Application of double-positive imidazolium salt ionic liquid in extraction of bisphenol compound and micro-extraction technology based on ionic liquid
A positive imidazolium salt, ionic liquid technology, applied in the field of analytical chemistry, can solve the problem of lack of micro-extraction technology, and achieve the effect of wide linear range, low detection limit and good reproducibility
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Embodiment 1
[0041] Experimental reagents: bisphenol A (BPA, 99% purity), bisphenol B (BPB, >98% purity), bisphenol AF (BPAF, 99% purity) and bisphenol Z (BPZ, 95% purity) were purchased from Sigma - Aldrich (West Chester, PA; USA). Chromatographic grade methanol and acetonitrile were purchased from Shanghai Merck Reagent Company. and 1-butyl-3-methylimidazolium tetrafluoroborate ([C4MIM]BF4) were purchased from Shanghai Chengjie Co., Ltd. The novel ionic liquid double-positive imidazolium bromide ([C4(MIM)2]Br2, [C6(MIM)2]Br2) was synthesized in the laboratory. Other chemical reagents were of analytical grade and purchased from Tianjin Chemical Reagent Co., Ltd.
[0042] Standard solution preparation: the preparation concentration is 1000μg mL -1 BPA, BPB, BPAF and BPZ mixed standard solution (4 ℃ standby).
[0043] Yili milk was purchased from Wenzhou Baixin Supermarket and stored at 4°C.
[0044] The water used in the experiment is ultrapure water (resistivity ≥ 18.2MΩ cm)
[0045] ...
Embodiment 2
[0073] Experimental reagent, instrument, process are as shown in embodiment 1, and its difference point is that used extraction agent is [C 6 (MIM) 2 ]Br 2 , adding LiNTf 2 Afterwards, ultrasonic treatment was performed for 1 to 9 minutes.
[0074] Experimental Results: Ultrasound Can Accelerate Organic Reaction, Contributes to LiNTf 2 Dissolve in the system solution, increase LiNTf 2 The probability of contact with the ionic liquid can accelerate the in-situ reaction, make the reaction more complete, and shorten the operation time.
[0075] Depend on Figure 9 It can be seen that when the ultrasonic time is between 1 and 9 minutes, the extraction rate is very considerable.
[0076] Among them, when the ultrasonic time increased from 1 minute to 3 minutes, the average extraction recovery of bisphenols increased from 74.08% to 84.60%; when the ultrasonic time continued to increase, the average extraction recovery of bisphenols appeared different degree of decline. The r...
Embodiment 3
[0078] Experimental reagent, instrument, process are as shown in embodiment 1, and its difference point is that used extraction agent is [C 6 (MIM) 2 ]Br 2 , The cooling time is 5-13 minutes.
[0079] Experimental results: if Figure 10 Shown, when cooling time is 5~13 minutes, its extraction rate is all very objective.
[0080] When the cooling time was increased from 5 minutes to 9 minutes, the average extraction recovery of bisphenols increased from 76.7% to 79.9%. This is because cooling can increase the viscosity of the ionic liquid, which is beneficial to its separation from water, and indirectly improves the extraction recovery rate of bisphenols. With the increase of cooling time, the recovery rate of bisphenols decreased from 79.9% to 73.4%, which may be due to the excessive cooling time and the high viscosity of the ionic liquid, which caused the ionic liquid to not be completely separated from the water phase during the centrifugation process. , thus reducing t...
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