The widths and overall profiles of dielectric grating lines can be determined by measuring the intensity of diffracted laser light from the sample over a specified range of incident beam angles. This technique, known as 2‐Θ scatterometry, is able to accurately and precisely measure photoresist structures in the subhalf micron regime. Moreover, a 2‐Θ scatterometer is capable of making measurements in a rapid and nondestructive manner. To test this technique we measured five identically processed wafers with nominal 0.5 μm line/0.5 μm space grating patterns. Each wafer comprised gratings in a Shipley 89131 negative photoresist exposed in a matrix of incremental exposure doses and focus settings. The scatterometry results were consistent with cross‐sectional and top‐down scanning electron microscopy (SEM) measurements of the same structures. The average deviation of 11 scatterometer linewidth measurements from top‐down SEM measurements, over a broad exposure range, is 14.5 nm. In addition, the repeatability (1σ) of the 2‐Θ scatterometer is shown to be excellent: 0.5 nm for consecutive measurements and 0.8 nm for day‐to‐day measurements.