Setting priorities in CNF particle size measurement: What is needed vs. what is feasible

Abstract

Measuring the size of cellulose nanomaterials can be challenging, especially in the case of branched and entangled cellulose nanofibrils (CNFs). The International Organization for Standardization, Technical Committee 6, Task Group 1—Cellulosic Nanomaterials, is exploring opportunities to develop standard methods for the measurement of CNF particle size and particle size distribution. This paper presents a summary of the available measuring techniques, responses from a survey on the measurement needs of CNF companies and researchers, and outcomes from an international workshop on cellulose nanofibril measurement and standardization. Standardization needs differed among groups, with Japanese companies mostly requiring measurements for product specification and production control, and other companies mostly needing measurements for safety/regulatory purposes and for grade definitions in patents. Among all the companies, average length and width with percentiles (D(10), D(50), D(90)) were the most desired measurands. Workshop participants concurred that defining the location(s) on the CNF at which to measure the width and the length is an urgent and complex question. They also agreed that methods are needed for rapid particle size measurement at the nanoscale. Our recommendation within ISO is to start work to revise the definition of CNFs and develop sample preparation and measurement guidelines. It was also recommended that further research be done to reproducibly prepare hierarchical branched CNF structures and characterize them, develop automated image analysis for hierarchical branched CNF structures, and develop a classification system encompassing measurements at multiple size ranges from micro- to nanoscale to fully characterize and distinguish CNF samples.