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Sykes and Rea spent all of practice trading top spot on the timesheets, and did so again in qualifying, with the former edging ahead to set the initial pace in SP2 with a 1m27.663s.
Both Kawasaki riders came under no threat as the rest of the SP2 runners put in their race tyre laps, and proved untouchable on their qualifying runs.
Championship leader Rea took provisional pole with a 1m26.956s with 30 seconds left on the clock, but was deposed by Sykes, who did a 1m26.663s, to better Troy Corser's pole record by one.
He claimed his first top spot on the grid since the Phillip Island round in February.
Althea BMW's Loris Baz secured his first front row start since returning to WSBK despite being almost seven tenths off the pace.
Lorenzo Savadori heads row two on his Milwaukee Aprilia, with the Italian leading the Yamaha duo of Alex Lowes and Michael van der Mark.
Eugene Laverty will start his home round from seventh on the second of the Aprilias ahead of SP1 graduates Toprak Razgatlioglu and Chaz Davies.
Bradley Ray put his British Superbike-spec Hawk Racing Suzuki 10th for his WSBK debut, with BSB rival Leon Haslam on the Puccetti Kawasaki and the second Ducati of Marco Melandri completing the top 12.
Leon Camier sat atop the SP1 timesheets or much of the session, and was still inside the SP2 progression places when the chequered flag was flown.
However, the Ten Kate Honda rider – who has been passed fit to race today, but will be assessed once again on Sunday – was knocked down a spot by Davies' final lap, and will start 13th ahead of MV Agusta's Jordi Torres and Ducati's Michael Ruben Rinaldi.
Barni Racing's Xavi Fores was the surprise scalp in the first part of qualifying, with the customer Ducati rider a lowly 22nd and 1.3s from the top two.
Wildcard Mason Law crashed at Redgate at the start of the session and was unable to set a laptime, leaving the Team WD40 Kawasaki rider last of the 25-strong field for race one.
|6||60||Michael van der Mark||Yamaha||1'27.472||0.809|
|14||81||Jordi Torres||MV Agusta||1'28.230||1.567|
|15||21||Michael Ruben Rinaldi||Ducati||1'28.376||1.713|
Injured Camier unsure if he'll race at Donington
Donington WSBK: Van der Mark holds off Rea for maiden win