Project title: Simultaneous elemental microanalytical method for environment and food control using passive sampling coupled with miniaturized instrumentation based on plasma microtorch optical emission spectrometry

Acronym: MULTIPASS

Contract no: 733PED / 27.06.2022

Contracting Authority: Executive Agency for Higher Education, Research, Development and Innovation Funding (UEFISCDI), P2 – Increasing the competitiveness of the Romanian economy through RDI

Abstract

The project aims to develop and validate new highly-sensitive microanalytical methods without matrix effects to determine Hg, Pb, Cd, As, Sb, Cu and Zn of interest for environmental and food quality control using passive preconcentration by gradient diffusion in thin layer (DGT) and detection by optical emission spectrometry in capacitively coupled plasma microtorch (DGT-SSETV-μCCP-OES). The starting level of the project is TRL3 through the existence of the miniaturized spectrometric experimental model and the TRL4 level is reached by validation of the methods applied to environmental and food samples. The duration of the project is 24 months, in two stages, and is carried out in partnership by Research Institute for Analytical Instrumentation Cluj-Napoca (CO-ICIA), Babes-Bolyai University Cluj-Napoca (P1-UBB) and Technical University Cluj-Napoca (P2-UTCN). The first stage is intended to increase the technological maturity of the SSETV-μCCP-OES system at TRL4 by in-situ and ex-situ DGT preconcentration. The preconcentration and spectral detection will be optimized in such a way as to develop simultaneous multielemental methods. Analytical performances will be compared with traditional methods based on inductively coupled plasma optical emission spectrometry, graphite furnace atomic absorption and thermal desorption atomic absorption spectrometry. The second stage is dedicated to the development and validation of DGT-SSETV-μCCP-OES microanalytical methods compared to traditional methods and European Commission requirements for official control laboratories. The analytical capability will be presented to potential users through a practical demonstration. The standard operating procedures will be implemented in the CO-ICIA and P1-UBB laboratories. The results will be disseminated through 4 articles in WoS journals and participation in conferences (4 national and 6 international). An application for a national patent will be considered.

Project objective

The main objective of the MULTIPASS project is to develop new microanalytical methods as TRL4 for the simultaneous determination of priority hazardous elements (Pb, Cd, Hg) and other elements (As, Sb, Se, Cu, Zn) in environment and food microsamples using a fully miniaturized laboratory experimental model based on direct liquid microsampling SSETV-μCCP-OES in tandem with DGT device for in-situ and ex-situ preconcentration and analyte separation.

Estimated results

  • Testing and optimization report on the working conditions for in-situ and ex-situ preconcentration of Hg, Pb, Cd, As, Sb, Se, Cu and Zn using the DGT devices;
  • Optimization report on the working conditions for SSETV as device for direct liquid microsampling after DGT preconcentration;
  • Software to control the thermal program of the Rh filament;
  • Optimization report on the working conditions for plasma microtorch interfaced with a low resolution microspectrometer for simultaneous multielemental determination by DGT-SSETV-μCCP-OES;
  • Report on improved analytical performance (limit of detection, quantification, and compensation of non-spectral effects) for DGT-SSETV-μCCP-OES methods in low power plasma microtorch after DGT analytes preconcentration/separation compared to direct liquid microsampling without DGT;
  • Comparative study of analytical performance of DGT-SSETV-μCCP-OES with traditional methods, GFAAS, TDAAS, ICP-OES and European Legislations demands for official laboratory control;
  • Validation report for microanalytical methods based on DGT-SSETV-μCCP-OES for simultaneous multielemental determination in environmental samples;
  • Validation report for microanalytical methods based on DGT-SSETV-μCCP-OES for simultaneous multielemental determination in food samples;
  • Microanalytical methods for environmental samples using DGT preconcentration and multielemental determination by implementation of DGT-SSETV-μCCP-OES as TRL4 on real samples;
  • Microanalytical methods for food samples using DGT preconcentration and multielemental determination by implementation of DGT-SSETV-μCCP-OES as TRL4 on real samples;
  • Demonstration of the utility and capability report for the new DGT-SSETV-μCCP-OES microanalytical methods for environment and food control quality;
  • 2 Internal Operating Procedures based on DGT-SSETV-μCCP-OES;
  • National patent application;
  • Dissemination of results through participation in scientific national and international events;
  • Dissemination of results through papers in WoS indexed journals.

Project start: 27/06/2022
Project end: 26/06/2024
Project duration: 24 months

Partners:

  • P1 – BABES BOLYAI UNIVERSITY Cluj-Napoca
    Project responsible: Prof. Dr. Tiberiu Frențiu
  • P2 – TECHNICAL UNIVERSITY OF CLUJ – NAPOCA
    Project responsible: Prof. Dr. Dorin Petreuș

Budget:

Project budget 598.795,00 RON
Co-financing: 0,00 RON

Contact

Project coordinator
Senior Researcher I Dr. Marin Senila
Str. Donath nr. 67, Cluj-Napoca, Romania
E-mail: marin.senila@icia.ro; icia@icia.ro
Tel/Fax: +40 264 420590 / +40 264 667

Obtained results – Stage 1

  1. Testing and optimization of the working conditions for in-situ and ex-situ preconcentration of Hg, Pb, Cd, As, Sb, Se, Cu and Zn using the DGT devices
  2. Optimization report of the working conditions for DGT-SSETV-µCCP-OES equipment for Zn, Cd, Cu, Hg and Pb determination
  3. Development of specialized software to control the thermal program of the Rh filament (electrothermal evaporation of Zn, Cd, Cu, Hg and Pb)
  4. DGT-SSETV-μCCP-OES experimental model developed at TRL4
  5. Participatio at national scientific events

Eniko Covaci, Zsofia Sandor, Bogdan Simion Angyus, Marin Senila, Tiberiu Frentiu. Optical emission spectrometry by electrothermal vaporization in a capacitively coupled plasma microtorch as a specific detector in simultaneous multielemental passive sampling by diffusive  gradients in thin films (DGT-SSETV-μCCP-OES): Preliminary studies on the optimization of working parameters. Conferința Națională de Chimie, ediția XXXVI, secțiunea Chimie anorganică, chimie-fizică și analitică, Călimănești-Căciulata, 04–07 octombrie 2022 – Oral communication

Zsofia Sandor, Eniko Covaci, Bogdan Simion Angyus, Marin Senila, Tiberiu Frentiu. Microanalytical method for monitoring of toxic elements in surface waters using passive sampling in diffusive gradients in thin films and detection by capacitively coupled plasma microtorch optical emission spectrometry with electrothermal vaporization  (DGT-SSETV-μCCP-OES). Conferința Națională de Chimie, ediția XXXVI, secțiunea Chimie anorganică, chimie-fizică și analitică, Călimănești-Căciulata, 04–07 octombrie 2022 – Poster