Toxi-triage - Ref. Ares(2019)5493611 - 30/08/2019 Situational … · 2019. 9. 17. · This project...
Transcript of Toxi-triage - Ref. Ares(2019)5493611 - 30/08/2019 Situational … · 2019. 9. 17. · This project...
Situational Awareness
End User
Clinical
Triage
ICT
D2.3 Triage verification facility
Tools for detection, traceability, triage and individual monitoring of victims
www.toxi-triage.eu This project has received funding from the European Union’s Horizon 2020 (H2020) research and innovation programme under the Grant Agreement no 653409.
Ref. Ares(2019)5493611 - 30/08/2019
D2.3 Triage verification facility
Grant agreement number: 653409
Start date of the project: 2015-09-01
Duration: 48 months
Due date of deliverable:
Actual submission date:
Lead Beneficiary: UH (Matti Kuula, Paula Vanninen)
Keywords:
Validation, ion mobility spectrometry, photoionization detector, hyperspectral technology, simulants, ANSI N42.43, ANSI N42.34, IEC 62327, IEC 62618, CZT detector, gamma spectrometry, validation, radionuclide identification
Dissemination level:
PU ☒
CO ☐
CI ☐
©TOXI-triage Consortium 2 August 2019
Release History
Version Date Description Released by
V1 2019-07-05 First version UH
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Table of Contents
Executive Summary ................................................................................................................................. 7
1 Conclusion ...................................................................................................................................... 10
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List of Tables
Table 1: Device testing at VERIFIN’s laboratory _______________________________________________ 7
Table 2: Table of Annexes and Appendixes of D2.3 (C-detection) ______________________________________ 8
Table 3: Device testing at laboratory ____________________________________________________________ 9
Table 4: Table of Annexes and Appendixes of D2.3 (RN-detection) _____________________________________ 9
List of Figures
No table of figures entries found.
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List of Acronyms
Abbreviation /
acronym
Description
CA Consortium Agreement
CAPEX Capital expenses, price of the system or subsystems or components
CBRN Chemical biological radiological and nuclear
CONOPS Concept of operations
CZT Cadmium Zinc Telluride (detector)
Decon Decontamination
DoW Description of work
EAB Ethical Advisory Board
EP Exploitation plan
FTX Field technical exercise
GA Grant Agreement
GC Gas chromatography
GC-IMS Gas Chromatography - Ion Mobility Spectrometry
HSI Hyperspectral Imaging
ICT Information and communication technology
IMS Ion mobility spectrometry
MIC Medical incident commander
NFC Near to field communication
OPCW Organisation for the Prohibition of Chemical Weapons
OPEX Operational expenses, mostly personnel costs and maintenance
OPsX Operational exercise
PAB Project Advisory Board
PII Personally Identifiable Information
PPE Personal Protective Equipment
RPAS Remote piloted airborne system (AKA drone)
SO Specific Objective
TAG Test atmosphere generator
WP Work Package
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Executive Summary
In TOXI-triage project one major task has been the establishment of a facility for testing and
performance verification of the detectors developed in the project.
The verification facility was involved three different tasks:
Task 2.3 Evaluation and validation/verification of stand-off, and environmental contamination
monitoring methods for C-detection and identification (UFZ).
Using the guidelines from T2.2 this task will evaluate the prototypes from Tasks 4.1 and4.2 in a
validated CBRN laboratory to generate exemplar data from the IMS, and hyperspectral systems that
will be have been developed and prepared. Priority threats will be addressed and the first library
release is envisaged to include: pesticides, chlorine, chloropicrin, sarin, and VX- nerve agents in a range
of matrices including: food, water, clothing (PPE) and building materials under a range of
environmental conditions. This task will be informed by the experience gained during recent VERIFIN
(UH) deployments to suspected C-attacks. This Operational exercise (OPsX) activity will be validated by
analytical gold-standards e.g. mass spectrometric methods. An important element in this task will be
the optimisation of methods and systems using simulants before transfer to UH for final verification
with live agents.
Participating partners (LU, UH, JyU)
All tested technologies and partners can be found on Table 1.
Table 1: Device testing at VERIFIN’s laboratory
Providing
Partner Device Name
Device
Type Mobility
Sampling
Medium /
Matrix
Schedule
AIR GDA-G
GDA-P IMS Handheld Air 2.-6.10.2017
UFZ
SLGE (Sprayed
Liquid Gas
Extraction)
Sampling
system Field-deployable Air 9.-13.10.2017
EOY ChemPro DM IMS
Handheld, Vehicle
mountable, UAV
mountable
Air 27.11.-1.12.2017
T4i T4i DOVER GC-PID Drone payload Air 22.-26.1.2018
LUH Prototype IMS Field-deployable Air 4.-8.2.2019
JYU Prototype Optical
detector Field-deployable
Solid and
liquid on
surfaces
and as
wiping
samples
9.-20.5.2016
7.-8.1.2016
24.-25.1.2017
Reports from tests are listed on Table 2.
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Table 2: Table of Annexes and Appendixes of D2.3 (C-detection)
Annex or Appendix number Title or Contributor Dissemination level
Annex 1 C-detection PU
Appendix 1 T4i CI
Appendix 2 AIR CI
Appendix 3 EOY CI
Appendix 4 LUH CI
Appendix 5 UFZ CI
Appendix 6 JYU CI
Appendix 7 NTUA CI
Task 2.4 Evaluation and validation/verification of methods for B- and toxin detection (LU).
Also defined by T2.2, methods for ion mobility spectrometry (IMS) and hyperspectral imaging are to
be tested for efficacy of B-contamination of a series of selected matrices: food, water, clothing and
building materials under conditions amenable to bacterial development. These OPsX activities will use
safe simulant organisms (Bacillus subtilis and Bacillus megaterium). As with T2.3, mass-spectrometric
validation will underpin the efforts with methods and systems transferred to UH for proof of principal
testing with ricin. The technology gap in rapid B-detection is widely acknowledged, and so some
resource will be devoted to assessing the suitability of the rapidly developing sensing field of aptamer-
based detection. The feasibility of establishing rapid-prototyping facilities for specific organism
aptamer sensors will be assessed.
Reports from these tests are provided in Deliverables D 2.5 Identification of bacterial strains with
multiplexed Aptamer sensing” Report assessing the potential of B-detection based on aptamer-based
methods and techniques and D4.6 Laboratory system for B detection
Task 2.5 Development and validation/verification of methods for R- & N- detection and identification
after CBRN exposure (LU).
Unlike B-detection R-& N- -detection systems are significantly more mature, and the consortium is able
to field remotely operable drone compatible instruments that exceed the specifications of the N42 34
ANSI isotope list. Further our systems are able to provide GIS tagged data on dose-rates, nucleotide
identification and significance, spectrum analysis accompanied by a range of haptic feedback for the
end-use. The nature of the challenge is associated with effective sampling and knowledge and
expertise of nucleotide migration in the environment. Guidelines for survey/sampling protocols to
identify hotspots, transport from matrices and assess chemical transformations will be developed.
Note the Radiochemistry Sections at LU and UH are licensed and equipped to handle a range of
radiological materials and the teams are acknowledged international authorities in environmental
radiochemistry and the containment of radioactive materials. Participating partners: LU, UH, EYO.
All tested technologies and partners can be found on Table 5.
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Table 3: Device testing at laboratory
Providing
Partner
Device
Name
Device
Type Mobility
Sampling
Medium /
Matrix
Schedule
EOY Ranid Fly CZT Drone payload Air November 2017
EOY Ranid Fly CZT Drone payload May 2018
Reports from tests are listed on Table 6.
Table 4: Table of Annexes and Appendixes of D2.3 (RN-detection)
Annex or Appendix number Title or Contributor Dissemination level
Annex 2 RN-detection PU
Appendix 1 EOY CI
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Conclusion
The two annexes are appended, and the eight technical appendices detail the analytical figures of merit
of the assembly of detection systems delivered elsewhere the project. The combined data provide
evidence of a traceable and rigorous verification facility that has been he foundation of the validation
of the chemical, biological and radiological detection effort in TOXI-triage.
The eight technical appendices are classified EU Restricted and are not publicly available. Enquiries
about specific detection system performance should be addressed to the technology provider.
www.toxi-triage.eu
Tools for detection, traceability, triage and individual
monitoring of victims
Situational Awareness
End User
Clinical
Triage
ICT
D2.3 Triage verification facility
Annex 1 – C-detection
Tools for detection, traceability, triage and individual monitoring of victims
www.toxi-triage.eu This project has received funding from the European Union’s Horizon 2020 (H2020) research and innovation programme under the Grant Agreement no 653409.
D2.3 Triage verification facility
Annex 1 – C-detection
Grant agreement number: 653409
Start date of the project: 2015-09-01
Duration: 48 months
Due date of deliverable:
Actual submission date:
Lead Beneficiary: UFZ (Helko Borsdorf, Mashaalah Zarejousheghani)
Contributing beneficiaries: AIR (Andreas Walte), EOY (Toni Leikas, Ville Julkunen), UH (Paula Vanninen,
Matti Kuula), LUH (Stefan Zimmermann, André Ahrens), JYU (Jaana Kuula), T4i (George Pallis, George
Psarras), NTUA (Milt Statheropoulos)
Keywords:
Validation, ion mobility spectrometry, photoionization detector, hyperspectral technology, simulants
Dissemination level:
PU ☒
CO ☐
CI ☐
©TOXI-triage Consortium August 2019
Release History
Version Date Description Released by
V1 2016-02-10 First draft Helko Borsdorf, Mashaalah Zarejousheghani
V2 2016-05-30 Second release version, modified on the basis of the project partner feedback and material
Helko Borsdorf, Mashaalah Zarejousheghani
V2.1 2016-07-17 Intermediate release with JYU and UH contribution
Paula Vanninen, Jaana Kuula
V3 2016-08-17 Third release version, modified on the basis of the project partner feedback and material
Helko Borsdorf, Mashaalah Zarejousheghani
V3.1 2016-11-16 Intermediate release with JYU and T4i contribution
George Pallis, Jaana Kuula
V4 2016-12-19 Fourth release version, modified on the basis of the project partner feedback and material
Helko Borsdorf, Mashaalah Zarejousheghani
V4.1 2017-01-02 Intermediate release with T4i contribution Paula Vanninen
V4.2 2017-01-10 Intermediate release with NTUA contribution Milt Statheropoulos
V5 2017-01-16 Fifth release version, modified on the basis of the project partner feedback and material
Helko Borsdorf, Mashaalah Zarejousheghani
V5 2017-01-19 Last-minute additions and language consistency check
Helko Borsdorf, Mashaalah Zarejousheghani Andreas Walte
V6 2017-08-24 Sixth release version, modified on the basis of experimental results by UFZ, AIR and EOY
Helko Borsdorf, Mashaalah Zarejousheghani Osmo Anttalainen Andreas Walthe
V7 2017-08-28 Added VERIFIN testing compounds and matrices
Paula Vanninen Marja-Leena Kuitunen Vesa Häkkinen Harri Kiljunen Matti Kuula
V8 2017-07-06 Added results of validation experiments of HU, NTUA, T4i, Air, UFZ, EYO
Helko Borsdorf, Mashaalah Zarejousheghani Osmo Anttalainen Andreas Walthe Paula Vanninen Milt Statheropoulos George Pallis
V9 2019-05-10 Whole report revised Added following annexes: Annex 1: C-detection Annex 2: R/N-detection Annex 3: B-detection
Matti Kuula Paula Vanninen
V10 2019-06-04 Whole report minor revision
Matti Kuula Paula Vanninen
V11 2019-06-06 Toni Leikas
V12 2019-06-12 George Psarras
V13 2019-06-14 Matti Kuula Paula Vanninen
V14 2019-06-14 André Ahrens
V15 2019-06-17 Helko Mashaalah
V16 2019-06-17 Jaana Kuula
V17 2019-07-05 Matti Kuula Paula Vanninen
V18 2019-07-12 Finalised with partner comments Matti Kuula
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Table of Contents
Executive Summary ................................................................................................................................. 5
General .................................................................................................................................................. 6
1 Introduction ..................................................................................................................................... 6
1.1 Validation of Monitoring Methods .......................................................................................... 7
2 Sample Introduction Systems .......................................................................................................... 9
2.1 Sample introduction system (UFZ) .......................................................................................... 9
2.2 Sample introduction system (EOY) ........................................................................................ 14
2.2.1 General Requirements ...................................................................................................... 14
2.2.2 Schematic of the Setup ...................................................................................................... 15
2.2.3 Overall test instructions .................................................................................................... 16
2.3 Miniature Trace Atmosphere Generator (NTUA) .................................................................. 17
2.3.1 Technical Description ........................................................................................................ 17
2.3.2 Validation procedure ......................................................................................................... 19
2.3.3 Simulants for preliminary validation ................................................................................. 19
3 Analytical Instruments ................................................................................................................... 21
3.1 Ion mobility spectrometers ................................................................................................... 21
3.1.1 Technical description ......................................................................................................... 21
3.1.2 Validation procedure ......................................................................................................... 21
3.1.3 Simulants for preliminary validation ................................................................................. 23
3.1.4 Presentation of Results ..................................................................................................... 24
3.2 Gas chromatography – PID .................................................................................................... 24
3.2.1 Technical description ......................................................................................................... 24
3.2.2 Simulants for preliminary validation ................................................................................. 28
3.2.3 Validation procedure ......................................................................................................... 28
3.3 Hyperspectral systems .......................................................................................................... 29
3.3.1 Technical description ......................................................................................................... 29
3.3.2 Validation procedure ......................................................................................................... 30
3.3.3 Simulants for preliminary validation ................................................................................. 31
