Following the Missouri Compromise, there were fears in the South that tariffs which protected Northern manufacturing profits were causing economic difficulty in the slave-holding South. Because of these tariffs, they argued, Southerners had to pay much higher prices for imported manufactured goods. A recession in the South during the 1820's was essentially blamed on the country's tariff policies. The South Carolina Senator and then Vice President under John Quincy Adams, John C. Calhoun, was among the leaders in the fight against there protective tariffs. As feelings of nationalism began to diminish among Southerners, Calhoun issued a doctrine that proclaimed it was "the right of any state overrule or modify not only the tariff but also any federal government law deemed unconstitutional. Nullification was a complete theory of government that placed the greatest powers on the state level rather than the national. With this proclamation of states' rights, Calhoun had come full circle in his political philosophy" (Davis, 38).
Although Calhoun was bold in his thinking, his proclamation failed its major test in 1832 when South Carolina formally rejected two national tariffs. President Andrew Jackson deemed the rejection as treasonous, and threatened the use of force to uphold the tariffs. After much debate, and because Calhoun could not gain enough support, a compromise had to be agreed to. However, despite this first failure, Calhoun began a campaign to muster support for solidarity among all the Southern states, and thus began the fight for states' right. The issue would not be fully resolved until the Civil War was won by the Union in 1865.
Source Used: Brother Against Brother: The War Begins. William C. Davis, 1983.