It was also the first time the Free Practices were held under the new qualifying regulations, meaning the line-up for Saturday's Q2 has now been established.
From 2013 onwards, the first three of four MotoGP practice sessions have a direct bearing on Qualifying. For this reason, there was much tension in the bottom half of the top ten as riders strived for a place in Saturday's pole position Q2 shootout.
The first session of the day did not see riders improve over Thursday due to the windy and dirty track conditions. As the second free practice session started there were worries in the paddock that rain, which had already affected earlier sessions, may return and break up the action. As it transpired, the showers stayed away and made for a dramatic climax to the night's action.
Delivering a lap time of 1'56.084 in the last knockings, Márquez confirmed that he will be able to fight for pole position on his MotoGP debut. He demoted champion Jorge Lorenzo by just one thousandth of a second, who was trying out his new chassis, which is near identical to the current bike but with a different stiffness.
Britain's Cal Crutchlow comfortably sealed a Q2 placing with third spot for Monster Yamaha Tech 3, as Lorenzo's teammate Valentino Rossi was fourth.
Shooting into the top five in the late stages was Andrea Dovizioso on his first Ducati Team weekend, showing that the new Desmosedici is certainly competitive in Losail, with Repsol's Dani Pedrosa having struggled for front end grip since the start of first practice, but still securing a Q2 effort with sixth.
As track conditions improved towards the end of practice, a dramatic battled raged while riders continued to push rivals out of the top ten. Álvaro Bautista went seventh for GO&FUN Honda Gresini, as the times suddenly became the tightest they have been all weekend.
In eighth spot was Nicky Hayden on the second Ducati Team bike, with British rookie Bradley Smith impressing on his first outing by achieving ninth for Tech 3. Stefan Bradl looked to have a challenge on his hands as the times came down, but snatched back tenth for LCR Honda MotoGP.
Ninth tenths of a second separate the top ten - a group in which may of the riders are split up by margins of just thousandths of a second.
At the end of Q1 on Saturday, grid positions 13 and downward will be decided. However, the fastest two riders will be promoted to Q2, making for a final top-12 contest.
Judging by the latest form, it looks as though that battle will be between Pramac pairing Andrea Iannone and Ben Spies, plus Power Electronics Aspar's Aleix Espargaró on the leading CRT machine; the trio ended Friday in positions 11 to 13.
Behind, Héctor Barberá was the leading Avintia Blusens representative in 14th from PBM's Yonny Hernández, Aspar's Randy de Puniet and NGM Mobile Forward Racing's Colin Edwards.
Karel Abraham and Cardion AB Motoracing were 18th as Hiroshi Aoyama and Danilo Petrucci completed the top 20 for Avintia and Came IodaRacing Project, respectively.
21st and 22nd places are split by less than a tenth, showing that the competition is just as tight at the back of the field between Bryan Staring, on Gresini's CRT bike, and Ioda's Czech newcomer Lukáš Pešek.
PBM's Michael Laverty continued to develop the team's own-built bike en route to 23rd, whereas Forward's Claudio Corti rounded off the timesheets after stopping on-track after his FTR-Kawasaki started smoking.