Dilution Methods in Flow Injection Analysis. Evaluation of Different Approaches as Exemplified for the Determination of Nitrosyl in Concentrated Sulphuric Acid

Abstract

Instigated by developing a flow injection procedure for assay of nitrosyl in concentrated sulphuric acid, different approaches for reliable and robust on-line dilution in FIA were evaluated. These comprised the application of mixing tees in conjunction with mixing coils (including knotted reactors) of different internal diameter, zone sampling, the use of a mixing chamber, micro-sampling, and sample injection by means of pseudo-hydrodynamic injection. The individual approaches are described in detail, their advantages and disadvantages being emphasized in regard to their practical applicability. For each approach the criteria stipulated were that the procedure should allow a dilution factor of approximately 100, yet without excessive zone spreading, so that it, on one hand, could effectively eliminate the pronounced Schlieren effect encountered when mixing concentrated sulphuric acid with an aqueous diluent, and, on the other hand, would permit the sample material to be appropriately conditioned for the ensuing chemical derivatization procedure. It was found that this most reliably could be effected by a combination of pseudo-hydrodynamic injection comprising a mixing point and the use of mixing tees in conjunction with knotted reactors of relatively large internal diameter (1.5 mm). The optimized FI-manifold was used with the Griess method for the spectrophotometric assay of nitrosyl (nitrite) in standards prepared in the matrix of concentrated sulphuric acid (detection limit 0.16 mg/1 NO⁺-N (3[sgrave])) and in practical WSA-samples.

Key Words:

• Elimination of Schlieren
• FIA dilution methods
• nitrosyl
• Griess reaction
• spectrophotomerry
• concentrated sulphuric acid matrix