AVS 66th International Symposium & Exhibition
    New Challenges to Reproducible Data and Analysis Focus Topic Wednesday Sessions
       Session RA+AS+BI-WeA

Invited Paper RA+AS+BI-WeA9
Complementary Measurements of Colloidal Nanoparticles and their Coatings by In-situ and Vacuum-based Methods

Wednesday, October 23, 2019, 5:00 pm, Room A124-125

Session: Addressing Reproducibility Challenges using Multi-Technique Approaches
Presenter: Caterina Minelli, National Physical Laboratory, UK
Correspondent: Click to Email

Engineered nanoparticles add high value to commercial products and have the potential to improve our quality of lives and boost prosperity. For example, they provide radical new approaches to cancer drug delivery, biosensing, medical imaging and catalysis. However, the effective implementation of these materials relies on the ability to measure and control their properties, such as their surface chemical identity, size and concentration. There are significant challenges in the analysis of nanomaterials due to, among other factors, the interdisciplinary nature of the field and the lack of adequate reference materials to calibrate analytical tools. The use of complementary tools provides opportunities for (1) deepening the quantitative understanding of these systems and, importantly, (2) a route to method validation. I will provide examples from our work on both these cases.

(1) We use a combination of methods to analyse nanoparticles which are employed in liquid media (in-situ) using techniques such as analytical centrifugation and dynamic light scattering and ex-situ with X-ray photoelectron spectroscopy (XPS). Sound sample preparation protocols are critical for meaningful and comparable measurements. This is especially important when using complementary methods for the analysis of the same samples. I will discuss our experience in the analysis of protein coated gold nanoparticles and polymeric core/shell nanoparticles and show how multimodal analysis is critical to the full understanding of the system.

(2) The lack of certified reference materials for nanoparticle number concentration has hindered the validation of laboratory methods, which resulted in a general distrust in commercially available instrumentation. We have led a collaborative effort to develop accurate methods based on small angle X-ray scattering (SAXS) and single particle inductively coupled plasma mass spectrometry (spICPMS) for the measurement of colloidal number concentration. We have then used these methods to assess and validate a range of laboratory methods. I will discuss the result of this work for both ideal and agglomerated nanoparticles and present the outcomes of a large VAMAS interlaboratory study which assessed four methods for the measurement of colloidal concentration.

Finally, I will look at unmet challenges in the characterisation of nanoparticles and discuss the benefits of a multimodal approach to them.