The 44-year-old found herself in the bottom two after public votes were announced, alongside boyband District 3.
Taking part in a tense sing-off, Masson belted out Duffy hit Stay With Me Baby, but it seems her impressive rendition wasn't enough to beat District 3's performance of Bryan Adams' Anything I Do.
Louis Walsh voted for his group contestants, as did Tulisa by his side. Gary Barlow swiftly added a vote for Melanie, while, after a long speech, Nicole Scherzinger took the vote to deadlock.
'First of all boys you did an amazing job, I know I gave you a hard time yesterday, but you knocked it out of the park at Bootcamp and you did it tonight,' she gushed.
'Melanie, I have to go off of the saving song that I just saw, you are the oldest in this competition, and I know you have been waiting for this your whole life and I felt it in that performance.'
'The act I'm saving is Melanie.'
With that, the decision was taken to the public, which gave Melanie the least amount of votes, sending her home.
Smiling, she said: 'I've absolutely enjoyed every single second of being here. It's just been the best experience and I've loved every minute of it.'
Gary Barlow, who stormed off stage when his act lost out last week added: 'For me Melanie is one of the best singers in the competition. I'm absolutely gutted for you.'
WATCH Melanie in action here...
Who got your vote on the X Factor this week? Was Melanie Masson the right contestant to go? Let us know on the comments box below...