4 Validation of Sample Preparation Techniques ............................................................................... 33
4.1 Paper filter as field deployable sampling techniques ........................................................... 33
4.1.1 Technical description ......................................................................................................... 33
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4.1.2 Validation procedure ......................................................................................................... 34
4.2 Sprayed liquid-gas extraction (SLGE) ..................................................................................... 34
4.2.1 Technical description ......................................................................................................... 34
4.2.2 Validation procedure ......................................................................................................... 35
4.3 Wipe tests (AIRSENSE Analytics) ........................................................................................... 36
5 Validation protocols at VERIFIN using live agents and various matrices ....................................... 38
5.1 Validation Plan of Analytical Instruments ............................................................................. 40
5.2 Matrices ................................................................................................................................. 41
5.3 Sample Preparation Reference Methods: Recommended Operation Procedures ............... 41
5.4 Tested Instruments ............................................................................................................... 42
5.4.1 Technical description ......................................................................................................... 42
6 Results ............................................................................................................................................ 43
7 Conclusion ...................................................................................................................................... 44
8 References ...................................................................................................................................... 46
1. ‘Appendix 1 – T4i’ (data from simulant and live agent testing)
2. ‘Appendix 2 – AIR’ (data from simulant and live agent testing)
3. ‘Appendix 3 – EOY’ (data from simulant and live agent testing)
4. ‘Appendix 4 – LUH’ (data from simulant and live agent testing)
5. ‘Appendix 5 – UFZ’ (data from simulant and live agent testing)
6. ‘Appendix 6 – JYU’ (data from simulant and live agent testing)
7. ‘Appendix 7 – NTUA’ (data from simulant and FTX testing)
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List of Tables
Table 1: Devices and technologies in TOXI-triage project ____________________________________________ 7
Table 2: Tested ion mobility spectrometers ______________________________________________________ 21
Table 3: Example of reporting of verification analysis at UH _________________________________________ 24
Table 4: Hyperspectral cameras that were tested in the laboratory ___________________________________ 30
Table 5: Selected chemicals for testing __________________________________________________________ 39
Table 6: List of WHO Classes of hazardous chemicals ______________________________________________ 39
Table 7: Preliminary test plan _________________________________________________________________ 40
Table 8: Performed tests: concentrations studied and estimated required time for those experiments _______ 43
Table 9: Purity of applied chemicals ____________________________________________________________ 43
Table 10: Device testing at VERIFIN’s laboratory __________________________________________________ 44
List of Figures
Figure 1: Communication and feedback between WP2 and WP4 ______________________________________ 5
Figure 2: Sample introduction system for spectrometers with an internal sample gas pump providing a flow rate
of 25 L/h (416 mL/min) _______________________________________________________________________ 9
Figure 3: System for the introduction of two different compounds depending on their concentration using
spectrometers with an internal sample gas pump _________________________________________________ 11
Figure 4: Sample introduction system for spectrometers with internal sample gas pumps with varying flow rates
_________________________________________________________________________________________ 12
Figure 5: Sample introduction system with controlled humidity ______________________________________ 13
Figure 6: Photograph of the sample introduction system with controlled humidity _______________________ 13
Figure 7: Laboratory test setup for ChemPro 100i _________________________________________________ 15
Figure 8: Pneumatic connection _______________________________________________________________ 16
Figure 9: The schematic of the device (permeation vial, external vial and oven have not integrated to the device;
ad hoc connections are used instead) ___________________________________________________________ 17
Figure 10: User interface _____________________________________________________________________ 18
Figure 11: Example of a running file ____________________________________________________________ 18
Figure 12: 3D technical drawing of the current T4i DOVER™ configuration _____________________________ 25
Figure 13: The SMS (Sampling Modulation Separation) _____________________________________________ 26
Figure 14: Sample modulation ________________________________________________________________ 26
Figure 15: Sample separation _________________________________________________________________ 27
Figure 16: The T4iDOVER hardware configuration _________________________________________________ 27
Figure 17: Structural configuration of JYU’s hyperspectral detection system ____________________________ 29
Figure 18: Testing design for hyperspectral imaging _______________________________________________ 30
Figure 19: Photograph of the traditional column and new developed disk format of SPE method ___________ 33
Figure 20: Manual filtration apparatus and hand-operated vacuum pump for in-field applications __________ 33
Figure 21: Schematics representation of SLGE method (under development by UFZ) _____________________ 35
Figure 22: Wipe pad. Fold with active area facing down (left), Collect sample by gently wiping the area in
investigation (right) _________________________________________________________________________ 36
Figure 23: Collect sample by gently wiping the area in investigation __________________________________ 37
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List of Acronyms Abbreviation /
acronym
Description
CA Consortium Agreement
BTEX Benzene, Toluene, Ethyl benzene and Xylene
CAPEX Capital expenses, price of the system or subsystems or components
CBRN Chemical biological radiological and nuclear
CONOPS Concept of operations
CWA Chemical Warfare Agent
Decon Decontamination
DMMP Dimethyl methylphosphonate
DEMP Diethyl methylphosphonate
DIMP Diisopropyl methylphosphonate
DoW Description of work
EAB Ethical Advisory Board
EP Exploitation plan
FTX Field technical exercise
GA Grant Agreement
GC Gas chromatography
GC-IMS Gas Chromatography - Ion Mobility Spectrometry
GC-PID Gas Chromatography – Photo ionisation detection
HSI Hyperspectral Imaging
ICT Information and communication technology
IMS Ion mobility spectrometry
MIC Medical incident commander
MIP Molecularly imprinted polymers
MSAL Methyl salisylate
NFC Near to field communication
OPCW Organisation for the Prohibition of Chemical Weapons
OPEX Operational expenses, mostly personnel costs and maintenance
OPsX Operational exercise
PAB Project Advisory Board
PII Personally Identifiable Information
PPE Personal Protective Equipment
RPAS Remote piloted airborne system (AKA drone)
SO Specific Objective
TAG Test atmosphere generator
TIC Toxic Industrial Chemical
UH University of Helsinki
WP Work Package
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Executive Summary
Task 2.3 Guideline
• Task 2.3 needs inputs from task 2.2, task 4.1 and task 4.2 as presented in Figure 1
• Using the information from these tasks (suitable simulants; suitable sample introduction
systems; operational specification for C-detection; technical outputs from WP4), EOY, UFZ,
AIR, LUH, T4i and JYU will evaluate the developed analytical methodologies with suitable
simulants using a standard operational protocol which is described here.
• Preliminary verification includes the laboratory-intern measurements with determined
simulants by the developer.
• After preliminary verification, methods and systems will be transferred to University of
Helsinki (UH) for final verification with live agents.
• Verification/validation studies with life agents were performed at UH between October 2017
and February 2019.
Figure 1: Communication and feedback between WP2 and WP4
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General Approach
1st step: Calibration of stand-alone ion mobility spectrometers and GC-PID for gaseous substances
under comparable conditions (temperature, humidity with the same substances at precise
concentrations) and hyperspectral techniques for liquid (and possibly solid) substances in lab.
2nd step: Validation of suitable sampling techniques in dependence of different matrices after the
finished development in WP4 (a detailed protocol can be developed after the definition and realization
of technical equipment). The results must be compared with those of GC-MS as standard method.
3rd step: After preliminary verification, methods and systems will be transferred to UH for final
verification with live agents.
4th step: Verification/validation with live agents were finalized February 2019.
1 Supporting Documents
1.1 D2.3 – Triage verification facility Annex 1 – C-detection Appendix 1 – T4i
1.2 D2.3 – Triage verification facility Annex 1 – C-detection Appendix 2 – AIR
1.3 D2.3 – Triage verification facility Annex 1 – C-detection Appendix 3 – EOY
1.4 D2.3 – Triage verification facility Annex 1 – C-detection Appendix 4 – LUH
1.5 D2.3 – Triage verification facility Annex 1 – C-detection Appendix 5 – UFZ
1.6 D2.3 – Triage verification facility Annex 1 – C-detection Appendix 6 – JYU
1.7 D2.3 – Triage verification facility Annex 1 – C-detection Appendix 7 – NTUA
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2 Introduction
2.1 Validation of Monitoring Methods
Different devices and technologies are under development and used within the TOXI-triage project.
The following Table 1 summarizes these devices. This overview was taken from WP 4
(https://newrepository.atosresearch.eu/index.php/apps/files/?dir=%2FTOXI-Triage%2FWPs%20
Documents%2FWP4) (author André Ahrens, LUH).
Device Name Device Type Mobility Task Sampling Medium /
Matrix Detection Environment
for TRL
Providing
Partner
1 T4i DOVERTM Fast GC compatible with PID or IMS
Drone payload 4.1 Air Toxics (TICs) Field T4i
2 BreathSpec GC-IMS 19” rack 3.1
4.3
Breath (air) Metabolites In field and clinic
GAS
3 Prototype Optical detector Hand-held, mobile, drone payload
4.1
4.2
Solids and liquids on surfaces and as wiping samples
CWA Lab, field JYU
4 Sprayed Liquid Gas Extraction
Sampling system Field-deployable 4.2 Air CWA Lab, field UFZ
5 Paper-based Solid Phase
Extraction Discs
Sampling system Backpack 4.2 Liquid CWA Lab, field UFZ
6 ChemPro DM Aspiration Ion Mobility Spectrometer
Handheld, Vehicle mountable, UAV mountable
4.1 Air samples, gas vapors CWA, TICs, generic chemical
alarm
Field EOY
7 RanidFly Radiation spectrometer
UAV mountable 4.1 RN sampling Radio nuclide detection, identification
Field EOY
8 EnviScreen SW Laptop 4.1 Part of UAV system data interface
Field EOY
9 Trace Atmosphere Generator
Production of reference gases for calibration of field chemical instruments
Device weighs less than 1kg but needs two external gas cylinders
4.1 Lab NTUA
10 GDA-FR Combination of IMS, PID, EC, MOS
Handheld device with dilution sampling system
4.2 Air, with special trapping tool for very low concentrations in air (with UFZ), with new desorption tool also
surfaces (with LUH)
CWA, TICs Field AIR (with UFZ and LUH)
11 GDA-P – special version
Combination of IMS with alternatively PID
or EC
Small handheld instrument
4.2 Air CWA, TICs, (Cl2)
Field AIR
CWA = chemical warfare agent; TIC = toxic industrial chemical
Table 1: Devices and technologies in TOXI-triage project
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The highlighted technical developments (red colour) are part of the verification/validation protocol of
stand-off and environmental contamination monitoring methods. The BreathSpec by GAS is originally
developed for metabolites in exhaled air and is therefore not part of the validation with simulants of
chemical warfare agents (CWAs) and toxic industrial chemicals (TICs). RanidFly is a radiation
spectrometer and it is included in the Annex 2 of this document. Furthermore, the ENVISreen data
interface is a technical development for data transfer and not an analytical technique.
Nearly all above-mentioned analytical instruments are suitable for the measurements of gaseous
compounds. The comparative validation of these devices requires the injection of sample gas streams
with defined concentrations and defined environmental conditions (e.g. the composition of sample
gas stream, its humidity). During the measurements, the concentration should be adjustable while the
other parameter should be kept as constant as possible. Furthermore, the application of these
analytical techniques for the determination of chemical warfare agents (CWAs) and toxic industrial
chemicals (TICs) requires comparatively low detection limits, which must be realizable. Such
introduction systems are a challenge for the validation of the different analytical devices. Therefore,
we describe in the first part of this report different introduction systems which were been developed
and are under development and which are available for all TOXI triage partners. Testing of studied
detectors are described in Appendices 1-7 of this Annex 1.
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3 Sample Introduction Systems
3.1 Sample introduction system (UFZ)
The precise (repeatable and reproducible) sample introduction is the most important step for
quantitative analysis with ion mobility spectrometers. Preliminary experiments for calibration of all
stand-alone instruments from different producers must be accomplished under comparable conditions
including: same temperature, same humidity and precise sample concentrations.
Regarding different technical parameters of the spectrometers, UFZ has developed several
introduction systems. The stand-alone ion mobility spectrometers from producers taken part in the
TOXI-triage project are equipped with an internal sample gas pump that primes the sample gas flow
with a constant flow rate. In the following, it will be shown only the introduction systems which have
been developed for such spectrometers. Figure 2 shows the developed system for introduction of one
sample to the BRUKER RAID 1 ion mobility spectrometer. Their internal pumps have usually a flow rate
of 416 mL min-1. The temperature can be easily adjusted with a refrigerated/heated bath circulator
whereas humidity cannot be controlled.
Figure 2: Sample introduction system for spectrometers with an internal sample gas pump providing a flow rate of 25 L/h (416 mL/min)
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The system shown in the figure above is suitable for the analysis of volatile and semi volatile substances
with a sufficient permeation rate through the walls of permeation tubes. About 300 μl of liquid samples
of investigated compounds were sealed in permeation tubes consisting of polyethylene. The
permeation tubes with a volume of 1 ml and a wall thickness of 0.5 mm were placed in a temperature-
controlled glass column (permeation vessel). The temperature of the permeation vessel was adjusted
using a circulator which pumped water at a defined temperature from a thermostat along the
permeation vessel. The solid samples were put into an open vessel and also placed in the glass column.
