DETECTION AND IDENTIFICATION OF DANGEROUS SUBSTANCES
USING ION MOBILITY SPECTROMETRY COUPLED WITH MASS SPECTROMETRY (MOBSPEC)
Project No. 81-023/14.09.2007
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.
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).
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.
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.
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:
·
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.
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.