-processing and recycling methods is helpful for reducing pollution emissions, establishing a green and friendly molecular sieve production process, and reducing the production cost of molecular...

Examples

Embodiment approach

[0054] According to a preferred embodiment of the present invention, in the sample to be tested, the mass ratio of the internal standard substance to the triethylamine solution to be tested is 0.0025-0.01:1, preferably 0.005-0.01:1. By adopting this preferred embodiment, more accurate measurement results can be obtained even if less internal standard substance is used.

[0055] According to a preferred embodiment of the present invention, the triethylamine solution to be tested comes from wastewater generated during the production of molecular sieves. The assay method of triethylamine content that the present invention provides is particularly suitable for the mensuration of triethylamine content in the solution that triethylamine content differs greatly, and the assay method of triethylamine content that prior art provides is relatively different for triethylamine content. The wastewater generated during the production of large molecular sieves is not very suitable.

[0056]...

Embodiment 1

[0073] This example is used to illustrate the assay method of the present invention.

[0074] (1) Preparation of standard samples

[0075] Add 2g of triethylamine and 38g of water into a 50mL volumetric flask, and then add 0.5mL of ethanol to prepare standard sample 1; add 40g of triethylamine and 0.5mL of ethanol into a 50mL volumetric flask to prepare standard sample 2.

[0076] (2) Preparation of samples to be tested

[0077] Add 40 g of the triethylamine solution 1 to be tested and 0.5 mL of ethanol into a 50 mL volumetric flask and mix well to obtain the sample to be tested.

[0078] (3) Determination of samples to be tested

[0079] The chromatographic conditions in Table 1 were used to measure the peak areas of standard sample 1, standard sample 2, triethylamine solution 1 to be tested and ethanol and triethylamine in the sample to be tested, and the number of determinations was 3 times. The test results and calculation results are listed in Table 3.

[0080] table ...

Embodiment 2

[0083] This example is used to illustrate the assay method of the present invention.

[0084] (1) Preparation of standard samples

[0085] Add 2g of triethylamine and 38g of water into a 50mL volumetric flask, then add 0.5mL of ethanol to prepare standard sample 1; add 38g of triethylamine and 2g of water into a 50mL volumetric flask, then add 0.5mL of ethanol to prepare Standard sample 2; Add 68g of triethylamine and 12g of water into a 100mL volumetric flask, then add 1mL of ethanol to prepare standard sample 3.

[0086] (2) Preparation of samples to be tested

[0087] Add 40g of the triethylamine solution 2 to be tested and 0.5mL of ethanol into a 50mL volumetric flask and mix well to obtain the sample to be tested.

[0088] (3) Determination of samples to be tested

[0089] The chromatographic conditions in Table 1 were used to measure the peak areas of standard sample 1, standard sample 2, standard sample 3, triethylamine solution 2 to be tested and ethanol and triethy...

technical field

[0001] The invention relates to the field of wastewater treatment, in particular to a method for determining the content of triethylamine. Background technique

[0002] Triethylamine is an important chemical raw material, mainly used as medicine, polymerization inhibitor, preservative, insecticide and industrial solvent. In the production of molecular sieves such as SAPO-5, SAPO-34, and ZSM-12, triethylamine as a template is one of the main components of raw material costs. During the production and use of triethylamine, if it is discharged into the ground or water, it will cause great harm to the water quality environment and human health.

[0003] In the synthesis reaction of molecular sieves, triethylamine as a template is not consumed, and the research on its post-processing and recycling methods is helpful for reducing pollution emissions, establishing a green and friendly molecular sieve production process, and reducing the production cost of molecular...

Examples

Embodiment approach

[0054] According to a preferred embodiment of the present invention, in the sample to be tested, the mass ratio of the internal standard substance to the triethylamine solution to be tested is 0.0025-0.01:1, preferably 0.005-0.01:1. By adopting this preferred embodiment, more accurate measurement results can be obtained even if less internal standard substance is used.

[0055] According to a preferred embodiment of the present invention, the triethylamine solution to be tested comes from wastewater generated during the production of molecular sieves. The assay method of triethylamine content that the present invention provides is particularly suitable for the mensuration of triethylamine content in the solution that triethylamine content differs greatly, and the assay method of triethylamine content that prior art provides is relatively different for triethylamine content. The wastewater generated during the production of large molecular sieves is not very suitable.

[0056]...

Embodiment 1

[0073] This example is used to illustrate the assay method of the present invention.

[0074] (1) Preparation of standard samples

[0075] Add 2g of triethylamine and 38g of water into a 50mL volumetric flask, and then add 0.5mL of ethanol to prepare standard sample 1; add 40g of triethylamine and 0.5mL of ethanol into a 50mL volumetric flask to prepare standard sample 2.

[0076] (2) Preparation of samples to be tested

[0077] Add 40 g of the triethylamine solution 1 to be tested and 0.5 mL of ethanol into a 50 mL volumetric flask and mix well to obtain the sample to be tested.

[0078] (3) Determination of samples to be tested

[0079] The chromatographic conditions in Table 1 were used to measure the peak areas of standard sample 1, standard sample 2, triethylamine solution 1 to be tested and ethanol and triethylamine in the sample to be tested, and the number of determinations was 3 times. The test results and calculation results are listed in Table 3.

[0080] table ...

Embodiment 2

[0083] This example is used to illustrate the assay method of the present invention.

[0084] (1) Preparation of standard samples

[0085] Add 2g of triethylamine and 38g of water into a 50mL volumetric flask, then add 0.5mL of ethanol to prepare standard sample 1; add 38g of triethylamine and 2g of water into a 50mL volumetric flask, then add 0.5mL of ethanol to prepare Standard sample 2; Add 68g of triethylamine and 12g of water into a 100mL volumetric flask, then add 1mL of ethanol to prepare standard sample 3.

[0086] (2) Preparation of samples to be tested

[0087] Add 40g of the triethylamine solution 2 to be tested and 0.5mL of ethanol into a 50mL volumetric flask and mix well to obtain the sample to be tested.

[0088] (3) Determination of samples to be tested

[0089] The chromatographic conditions in Table 1 were used to measure the peak areas of standard sample 1, standard sample 2, standard sample 3, triethylamine solution 2 to be tested and ethanol and triethy...

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