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WP 6 Analytical Methods for In-situ Determination of Nanoparticles Fate

WP6 Objectives

The overall goal is the development and application of analytical methods and protocols for in-situ measurement, detection and studies of the fate of nanoparticles. This will be achieved by research activities covering three main areas:

  Optimisation of monitoring and tracing tools for laboratory and field use.

  Application of modern high performance analytics for on-site measurements and in-situ characterization of natural and engineered nanoparticles, and development of protocols. Methods for detection of Carbo-Iron and Fe-zeolites in sediment matrices will be developed.

  Laboratory and field tests of the methods developed will be conducted, providing documentation of “fit for purpose”, detection limits and costs, and assessments of the potential for routine application in a wider context of product safety and monitoring.

A major challenge in assessing the performance of engineered nanoparticles is the detection of those nanoparticles in environmental media, and in particular their isolation from natural nanoparticles and colloidal material. This represents a particular hurdle for the use of Fe-based nanoparticles in remediation, owing to high levels of naturally occurring iron. Many techniques are routinely applied to characterise nanoparticles under controlled laboratory conditions. A number of these could be applied to samples collected under field testing conditions, but the techniques require further method development and validation, and methods also need to be developed for new remediation nanoparticles (e.g. Fe-zeolites and Carbo-Iron). As one of the main ambitions of the project is to move from the realm of laboratory tests on nanoremediation to field and in-situ testing of the particles, the development and application of suitable analytical techniques forms a central role in demonstrating the viability of nanoremediation.

An analytical toolbox will be available which refers to all methods to support laboratory and field studies on the reactivity, fate and bioavailability of the nanoparticles of interest. According to where they can be applied, these can be divided into three main types of methods: i) techniques for laboratory use (e.g. for particle characterisation and stability); ii) techniques with a capability for on-site use in the field (i.e. requiring some sampling and infrastructure but providing immediate data); and iii) techniques that can be used in situ (i.e. providing data with a high resolution in space and time). On site and in-situ methods include techniques that monitor within the aquifer and those that rely on site sampling (e.g. ultrafiltration for size distribution) followed by laboratory analysis. The methods have different detection limits in terms of particle concentration, particle size distribution and most importantly their ability to detect above background colloids. In-situ techniques can be used to directly monitor levels of nanoparticles in-situ, using for example their magnetic properties or chemical reactivity through measurement of redox or hydrogen production, but these rely on relatively high concentrations of nanoparticles. Tracing methods (e.g. isotope or rare earth element analysis) can be applied to follow the movement of particles and reaction products out of the aquifer. Isotope labelling techniques allow sensitive and specific location of nanoparticles and their products in laboratory studies - where the ease of detection makes radiolabelling useful for high throughput experiments – and field studies where stable or short-lived isotopes can be used. Dual labelling, including with rare earth metals and stable isotopes, can be applied to study particle dissolution and reaction products.


On site and in-situ methods include techniques that monitor within the aquifer and those that rely on site sampling (e.g. ultrafiltration for size distribution) followed by laboratory analysis. The methods have different detection limits in terms of particle concentration, particle size distribution and most importantly their ability to detect above background colloids. In-situ techniques can be used to directly monitor levels of nanoparticles in-situ, using for example their magnetic properties or chemical reactivity through measurement of redox or hydrogen production, but these rely on relatively high concentrations of nanoparticles. Tracing methods (e.g. isotope or rare earth element analysis) can be applied to follow the movement of particles and reaction products out of the aquifer. Isotope labelling techniques allow sensitive and specific location of nanoparticles and their products in laboratory studies - where the ease of detection makes radiolabelling useful for high throughput experiments – and field studies where stable or short-lived isotopes can be used. Dual labelling, including with rare earth metals and stable isotopes, can be applied to study particle dissolution and reaction products. 
Since nanopoarticle stability is a key performance issue, reaction products are an important focus. Rapid freezing Mössbauer spectroscopy can distinguish and quantify various Fe-bearing phases, and can be applied for ex-situ identification of transformation products of a variety of Fe-based nanoparticles. In the case of ferrate nanoparticles, it is possible to discern and quantify various oxidation states. NanoRem will adapt and develop these techniques for a controlled study of iron-based nanoparticles. 
  •   Monitoring and tracing tools based on measurement of the ferro-magnetic properties (susceptibility) of iron as well as chemical reactivity of nanoparticles (redox, hydrogen production) will be optimised to follow iron reactivity in the field.

  •   On-site measurements and in-situ characterisation of natural and engineered nanoparticles will be carried out through the development of method protocols and the application of modern high performance site-specific analytics (e.g. Time of Transition measurement, in-situ turbidity and fluorescent measurements). Methods for detection of Fe-zeolites in aquifers will be developed. A range of different techniques will be tested, including indirect methods that can potentially be applied cheaply and continuously in the field (e.g. redox measurement).

  •   Field and laboratory tests of the methods developed will be conducted, providing documentation of “fit for purpose”, detection limits and costs, and assessments of the potential for routine application (e.g. wastewater) in a wider context of product safety and monitoring. Their applicability for other applications will be assessed. Field measurement data necessary for the assessment of the efficiency of the nanoremediation will be provided, together with application of analytical and sampling methodologies in field site studies (WP10).

Taking Nanotechnological Remediation Processes from Lab Scale to End User Applications for the Restoration of a Clean Environment.
This project has received funding from the European Union Seventh Framework Programme (FP7/2007-2013) under grant agreement No. 309517
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