However, solid samples can only be investigated using this system if their vapour pressure is sufficient
for trace amounts to evaporate. Purified and dried ambient air was pumped through the glass column
containing the permeation tube at a constant flow of 416 mL min-1. Nitrogen or ambient air was used
as a carrier gas. Purification and gas-drying were mainly performed using silica gel and charcoal or
special moisture traps. The moisture content of the gas streams was controlled by an AMX1
(Panametrics) moisture sensor. The sample gas stream was split using flow controllers. A defined
amount of the sample gas stream was rarefied with purified and dried ambient air. The flow rate of
this total gas stream was kept constant (416 mL min-1). The gas stream was primed by the ion mobility
spectrometer’s internal sample gas pump, which also had a capacity of 416 mL min-1. The analytes
were transported to the ion mobility spectrometer in this way. All the connections between the
permeation vessel, flow meters and spectrometer were made using Teflon tubes. However, the
optimization of the diameters of the connecting tubes required a long period of time due to the
different pressure ratios depending on the distances to the flow meters and the sample gas pump of
the spectrometer, so the diameters of the connecting tubes were therefore optimized empirically. All
the flow controllers used in this and the other introduction systems were calibrated using a bubble
meter. The concentration of the compounds in the sample gas stream was calculated using the weight
loss of the permeation tube over a certain time. The weight loss was determined using a microbalance.
Using the weight loss, the total amount of gas flow through the permeation vessel and the additional
rarefaction of gas streams, the concentration in the sample gas stream into the ion mobility
spectrometer was calculated and was reported in ng or μg of substance per litre of carrier gas. Before
we started the measurements, the permeation tubes were conditioned. For this purpose, a pre-
permeation station was used. The permeation tubes were placed in glass columns similar to the
permeation vessels. A constant gas flow of purified and dried ambient air with the same flow rate as
used in the permeation vessels of the sample introduction system was pumped through these glass
columns. After certain time, the permeation tubes were weighed and the permeation rate within this
time was determined depending on the gas flow. This procedure was repeated up to a constant
permeation rate.
Figure 3 shows the introduction systems that permits the simultaneous introduction of two different
compounds depending on their concentration. The principle of this system is the same as mentioned
above.
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Figure 3: System for the introduction of two different compounds depending on their concentration using spectrometers with an internal sample gas pump
The gas stream through each permeation vessel was held at a constant flow rate of 416 mL min-1. The
concentration of each substance was adjusted by splitting these gas flows using flow controllers. The
sample gas streams coming from the permeation vessels and an additional flow of carrier gas are
combined within a special mixing-chamber. This combined gas stream was split once more. One
portion of this sample gas stream with a flow rate lower than 400 mL min-1 was also rarefied with the
carrier gas up to a flow rate which corresponds with the capacity of the spectrometer’s internal sample
gas pump (416 mL min-1). The concentrations of substances in the sample gas flow were determined
as described above.
However, we established a considerable variation in flow rates of BRUKER RAID 1 ion mobility
spectrometers as the operating time of the pumps increased. For a better compensation of these
differences, we developed an additional introduction system as shown in Figure 4.
The mass flow controller (1) provides a constant flow rate through the permeation vessel (100 ml min-
1). For the determination of the spectrometer’s pump capacity, valve (V2) is closed and valve (V3)
permits only the gas flow from the mixing chamber to the spectrometer. The wash bottle on valve (V1)
was replaced by a bubble meter. The gas flow provided by the mass flow controller (2) was adjusted
so that no motion of soap bubbles in the bubble meter was observable.
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Figure 4: Sample introduction system for spectrometers with internal sample gas pumps with varying flow rates
Therefore, the gas flow provided by mass flow controllers (1) and (2) corresponds exactly with the flow
rate which is primed by the spectrometer’s internal pump. The adjustment of different concentrations
was realized using an additional gas flow of carrier gas provided by mass flow controller (3). The
excessive gas is withdrawn via valve (V1). During the measurements, valve (V3) is adjusted as described
above. The other position is only used for purging the system in the case of contaminations. The
concentrations were calculated using the weight loss over a certain time and the gas flows as described
above.
Figure 4 represent the introduction system with controlled humidity. Purified and dried carrier gas was
passed through the glass column with an adjusted flow rate. This flow through the permeation vessel
was held constant for at least 8 hours. Using a needle valve and controlled by a mass flow meter, this
sample gas stream was split and a portion of flow was guided into a mixing chamber where the sample
gas stream can be additionally diluted by two mass flow controllers. An aliquot of this diluted sample
gas stream is transported into a second mixing chamber via a rotary vane pump. The second mixing
chamber permits the additional dilution of sample gas and its humidification. The gas stream for
humidification is generated by mixing gas flows of 0% and 100% relative humidity. Both gas flows can
be adjusted with needle valves. The resulting gas flow into the mixing chamber is also controlled by a
mass flow meter. The carrier gas stream into the IMS was taken from this mixing chamber via a rotary
vane pump.
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Figure 5: Sample introduction system with controlled humidity
The humidity of this final gas flow was monitored with a moisture sensor AMX1 (Panametrics, Hofheim,
Germany). All mass flow meters and mass flow controllers must be calibrated using a bubble meter
before use. In Figure 5 a photograph of the sample introduction system with controlled humidity is
shown.
Figure 6: Photograph of the sample introduction system with controlled humidity
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3.2 Sample introduction system (EOY)
Chemical agent detector ChemPro100i is designed to operate in open-air conditions. However, the
best way to find out the ChemPro100i's agent performance is to test it by using the specific laboratory
test setup. In this section, special features of the laboratory testing of the ChemPro100i are described.
3.2.1 General Requirements
Normally the ChemPro100i is tested in a test setup containing basically conditioning air (clean air) flow,
agent flow and equipment (solenoid valve) to challenge it with clean air or with agent contaminated
air. Clean airflow rate of the setup must exceed the flow rate of the ChemPro100i, which means >3
l/min. The airflow through the detector must be continuous with no blockings i.e. the flow-rates at the
setup must not generate any extra pressure to the ChemPro100i. Solenoid valves are recommended
because of their consistent speed of operation. Generally, there should be no pressure changes or
humidity changes when switching from clean air to agent air. Thus, the clean air has the same pressure,
temperature and humidity as the agent air. It's possible to use the ChemPro100-UIP software to check
whether there is system induced effects at the setup.
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3.2.2 Schematic of the Setup
A schematic drawing in Figure 6 describes one example of suitable test setup for reliable testing of the
ChemPro100i. Suitable flow line materials are Teflon® PFA or glass. The ChemPro100i is connected
pneumatically to the setup with a special Fixed System Monitoring Cap (CP100-MOC2) as shown in
Figure 7 The air supply is compressed clean air, which is cleaned, dried, further humidified and finally
divided into dilution flow (clean air) and agent flow, which are controlled. The primary concentration
can be generated in several ways (infusion pump, oven, permeation tube etc.).
Figure 7: Laboratory test setup for ChemPro 100i
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3.2.3 Overall test instructions
1. Connect the ChemPro100i into the vapour generation system (see Fig. 7), start the airflow, set
the desired humidity level and start the detector. If possible monitor the ChemPro100i’s
responses using the Chempro100-UP software.
2. Test the system background air by switching the solenoid valve on and off (blank testing
without an agent). Test is OK if there are no responses observed in any of the ChemPro100i's
sensors (IMCell, SCCell, humidity and temperature).
3. Start testing with the agent. Record the exposures using the ChemPro100-UIP software, if
possible.
4. Always let the ChemPro100i stabilize for 5 minutes in clean air prior to each agent exposure
under new conditions (RH, temp).
5. The vapour generation system should be allowed to clean itself from residual gases from
previous challenges. If small residual carries over is present, the ChemPro100i may be able to
detect the previous sample. This could lead to misinterpretation of the test data.
6. When testing is finished, check the background signal again to verify that all samples have
vaporized and the system is clean. Let the system clean itself by running the system with clean
air for an extended time, overnight if necessary.
7. Shut down the ChemPro100i and vapour generation system.
Figure 8: Pneumatic connection
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3.3 Miniature Trace Atmosphere Generator (NTUA)
3.3.1 Technical Description
Miniature Trace Atmosphere Generator (TAG, dimensions 165x105x60 mm) is the prototype of an
automated pneumatic and electronic device for the production of reference gas mixtures with a
predefined concentration of analytes. These mixtures can be used for the calibration of chemical
monitoring devices. The device is equipped with the firmware of the device’s microcontroller, as well
as, the device’s control software
The electronic device is designed around the PIC32MX795F512L microcontroller which is responsible
for the digitization and the processing of the analogue signal coming from four flow sensors. Using a
PID based control algorithm the microcontroller creates the PWM signals that drive four proportional
solenoid gas valves. The target gas flow values for each flow sensor – valve pair are chosen by the user
using the software that was developed with Python® and runs on Windows® and Linux®. The design of
the device’s PCB was performed using the «design for manufacturing and assembly (DFMA) approach
which simplifies the end result and minimizes cost. In Figure 9 schematic of the device is given. In Figure
10 an example of a running file is presented.
Figure 9: The schematic of the device (permeation vial, external vial and oven have not integrated to the device; ad hoc connections are used instead)
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Figure 10: User interface
Figure 11: Example of a running file
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3.3.2 Validation procedure
The miniature TAG has Viton tubes and the validation procedure aims at testing the low limit of
concentration that the device are achieved. The device is connected to the UFZ system and gets as
input the stream output of UFZ system with the aim of generating lower concentrations. The TAG
output is measured using one of the TOXI IMS. Then the UFZ system generates the same low
concentration and the two outputs are compared. These tests will assist to identify how valves, flow
meters, firmware, software and tubes perform. The tag is not heated for the moment but this can be
part of the future development. An example of the tests will look like this: UFZ system develops 1ppm
concentration of a selected compound, and then TAG is set up to generate 500ppb. The response is
measured with IMS. Then UFZ system produces 500ppb of the same compound. The response that the
same IMS is giving to the UFZ stream at 500ppb is compared with the TAGs.
3.3.3 Simulants for preliminary validation
Simulants used for IMS calibration and Benzene, Toluene, Ethyl benzene and Xylene (BTEX) can be
used.
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4 Analytical Instruments
The validation procedures for analytical instruments which are under development in this project
therefore include:
1. Stand-alone ion mobility spectrometers at field level (TRL 6-9)(see Table 2)
2. GC-PID at lab level (TRL 4) and prototype level (TRL 7)
3. Hyperspectral Imaging at lab/field level (TRL 6-7)
4.1 Ion mobility spectrometers
4.1.1 Technical description
Within the TOXI-triage consortium and according the device table, three different ion mobility
spectrometers were used. The Table 2 summarizes their basic configuration.
Air (GDA-P) Air (GDA-FR) EYO (ChemPro) LUH (mini-IMS)
IMS type Time-of-flight Time-of-flight Aspiration Time-of-flight
Ion source 63Ni (100 MBq) 63Ni (100 MBq) Am241 (5.92MBq) X-Ray (3kV acceleration
voltage)
Sample inlet Silicon rubber membrane (80°C)
Silicon rubber membrane (80°C)
Open Direct inlet (250µl sample loop)
Drift gas Air (closed circuit) Air (closed circuit) Ambient air Air (closed circuit)
Drift gas flow Internal circuit Internal circuit Sample pump 120mls/min
Drift tube 6 cm (50 °C) 6 cm (50 °C) Aspiration 4 cm, ambient temperature
Additional sensors PID or EC PID, EC, MOS Several MOS / FE sensors, RH/AH, P, T,
Flow
-
Table 2: Tested ion mobility spectrometers
4.1.2 Validation procedure
In order to calibrate stand-alone ion mobility spectrometers, following characteristics must be
considered for validation:
• Detection limit and limit of quantification with LOQ = 3*LOD
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• Linear range of calibration
• Precision
o Repeatability (Intra Assay Variation): At least 5 repeated measurements for one
experiment at low, medium and high concentrations for a substance.
o Reproducibility (Inter Assay Variation): Repeated at least three experiments using
different/same equipment and operators at different/same days.
• Recovery time at high and low concentrations
Calculation of the above mentioned characteristics with different spectrometers and by different
group needs absolute clarity about the two following issues:
1. Suitable simulants
a. DMMP as sarin-type nerve agent and MSAL as simulant for blister agents
2. Sample introduction systems
a. Laboratory temperature (18-25°C)
b. Three humidity level (dry conditions, medium level, higher level)
4.1.2.1 ChemPro100i Confidence sample
ChemPro100i is calibrated and tested in factory after manufacture before is it sent to end-user. After
that ChemPro100 do not need any calibration and laboratory level validation but only confidence
check.
ChemPro100i continuously monitors the internal health of itself. This operation is called the Built-in
Test (BIT). After starting the unit, the ChemPro100i immediately begins the BIT self-diagnostic
sequence that verifies the operability of the detection system. The operator is informed when the unit
is ready for a detection mission. After the start-up the BIT is run as part of the program cycle.
