Radioactivation of sulfur is a common technique used to measure fast neutron fluences in test and research reactors. Elemental sulfur can be pressed into pellets and used as monitors. The 32S(n, p)32P reaction has a practical threshold of about 3 MeV and its cross section and associated uncertainties are well characterized . The product 32P emits a beta particle with a maximum energy of 1710 keV . This energetic beta particle allows pellets to be counted intact. ASTM Standard Test Method for Measuring Reaction Rates and Fast-Neutron Fluences by Radioactivation of Sulfur-32 (E265)  details a method of calibration for counting systems and subsequent analysis of results. This method requires irradiation of sulfur monitors in a fast-neutron field whose spectrum and intensity are well known. The resultant decay-corrected count rate is then correlated to the known fast neutron fluence. The Radiation Metrology Laboratory (RML) at Sandia has traditionally performed calibration irradiations of sulfur pellets using the 252Cf spontaneous fission neutron source at the National Institute of Standards and Technology (NIST)  as a transfer standard. However, decay has reduced the intensity of NIST's source; thus lowering the practical upper limits of available fluence. As of May 2010, neutron emission rates have decayed to approximately 3e8 n/s. In practice, this degradation of capabilities precludes calibrations at the highest fluence levels produced at test reactors and limits the useful range of count rates that can be measured. Furthermore, the reduced availability of replacement 252Cf threatens the long-term viability of the NIST 252Cf facility for sulfur pellet calibrations. In lieu of correlating count rate to neutron fluence in a reference field the total quantity of 32P produced in a pellet can be determined by absolute counting methods. This offers an attractive alternative to extended 252Cf exposures because it can be performed regardless of the characterization of the exposure environment. Count rates produced by sulfur pellets are correlated to the measured quantity of separated 32P. A posteriori spectral and cross section determination can be used to correlate the quantity of phosphorus back to a neutron fluence in a reference field. This paper outlines a method for the setup, calibration, and use of the detector systems, 32P sample preparation, and analysis of the beta spectrum. An uncertainty analysis and comparison to ASTM E265 is also included.