New methods for critical dimension (CD) measurements may be needed to enable the detailed characterization of nanoscale structures produced in the semiconductor industry and for nanotechnology applications. In earlier work, small angle x‐ray scattering (SAXS) measurements with synchrotron sources have shown promise in meeting several grand challenges for CD metrology. However, it is not practical to depend upon x‐ray synchrotron sources, which are large national facilities with limitations in the number of available instruments. To address this problem, a laboratory scale SAXS instrument for critical dimension measurements on periodic nanoscale patterns has been designed, installed, and tested. The system possesses two configurations, SAXS and ultra‐small‐angle x‐ray scattering (USAXS), with a radiation target of either copper or molybdenum. With these configurations, the instrument is capable of accessing scattering angles that probe length scales ranging from ca. 0.5 nm to 2 μm. In this work, we compare CD‐SAXS measurements taken from a synchrotron‐based SAXS at the Advanced Photon Source of the Argonne National Laboratory with those from the National Institute of Standards and Technology laboratory‐scale SAXS instrument. The results from standard line/space gratings possessing periodic line‐space patterns with CDs of tens to hundreds of nanometers show that the laboratory‐scale system can quantitatively measure parameters, such as the pitch, line width, height, line‐width roughness and sidewall angle. These results show that laboratory‐scale measurements are feasible and can be used for research and development purposes or to assist calibration of optical scatterometry and CD‐scanning electron microscopy instruments. The primary limitation of the measurement is that the data collection rate is unacceptably slow for production metrology because of the significantly lower x‐ray beam fluxes currently available.New methods for critical dimension (CD) measurements may be needed to enable the detailed characterization of nanoscale structures produced in the semiconductor industry and for nanotechnology applications. In earlier work, small angle x‐ray scattering (SAXS) measurements with synchrotron sources have shown promise in meeting several grand challenges for CD metrology. However, it is not practical to depend upon x‐ray synchrotron sources, which are large national facilities with limitations in the number of available instruments. To address this problem, a laboratory scale SAXS instrument for critical dimension measurements on periodic nanoscale patterns has been designed, installed, and tested. The system possesses two configurations, SAXS and ultra‐small‐angle x‐ray scattering (USAXS), with a radiation target of either copper or molybdenum. With these configurations, the instrument is capable of accessing scattering angles that probe length scales ranging from ca. 0.5 nm to 2 μm. In this work, we compare...