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By Wolfgang J. Kirsten
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Extra resources for Organic Elemental Analysis. Ultramicro, Micro, and Trace Methods
Sample text
When large samples are analyzed using an oxygen supplying catalyst like nickel oxide at a temperatur e above 1000°C, the catalyst sinters slowly and looses a part of its activity. This causes formation of methane in the combustion. The methane is measured as nitrogen. It is, therefore, recommended to carry out an analysis of a nitrogen-free substance like sucrose now and then. When unacceptably high nitrogen blanks are obtained the nickel oxide must be replaced with a new charge. When the flash compartment of the combustion tube is filled with residues from capsules and samples so that additional samples will not become hot enough to give efficient flash combustion (which can be observed through the window in the sampler), take out the tube and scratch out the residues with a steel hook until the quartz splinters begin to appear.
The methane is measured as nitrogen. It is, therefore, recommended to carry out an analysis of a nitrogen-free substance like sucrose now and then. When unacceptably high nitrogen blanks are obtained the nickel oxide must be replaced with a new charge. When the flash compartment of the combustion tube is filled with residues from capsules and samples so that additional samples will not become hot enough to give efficient flash combustion (which can be observed through the window in the sampler), take out the tube and scratch out the residues with a steel hook until the quartz splinters begin to appear.
Put a few empty capsules into the drum and analyze them according to the manual, using different sample inlet delay times (say, 17, 20, 25, and 30 s), and observe the flashes in the combustion tube. Adjust the inlet delay to about 3 s before the maximum flash. , when the copper has been reduced with impure hydrogen). In this case nitrogen blanks are obtained with nitrogen-free samples, but no nitrogen blanks are obtained without samples: Carbon dioxide and water from samples react with the carbon from the impurity to form carbon monoxide and hydrogen, which are measured as nitrogen.