No it will not work, not that way anyway.
Are you trying to just gain access to files on the drive, or trying to use it as a bootable drive??
This will make a difference, plus if the files on your XP drive were protected, it will be difficult to get those files off of it.
Basically when you properly install the two OS's, when you start the computer a "boot loader screen" will come up, basically an option screen that will ask you which OS you wish to run.
BUT
You need to install the OS's properly in a specific way for it to work. For me, a clean install of both OS's is the best way to go, installing XP first, then Vista, since Vista will recognise the older OS (XP), and allow you to install it as a secondary OS, even though it will be the default OS if you do not make the choice while restarting the computer (don't worry, you still are able to choose everytime you reboot the system).
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