The BIT:
• checks and adjusts the air flow
• checks the processor board
• checks the sensor boards
After the start-up, the BIT is run continuously as a part of normal program execution, but is not visible
to the user until some problems exist.
The ChemPro100i’s detection capability can be tested by using a confidence sample (Test Tube)
provided within the Standard Accessory Kit. The Test Tube contains a mixture of two chemicals, DIMP
and 1-propanol. The test is performed during a special Sensor Test mode selected from the user
interface.
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4.1.3 Simulants for preliminary validation
A report for simulants named “Selection of C simulants in TOXI-triage project” version 1.1 was
uploaded to the repository by Helsinki University. Airsense has also provided information for the
applicable simulants with ion mobility spectrometers.
Till May 2019, two stand-alone ion mobility spectrometers were available as operational instruments
from two providers: Chempro (Aspiration IMS) from Environics and GDA (Drift-IMS is also included)
from Airsense.
Furthermore, a GC-IMS coupling (T4i and LUH) and hyperspectral techniques (JYU) are under
development and the current configurations are defined in this document.
The initial validation includes a comparison of analytical data of the above-mentioned ion mobility
spectrometers regarding detection limit, linearity range and precision which is restricted to gas-phase
measurements without additional matrix effects. In dependence on the operational conditions of
spectrometers, different introduction systems can be used. The simulants must be selected regarding
the detectability in IMS and their suitability for calibration in the gas phase. The selected simulants
must therefore have a low volatility. We therefore suggest to use:
➢ DMMP (Dimethyl methylphosphonate) as sarin-type nerve agents
and
➢ MSAL (methyl salicylate) as simulant for blister agents.
the initial validation in the gas phase.
Due to the low-volatility of Malathion as the simulant for VX nerve agent, it may be able to be analysed
by GDA-X detector of Airsense.
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4.1.4 Presentation of Results
All data are to be collected under the following table and after experiments with simulants delivered
for the verification analysis at UH.
Tem
pe
ratu
re
(°C
)
Hu
mid
ity
Sim
ula
nt
De
tec
tio
n L
imit
Lin
ea
rity
Ra
ng
e
Re
pe
ata
bility
(Lo
w C
on
c.)
Re
pe
ata
bility
(Me
diu
m
Co
nc
.)
Re
pe
ata
bility
(Hig
h C
on
c.)
Re
pro
du
cib
ilit
y
Re
co
ve
ry T
ime
(Lo
w C
on
c.)
Re
co
ve
ry T
ime
(Hig
h C
on
c.)
Instrument 1 T1 H1 DMMP
Instrument 1 T1 H2 DMMP
Instrument 1 T1 H3 DMMP
Instrument 1 T1 H1 MSAL
Instrument 1 T1 H2 MSAL
Instrument 1 T1 H3 MSAL
Table 3: Example of reporting of verification analysis at UH
4.2 Gas chromatography – PID
4.2.1 Technical description
T4i DOVER™ is a fast GC-PID based chemical detector equipped with a front-end for Sample
Modulation and Separation (SMS), currently coupled with a photo ionization detector (PID). It is
designed especially for use on-board UAVs with the scope of DIM of CWAs and TICs. T4i DOVER™ is a
multi-sensor detector that overlays geo-referenced and time-stamped data with chemical real-time
measurements to provide temporal and spatial (in 3D) chemical information.
T4i DOVER™ allows for periodic gas sampling with “injection” times as low as 200 milliseconds. The
sample is injected into the fast GC, providing fast chromatographic analysis and it then introduced into
the detector, which is a commercial off the shelf (COTS) PID with a few seconds response time.
The 3D technical drawing presented in Figure 12 shows the current T4i DOVER™ configuration.
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Figure 12: 3D technical drawing of the current T4i DOVER™ configuration
T4i sample introduction system is valve-less (i.e. without the sample interacting with any pneumatic
component), providing very fast periodic sampling (“injections”).
The work will validate basic analytical performance of T4i DOVER™ using a vapour generator to
produce low concentrations of TICs and CWA simulants. Using a series of measurements, LoD, linearity
range and reproducibility will be estimated. Reproducibility will include GC retention times of
compounds and PID responses. In addition, GC performance in mixture analysis will be validated. The
work will also cover evaluation of basic operational parameters such as total analysis time.
T4iDOVER is a fast-GC PID detector that has at the front end the SMS which is a sampling unit that
allows dynamic, real-time sampling. The SMS is based on well-proven principles of fast pneumatic
periodic sampling and has been previously published ([1], [2], [3], [4]). These allow very fast
alternations between sampling and non-sampling periods that provide real-time monitoring capability.
In the Figures 13 - 16, the basic principles of the SMS unit of T4i DOVER™ are presented.
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Figure 13: The SMS (Sampling Modulation Separation)
How the SMS works during sample injection (Sampling ON) period:
1. Sample inlet through different nozzle types and isokinetic sampling
2. Small tube (20mm OD, 12cm long) for sharp sample injections as short as 100ms
3. COTS capillary column (30cm – 5m long)
4. Low Thermal Mass Gas Chromatography
5. Micro Photo Ionization Detector cleaning
Figure 14: Sample modulation
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How the SMS works during analysis (Sampling OFF) period:
6. Continuous introduction of ambient air
7. Introduction of clean air that prevents sampling
8. Analytical scale GC
9. Micro Photo Ionization Detector response
10. Sample exhaust
Figure 15: Sample separation
Figure 16: The T4iDOVER hardware configuration
• Valve-less sample introduction due to principle of operation. No electro-mechanical valve
comes in contact with the actual sample.
• Elimination of surface chemistry phenomena and iso-kinetic sampling by design.
• Ultra-low footprint.
• Ultra-low power consumption (less than 30W).
• No need to use pressurized gas cylinder.
Sample
modulation
Nozzle
TIC detection and
identification
Sample
separation
Pneumatics
board
Main board
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• Real time monitoring.
4.2.2 Simulants for preliminary validation
Initial measurements for developing the method have been carried out in LU. An elaborated,
systematic experimental design was carried out using Benzene, Toluene, Ethyl benzene and Xylene
(BTEX), a series of alcohols, ketones and, if possible, amino- or sulphur- compounds. Preliminary
validation was carried out with simulants DMMP and MSAL. The GC-IMS system was therefore tested
using the same simulants selected as used for the ion mobility spectrometers.
4.2.3 Validation procedure
• Generation of ultra-low concentrations for a set of compounds with vapour pressure in the
range of 10-1 to 10-2 mmHg.
• Monitoring of the vapour stream from the generator up to 1 h.
• Concentrations generated in the range of 200 ppb to 1 ppm or from 1 ppm to 300 ppm taking
into consideration toxicity levels.
Results are given Appendix 1 - T4i.
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4.3 Hyperspectral systems
4.3.1 Technical description
In Toxi-Triage project, JYU has developed and tested a holistic hyperspectral system for the field
detection of CBRNE. The core of the system is a newly generated wireless software that retrieves and
analyses in real time hyperspectral imaging data and generates alerts and warnings into integrator and
other selected systems. Hyperspectral cameras (sensors), operating platforms (e.g. drones), remote
control devices, Wi-Fi equipment, processors and other technical equipment are commercial of-the-
shelf (COTS) devices or tailored prototypes. The system is designed scalable, so that it can be used
alternatively with one or many different hyperspectral cameras and different operating platforms at
the same time. In addition, the system emphasizes precision investigation at the CBRNE site, and it is
also usable for long distance detection of CWAs and TICs from the outside of the Hot Zone. Overall
configuration of the scalable hyperspectral detection system is presented in Figure 17. The overall
design, all software, analysing procedures and integration/telecommunication parts of the system are
produced and constructed by JYU. Additional technical features of the system are seen in Table 4.
Figure 17: Structural configuration of JYU’s hyperspectral detection system
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Hyperspectral Cameras
Detection method Rapid
Type of camera Passive infrared cameras
Type of samples Solid, liquid
Detection environment Surfaces
Alternative types of sampling 1. Direct detection on the target without touching the target 2. Wiping sample + direct detection on the wipe without touching the sample
Recovery procedures 1. Not needed if there is no physical contact with the agent 2. Cleaning needed if the lens has a physical contact with the agent
Table 4: Hyperspectral cameras that were tested in the laboratory
4.3.2 Validation procedure
In the first stage of the project, capability tests were made in the laboratory with high-capability
hyperspectral cameras that are designed especially for industrial and laboratory use. After developing
the needed software for the field detection system, field tests and field experiments FTX Focus and
FTX Disperse were carried out with simulants with small hyperspectral cameras.
The hyperspectral system is validated for the hyperspectral cameras’ part in the laboratory according
to the following procedure (see also Figure 18):
1. Hyperspectral camera is placed steadily in a fume cupboard.
2. Conditions in the fume cupboard are set according to the used agent.
3. An exact amount of the test agent is dosed on glass or other predefined matrix in a Petri dish.
4. The Petri dish is placed in a fixed position under the hyperspectral camera ca. 15 cm from the
lens (with applicable optics).
5. The sample is measured with the hyperspectral camera.
6. The detection result is confirmed with an applicable secondary device.
Figure 18: Testing design for hyperspectral imaging
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4.3.3 Simulants for preliminary validation
Preliminary validation of hyperspectral devices was made with two simulants of organophosphorus
nerve agents and blistering agents. Validation for organophosphorus agents (sarin) was made with
DIMP and for blistering agents (sulphur mustard) with 2-Chloroethyl ethyl sulphide. Also many other
samples were used.
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5 Validation of Sample Preparation Techniques
5.1 Paper filter as field deployable sampling techniques
5.1.1 Technical description
Paper-filter disk extraction is a modified solid-phase extraction (SPE) format which is more suitable for
in-site application. Paper which is an inexpensive stable natural polymer is used as the substrate,
disperser and protector to fabricate low-cost selective extraction disks, which are robust, reproducible
and easy to handle also under field conditions. Figure 17 shows the photograph of the new developed
disk format compared to the traditional SPE column.
Figure 19: Photograph of the traditional column and new developed disk format of SPE method
Commercial laboratory filter-paper is simply converted to pulp, mixed with 50 to 400 mg of molecularly
imprinted polymer (MIP) particles and reconverted easily to a selective porous filter paper. Using a
simple preparation procedure, selective filter-papers can be easily prepared in different geometries
and sizes. We adjusted our circular-disk diameter to 47 mm in order to use it with a manual extraction
device (shown in Fig. 18) which is suitable for field application.
Figure 20: Manual filtration apparatus and hand-operated vacuum pump for in-field applications
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5.1.2 Validation procedure
The following parameters must be optimized for a chemical target:
• Molecularly imprinted polymer for the desired target
• Pulp to polymer ratio for the preparation of a stable disk
• Sample flow-rate
• Sample volume
• Washing and elution step
Firstly, an ion-exchange MIP, synthesized for a well-known anthropogenic marker, was used as an
example of nano-sized selective particles to evaluate and develop the new concept. The developed
paper disks were used in-field for the selective extraction of target compounds which transferred to
the laboratory for further analysis.
MIP adsorbents (termed by the company: RENSA™ 101) for the target molecule Malathion, as the
stimulant for VX nerve agent, was prepared from Biotage company. MIP polymer particles work based
on silver ion chromatography concept. Polymer particles could be used for complete purification of
Malathion from liquid samples. After Malathion removal by polymer particles, various elution solvents
were tested to elute the Malathion molecules from polymer. Surprisingly, none of the used solvent
could help to elute the adsorbed target molecules from polymer particles. That shows the successful
application of the polymer for the purification or decontamination of the contaminated samples, while
it cannot be used for sample-preparation purposes.
5.2 Sprayed liquid-gas extraction (SLGE)
5.2.1 Technical description
SLGE is under development by UFZ as a new sampling method for the low-volatile organic compounds
in gaseous phase using small-air sampling method. Figure 19 shows a schematic of the SLGE method
in which low volume of a liquid extractor is used for the fast collection of chemical molecules from high
volume of gas samples.
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Figure 21: Schematics representation of SLGE method (under development by UFZ)
Few mL of liquid extractor is dispersed (as the micro droplets) into large volume of gas sample
containing the molecules of chemical targets and collected in a test tube. Theoretically and due to the
high surface area of the extractor in contact with gaseous sample, the equilibrium state can be
achieved quickly and, therefore, the extraction time is very short. Following first step extraction using
SLGE method (the target chemical’s transfer from the gas into liquid phase), further sample
preparations like mini-scale liquid-liquid extraction can be easily implemented I) to increase the
enrichment factor and II) to make the samples easily injectable for the laboratory instruments (GC-MS)
or field deployable instruments (GDA-X from AirSense).
5.2.2 Validation procedure
For the especial targets following parameters must be optimized:
• Nature of the extractor
• Extractor flow-rate and extraction time
• Sample flow-rate
Malathion (VP: 3.97X10-5 mm Hg at 30 °C) as the simulant for VX nerve agent, dimethoate (VP:
1.875X10-5 mm Hg at 25 °C) as the simulant for pesticides and 4-Chloro-3-methylphenol (VP: 5.00X10-
2 mm Hg at 20 °C) have been selected as simulant for method optimization. Results are given in
Appendix 5 of this Annex 1.
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5.3 Wipe tests (AIRSENSE Analytics)
For liquid or solid samples which are present as a thin film on a surface, sampling by wiping is also
possible. The wipe tests are described for the available procedure from AIR. The wipe pads and their
handling are optimized for the use of the GDA-X ion mobility spectrometer with an attached desorber-
tool.
