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, especiall

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

Example Embodiment

[0053]Example 1

[0054]1. Rotary evaporation and re-processing recovery mixed solvent: The total volume of 60.00 ml is steam under conditions 42 ° C, vacuum degree of 0.09 MPa.

[0055]2, using gas chromatography-mass spectrometer using gas chromatography and mass spectrometry test conditions:

[0056]Gas chromatography conditions:

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

[0058]The program was warmed: at the initial temperature of 40 ° C, maintained for 5 min, raised at 20 ° C to 220 ° C for 5 min;

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

[0060]Inlet temperature: 230 ° C

[0061]Inject volume: 1μL, shunt ratio: 60: 1

[0062]Mass spectrometry:

[0063]Electronic bombardment ion source (EI);

[0064]Ion source temperature: 230 ° C;

[0065]Chromatographic mass spectrum transmission rod temperature: 250 ° C;

[0066]Quality scan range: 29-650AMU;

[0067]Quality: He, flow rate: 2.25ml / min;

[0068]Collision gas: N2, Flow rate: 1.5 mL / min;

[0069]Detection method: Multiple re...

Example Embodiment

[0090]Example 2

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

[0092]2. Detection was carried out using a gas chromatography-mass spectrometer using a gas chromatography-mass spectrometer, as in Example 1.

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

[0094]4, setting of MRM measurement: As in Example 1.

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

[0096]6. To analyze the formulation and steam of pure ethyl acetate and petroleum ether mixed solvent: as in Example 1.

[0097]7. ODURTIVATION Samples: According to the above detection conditions, mix the solvent injection before and after the above steps, resulting in a peak area to substituting the curve equation in Example 1 to calculate the extracetonate volume percentage content, result See Table 6, the result showed that the content of ethyl acetate before and after steaming was not significantly changed, EA: PE volume ratio of 1: 1 changed to 10.47% for accidental errors, may be beca...

Example Embodiment

[0106]Example 3

[0107]1. Rotary evaporation Recycled acetate and petroleum ether mixed solvent: as in Example 1.

[0108]2. Detection was carried out using a gas chromatography-mass spectrometer using a gas chromatography-mass spectrometer, as in Example 1.

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

[0110]4, setting of MRM measurement: As in Example 1.

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

[0112]6. To analyze the formulation and steam of pure ethyl acetate and petroleum ether mixed solvent: as in Example 1.

[0113]7. ODRC analysis Sample: According to the above detection conditions, mix the solvent injection before and after the above steps, resulting in the standard curve equation of the peak area into Embodiment 1 to calculate the amount of ethyl acetate volume, The results are shown in Table 8, and the results show that there is no significant change in the content of ethyl acetate before and after steam.

[0114]Table 8 Detection results of ethyl acet...

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PUM

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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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