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Gas chromatography-mass spectrometry detection method of hydrofluoroether solvent

A gas chromatography and mass spectrometry detection technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of ethyl nonafluorobutyl ether and ethyl perfluorobutyl ether substance detection, determination of purity, etc. , to achieve the effects of small matrix interference, good reproducibility, and improved detection accuracy

Active Publication Date: 2021-02-19
广电计量检测集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] So far, there are no reports on the detection and purity determination of ethyl nonafluorobutyl ether and ethyl perfluorobutyl ether in hydrofluoroether solvents

Method used

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  • Gas chromatography-mass spectrometry detection method of hydrofluoroether solvent
  • Gas chromatography-mass spectrometry detection method of hydrofluoroether solvent
  • Gas chromatography-mass spectrometry detection method of hydrofluoroether solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] This example provides the optimization steps of the gas chromatography-mass spectrometry detection method of ethyl nonafluorobutyl ether and ethyl perfluorobutyl ether, as follows:

[0067] S1. Preparation of standard sample solution;

[0068] Accurately weigh 0.10 g of ethyl nonafluorobutyl ether and ethyl perfluorobutyl ether standard substances with a 100,000 graded analytical balance, dissolve them in methanol and set the volume to a 10 mL volumetric flask, and prepare ethyl nonafluorobutyl ether Both ether and ethyl perfluorobutyl ether are 10g / L standard stock solutions, and then diluted into 20mg / L, 100mg / L, 200mg / L, 600mg / L, 1000mg / L, 2000mg / L standard sample solutions.

[0069] S2. Preparation of test solution:

[0070] Weigh 2.0000g of hydrofluoroether solvent sample, add methanol and dilute to a 25mL volumetric flask, shake well, filter through a 0.45μm microporous membrane to obtain the test solution;

[0071] S3. Detection:

[0072] The standard sample s...

Embodiment 2

[0107] This example provides an optimized gas chromatography-mass spectrometry detection method for ethyl nonafluorobutyl ether and ethyl perfluorobutyl ether. The specific operation steps are as follows:

[0108] S1. Preparation of standard sample solution;

[0109] Accurately weigh 0.10 g each of ethyl nonafluorobutyl ether and ethyl perfluorobutyl ether standard with a 100,000 graded analytical balance, dissolve in acetonitrile and set the volume to a 10 mL volumetric flask, and prepare ethyl nonafluorobutyl ether Both ether and ethyl perfluorobutyl ether are 10g / L standard stock solutions, and then diluted into 20mg / L, 100mg / L, 200mg / L, 600mg / L, 1000mg / L, 2000mg / L standard sample solutions.

[0110] S2. Preparation of test solution:

[0111] Weigh 2.5000g of hydrofluoroether solvent sample, add acetonitrile to it and dilute it to a 25mL volumetric flask, shake well, and filter through a 0.45μm microporous membrane to obtain the test solution;

[0112] S3. Detection:

[...

Embodiment 3

[0165] Compared with Example 2, this example differs in that: the DB-WAX chromatographic column is replaced by an Ultra2 chromatographic column.

[0166] The detection result is consistent with the detection result of Example 2. It shows that the type of chromatographic column has little effect on the detection of ethyl nonafluorobutyl ether and ethyl perfluorobutyl ether, the main components of hydrofluoroether solvent.

[0167] From the above analysis, it can be seen that the detection method of the present invention can detect ethyl nonafluorobutyl ether and ethyl perfluorobutyl ether, have a better peak time, and obtain a better peak shape in a normal distribution. The matrix interference is small, the reproducibility is good, and the detection accuracy is high. The detection limit (3 times signal-to-noise ratio) is 1.146 mg / L, the quantification limit is 3.820 mg / L, and the recovery rate of standard addition is 94% to 107%, which can meet the Test requirements for ethyl ...

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Abstract

The invention provides a gas chromatography-mass spectrometry detection method of a hydrofluoroether solvent. The main components of the hydrofluoroether solvent are ethyl nonafluorobutyl ether and ethyl perfluorobutyl ether; the ethyl nonafluorobutyl ether and the ethyl perfluorobutyl ether can be separated from the hydrofluoroether solvent by selecting a chromatographic column with a specific length; the heating procedure of the chromatography is further optimized, so better peak appearance time can be obtained, better peak patterns in normal distribution can be obtained, matrix interferenceis small, and reproducibility is good; and by optimizing mass spectrum parameters, detection precision can be improved, a detection limit (three times of a signal-to-noise ratio) is 1.146 mg / L, a quantification limit is 3.820 mg / L, a standard-added recovery rate is 94%-107%, and test requirements on ethyl nonafluorobutyl ether and ethyl perfluorobutyl ether can be met.

Description

technical field [0001] The invention belongs to the technical field of detection, and in particular relates to a gas chromatography-mass spectrometry detection method of a hydrofluoroether solvent. Background technique [0002] With the development of science and technology, the integration of electronic products is getting higher and higher. To ensure the normal function of the products, the cleaning of the products has become extremely important. CFC (CFC-113), which was commonly used in the electronics industry in the past, will cause ozone layer damage and greenhouse effect, and has been banned. Its substitute HCFC (HCFC-141b, HCFC-225) can only be used as a transitional alternative cleaning solvent because it still contains chlorine. [0003] In response to this development trend, 3M has developed a series of NovecTM HFE hydrofluoroether solvents (mainly composed of ethyl nonafluorobutyl ether and ethyl perfluorobutyl ether) (such as HFE-7100 / 7200). Unlike transitiona...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/60G01N30/72
CPCG01N30/02G01N30/60G01N30/72
Inventor 张兰兰何毅华丁恩恩陈礼懿
Owner 广电计量检测集团股份有限公司
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