A wipe pad must be clean and free of chemicals and dust in order to avoid contamination or carry over.
But a wipe pad can be reused as long as no explosives were measured. Do not touch the active area in
order to avoid contamination of the wipe pad before analysis. Gently wipe the surface for investigation
with the active area of the wipe test facing down. Do not use too much force during wiping in order to
avoid scratching of the surface. Treat the sample carefully to avoid cross contamination by unintended
contact with other surfaces (see Figure 20).
Figure 22: Wipe pad. Fold with active area facing down (left), Collect sample by gently wiping the area in investigation
(right)
The desorber-tool must be aligned correctly. The instrument will elevate the desorber temperature
and prepare to receive the sample. After preparation, the status LED on the desorber-Tool of GDA-X
(AIR) will blink blue and the instrument prompts the operator to introduce the sample. Introduce the
wipe pad with the active sampling area facing down into the desorber-tool. The desorber-tool detects
the wipe pad and checks for its correct alignment. As the wipe pad is inserted correctly, the instrument
demands to close the cover lid. This will start the measuring procedure automatically (see Figure 21).
Results for this device are given in Appendix 2 of this Annex 1.
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Figure 23: Collect sample by gently wiping the area in investigation
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6 Validation protocols at VERIFIN using live agents and various matrices
Validation protocols performed at VERIFIN includes testing of instruments with live agents like pesticides, chlorine, chloropicrin, sarin, VX, HD and various
degradation products. In the Table 5 are given chemical properties of the selected chemicals, which could be tested using TOXI-triage detectors. Not each
chemical is used in testing of all instruments. Compounds are selected on basis of their suitability to test a selected instrument.
Chemical Class CAS Structure Schedule MW [g/
mol]
Bp [°C]
KH
Vapour pressure at 25 °C [mmHg]
Oral toxicity [mg/kg] WHO class
Rat Mouse
Chlorpyrifos Pesticide 2921-88-2
– 350 decomp at 160 °C
3.6∙10-5 2.1∙10-5 82–320 60–150 II
Dimethoate Pesticide 60-51-5
– 229 107
(0.05 mmHg)
2.4∙10-10 1.9∙10-6 240–680 60–160 II
Chlorine TIC 7782-50-5 Cl2 – 71 -34 4.6∙10−5 5.8∙103
Chloropicrin1,2 TIC 76-06-2
3.A.04 164 112 24 250 II
Sarin1 Nerve agent 107-44-8
1.A.01 140 158 3.8∙10-4 2.1 0.1–1.1 0.29 Ia
VX Nerve agent 50782-69-9
1.A.03 267 298 1.4∙10-7 7∙10-4 0.077–0.13 Ia
Dipropylene glycol monomethyl ether
Nerve agent simulant
34590-94-8 – 148 184-190 4.7∙10-8 0.55 5200–5400 III
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Table 5: Selected chemicals for testing
GC-MS-technique is a so-called Golden Standard method. In validation report all instrumental parameters used in validation must be reported both for the
tested instrument as well as for the reference method.
Purity of all chemicals are tested before tests with NMR and reported in the validation report. Purity has to be checked and it should be at least 70%. Actual
amount of compound is calculated against to the purity. Purity of used compounds can be found on Table 7.
Table 6: List of WHO Classes of hazardous chemicals
Diethyl phosphite Nerve agent simulant
762-04-9
– 138 204 5.8∙10-6 11 3900 >2000 III
Malathion3 Nerve agent simulant
121-75-5
– 330 156 2.0∙10-7 3.4∙10-6 290 190 II
Propan-1-ol Nerve agent simulant
71-23-8 – 60 97 7.4∙10-6 21 1900 6800 II
1 Chloropicrin and Sarin hydrolyse quite fast in aqueous conditions 2 Chloropicrin is quite volatile and evaporates fast from solid surfaces 3 Malathion cannot be used if TENAX® tubes are used for sampling because of degradation
TIC= Toxic industrial chemical; MW = molecular weight; Bp = boiling point; KH = ; WHO = World Health Organization
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6.1 Validation Plan of Analytical Instruments
Preliminary test plan is shown at Table 7.
Chemical Matrix Concentration Instrument
Chlorpyrifos Air (sniff) Pure agent EOY/IMS
Dimethoate AIR/GDA-FR
Malathion AIR/GDA-P
Chloropicrin AIR/Wipe tests-AIR/GDA-FR
Sarin UFZ/SLGE and AIR/GDA-FR
VX UFZ/paper filter and AIR/GDA-FR
LUH/Mini-IMS
T4i/Dover
Sarin Air 0 mg/m3 EOY/IMS
VX 0.1 mg/m3 AIR/GDA-FR
0.2 mg/m3 AIR/GDA-P
0.3 mg/m3 UFZ/SLGE and AIR/GDA-FR
0.4 mg/m3 LUH/Mini-IMS
0.5 mg/m3 T4i/Dover
Chlorine Air 0 ppm EOY/IMS
0.1 ppm AIR/GDA-FR
0.5 ppm AIR/GDA-P
1 ppm LUH/Mini-IMS
2 ppm T4i/Dover
5 ppm
Chlorpyrifos Steel 0.1 µg EOY/IMS
Dimethoate PPE 1 µg AIR/GDA-FR
Malathion Cotton 10 µg AIR/GDA-P
Chloropicrin Glass* 50 µg AIR/Wipe tests-AIR/GDA-FR
Sarin 100 µg UFZ/SLGE and AIR/GDA-FR
VX 200 µg (not Sarin or VX) UFZ/paper filter and AIR/GDA-FR
500 µg (not Sarin or VX) LUH/Mini-IMS
JYU/HSI (* matrix only with this
technique)
Table 7: Preliminary test plan
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6.2 Matrices
1. Stainless steel plates were used as building material
Regular stainless steel plates: size approx. 2 * 2 cm and thickness 1 mm, supply from University of
Helsinki
2. Fire escape suit is used as Personal Protective Equipment. It was obtained from SSAV (South-Savo
Regional Fire Service, Mikkeli, Finland). It is made of Nomex®1. Before used as matrix the suit was
cleaned by washing with water as instructed in the care label.
3. Cotton fabric to simulate regular clothing
4. Air
Centralised air compressor is used for pressurised used air. Moist and oil is filtered from compress air. Analytes are added using syringe dispenser together with sample introduction system with controlled humidity.
6.3 Sample Preparation Reference Methods: Recommended Operation
Procedures
ROP 2B IV: Recommended Operation Procedure, Section Sample Preparation, Part B, Chapter IV, Air
samples
• The concentration of a chemical in the spiking solution is adjusted using syringe dispenser with
sample introduction system with controlled humidity
ROP 2B V: Recommended Operation Procedure, Section Sample Preparation, Part B, Chapter V, Solid
materials
• Personal Protective Equipment, Extraction: The sample is analysed immediately after spiking
after the solvent has been evaporated. The concentration of a chemical in the spiking solution
is adjusted so that the spiked volumes are between 5-100 µl. Multiple tip pipette is used.
• A piece of 4 cm x 4 cm is spiked
ROP 2B V.C: Recommended Operation Procedure, Section Sample Preparation, Part B, Chapter V.C,
Wipe samples
• Stainless steel plates: The sample is analysed immediately after spiking after the solvent has
been evaporated. The concentration of a chemical in the spiking solution is adjusted so that
the spiked volumes are between 5-100 µl. Multiple tip pipette is used.
• Teflon is used as wipe material
1 The main component of Nomex® is meta-aramid
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6.4 Tested Instruments
6.4.1 Technical description
Within the TOXI-triage consortium and according the device table, three different ion mobility
spectrometers will be used. The following table summarizes their basic configuration.
Chemical Matrix Concentration Instrument
Chlorpyrifos Air (sniff) Pure agent EOY/IMS
Dimethoate AIR/GDA-FR
Malathion AIR/GDA-P
Chloropicrin LUH/Mini-IMS
Sarin T4i/Dover
VX
Sarin Air 0 mg/m3 EOY/IMS
VX 0.05 mg/m3 * AIR/GDA-FR
0.07 mg/m3 * AIR/GDA-P
0.1 mg/m3 UFZ/SLGE and AIR/GDA-FR
0.2 mg/m3 LUH/Mini-IMS (* levels only with
this technique)
0.3 mg/m3 T4i/Dover
0.4 mg/m3
0.5 mg/m3
Chlorine Air 0 ppm AIR/GDA-FR
0.1 ppm AIR/GDA-P
0.5 ppm
1 ppm
2 ppm
5 ppm
Chlorpyrifos Steel 0.1 µg EOY/IMS
Dimethoate PPE 1 µg AIR/GDA-FR
Malathion Cotton 10 µg AIR/GDA-P
Chloropicrin Glass # 50 µg AIR/Wipe tests-AIR/GDA-FR
Sarin 100 µg UFZ/SLGE and AIR/GDA-FR
VX 200 µg (not Sarin or VX) UFZ/paper filter and AIR/GDA-FR
500 µg (not Sarin or VX) LUH/Mini-IMS
JYU/HSI (# matrix only with this
technique)
1-propanol Air High concentration EOY/IMS
AIR/GDA-FR
AIR/GDA-P
LUH/Mini-IMS
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Chemical Matrix Concentration Instrument
T4i/Dover
Dimethyl
methylphosphonate
Air Different concentration
levels
T4i/Dover
Diethyl
methylphosphonate
Diisopropyl
methylphosphonate
Dithiane
Divinyl sulfoxide
Mustard gas
Oxathiane
Table 8: Performed tests: concentrations studied and estimated required time for those experiments
Spiking Chemical Purity
Sarin 69 %
VX 90 %
Chlorpyrifos 97 %
Chloropicrin 99 %
Dimethoate 36 % *
Malathion 92 %
* Solubility issue in hexane/EtOAc
Table 9: Purity of applied chemicals
7 Results
All the results are included in Appendixes 1-7 of this Annex 1.
‘Appendix 1 – T4i’ (data from simulant and live agent testing)
‘Appendix 2 – AIR’ (data from simulant and live agent testing)
‘Appendix 3 – EOY’ (data from simulant n and live agent testing)
‘Appendix 4 – LUH’ (data from simulant and live agent testing)
‘Appendix 5 – UFZ’ (data from simulant and live agent testing)
‘Appendix 6 – JYU’ (data from simulant and live agent testing)
‘Appendix 7 – NTUA’ (data from simulant and FTX testing)
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8 Conclusion
Table 10 show instrument testing in VERIFIN’s lab
Providing
Partner
Device
Name
Device
Type Mobility
Sampling
Medium /
Matrix
Schedule
AIR GDA-G
GDA-P IMS Handheld Air 2.-6.10.2017
UFZ
SLGE
(Sprayed
Liquid Gas
Extraction)
Sampling
system Field-deployable Air 9.-13.10.2017
EOY ChemPro
DM IMS
Handheld, Vehicle
mountable, UAV
mountable
Air 27.11.-1.12.2017
T4i T4i DOVER GC-PID Drone payload Air 22.-26.1.2018
LUH Prototype IMS Field-deployable Air 4.-8.2.2019
JYU Prototype Optical
detector Field-deployable
Solid and
liquid on
surfaces
and as
wiping
samples
9.-20.5.2016
7.-8.1.2016
24.-25.1.2017
Table 10: Device testing at VERIFIN’s laboratory
T4i DOVER™ was able to detect DMMP at 10ppm which was the limit of detection of the system for
this compound using the current configuration (column, PID lamp). DIMP and DEMP were not detected
at the concentrations which were used. Regarding C agents, HD was detected and it was proven using
GC-MS analysis that GB was being passed through the GC module and transferred to the detector. T4i
DOVER™ was also able to detect degradation products of GB thus allowing the determination of
residuals from the use of the agent.
GC resolution proved to be adequate when the system was exposed to mixtures with less than 10
compounds and its repeatability was satisfactory.
The total analysis time for one measurement proved to be under 90 seconds even when sampling high
boiling point compounds.
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JYU carried out the laboratory tests in the early stage of the project in order to confirm the need and
reason for creating a new CBRNE detection system especially with small size hyperspectral technology.
In the laboratory tests at Verifin, altogether 23 live agents and simulants were tested, and
hyperspectral image and spectrum were successfully produced for plenty of substances. For some
agents a weak image was produced without a readable spectrum. The tests were made with laboratory
type of heavy weight hyperspectral cameras before building up the wireless system especially for small
and light weight hyperspectral cameras. At the time of carrying out the tests there was no significant
capability of detecting CWAs and TICs with the small hyperspectral cameras that were available on the
open market.
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9 References
[1] McClennen, W. H., Vaughn, C. L., Cole, P. A., Sheya, S. N., Wager, D. J., Mott, T. J., ... & Meuzelaar, H. L. C. (1996). Roving GC/MS: mapping VOC gradients and trends in space and time. Field Analytical Chemistry & Technology, 1(2), 109-116
[2] Snyder, A. P., Harden, C. S., Brittain, A. H., Kim, M. G., Arnold, N. S., & Meuzelaar, H. L. (1993). Portable hand-held gas chromatography/ion mobility spectrometry device. Analytical Chemistry, 65(3), 299-306
[3] Arnold, N. S., McClennen, W. H., & Meuzelaar, H. L. (1991). Vapor sampling device for direct short column gas chromatography/mass spectrometry analyses of atmospheric vapors. Analytical chemistry, 63(3), 299-304.
