Louis W. Doher - Rocky Flats Plant, Rockwell International
John D. Livingston - N/A
During the normal operation of an analytical SS surveillance program, some difficulty is experienced in the preparation of standard solutions for control programs. The most common problems are: (1) Obtaining a stoichiometric standard compound. (2) Synthesis of a control sample which is representative of the material being routinely measured by the measurement facility. (3) Reduction of the errors involved in the preparation of the control samples to a level which is not significant when compared to the errors involved in the analytical procedure being tested. A section of the Analytical Laboratories of Rocky Flats Plant is preparing a paper dealing with point one. As for point two, these problems range from the arguments of homogeneity of samples and possible particle sizes through known impurities of both the stream and the sample. Since all of these points are relative to the particular sample in question, and the purity of the process stream, let it suffice to say that these problems are being attacked, and to the best of the authors' knowledge, continual improvements are being made. This paper is concerned with point three, wherein an accurate standard solution can be synthesized on a semi-micro scale, with complete mixing and ease of handling with isolation techniques, and a minimum of equipment. The criteria of a good control program prevent the chemist from preparing solutions measured in a mass-per-unit-volume manner using normal volumetric equipment. This problem is amplified by such factors as the necessity for micro and sub-micro techniques, and dry box methods, in addition to the usual hazards of standards preparation. The authors were confronted by these problems when a plutonium analytical laboratory changed its technique for reporting concentrations in plutonium-bearing liquids from a mass-per-unit—mass measurement to that of mass-per-unit-volume.