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DETECTION AND IDENTIFICATION OF DANGEROUS SUBSTANCES USING ION MOBILITY SPECTROMETRY COUPLED WITH MASS SPECTROMETRY (MOBSPEC)

 

Project No. 81-023/14.09.2007

 

Description  Objectives  Activities  Results  Results disemination  Team Partners

 

Description:

 

The danger of terrorism acts against public institutions, facilities and buildings with a large number of people rose dramatically in the latest years. This fact imposes the necessity of developing efficient alarm systems against the presence of some dangerous substances, like chemical warfare agents (CWAs), biological warfare agents (BWAs) and explosives, and also like controlled substances such as illegal drugs.

 

Ion mobility spectrometry (IMS) is a proven, cutting-edge technology, aimed to the trace detection and identification of dangerous substances. Because of their extremely high sensitivity for the chemicals with elevated electronegativity (like is the case for explosives) or with elevated proton affinity (like chemical warfare agents), because of the fast response time and their capability for miniaturization, the ion mobility analyzers are ideals for detecting ultra-traces of toxic or explosive chemicals, at concentration levels of sub-p.p.b. (parts-per-billion).

 

However, due to the fact that the resolution of ion mobility spectrometers is relatively low, for an accurate identification of the target analytes a coupling with a mass spectrometer is recommended, acquiring this way confirmatory information. This coupling is made through an interface, which must ensure:

-         The pressure drop from atmospheric pressure (as in IMS instrument) to the vacuum pressure in the mass spectrometer (10-6 bar);

-         Ion transfer from the IMS spectrometer zone within the mass spectrometer zone, at the appropriate energies for analysis.

 

The general objective of this project is the realization of an experimental model of tandem (coupled) instrument ion mobility spectrometer (IMS) having a non-radioactive ionization source - quadrupole mass spectrometer (QMS), with which the dangerous substances could be detected and identified. The accomplishment of this general objective will be done by mean of a series of specific objectives mentioned in the paragraphs below.

 

The originality of this proposal relies in the construction in premiere in Romania of this kind of tandem instrument IMS-QMS; this implies solving, using innovative solutions, a couple of complex problems, such as: ensuring the stability of ion beam generated by the non-radioactive ionization source with corona discharge, transfer with a good efficiency of ion current from the IMS analyzer within the QMS spectrometer, and the realization of a special electronic circuit which will ensure detection of both positive and negative ions.

 

The interface that will ensure the ion transfer between the two spectrometers would be the object of a patent proposal.

 

To solve these complex problems of this project, a consortium has been formed, consortium that reunites four prestigious Romanian institutions: two national research institutes and two universities. Moreover, the realization of the proposed objectives will definitely allow the initiation and participation to international scientific collaborations, especially in preparing project proposals in the E.U. FP7.

 

All activities that will be deployed within this project are of fundamental research and industrial research types.

 

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Objectives:

 

General objective of the project:

Realization of an experimental model for a tandem ion mobility spectrometer - quadrupole mass spectrometer, for detection and identification dangerous substances from the chemical warfare agents’ category.

 

Specific objectives are:

-         O-1. Analysis of the ionic transport system and vacuum system, for design and construction of the interface and of the non-radioactive ionization source.

-         O-2. Design of mechanical and electronic components of the ion mobility analyzer.

-         O-3. Design of mechanical and electronic components of the quadrupole mass analyzer.

-         O-4. Construction and testing of the mechanical and electronic components of the tandem IMS-QMS.

-         O-5. Conception and realization of software products dedicated for controlling the IMS-QMS tandem instrument.

-         O-6. Elaboration of a methodology for operating the equipment.

-         O-7. Experimentation and verification, then presentation and demonstration of the functionality for the tandem analyzer of IMS-QMS type, by using simulant substances (chemical compounds having chemical structure very similar with that of CWAs, but much lower toxicity).

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Activities:

 

Stage I. Comparative analysis of the solutions for an ion mobility spectrometer (IMS) coupled to a quadrupole mass spectrometer (QMS). Choosing the optimum variant. – Correlation with O-1.

Activities: A I.1. Analysis of the systems for ionization and command; A I.2. Study of the vacuum systems for the interface and quadrupole spectrometer; A I.3. Study of ion transport systems and ion focusing; A I.4. Elaboration of methods for numerical controlling the supplies, high-voltage sources, high-frequency sources; A I.5. Studies of charge transport at atmospheric pressure; influence of gas parameters on mobility.