[4] Arnold, N. S., Dworzanski, J. P., Sheya, S. A., McClennen, W. H., & Meuzelaar, H. L. (2000). Design considerations in field-portable GC-based hyphenated instrumentation. Field Analytical Chemistry & Technology, 4(5), 219-238
www.toxi-triage.eu
Tools for detection, traceability, triage and individual
monitoring of victims
Situational Awareness
End User
Clinical
Triage
ICT
D2.3 Triage verification facility
Annex 2 – RN-detection
Tools for detection, traceability, triage and individual monitoring of victims
www.toxi-triage.eu This project has received funding from the European Union’s Horizon 2020 (H2020) research and innovation programme under the Grant Agreement no 653409.
D2.3 Triage verification facility
Annex 2 - RN-detection
Grant agreement number: 653409
Start date of the project: 2015-09-01
Duration: 48 months
Due date of deliverable:
Actual submission date: 25.6. 2019
Lead Beneficiary: UH (Susanna Salminen-Paatero, Paula Vanninen, Matti Kuula)
Contributing beneficiaries: EOY (Osmo Anttalainen, Jukka Härkönen, Jani Kartano), JYU (Jaana Kuula)
Keywords:
ANSI N42.43, ANSI N42.34, IEC 62327, IEC 62618, CZT detector, gamma spectrometry, validation,
radionuclide identification
Dissemination level:
PU ☒
CO ☐
CI ☐
©TOXI-triage Consortium August 2019
Release History
Version Date Description Released by
V1 2019-06-24 The first version merged from two separate
drafts
Susanna Salminen-Paatero
V2 2019-07-03 Report updated to Toxi-Triage template Matti Kuula
D2.3.3 653409 TOXI-TRIAGE DELIVERABLE TRIAGE VERIFICATION FACILITY AN2 RN DETN
©TOXI-triage Consortium 1 August 2019
Table of Contents
Executive Summary ................................................................................................................................. 4
1 Introduction ..................................................................................................................................... 5
2 Validation procedure ....................................................................................................................... 7
2.1 Environmental conditions before starting the tests ............................................................... 7
2.2 Physical and radiological demands for a mobile spectrometer .............................................. 8
2.2.1 Physical requirements ......................................................................................................... 8
2.2.2 Radiological requirements ................................................................................................... 8
2.2.3 Alarm requirements ............................................................................................................ 9
2.2.4 Requirements for power source........................................................................................ 10
2.2.5 Requirements for energy range of the detector ............................................................... 11
2.2.6 Requirements for communications protocol .................................................................... 11
2.2.7 Requirements for user interface ....................................................................................... 11
2.3 Radiological tests ................................................................................................................... 13
2.3.1 Tests in laboratory ............................................................................................................. 13
2.4 Requirements for environmental performance .................................................................... 26
2.5 Requirements for mechanical performance ......................................................................... 27
2.6 Tests in field ........................................................................................................................... 27
2.6.1 Preliminary test plan for field ............................................................................................ 28
3. Conclusions ........................................................................................................................................ 30
References ............................................................................................................................................. 31
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List of Tables
Table 1. Testing conditions in laboratory (modified from ANSI N42.34, ANSI N42.43, IEC 62327, and IEC 62618). 7
Table 2. Radionuclide test samples used for validation. ____________________________________________ 16
Table 3. A nuclide library that a gamma spectrometer should be able to identify at least. The classification of the
radionuclides has been published by IAEA Safety Guide No. RS-G-1.9 (2005) [6]. ________________________ 20
Table 4. Acceptable daughter nuclides and expected impurities [3][4]. ________________________________ 22
Table 5. Radiation sources used in tests in May 2018. ______________________________________________ 26
Table 6. Probable environmental conditions during field testing. _____________________________________ 27
Table 7. Parameter combinations to be tested in the first field exercise (November 2017). ________________ 29
List of Figures
Figure 1: GR1-A® - CZT Gamma Ray Spectrometer (www.kromek.com). The detector is a small sized (25mm x
25mm x 63mm) and its weight is only ~60 grams. Detection area (detection window) of GR1-A® CZT is 10 mm x
10 mm x 10 mm. ____________________________________________________________________________ 6
Figure 2. Radiation source is positioned in the middle of the detection area of the detector window during
measurements. The source can be kept still in front of the detector window (static testing) or moved either from
far to near, or vice versa (dynamic testing). Thus start position and final position can change places depending
on the test. ________________________________________________________________________________ 16
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List of Acronyms
Abbreviation/acronym Description
AA Battery size, equal to IEC: LR 6
AC Alternating current
ANSI American National Standards Institute
COV Coefficient of variation
CsI(Tl) Cesium Iodide Thallium (detector)
CZT Cadmium Zinc Telluride (detector)
DC Direct current
DU Depleted uranium
GA Grant Agreement
GPS Global positioning system
HEU Highly enriched uranium
HDPE High-density polyethylene
HPGe High-Purity Germanium (detector)
IEC International Electrotechnical Commission
NaI Sodium iodide (detector)
NIST National Institute of Standards and Technology
NORM Naturally Occurring Radioactive Material
NPL National Physical Laboratory
PC Personal computer
RGPu Reactor grade plutonium
SNM Special nuclear material
TRL Technology readiness level
VDC Volts of direct current
WP Work Package
WGPu Weapons grade plutonium
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Executive Summary
Properties of a CZT gamma detector purchased by EOY and user interface developed by EOY were
tested in laboratory and, attached to a drone, in field conditions in Helsinki in November 2017. The
validation plan was modified from the standards ANSI N42.34, ANSI N42.43, IEC 62327, and IEC 62618
before the tests. Identification ability of the detector was tested using standard radionuclide sources.
A second test series for a CZT detector was conducted in 3rd of May 2018, again in University of Helsinki.
In this second test procedure, the capability of the gamma spectrometer for radionuclide identification
and repeatability of the measurement results were evaluated in a simpler and more quantitative way
than in the first validation tests.
Here the planned and for the most part also executed testing program for a RN detector is presented.
All measurement results, observations during the testing and conclusions are summed in a separate
Appendix.
1 Supporting Documents
1.1 D2.3 Triage verification facility Annex 2 – RN-detection Appendix 1-UH
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2 Introduction
Among different gamma detectors, CZT (Cadmium Zinc Telluride) detectors are a kind of compromise
between NaI or CsI detectors (operated at room temperature, low energy resolution) and HPGe
detectors (needs cooling system, good energy resolution). CZT and other wide-bandgap semiconductor
detectors can be operated at room temperatures. However, the size of the CZT detectors is limited
due to technical difficulties in growing large CZT crystals, leading to lower efficiency than of larger-
sized NaI or CsI detectors. The energy resolution of the CZT detector is better than of NaI and CsI, but
slightly poorer than of HPGe.
GR1-A® - Gamma Ray Spectrometer is a CZT detector manufactured by Kromek. Small size (25mm x
25mm x 63mm) and low weight (~60 grams) of GR1-A® make the detector ideal to be installed to a
drone and for aerial survey of gamma-emitting R & N agents (Figure 1). EOY has purchased a GR1-A®
to be connected to a drone and further establishing a new product called RanidFly. The software used
for operating the detector is developed by EOY. This detector has been chosen by EOY based on their
previous positive experiences of similar detector types.
Before installing GR1-A® CZT detector to a drone, a thorough validation procedure was executed,
covering essential factors and adequate statistics of analytical results. Pohjonen Group provided a
drone and necessary knowhow for flying it in this experiment. EOY has provided preliminary
information about the detector and drone and participated to writing the test plan.
R,N detector tests were conducted first in 20-23 November 2017 in Helsinki, Finland. The tests had
been planned according to standards ANSI N42.43, ANSI N42.34, IEC 62327, and IEC 62618 [1-4]. The
tests performed in November 2017 were diverse and fundamental and the following test report v1
(“D2.3 Triage verification facility - CZT (R&N) detector tests in lab and field, 20-23 November 2017,
Helsinki”) was a detailed description about the first validation attempt.
In the second tests in the laboratory in May 2018 and the following test report, the emphasis was in
parallel (repeat) measurements of fewer radiation sources, for achieving quantitative information
about the functionality of the CZT detector, instead of qualitative. Correct radionuclide identification
and repeatability of the measurements were the objects of this test series.
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©TOXI-triage Consortium 6 August 2019
Figure 1: GR1-A® - CZT Gamma Ray Spectrometer (www.kromek.com). The detector is a small sized (25mm x 25mm x
63mm) and its weight is only ~60 grams. Detection area (detection window) of GR1-A® CZT is 10 mm x 10 mm x 10 mm.
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3 Validation procedure
3.1 Environmental conditions before starting the tests
Environmental conditions should be selected according to parameters in Table 1: “Testing conditions
in laboratory”, while testing detector at the first phase in laboratory. Table 1 is modified from ANSI
N42.34, ANSI N42.43, IEC 62327 and IEC 62618 standards [1-4]. The values for temperature, humidity
and atmospheric pressure should be recorded during the tests. The unit Sievert (Sv) is used for
radiation dose throughout the validation procedure, instead of other commonly used unit Roentgen
(R), because Sievert is an SI-unit and it is newer than Roentgen. Only SI-units will be used throughout
the validation procedure.
Environmental factor Value
Temperature 18-25 °C
Humidity ≤ 75% RH
Atmospheric pressure 70-106.6 kPa (525-800 mm
of mercury at 0 °C)
Gamma background including
cosmic radiation
≤ 250 nSv/h
Electromagnetic field of external
origin
Natural conditions without
man-made generators
Magnetic induction of external
origin
Natural conditions without
man-made generators
Table 1. Testing conditions in laboratory (modified from ANSI N42.34, ANSI N42.43, IEC 62327, and IEC 62618).
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3.2 Physical and radiological demands for a mobile spectrometer
3.2.1 Physical requirements
If the mobile spectrometer undergoes crash, the components should not get separated, so mounting
technique is a very important factor in designation. Attention has to be paid for preventing instrument
from damaging during transit, and from mechanical shock and vibration.
3.2.2 Radiological requirements
a) The spectrometer is capable to store at least 8 h of measurement data, which contains
information as follows.
b) Each measurement data set or output set should contain the following information, described
in ANSI N42.42 [5]:
1. manufacturer name
2. instrument model
3. serial number
4. software version
5. instrument class (e.g., mobile)
6. the type of gamma detector (e.g., sodium iodide (NaI), Geiger Müller tube, cadmium-
zinc-telluride (CdZnTe, CZT)
7. date and time of measurement
8. measured background radiation levels (i.e., count rate)
9. measured gamma radiation level (i.e., count rate)
10. gamma-ray alarm indication
11. GPS-localization
12. (speed), or coordinates and time label
In addition, the data file should contain following information concerning nuclide
identification:
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13. unprocessed background spectrum
14. live time and real time for background spectrum
15. unprocessed measured spectrum
16. live time and real time for the measured spectrum
17. energy calibration for the measured spectrum
18. radionuclide identification results
19. confidence indicator, if provided
c) The spectrometer can store gamma photon count rate, combined with time and GPS data, and
it is capable of transferring data to an external device (like computer).
d) If the instrument cannot identify a radionuclide, an indication like “not identified” must be
given.
e) If the exposure rate is too high or low for identification, an indication for that must be given.
3.2.2.1 Test for verifying the functionality of the instrument
This test is performed to check, if the instrument fulfills the requirements described in 2.2.2
(Radiological requirements). The test results should be documented.
1. the spectrometer is visually checked
2. the documentation provided by manufacturer is reviewed and the specifications of
the spectrometer given by the manufacturer are verified
3. a 137Cs source is moved horizontally through the middle of the detection zone, with a
source-detector distance adequate to produce background count rate at least three
times of the background count rate
4. over-range indication mentioned above in 2.2.2 e) is tested as in section 2.3.1.4
5. the output data file is opened and it is verified, that the required data are contained
within the file
3.2.3 Alarm requirements
Any external alarm component, either visual or audible, should be tested before use. It should be
possible to test alarm features without any radiation source, e.g. lamp test. An option for switching
alarm indication (light or sound) on/off is needed. The spectrometer should also have ability to re-
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alarm without reset or acknowledge, after being activated, thus registrating several separate alarms.
All alarm indicators shall not be possible to be switched off at the same time.
3.2.3.1 Test for checking, that the spectrometer is functional even in alarm state
1. the spectrometer is induced to make an alarm with a radiation source
2. the alarm is silenced and it is verified that the visual alarm stays on
3. the radiation source is removed, but alarm is not acknowledged or reset
4. after delay time of 10 seconds , the spectrometer is re-induced to make an
alarm with the radiation source and the alarm state is verified from
spectrometer’s display
5. the radiation source is removed and alarm is acknowledged or reset
6. the saved alarm data files are checked to observe two separate alarms in
storage
3.2.4 Requirements for power source
The power source of the spectrometer depends on the drone where it will be attached to, and by the
testing time (November 2017), the technical details and capacities of the drone were not known.
Therefore, detailed requirements for power source cannot be given. The following requirements from
ANSI N42.34 and N42.43 are recommended to be reviewed, after properties of drone have been found
out:
The spectrometer should be able to utilize multiple power sources in operation. Batteries should be
easily changeable and widely available, like AA, 9V.
