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
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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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