 

Stage II. Computer simulation of ionic trajectories for obtaining design data for ionization source, ion mobility analyzer, and ion transport systems. Mechanical and electronic design of these components. Realization of ionization source for the IMS. – Correlation with O-2 and O-3.

Activities: A II.1. Computer simulation of ionic trajectories in the interface’s lenses system; A II.2. Research – mechanical design of sample inlet systems, gas flow and purification of drift gases; A II.3. Mechanical design of ionization source, ion mobility analyzer, and interface. Elaboration of technical documentation; A II.4. Design of electronic circuits for the units of IMS; A II.5. Conception of integrate intelligent systems that will correlate the functions of the subsystems ensuring the IMS work; A II.6. Execution and building of ionization source; AII.7. Dissemination of results.

 

Stage III. Realization of experimental models for sample inlet system, gas flow & purification system, analyzer cell, and interface. Mechanical and electronic design of quadrupole analyzer and of detection system for ionic currents. Design of vacuum system of the interface that couple the IMS with the quadrupole analyzer and of the quadrupole. – Correlation with O-3 and O-4.

Activities: A III.1. Execution of the sample inlet system and drift gas systems; A III.2. Execution and mounting of the analyzer cell and of the interface; A III.3. Mechanical and electronic design of components for quadrupole analyzer. Elaboration of technical documentation; A III.4. Design of vacuum system of the tandem; A III.5. Elaboration of advanced signal processing methods; A III.6. Dissemination of results.

 

Stage IV. Realization of experimental model for quadrupole mass analyzer and for vacuum system. Realization of electronic units for the IMS. Realization of experimental model of the IMS. Conception of dedicated software products for controlling the IMS-QMS tandem. – Correlation with O-4 and O-5.

Activities: A IV.1. Realization of mechanical components for the quadrupole and of its electronic units. Mounting these components; A IV.2. Realization and testing the electronic units of the IMS; A IV.3. Mounting mechanical and electronic components of the IMS; A IV.4. Realization of vacuum system of the tandem; A IV.5.  Realization of numerical control of the electronic systems for generating voltage pulses on grids; A IV.6. Organizing a workshop with partners; A IV.7. Dissemination of results.

 

Stage V. Mounting the tandem analyzer IMS-QMS, its first starting and checking of the designed parameters. – Correlation with O-4.

Activities: A V.1. Experimentation of the IMS; A V.2. Experimentation of the QMS; A V.3. Mounting the tandem, its experimentation, and checking the designed parameters; A V.4. Experimentation of the advanced signal processing signal system; A V.5. Dissemination on a large scale by communicating and publishing the results at national and international level.

 

Stage VI. Presentation and demonstration of functionality of the analyzer tandem IMS-QMS using a group of simulant substances. Elaboration of working methodology with the equipment, concerning collection, introduction and analysis of samples. – Correlation with O-6 and O-7.

Activities: A VI.1. Choosing of substances groups that simulate the best chemical warfare agents; A VI.2. Sample treatment and their preparation for analysis; A VI.3. Elaboration of working methodology for the equipment; A VI.4. Testing the software for controlling the IMS-QMS tandem. Data acquisition and data advanced processing; A VI.5. Demonstration of functionality of the analyzer tandem IMS-QMS; A VI.6. Dissemination of results.

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Results:

 

The final result of the research deployed in this project will be an experimental model of tandem analyzer ion mobility spectrometer – quadrupole mass spectrometer, ultra-sensitive, with high precision, for detection and identification of dangerous substances. The apparatus may be used to detect chemical warfare agents.

 

Other results: 1.Data concerning the influence of ion-molecule collisions on ionic mobilities in gases, at atmospheric pressure. Data concerning the influence of pressure and duty cycle of analyzer on ionic mobility. 2. Data regarding the electric charge transport at or near atmospheric pressure in electric fields having different configurations and intensities. 3. An ion mobility spectrometer with non-radioactive ionization source, which can be used separately for analysis of chemical compounds (with the same detector built for the tandem). 4. A quadrupole mass spectrometer that, with an ionization source attached may function as an autonomous analyzer. 5. Software for electronic command of impulses and time distribution of these impulses applied to the command systems of ion bunches. 6. Software for data acquisition and processing. 7. Patents and scientific papers.

 

Results stage I:

 

·        The ionizing systems and commands were studied and the option was for a corona discharge source. The parameters of the source were established.

·        Following the study of some variants, a tandem FAIMS mobility spectrometer-quadrpole mass spectrometer was elected to be manufactured.

