Sample, selection 2, gross

The procedure followed entails the removal of gross interferences by solvent extraction, and the selective extraction and concentration of the trace metal by use of a chelating agent. The alloy used should not contain more than 0.1 g of copper in the sample weighed out. 

It is clear that neither NMEA nor NDPA is appropriate for an internal standard in NDMA determination if criteria are interpreted strictly, but both compounds have been used for this purpose. Addition of a nitrosamine, not normally present in the sample, is helpful in detecting any gross errors in the procedure, but the addition should not be considered to be internal standardization. Utilization of NMEA or NDPA to indicate recovery of NDMA can lead to significant errors. In most reports of the application of these "internal standards", recovery of all nitrosamines was close to 100%. Under these conditions, any added compound would appear to be a good internal standard, but none is necessary. NDMA is a particularly difficult compound for use of internal standardization because of its anomalous distribution behavior. I mass j ectrometry is employed for quantitative determination, H- or N-labeled NDMA could be added as internal standard. Because the labeled material would coelute from GC columns with the unlabeled NDMA, this approach is unworkable when GC-TEA is employed or when high resolution MS selected ion monitoring is used with the equipment described above. 

To collect a representative primary or gross sample, see Figure 1. First, the appropriate container or containers must be selected from the population of M containers. Second, a representative sample must be withdrawn from each of the selected containers. 

Gross dissolution of the waste can be measured from the loss of weight of the sample or by determination of the appearance in the leaching medium of the major matrix constituent e.g. glass). However, the selective leaching of important fission product elements has been observed in this work to be significantly different from that of the bulk waste matrix. The units normally used to describe leach rates, g/cm day, appear to imply... 

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