Four years of experience in applying inductively coupled plasma-mass spectrometry (ICP-MS) to the analysis of actinides and fission products in high level waste (HLW) samples at the Savannah River Site has led to the development of a number of techniques to aid in the interpretation of the mass spectral data. Our goal has been to develop rapid and reliable analytical procedures that provide the necessary chemical and isotopic information to answer the process needs of the customers. Techniques that have been developed include the writing of computer software to strip the experimental data from the instrument data files into spreadsheets or into a spectral data processing package so that the raw mass spectra can be overlain for comparison or plotted with higher output resolution. These procedures have been applied to problems ranging from the analysis of the high level waste tanks to reactor moderator water as well as environmental samples. Criticality safety analyses in some HLW waste treatment processes depend upon actinide concentration and isotopic information generated by ICP-MS, particularly in tanks with high concentrations of 137Cs and 90Sr. Experimental results for a number of these applications will be presented. These procedures represent a considerable saving in time and expense as compared to conventional chemical separation followed by radiochemical analyses, as well as decreased radiation exposure for the analysts.

Authoritative reference providing the principles, practical techniques, and procedures for the accurate measurement of radioactivity.

A VG Elemental Inductively coupled plasma-mass spectrometer (ICPMS), PlasmaQuad 1 (PQ1) Model No. 4, installed in a radiological controlled hood, is used by the Savannah River Technology Center to provide non-routine mass measurements for environmental monitoring, waste tank characterization studies, isotope ratios for criticality determinations, and the measurement of elemental, fission product, and actinide mass distributions of the glass product from the Defense Waste Processing Facility (DWPF).

High-resolution Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) is a variant of the more conventional ICP-AES that is widely used for environmental monitoring. The relevance of high-resolution capabilities of three such analytical problems are discussed herein. (1) Pu in very complex, radioactive matrices can be determined with good accuracy without the need for prior chemical separations. Isotopically resolved spectra from actinides in fuel dissolver solutions can be obtained after a simple ion-exchange step. (2) High-resolution methods permit the simultaneous determination of fission products and actinides in simulated high-level nuclear waste solutions. Such measurements can be useful for both safeguards and waste processing. (3) The ICP-AES technique, with a photodiode array detector, can be used to determine the composition of nuclear waste glasses. Such measurements can assist the glass producer as well as providing predictors of nuclear waste form performance in a repository. 16 refs., 5 figs., 4 tabs.

Over the past decade significant progress has been achieved in the development of waste characterization and control procedures and equipment as a direct response to ever-increasing requirements for quality and reliability of information on waste characteristics. Failure in control procedures at any step can have important, adverse consequences and may result in producing waste packages which are not compliant with the waste acceptance criteria for disposal, thereby adversely impacting the repository. The information and guidance included in this publication corresponds to recent achievements and reflects the optimum approaches, thereby reducing the potential for error and enhancing the quality of the end product. -- Publisher's description.