Grantee Research Project Results
Final Report: Development of a near-real-time analytical system for measurement of N-nitrosamines in water reuse
EPA Contract Number: 68HERC21C0008Title: Development of a near-real-time analytical system for measurement of N-nitrosamines in water reuse
Investigators: Griffiths, Duncan
Small Business: Hyperion Analytical LLC
EPA Contact: Richards, April
Phase: I
Project Period: March 1, 2021 through August 31, 2021
Project Amount: $99,954
RFA: Small Business Innovation Research (SBIR) - Phase I (2021) RFA Text | Recipients Lists
Research Category: Small Business Innovation Research (SBIR) , SBIR - Water , SBIR - Clean and Safe Water
Description:
This project successfully developed two versions of an analytical instrument for the measurement of N-nitrosamines in recycled water and other sample matrices. From earlier proof of concept work published in the scientific literature, the task for Phase I was to convert these concepts into a working prototype using commercial components and initial software development to run the system.
The first stage was to use a standard HPLC front end for a laboratory-based prototype system along with the multi-step sample conditioning and detector system. A second stage was to construct a fully automated and integrated system that could be operated in a continuous-operation, unattended, online configuration. These systems were targeted to have unparalleled detection performance at a fraction of the cost of the current standard mass spectrometry based analytical systems.
Summary/Accomplishments (Outputs/Outcomes):
The HPLC-based system was designed after careful consideration of previous published work and consideration of advances in each component of the system. Incremental advances in performance, enhanced usability and local commercial availability yielded a system that has the potential for better performance than previous research systems and commercially available mass spectrometer based systems.
The laboratory benchtop system operated in combination with the HPLC to provide results that validated the basic premise of the project. Lower limit of detection was determined to be below 10 ng/L. The target is in the single ng/L range so the initial result is promising considering the limited development time and already identified avenues for further performance improvements.
Notwithstanding the normal setbacks and delays of a short development project, the engineering and assembly of the initial system was relatively straightforward. Working closely with vendors meant basic functionality was usually provided with the first iteration of most components. Adapting components to a specialized purpose and searching for a high level of performance meant several challenges arose to make certain modules work as needed in this system. Several delays due to vendor lead times during the COVID crisis compromised the schedule and the full scope of work that could be accomplished.
However, sufficient data was generated and operational evaluation completed to confirm the performance and the suitability for further development. Besides the laboratory system, a fully automated online system was developed that was able to measure samples continuously as long as the necessary supplies were replenished. Software control of multiple additional functions was incorporated and will be incorporated into the laboratory system as that evolves.
Conclusions:
The work carried out proves the HPLC based system is capable of measurement performance that is competitive with current commercial offerings. Furthermore, the system can be built either as an accessory to an existing HPLC system or a complete integrated system for fully automated online analysis. Further refinement and optimization is needed to find the limits of the technique and to fully characterize all measurement parameters.
The result of this Phase I project is a working prototype in need of refinement into a commercial product. The results generated show the potential of our technical approach and conversations with potential commercial partners and end users confirm the high level of interest from the marketplace for this cost-effective and capable analytical tool. Besides having equivalent, or potentially better, measurement performance to the mass spectrometry-based systems costing 3-5 times as much, the ability to operate online and unattended enhances the market appeal greatly. Further engineering development will result in a robust and user-friendly product that will meet market requirements.
Further funding will be sought to continue the development and launch the products on the market.
SBIR Phase II:
Development of a Near-Real-Time Analytical System for Measurement of N-nitrosamines in Water ReuseThe perspectives, information and conclusions conveyed in research project abstracts, progress reports, final reports, journal abstracts and journal publications convey the viewpoints of the principal investigator and may not represent the views and policies of ORD and EPA. Conclusions drawn by the principal investigators have not been reviewed by the Agency.