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Recovery and analytical test method of ethyl acetate and petroleum ether mixed solvent

A technology of ethyl acetate and mixed solvent, which is applied in the field of recovery and analysis and testing of ethyl acetate and petroleum ether mixed solvent, can solve problems such as difficulty in qualitative analysis, and achieve the effect of good recovery effect and good linear relationship.

Pending Publication Date: 2021-04-30
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Mass spectrometry can perform effective qualitative analysis, but it is powerless for the analysis of complex organic compounds; while chromatography is an effective separation and analysis method for organic compounds, especially suitable for quantitative analysis of organic compounds, but qualitative analysis is more difficult. Difficulty, the effective combination of the two can efficiently carry out qualitative and quantitative analysis of the target

Method used

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  • Recovery and analytical test method of ethyl acetate and petroleum ether mixed solvent
  • Recovery and analytical test method of ethyl acetate and petroleum ether mixed solvent
  • Recovery and analytical test method of ethyl acetate and petroleum ether mixed solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] 1. Rotary evaporation and reprocessing to recover the mixed solvent: the mixed solution with a total volume of 60.00 mL was subjected to rotary evaporation at 42°C and a vacuum of 0.09 MPa.

[0055] 2. Use gas chromatography-mass spectrometry for detection, and the gas chromatography and mass spectrometry detection conditions are:

[0056] Gas chromatography conditions:

[0057] Chromatographic column: TG-624 chromatographic column (30m×0.32mm×1.8μm);

[0058] Programmed temperature rise: initial temperature 40°C, keep for 5 minutes, increase to 220°C at 20°C / min and keep for 5 minutes;

[0059] Carrier gas: helium (purity ≥ 99.999%), flow rate: 1.5mL / min;

[0060] Inlet temperature: 230°C

[0061] Injection volume: 1μL, split ratio: 60:1

[0062] Mass Spectrometry Conditions:

[0063] Electron bombardment ion source (EI);

[0064] Ion source temperature: 230°C;

[0065] Chromatography mass spectrometer transfer rod temperature: 250°C;

[0066] Mass scanning range...

Embodiment 2

[0091] 1. Rotary evaporation recovery mixed solvent: as in Example 1.

[0092] 2. Detection by gas chromatography-mass spectrometry, as in Example 1.

[0093] 3. Selection of quantitative objects and methods: as in Example 1.

[0094] 4. Setting of MRM measurement method: as in Example 1.

[0095] 5. Draw a standard curve: as in Example 1.

[0096] 6. Preparation and rotary evaporation of mixed solvent of pure ethyl acetate and sherwood oil for analysis: as in Example 1.

[0097] 7. Quantitative analysis of samples by external standard method: according to the above detection conditions, the mixed solvent before and after the rotary evaporation obtained in the above steps was taken for sample injection, and the peak area obtained was substituted into the standard curve equation in Example 1 to calculate the volume percentage of ethyl acetate. The result See Table 6, the results show that there is no significant change in the content of ethyl acetate before and after the rot...

Embodiment 3

[0107] 1. The mixed solvent of ethyl acetate and sherwood oil is recovered by rotary evaporation: as in Example 1.

[0108] 2. Detection by gas chromatography-mass spectrometry, as in Example 1.

[0109] 3. Selection of quantitative objects and methods: as in Example 1.

[0110] 4. Setting of MRM measurement method: as in Example 1.

[0111] 5. Draw a standard curve: as in Example 1.

[0112] 6. Preparation and rotary evaporation of mixed solvent of pure ethyl acetate and sherwood oil for analysis: as in Example 1.

[0113] 7. Quantitative analysis of samples by external standard method: according to the above detection conditions, the sample injection of the mixed solvent before and after the rotary evaporation obtained in the above steps is taken, and the obtained peak area is substituted into the standard curve equation in Example 1 to calculate the volume percentage of ethyl acetate. The results are shown in Table 8, and the results show that there is no significant cha...

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Abstract

The invention discloses an ethyl acetate and petroleum ether mixed solvent recovery and analytical test method. The method comprises the following steps of (1) carrying out recovery treatment on an ethyl acetate and petroleum ether mixed solvent sample to be recovered by using a rotary evaporator to obtain a recovered mixed solution; (2) detecting the sample by using a gas chromatography-mass spectrometer combined method, and setting gas chromatography and mass spectrometry detection conditions; (3) selecting ethyl acetate as a quantitative object; (4) setting a multi-reaction monitoring detection mode: selecting proper ions as qualitative and quantitative ions according to a mass spectrogram of analytically pure ethyl acetate; (5) preparing an ethyl acetate standard solution by taking petroleum ether as a solvent; (6) constructing a standard curve; (7) quantitatively analyzing an actual sample by an external standard method; and (8) qualitatively determining actual sample components by a GCMS (Gas Chromatography Mass Spectrometry) method. The ethyl acetate and petroleum ether mixed solvent recovery and analytical test method can realize recovery and reutilization of the mixed solvent.

Description

technical field [0001] The invention relates to a method for recovery, analysis and testing of a mixed solvent of ethyl acetate and petroleum ether. Background technique [0002] With the rapid development of my country's economic construction, the problem of environmental pollution is becoming more and more prominent. Environmental protection and governance are of great significance to the implementation of "sustainable development strategy". The amount of chemical substances discharged each time in the chemical laboratories of colleges and universities is not much, but the impact on the environment caused by the accumulation of time cannot be ignored. [0003] Ethyl acetate and petroleum ether are commonly used chromatography solvents in laboratories, and are consumed in large amounts in organic synthesis laboratories. Choosing an appropriate method for recycling can not only reduce the discharge of waste liquid, which is beneficial to environmental protection, but also c...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 李国华胡叶慧叶飞孙欣颖李雨佳张朱涛
Owner ZHEJIANG UNIV OF TECH
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