 

  • PROCES VERBAL DE AVIZARE A LUCRARILOR DE CERCETARE  - DEZVOLTARE (PVA)  ( PVA_INCDTIM.doc )

 

 

 

 

Results stage II:

·         Ion trajectories computer simulations in interface lens system and electric field computer simulation in ion source and analyzer cell;

·         Technical documentation for the corona ion source, FAIMS analyzer, classic analyzer and interface;

·         The realization, the assembly and the test of the corona ion source;

·         Results dissemination.

 

Results stage III:

·         The realization, the assembly and the testing of the FAIMS parallel plates cell analyzer;

·         The realization and the assembly of the IMS-QMS interface;

·         The mechanical and electronic design of the quadrupole analyzer;

·         The calculus and the design of the vacuum system;

·         The realization of the inlet system and the drift gas system;

·         The calculus and the elaboration of a new method for the advanced signals processing;

·         The results dissemination by publications and WEB page.

 

Results stage IV:

 

Results stage V:

 

Results stage VI:

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Results disemination:

1.     Web page

2.     Scientific contributions

·        C. Cuna, St. Popescu, M. Kaucsar, Digital signal acquisition with non  National Instruments input/output board, Isotopic and Molecular Processes, Cluj-Napoca, 2007, Sept. 20-22

·        C. Cuna, E. Indrea, St. Popescu, D. Ursu, Analog signal acquisition with non National Instruments input board, Isotopic and Molecular Processes, Cluj-Napoca, 2007, Sept. 20-22

·        Victor Bocos-Bintintan, Georgiana-Maria Pop, Trace detection of ammonia by ion mobility spectrometry, 6-th Symposium “Environment-Research, Protection and Management”, October 26-28, Cluj Napoca, 2007

·        Stela Cuna, Negoita Teodor, Petre Berdea, The use of isotopic signals for the study of the response of polar ecosystems to environmental changes, 2-nd National Symposium of  Polar Scientific Research, November 16-17, Bucharest, 2007

·        C. Cuna, M. Leuca, N. Lupsa, V. Mirel, C. Festila, Eva Dulf, Stela Cuna, Florina Tusa, The calculus and the design of a field asymmetric waveform ion mobility spectrometer, 27th IMMS, 3-8 May, 2009, Retz, Austria.

·        C. Cuna, M. Leuca, N. Lupsa, V. Mirel, V. Bocos-Bintintan, Stela Cuna, Florina Tusa, Ion mobility analyzer-quadrupole mass spectrometer system design, Conferinta Internationala ”Processes in Isotopes and Molecules”, 24-26 September, Cluj-Napoca, Romania.

·         Eva Dulf, C.Festila, C.Cuna, Asymmetric High Frequency Square Wave Generator with DC Component Control for Ion Mobility Spectrometers, 5th International Symposium on Applied Computational Intelligence and Informatics, May 28-29, 2009, Timisoara, Romania.

 

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Team:

  • Cuna Cornel Director proiect - Physcist
  • Cosma Viorel Colaborator – Electro-Mechanical Engineer
  • Pamula Adrian Colaborator - Physcist
  • Ioanoviciu Damaschin Colaborator - Physcist
  • Cuna Stela Colaborator - Physcist
  • Lupsa Nicolae Colaborator -Engineer
  • Leuca Moise Colaborator - Engineer
  •  Mirel Valentin Colaborator - Physcist
  • Balas Gabriela Colaborator - Physcist
  • Tusa Florina Colaborator -Chemist
  • Szilaghy Edina Colaborator - Physcist
  • Magdas Alina Colaborator - Physcist
  • Gligan Nicolae Colaborator - Mechanical engineer
  • Dobocan Ioan Colaborator - Mechanical engineer
  • Petrica Nicoleta Colaborator - Technician
  • Oltean Simion Colaborator - Technician
  • Baciu Gheorghe Colaborator - Technician

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Partners:

1.     National Institute for Research and Development of Isotopic and Molecular Technologies, Cluj-Napoca - Coordinator

Cuna Cornel - Project manager - Physicist dr. CS I

 

2.     Babes-Bolyai University Cluj-Napoca

Bocos-Bintintan Victor - Project responsible - Assistant Prof. Dr.

 

3.     National Institute for Research and Development of Cryogenic and Isotopic Technologies-ICSI, Rm. Valcea

Iliescu Mariana - Project responsible - Engineer

 

4.     Technical University Cluj – Napoca

Eva Dulf  - Project responsible -  Assistant Prof. Dr.

 

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