The 234U/238U activity ratio (AR) is extensively used as a geochemical tool to investigate movement and flow relationships in major hydrological units, information that is particularly important when considering nuclear waste disposal. It is usually determined by radiochemical separation and concentration of U, followed by energy-specific alpha particle counting. Alternatively, sector field inductively coupled plasma mass spectrometry (SF-ICP-MS) can be used to measure U isotopic signatures directly in groundwater samples. Here, we compare the two methods for samples of spring and groundwater from southern Nevada. Results for samples stripped from stainless steel disks, previously used for alpha counting, and for splits of groundwater samples show good agreement between the methods. However, SF-ICP-MS is faster, requires much less sample, and produces essentially no waste. We demonstrate applicability of the SF-ICP-MS method for groundwater collected from over 25 wells on and near the Nevada Test Site during 2003. Uranium concentrations ranged from 0.17 to 9.87 ppb with a mean of 2.9 ppb, while 234U/238U AR values ranged from 1.9 to 11.5 with a mean of 4.3. Groundwater collected from deep wells in the northern part of the study area tended to have moderate to high U concentrations and AR values, possibly representative of older volcanic-type waters, whereas groundwater from wells in the Fortymile Wash area had relatively low AR and U concentrations, suggesting younger waters with a possible local recharge component.