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.
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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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