Sample preparation by borate fusion of catalysts and high silica samples for ICP-OES analysis: method development and results

The analysis and determination of metals and trace metals in high silica and alumino-silicate samples such as catalysts and Zeolites are never easy, mainly because of the dissolution process. Samples containing silica often need hazardous chemicals (HF), strong acids (HClO4) or microwave digestions.

This application note describes a new approach using lithium borate fusion as the sample preparation method as well as the optimization of ICP-OES parameters. Many elements showed a signal suppression varying from 0 to 40 % while Plasma ionization effects from the borate solution enhanced the K, Na, and Rb signals.
High levels of Si, Al, Ca and Na from the sample and Li from the matrix required a strict scheme to correct all spectral interferences. The PerkinElmer® WinLab 32 software for the Optima™ ICP-OES allowed for three spectral correction techniques and they were used as follows:
• Background correction if no wing lines nearby;
• Multi-component spectral fitting ( MSF ) when there is a partial overlapping;
• Inter-element corrections ( IEC ) when lines are completely overlapped.

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