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Method for detecting content of hydrazine compounds in water sample

A technology for hydrazine compounds and content, which can be used in measurement devices, instruments, scientific instruments, etc., can solve problems such as mutual interference and affect the reliability of analysis results, simplify test steps, improve the detection sensitivity of electrospray mass spectrometry, and eliminate mutual interference. Effect

Pending Publication Date: 2021-10-15
北京航天凯恩新材料有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Many methods rely on derivatization reactions to improve the detection sensitivity and method selectivity of hydrazine compounds, requiring tedious sample pretreatment, which may not only introduce more sources of error, but also put forward higher requirements for personnel skills and test conditions
When there are multiple hydrazine compounds in the sample, there may be mutual interference between different hydrazine compounds, which will affect the reliability of the analysis results

Method used

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  • Method for detecting content of hydrazine compounds in water sample
  • Method for detecting content of hydrazine compounds in water sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: The water sample containing hydrazine was diluted with 80% isopropanol and then injected for analysis. Record the ion chromatograms of mass-to-charge ratio 33 (molecular weight of protonated hydrazine) and mass-to-charge ratio 74 (molecular weight of protonated hydrazine-acetonitrile adduct), the results are shown in the attached figure 1 shown. The ion chromatograms with mass-to-charge ratio 33 and mass-to-charge ratio 74 both detected hydrazine at the same retention time, but the peak area and height of the ion chromatogram with mass-to-charge ratio 74 were much higher than those with mass-to-charge ratio 33.

Embodiment 2

[0027] Example 2: Water samples containing hydrazine, methylhydrazine, and unsymmetrical dimethylhydrazine were diluted with 70% methanol and 70% isopropanol respectively, and then 4 μL was injected for analysis. The mobile phase was 70% acetonitrile, 10 mM ammonium formate , pH4.0. Record the ion chromatograms containing the three analyte ions to be measured, and the results are shown in the attached figure 2 shown. When the sample was diluted with 70% methanol, the chromatographic peak of hydrazine bifurcated; when the sample was diluted with 70% isopropanol, the peak shape of hydrazine was better.

Embodiment 3

[0028] Example 3: After diluting the water sample containing methylhydrazine and unsymmetrical dimethylhydrazine with 50% isopropanol, inject 5μL for analysis, the mobile phase is 85% acetonitrile-15% water, 5mM ammonium formate, pH2.5 . Selected ion detection mode was adopted for mass spectrometry detection, and the ion chromatograms of protonated methylhydrazine and protonated unsymmetrical dimethylhydrazine were recorded. Baseline separation was achieved for methylhydrazine and unsymmetrical dimethylhydrazine, with good detection sensitivity for both analytes.

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Abstract

The invention relates to a method for detecting hydrazine compounds and particularly relates to a method for detecting hydrazine compounds in a water sample by using a hydrophilic interaction chromatography-mass spectrometry technology. According to the method, hydrazine compounds in a water sample are separated by using hydrophilic interaction chromatography, and then the hydrazine compounds are detected by using electrospray ionization mass spectrometry. A sample does not need to be subjected to derivatization treatment before sample introduction analysis and only needs to be diluted by using an organic solvent. The method provides a simple, convenient, rapid and effective analysis means for testing the content of the hydrazine compound in the water body.

Description

technical field [0001] The invention relates to a method for detecting hydrazine compounds, in particular to a method for detecting hydrazine compounds in water samples using hydrophilic interaction chromatography-mass spectrometry technology. Background technique [0002] Hydrazine compounds such as hydrazine, methylhydrazine, and unsymmetrical dimethylhydrazine have high reactivity and high energy density, and are commonly used in aerospace liquid propellants. At the same time, hydrazine compounds are also widely used in chemical, pharmaceutical, metallurgical and other fields. [0003] However, hydrazine compounds are also highly toxic and can cause harm to the human body through various exposure routes. Hydrazine compounds in the aquatic environment can also threaten the safety of aquatic organisms. Therefore, the relevant national standards have made clear regulations on the content of hydrazine compounds in various water bodies. [0004] Hydrazine compounds in water...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72
Inventor 徐林楠张旭贾冬雪赵坦贾月毛亚南孟醒米思巍李俊
Owner 北京航天凯恩新材料有限公司
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