The ability to reliably measure electromechanical properties is crucial to the advancement of materials design for applications in fields ranging from biology and medicine to energy storage and electronics. With the relentless miniaturization of device technology, the ability to perform this characterization on the nanoscale is paramount. Due to its ability to probe electromechanical properties on the micro- and nano-scales, piezoresponse force microscopy (PFM) has become the premier tool for piezoelectric and ferroelectric characterization of a new generation of smart, functional materials. Despite its widespread use and popularity, PFM is a highly nuanced technique, and measurements on similar samples using different machines and/or in different laboratories often fail to agree. A comprehensive protocol for accurate quantitative measurements has not been presented in the literature, slowing the general uptake of the technique by reducing the ability of research groups to take full advantage of PFM for their characterization needs. Here, we present a procedure for PFM measurements, which outlines the practical aspects of quantitative PFM, from sample preparation to probe choice and use of control samples, and we substantiate these steps with original data on lithium niobate control samples. This quantitative characterization protocol is critical as society looks to smaller, greener alternatives to traditional piezoelectric materials for applications such as drug delivery, bio-microelectromechanical system sensors and actuators, and energy harvesting. (c) 2021 Author(s).