The extraction with petroleum ether was performed under optimized conditions: temperature, 160°C; static extraction time, 10 min; pressure, 1500 psi; flush volume, 40%; static cycle 1 and one for the number of extraction.
Mirivel and co-workers determined the PLE recoveries of various OPAHs (including BAQ and BaAQ) spiked onto filters to be in the order of 79 107%% (PLE with methanol and one 8-min static cycle at 100 °C) [ 24], and Walgraeve and co-workers obtained recoveries of 99 ± 4 % and 101 ± 4 % for BAQ at ambient temperature and at 40 °C, respectively (PLE with ethyl acetate and three 5-min static cycles).
Hernández's "Silencio" differs greatly from the "Buena Vista" version: it bobs and weaves, changing its rhythmic background against static cycles of melody.
A factorial design was used to identify the optimal PLE operational conditions: 2 static cycles of 5 min at 80 °C.
The optimised PSE procedure implies the use of 1 g of sample, without preliminary clean-up step, sea sand as dispersant, temperature of 105 °C, methanol (63%) in water as solvent, and 5 min of extraction time (2 static cycles).
For each solvent mixture, two static cycles were applied.
The operational settings were as follows: extraction temperature 70 °C, extraction pressure 2,000 psi, static time 5 min, flush volume 60%, purge time 120 s, and two static cycles.
A total of five static cycles were used at 5 min per cycle, with a final flush of solvent equal to 75% of the cell volume (approx. 11 mL).
Extraction was performed using pressurized liquid extraction (ASE 350, Dionex Europe, U.K). using hexane/dichloromethane (1 1, v/v) at 45°C and 1500 psi with a heating time of 5 min, static 4 min, purge time 90 s, flush volume 50%, with three static cycles.
Three of the beams were subjected to uni-directional, static loading and the remainder were loaded under constant-range, quasi-static cycles.
Test specimens were loaded in quasi-static cycles with successively increasing loads, and damage development in the vicinity of the bolt holes was detected using different methods such as strain measurements, acoustic emission, X-ray and microscopic examination.