The requirements for different power sources are:
1. AC: single-phase AC supply voltage 100 V – 240 V, 47 Hz – 63 Hz [2]
2. DC: 11 V – 14.5 V [2], nominal 12 VDC [1] (nominal voltage 12 V)
3. Battery pack supplying 9 VDC to 14 VDC
4. A 12 VDC power supply working with utility power
5. Battery chargers fulfil the electrical standards of EU
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3.2.5 Requirements for energy range of the detector
The effective range for gamma photon energy should be at least from 40 keV to 3 MeV, and it is defined
by the manufacturer (EOY). For comparison, the required energy range in ANSI-standards is from 25
keV to 3 MeV [1] and from 40 keV to 3 MeV [2].
3.2.5.1 Test for energy range
The requirements for energy range are verified by evaluating the documents provided by
manufacturer. The results of this test are documented.
3.2.6 Requirements for communications protocol
The spectrometer should be able to send data to a computer or other external device via USB,
Ethernet, wireless or other technique. If wireless techniques are used, the data should be encrypted.
3.2.6.1 Test for communications protocol
The requirements for communications protocol are verified by evaluating information provided by
manufacturer, in EnviScreen data interface document.
3.2.7 Requirements for user interface
3.2.7.1 Test for the function of user interface
At least three different persons, having previous experience from similar instruments, should read the
instructions provided by manufacturer. Every test person should verify that the spectrometer fulfils
the requirements presented in 2.2.7.2 and 2.2.7.3. The existence of visual and warning indicators
(2.2.7.4 and 2.2.7.5) are verified by reviewing the manual, or if the manual does not exist, by following
functionality of measurement program from the display.
3.2.7.2 User/Routine mode
1. easy and user-friendly program structure
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2. radionuclide identification and categorization (e.g., nuclear, medical, industrial,
NORM) and confidence level for identification
3. save of identification data
4. saved measurement data is accessible
5. visual, acoustical, and optionally vibration alarm indications exist
6. both source indication alarm and personal protection safety alarm exist
7. alarm threshold levels are adjustable, for example via external PC
8. mapping in real time and alarm locations are accessible
9. data file transfer is allowed
10. possibility of using gloves, even weather-protective, has to be noted when designing
controls, switches, etc.
3.2.7.3 Supervisory-user/Restricted mode
The following procedures allowed for a supervisor-level user should be included in the technical
manual, provided by manufacturer:
1. measurement data settings, like nuclide library, peak fitting, integration time, etc.
are accessible
2. datalog is accessible
3. calibration information, either energy and/or efficiency, is accessible
3.2.7.4 Display and visual indicators
The following visual indicators should be present in the computer display connected to the
spectrometer:
1. gamma alarm
2. gamma counts per real-time, presented as strip-chart, water fall, etc.
3. saved measurement data
4. GPS data and alarm locations are presented as real-time mapping
5. excess amount of gamma counts is expressed as «over-range» or «high counts», or
similar
6. operating mode
7. operational status (normal/calibration needed/stabilization needed/other)
8. result of gamma emitter identification and if provided, a confidence indicator
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9. the detected radionuclide cannot be identified («unknown», «not identified», etc.)
10. too high gamma count rate for radionuclide identification
11. spectral display
3.2.7.5 Requirements for warning indicators
At least the following indications should be shown on the display:
1. detector failure condition
2. invalid or inacceptable energy stabilization
3. monitor failure
3.3 Radiological tests
3.3.1 Tests in laboratory
3.3.1.1 Background measurements
Before starting sample measurements, a background measurement is performed to ensure that the
radioactive background is at the level that agrees with Table 1 and it consists of natural background
radionuclides (40K, 232Th series, 238U series) only. In addition to the spectrometers to be validated, this
background measurement is also performed with another spectroscopic detector, like NaI or HPGe.
3.3.1.2 Test configuration and influencing parameters
Radiation sources used in tests should be traceable to an accredited organization, like NIST, NPL, or
similar. A spotlike radiation source, listed in Table 2 and example in Figure 2, is positioned in front of
the middle point of the detector window, with a source-detector distance that is adequate for
producing a count rate of at least three times the background count rate. Both static (the radiation
source stays still in the centre of the detection area) and dynamic (the radiation source is moved
horizontally along the centre line of the detection area) tests will be performed. In dynamic testing, a
minimum delay of 10 s is kept between the measurements and during that time, the radiation source
will be either moved so far from the detector, that its influence on the detector does not deviate from
the background radiation, or it will be shielded. For static test, the radiation source is not moved
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between the measurements of the series and the test time is 2 min. The selected positions and tracks
of the radiation sources during static and dynamic tests are marked for repeats.
Radionuclide Activity Physical half-life Gamma
energy (keV)
Gamma
intensity (%)
Sample
description
137Cs, Serial No. C-
148-20
25 kBq
(21.11.2017)
30.07 years 661.657 85.1 Standard
radiation source
241Am, CAL 2600 38 kBq
(21.11.2017)
432.2 years 59.5412 35.9 Standard
radiation source
57Co, E-20-31 1.6 kBq
(21.11.2017)
271.79 days 122.0614
136.4743
85.60
10.68
Standard
radiation source
60Co, E-20-32 16 kBq
(21.11.2017)
5.2714 years 1173.237
1332.501
99.9736
99.9856
Standard
radiation source
133Ba, D-71-7,
3/02
13 kBq
(21.11.2017)
10.51 years 356.017
80.997
302.853
62.05
34.06
18.33
Standard
radiation source
226Ra, No 743 37 kBq
(21.11.2017)
1600 years 186.211 3.59 Liquid in a closed
bottle
131I 26 MBq
(21.11.2017)
8.0207 days 364.489
636.989
284.305
80.185
81.7
7.17
6.14
2.62
Capsule in a
closed bottle
99mTc 125 kBq
(20.11.2017,
10:00 AM)
6.01 hours 140.511 89 Liquid in a closed
bottle
232Th 26 kBq 1.405 x 1010 years 63.83 0.263 Th-acetate
powder in a
closed bottle,
about 13 grams
238U There was no
100% pure 238U
available
4.468 x 109 years 49.55 0.064 Solid powder in a
closed bottle
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Radionuclide mixtures
DU, RLIAE222 Total U activity
of the sample is
64.01 kBq, of
which 2.85 kBq is
235U and 61.16
kBq 238U.
several, including
1001.03 (234mPa),
49.55 (238U)
0.837
(234mPa),
0.064 (238U)
Uranium dioxide
powder in a
closed bottle.
4.9551 g, of which
is 0.72% 235U, i.e.
0.0357 g of 235U.
HEU, RLRCC250 233U, 46 MBq 42.44 (233U) 0.0862 (233U) 0.1275 g of pure
solid 233U in a
closed bottle
WGPu, RLNBS204 239Pu, 240Pu,
241Pu, 242Pu,
238Pu (Original
arrival date:
10.3.1975,
original activity:
~560 MBq)
several, including
375.045 (239Pu),
45.242 (240Pu)
0.001554
(239Pu),
0.0450 (240Pu)
0.250 g of solid
plutonium sulfate
tetrahydrate in a
closed bottle.
91.574% 239Pu,
7.914% 240Pu,
0.468% 241Pu,
0.033% 242Pu,
0.011% 238Pu
(atom-
percentages)
NORM-sample
RLORE982/1-5,
containing 238U,
232Th, 226Ra, 228Ra,
222Rn, 210Pb, 210Po,
210Bi, 40K, etc.
210Bi: produces
Bremmstrahlung
with endpoint
energy of 1161
keV that increases
the detection limit
of other gamma
emitters in the
spectrum [7].
5 subsamples, in
total 920.680 g
→25 MBq
#
49.55 (238U),
1001.03 (234mPa)
63.83 (232Th),
186.211 (226Ra),
16.2 (228Ra)*, 511
(222Rn), 46.539
(210Pb), 803.10
(210Po), 1460.830
(40K)
0.064 (238U),
0.837
(234mPa),
0.263 (232Th),
3.59 (226Ra),
0.72 (228Ra)*,
0.076 (222Rn),
4.25 (210Pb),
0.00121
(210Po),
11 (40K)
Ore in closed
bottles
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* = not detectable with these gamma detectors to be tested due to low energy.
# = Note that if 226Ra is also present, the strongest gamma peaks of 226Ra (186,211 keV, I= 3,59%) and 235U will overlap in the gamma
spectrum. 226Ra has, however, other smaller gamma peaks (262,27 keV, I = 0,005%, 600,66 keV, I = 0,0005%) that can be searched in case
of mixed uranium and radium sample.
Source for gamma energies and intensities: http://nucleardata.nuclear.lu.se/toi/
Table 2. Radionuclide test samples used for validation.
Figure 2. Radiation source is positioned in the middle of the detection area of the detector window during
measurements. The source can be kept still in front of the detector window (static testing) or moved either from far to
near, or vice versa (dynamic testing). Thus start position and final position can change places depending on the test.
3.3.1.3 Criteria for the test results
From the recorded results, mean value, standard deviation, and coefficient of variation (COV) will be
calculated for dose rate and/or count rate. COV should be ≤ 12 % for gamma dose rate and count rate
and in the case of COV exceeding 12 %, the distance between radiation source and detector should be
decreased for improving the counting statistics. The acceptable range of dose rate and count rate is
±15 % of the calculated mean value.
The acceptable amount for false alarms or false identifications is less than 1:1000, without the
radiation source in the detection zone.
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3.3.1.4 Over-range condition: indication and testing
If the measurable radioactivity level exceeds the exposure limit given by the detector manufacturer,
the detector is in over-range state. This prevents detector from fully registrating all radiation events.
The instrument should be designed to give a visual sign when being at over-range state, to inform that
it is not functioning properly, even if the alarm is reset by a user. The time between decreasing
radiation field to the background level and return of the detector from the alarm state to the non-
alarm state (without any resetting or switching off by a user) should be 2 min or less.
The over-range actions are tested as follows:
A 137Cs radiation source (Table 2) is positioned to produce a radiation field to 90% of the maximum
exposure stated by the detector manufacturer. The radiation source is kept for 2 min in that position
and the over-range state is observed from the display. The over-range state should continue until
removing the radiation source and exposure level returning to the background level. Before removing
the radiation source, the over-range alarm is reset/acknowledged, and the visual indication of over-
range state should still be observable. After removing the radiation source, the time interval between
removal and the detector being fully operational again, is measured. This test is performed 8 times
and the functionality of the detector is verified, if the instrument identifies correctly 137Cs in 8 out of 8
trials and if time interval between alarm- and non-alarm states is 2 min or less, after removing the
radiation source from proximity of the detector.
3.3.1.5 Detector in mobile use, background changes
Different construction materials, roads or landfills may give different radioactive background to the
mobile detector, and the background level may change widely. The detector should give a warning
indication, if the background change is significant enough to effect on alarm probability of the detector,
but still no actual alarm should appear because of changing background.
Testing the effect of increasing/decreasing background on the detection:
1. First, the spectrometer is started to measure at normal background level for 2 min.
2. A NORM-radiation source (Table 2), that is used here as an artificial background radiation, is
moved vertically from far (where only normal ambient background level is observed)
towards the middle point of the detection area with a final source-detector distance, that
produces 3 times higher count rate than ambient background.
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3. The transferring time is 30 s.
4. Either detector or NORM-source can be transferred this way, to increase the radiation level
from NORM.
5. During transfer time, the spectrometer may identify the NORM, but any kind of alarm should
not be activated.
6. The instrument is allowed to measure the artificial background for 2 min. Then either the
detector or the NORM-source is moved to far (where only ambient background level is
observed) during 30 s.
7. The spectrometer is allowed to measure normal ambient background level for 2 min.
8. This test is repeated for two times, and no alarms should be activated due to NORM
radiation and no other radionuclides than NORM should be identified during all three
measurements.
9. The test can also be performed vice versa, by starting with the NORM source being at the
closest position in respect to the detector (producing 3 times higher radiation level
compared to the ambient background), and then increasing the source-detector distance.
Testing the changing background with both NORM- and 137Cs-sources:
The test is otherwise similar with the test for NORM-source only (described above), but during the 30
s transferring time between the far and close source-detector distance, a 137Cs-source (Table 2) is
moved (similarly with 2.2.2.1) through the middle point of the detection zone and the results are
recorded. At the end of 2 min exposure to artificial NORM-background (closest distance between
NORM-sample and the detector), the 137Cs-source is moved again across the detection area. The test
is repeated three times, thus the test set contains six dynamic tests of 137Cs. The test is completed, if
all six 137Cs-tests cause alarm.
