63Ni determination

Kallos GJ. 1981. Oxygen-induced response enhancement in determination of bis(chloromethyl) ether by gas chromatography with 63Ni electron capture detection. Anal Chem 53 963-965. 

Scheuerer et al. [5] determined 63Ni in soils. The method is applicable to analytical measurements needed during the decommissioning of nuclear power plants. 

The radioanalytical methods of determining 55Fe and 63Ni were worked out by Holm et al.6 and Skwarzec et al.11 Figures 11.1 and 11.2 illustrate the procedures for the radiochemical analysis of 55Fe and 63Ni in aquatic environmental samples. 

Figure 11.2 shows a scheme for the radioanalytical determination of 63Ni in aquatic samples.11 The method for determining nickel activity is based on the separation of this element from other radionuclides, particularly 55Fe. To separate 63Ni, the stable dimethylglyoxime (DMG) complex (DMG)2Ni is formed in ammonia and extracted with chloroform. 

FIGURE 11.2 Radioanalytical determination of 63Ni in aquatic samples. 

Skwarzec, B., E. Holm, and D. Strumiriska. 2001. Radioanalytical determination of 55Fe and 63Ni in the environmental samples. Chem. Anal. (Warsaw) 46 23-30. 

For the GC analysis of these substances trimethylsilyl derivatives are mostly prepared. Chloramphenicol is silylated with the aid of BSA [520,521 ]. Some workers [522], however, prefer an HMDS—TMCS mixture in pyridine as it is said to result in a more uniform product. The analysis is performed on silicone stationary phases of the SE-30 and OV-17 types. The related thiamphenicol is converted into the TMS derivative by treatment with BSA [523,524] and the same stationary phases are used for GC. If this method is applied to the determination of these substances in plasma and body fluids, and a selective detector is used (63Ni ECD), a sensitivity of determination of 0.1 jug/ml can be reached. 

Savory et al. [635] determined chromium in serum. The sample was wet ashed by treatment with sulphuric, nitric and perchloric acids. Finally, the pH was adjusted to 6.0 with a buffer and chelation was effected with a dilute solution of trifluoroacetylacetone at 70°C. The analysis was carried out on 5% of QF-1 on Chromosorb W with the use of a 63Ni ECD. Booth and Darby [636] applied a very similar procedure to soft tissues and serum. They performed the chelation reaction also at 70°C for 1 h. Recoveries of chromium in serum and liver homogenates were 94 and 88—104%, respectively. Ross and Shafik... 

Khan, S.U. Determination of Terbacil in Soil by Gas-Liquid Chromatography with 63Ni Electron Capture Detection, Bull Environ. Contam. Toxicol, 18(l) 83-88 (1977). 

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