Abstract

Turbidity measurements are frequently implemented for the monitoring of heterogeneous chemical, physical, or biotechnological processes. However, for quantitative measurements, turbidity probes need calibration, as is requested and regulated by the ISO 7027:1999. Accordingly, a formazine suspension has to be produced. Despite this regulatory demand, no scientific publication on the stability and reproducibility of this polymerization process is available. In addition, no characterization of the optical properties of this calibration material with other optical methods had been achieved so far. Thus, in this contribution, process conditions such as temperature and concentration have been systematically investigated by turbidity probe measurements and Photon Density Wave (PDW) spectroscopy, revealing an influence on the temporal formazine formation onset. In contrast, different reaction temperatures do not lead to different scattering properties for the final formazine suspensions, but give an access to the activation energy for this condensation reaction. Based on PDW spectroscopy data, the synthesis of formazine is reproducible. However, very strong influences of the ambient conditions on the measurements of the turbidity probe have been observed, limiting its applicability. The restrictions of the turbidity probe with respect to scatterer concentration are examined on the basis of formazine and polystyrene suspensions. Compared to PDW spectroscopy data, signal saturation is observed at already low reduced scattering coefficients.

Highlights

  • Process analytical technologies (PAT) are important to ensure quality, efficiency, and safety during chemical, physical, and biotechnological processing [1]

  • This strongly disagrees with the stated reproducibility of formazine suspensions of about 1 % [11, 18]

  • Besides the saturation and calibration problem of a turbidity probe, multiwavelength measurements are highly recommended for turbidity measurements as well as for Photon Density Wave (PDW) spectroscopy

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Summary

Introduction

Process analytical technologies (PAT) are important to ensure quality, efficiency, and safety during chemical, physical, and biotechnological processing [1]. Photon Density Wave (PDW) spectroscopy [12,13,14,15,16] is well suited for this polymerization reaction, since it absolutely and independently quantifies the optical properties of the formazine suspension, i.e., the absorption coefficient (μa) and the reduced scattering coefficient (μs′).

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