On December 19, 1828, Vice President Calhoun submitted a report to the South Carolina State House about the hated Tariff of 1828 (the Tariff of Abominations), which soon had copies of the 35,000-word document printed and distributed at its own expense. It was a statement against the tariff, but more than that. Known to history as the South Carolina Exposition and Protest, the document argued for nullification -- the right of the states to reject federal law.
Calhoun wrote (anonymously at first, though word got out soon enough): "If it be conceded, as it must be by every one who is the least conversant with our institutions, that the sovereign powers delegated are divided between the General and State Governments, and that the latter bold their portion by the same tenure as the former, it would seem impossible to deny to the States the right of deciding on the infractions of their powers, and the proper remedy to be applied for their correction. The right of judging, in such cases, is an essential attribute of sovereignty, of which the States cannot be divested without losing their sovereignty itself, and being reduced to a subordinate corporate condition. In fact, to divide power, and to give to one of the parties the exclusive right of judging of the portion allotted to each, is, in reality, not to divide it at all; and to reserve such exclusive right to the General Government (it matters not by what department to be exercised), is to convert it, in fact, into a great consolidated government, with unlimited powers, and to divest the States, in reality, of all their rights, It is impossible to understand the force of terms, and to deny so plain a conclusion."
In early 1833, President Jackson was prepared to -- and authorized by Congress to -- take military action against South Carolina for its act late in the previous year of nullifying the Tariffs of 1828 and 1832. Old Hickory wasn't known to be a bluffing sort, so South Carolina backed down, and nullification per se was discredited. But not, as it turned out, broader notions of states' rights that weren't settled until 1865.