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Isn't it that NLS_LANG is an Environment variable and for the session its NLS_LANGUAGE?
Also read this Faq about the same,
And this page about Alter session and NLS settings,
NLS_LANG is an environment variable, i.e. which can't be at session level using ALTER SESSION.
If you are on Windows, try as follows.
C:\> set NLS_LANG=AMERICAN_AMERICA.WE8MSWIN1252
$ export NLS_LANG=AMERICAN_AMERICA.WE8MSWIN1252
Other NLS Parameters can be set in the initialization parameter, As environment variables , and With the ALTER SESSION statement.
Hope this helps.