Detection of iron and iron-cobalt labeled cellulose nanofibrils using ICP-OES and XμCT

When studying the properties of cellulose nanofibrils (CNF) enriched fiber products, it is essential to be able to determine the retention and the spatial distribution of the CNF inside the end-product. That is, to determine how much and where the CNF has been attached. As the CNF and cellulose fibers share the same density and chemical composition, labeling of the CNF is required to distinguish them from each other. In this work, we have applied iron and iron-cobalt -labeling. Labeling with iron is more desirable because of the carcinogenic and toxic properties of cobalt chloride. The benefits of our labeling method are the possibility to determine the retention of the labeled nanocellulose using inductively coupled plasma optical emission spectroscopy (ICP-OES), and to define the spatial distribution using X-ray micro-computed tomographic (XμCT). With XμCT we were able to measure fairly large samples (2 cm × 5 cm × 5 cm). Our study found that the retention of iron-labeled CNF was about 95 % and that of iron-cobalt labeled CNF was 84-94 %. Labeling of CNF improves the contrast of X-ray images. Labeled CNF is attached to fiber network also in the inner structures of the sample. Furthermore, when making thick porous structures using cationic starch, there might be agglomerates in the sample that cannot be visually detected by looking the sample.