Ok, try this:
1) plug in your usb disk
2) type  "mount"  in a terminal to see which device it is (something starting 
with /dev)
3) then type "sudo umount /dev/...", where /dev/,,, is what you found in step 2
make sure no open nautilus windows are displaying the contents of this disk...

tell us what the output of step 3 was...
good luck

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Cannot unmount the volume 'USB DISK'
https://bugs.launchpad.net/bugs/262046
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