3.3.1.6 Identification of radionuclides
A spectrometer should be able to identify and classify the identified radionuclides, in extent that is
stated by the spectrometer manufacturer. However, the minimum requirement of identifiable
radionuclides is listed in Table 3. Classification of the radionuclides is based on either the categorization
by ANSI [1] or by IAEA (2005) [6]. The categories are neither all-inclusive nor restricted, one
radionuclide can belong to several groups. Classification by IAEA [6] is made as follows:
1 Radioisotope thermoelectric generators (RTGs), Irradiators, Teletherapy sources, Fixed, multi-
beam teletherapy (gamma knife) sources
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2 Industrial gamma radiography sources, High/medium dose rate brachytherapy sources
3 Fixed industrial gauges that incorporate high activity sources, Well logging gauges
4 Low dose rate brachytherapy sources (except eye plaques and permanent implants), Industrial
gauges that do not incorporate high activity sources, Bone densitometers, Static eliminators
5 Low dose rate brachytherapy eye plaques and permanent implant sources, X ray fluorescence
(XRF) devices, Electron capture devices, Mossbauer spectrometry sources, Positron emission
tomography (PET) check sources
Category 1 represents the possibly most dangerous radioactive sources, Category 5 is not dangerous,
and all other categories are in between these two dangerous levels. The verification of radionuclide
list and classification can be made by checking the documents given by the manufacturer, and the
radionuclide identification library of the spectrometer.
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Radionuclide Category, according to ANSI N42.34 [1]
Category, 1-5 [6]
241Am Industrial 4, 5 133Ba Industrial 2 57Co Industrial 5 60Co Industrial 1, 2, 3, 4 137Cs Industrial 1, 2, 3, 4 67Ga Medical - 131I Medical 4
99mTc Medical - 201Tl Medical -
226Ra Industrial 4, 5 232Th NORM NORM 192Ir Industrial 2, 4
238U (DU) SNM SNM 235U (HEU) SNM SNM
239Pu (WGPu) SNM SNM Table 3. A nuclide library that a gamma spectrometer should be able to identify at least. The classification of the
radionuclides has been published by IAEA Safety Guide No. RS-G-1.9 (2005) [6].
Identification of single radionuclides:
The spectrometer should be able to identify 241Am, 133Ba, 60Co, 137Cs, 67Ga, 131I, 99mTc, 201Tl, 226Ra, 232Th,
238U (DU), 235U (HEU) and 239Pu (WGPu). The identification tests are performed both in dynamic and
static mode, and with radiation sources from Table 2.
Dynamic testing
The radiation source is moved horizontally through detection area at appropriate source-detector
distance. Identification results and confidence indicators (if available) are stored. Alarm function is
reset. This test is repeated 4 times and there should be a 10 s delay between the tests, when the
radiation source is at the distance where it does not have influence on the detector. The test series of
5 repeats is performed only for two radionuclides: a low gamma energy source 133Ba and a high gamma
energy source 60Co.
Static testing
A radiation source is positioned to middle point of detection window with appropriate source detector
distance. The measurement time is 2 min. Identification results and confidence indicators (if available)
are stored. Alarm function is reset. The measurement is repeated 4 more times. The source is not
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moved between 10 tests. The test series of 5 repeats is performed for all radiation sources in Table 2,
except NORM-source, and medical nuclides 99mTc and 131I are measured both as shielded and
unshielded.
Both dynamic and static test results are accepted, if the detector identifies the radionuclide correctly
in 5 out of 5 parallel static tests and 8 out of 8 dynamic tests per radionuclide. For medical nuclides,
the acceptable identification amount is 10 out of 10 parallel static tests (5 unshielded and 5 shielded).
Daughter nuclides and other accepted impurities
SNMs are mixtures of several isotopes of Pu, U, Am, and daughters (decay products) of U. Also NORMs
contain a mixture of several radionuclides and decay products of 238U. These mixtures often produce
complex gamma spectra with interfering or overlapping peaks that cannot be separated from each
other or identified as a single isotope. Also combinations of medical radionuclides and SNM give
identification result for several radionuclides with both medical and SNM category. In these cases,
several options can be accepted as correct identification. Further confirmatory analysis of spectrum or
sample (if available) is recommended, if exact composition of radionuclides is needed. For example, if
239Pu is present in gamma spectrum, then a more detailed analysis of Pu isotope fractions in a particular
sample is needed for telling if it is WGPu, RGPu or other.
Certain simplifications make categorization and identification of radionuclides easier, reducing false
alarms and leaving the possibility for later further examinations open, if needed. The requirements are
summarized below in the next box and in Table 4.
Special requirements in categorization of iodine, uranium, plutonium, and thorium [3]
The manufacturer and user can make an agreement, that
1. any iodine isotope detected can be classified as “medical iodine”
2. any uranium isotope detected can be classified as “uranium”
3. any plutonium isotope detected can be classified as “nuclear plutonium”
4. any 232Th and its decay product detected can be classified as “NORM thorium”
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Radiation source Required radionuclides Probable daughters or impurities
201Tl 201Tl 202Tl
Natural uranium (uranium ore) 238U 226Ra
DU 238U 235U, 226Ra
RGPu 239Pu 242Pu, 241Pu, 240Pu, 238Pu, 241Am,
237U, 242Pa, 233U, 252Cf, 249Cf, RGPu,
Plutonium
WGPu 239Pu 242Pu, 241Pu, 240Pu, 238Pu, 241Am,
237U, 242Pa, 233U, 252Cf, 249Cf,
WGPu, Plutonium
HEU 235U 238U, 234mPa, HEU, Uranium
(226Ra + 232Th) + WGPu 239Pu 242Pu, 241Pu, 240Pu, 238Pu, 241Am,
237U, 242Pa, 233U, 252Cf, 249Cf, 232U,
214Pb, 214Bi, 228Th, 232Th, 226Ra,
WGPu, Plutonium
(226Ra + 232Th) + HEU 235U 238U, 234mPa, 228Th, 232U, 214Bi,
214Pb, 232Th, 226Ra, HEU, Uranium
131I + WGPu 239Pu + 131I 242Pu, 241Pu, 240Pu, 238Pu, 241Am,
237U, 242Pa, 233U, 252Cf, 249Cf,
WGPu, Plutonium
99mTc + HEU 235U + 99mTc 238U, 234mPa, 99Mo, HEU, Uranium
99mTc 99mTc 99Mo
232Th 232Th 228Th, 232U
226Ra 226Ra 214Bi, 214Pb
241Am (smoke detectors, gauging
sources, and other sources that
don’t contain plutonium)
241Am RGPu and WGPu both contain
241Am. It is difficult to distinguish
RGPu from WGPu by
spectroscopy. False plutonium
identification can lead to
operational problems.
Table 4. Acceptable daughter nuclides and expected impurities [3][4].
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Identification of shielded single radionuclides
Radionuclides have to be measured as shielded in certain situations, for radioprotectional and
spectroscopically reasons. Shielding is used for minimizing radiation exposure from highly active
source, or if the radiation source contains some isotope emitting very penetrating beta or gamma
radiation. Shielding is also needed to avoid false radionuclide identification due to one strong
overlapping peak in the produced spectrum. Shielding reduces the influence of certain isotope, whose
presence and quantity is not as important to know as some other isotope. For example, RGPu contains
241Am, that emits gamma radiation of 59.54 keV with much higher intensity than gamma emissions of
239Pu and 240Pu. On the other hand, the low energy of 241Am gamma emission enables blocking of these
gamma photons with only 1.2 mm of lead. It is therefore necessary to shield the RGPu source before
the measurements, for reducing the interference from 241Am in the gamma spectrum. The same goes
with WGPu.
The capability of the spectrometer to identify shielded radioactive material is investigated in the
following test, performed with 60Co and 137Cs (Table 2), which are enclosed with 1 cm of steel and 8 cm
(10%) of HDPE. Steel and HDPE form a mixed shielding material in this test. Testing of shielded
radionuclides’ identification goes otherwise similarly as testing of single radionuclides – 5 dynamic and
5 static tests for both 60Co and 137Cs sources – but the radioactive source is shielded with a steel and
HDPE container during testing. The test results give information about the capability of the
spectrometer for identifying shielded sources, but there is no pass/fail criteria based on the test
measurements.
Identification of mixed radionuclides
The spectrometer should be able to identify several radionuclides simultaneously. This property is
needed because medical nuclides are used for masking nuclear material and HEU can be masked with
NORM radionuclides for smuggling. The ability for identifying mixed radionuclides can be tested as
follows:
Radionuclide sources are measured as pairs
137Cs and DU
99mTc and HEU
131I and WGPu
(NORM and HEU)
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Each radiation source pair is positioned in one’s turn to the middle point of the detection window, with
an initial source-detector distance of 50 cm. The sources have to be positioned the way that they do
not shield each other. The exposure rate (or count rate) from this distance is recorded.
The dynamic test is performed by moving the radiation source pair horizontally across the detection
area. Identification results and confidence indicators (if possible) are stored. Alarm is reset after the
measurement. This test is repeated 4 more times and a minimum delay time of 10 s is kept between
the measurements, during this delay the sources are kept at the distance where they don’t have an
effect on background count rate. The dynamic test procedure of 5 parallel measurements is performed
with all source pairs, except the NORM-containing pair.
For static test, a source pair is positioned in the middle of the detection window, at appropriate source-
detector distance. The source pair is measured during 2 min counting time. Identification results and
confidence indicators are stored. The alarm is reset. The source pair is not moved and 4 more
measurements are performed, to produce 5 parallel measurements. The test is repeated for all other
source pairs, except the NORM-containing pair.
The spectrometer’s ability to identify simultaneously artificial and NORM-nuclides is tested by
positioning the source pair NORM + x to appropriate distance from the detector. To simulate the
common matrix of NORM-nuclides, 25 kg of KCl is located to the distance that produces a clear gamma
peak of 1460 keV. Instead of KCl, some other NORM-rich source can be used for producing the same
gamma peak of 40K. The same 5 dynamic and 5 static tests are performed with the NORM + x pair, as
with other source pairs.
The tests are accepted, if the spectrometer makes a correct identification in 5 out of 5 tests, both static
and dynamic.
Radionuclides not in the nuclide library
The spectrometer should be able to express the unidentifiable (within the confidence limits defined by
the manufacturer) radiation source as “unknown”, “not in library”, or similar. Following dynamic and
static tests are performed for checking the identification of nuclide not in library:
A radiation source is selected from Table 2. It is recommended to choose single energy or simple
spectrum source (137Cs, for example). The nuclide identification library of the spectrometer is edited,
according to the instructions by the manufacturer, and the selected radiation source is removed from
the list of identification.
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The dynamic test is performed by moving the radiation source horizontally with appropriate source-
detector distance, through the middle of the detection zone. The identification results and the
confidence indicator (if available) are stored. The alarm is reset. The test is repeated 4 more times, and
between the tests a minimum of 10 s is kept as delay time, while the radiation source is kept away or
shielded from affecting the background count rate.
For static test, the radiation source is positioned in the middle of the detection zone with appropriate
source-detector distance. The measurement time is 2 min. The identification results and confidence
indicators (if applicable) are stored and the alarm is reset. The measurement is repeated 4 more times,
without removing the radiation source from its position.
The test results are acceptable, if they agree with the stated indication requirements.
3.3.1.7 Radionuclide identification in later tests in May 2018
Nuclide identification test was greatly simplified from the previous test procedure in November 2017.
Five different radiation sources were selected (Table 5), the selection was based on either adequate
activity of the radiation source (preferably 1 MBq or more) or in the case of 235U (HEU), better suitability
of the radiation source due to nuclide library content of the spectrometer.
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Radionuclide/mixture
Activity Half-life Gamma energy (keV) Gamma intensity (%)
241Am 1 MBq 432.2 years 59.5412 35.9
60Co 9.16 MBq 5.2714 years 1173.237
1332.501
99.9736
99.9856
NORM
RLORE982/1-5
25 MBq (contains 238U, 232Th, 226Ra, 228Ra, 222Rn, 210Pb, 210Po, 210Bi, 40K,
etc.)
#
49.55 (238U),
1001.03 (234mPa)
63.83 (232Th), 186.211
(226Ra), 16.2 (228Ra)*,
511 (222Rn),
46.539 (210Pb), 803.10
(210Po), 1460.830 (40K)
0.064 (238U),
0.837 (234mPa),
0.263 (232Th),
3.59 (226Ra),
0.72 (228Ra)*,
0.076 (222Rn),
4.25 (210Pb),
0.00121 (210Po),
11 (40K)
WGPu
RLNBS204
239Pu, 240Pu, 241Pu, 242Pu, 238Pu
(Original arrival
date: 10.3.1975,
original activity:
~560 MBq)
several, including 375.045
(239Pu),
413.707 (239Pu),
51.624 (239Pu),
45.242 (240Pu)
59.5412 (241Am)¤
0.001554 (239Pu),
0.001466 (239Pu),
0.0271 (239Pu),
0.0450 (240Pu),
35.9 (241Am)¤
235U (HEU) 58 kBq 185.712
143.764
163.358
205.309
57.2
10.96
5.08
5.01
# = Note that if 226Ra is also present, the strongest gamma peaks of 226Ra (186.211 keV, I=3.59%) and 235U (185.712 keV, I=57.2%) will overlap
in the gamma spectrum. 226Ra has, however, other smaller gamma peaks (262.27 keV, I = 0.005%, 600.66 keV, I = 0.0005%) that can be searched
in case of mixed uranium and radium sample.
¤ = 241Am is a daughter nuclide of 241Pu. The stronger gamma emission of 241Am will dominate the weaker gamma emissions of Pu isotopes in
the gamma spectrum of WGPu, unless the WGPu source is shielded.
* = not detectable with these gamma detectors to be tested due to low energy.
Table 5. Radiation sources used in tests in May 2018.
3.4 Requirements for environmental performance
The functionality of the detectors with varying temperatures and relative air humidity will be tested
separately later. These tests will be performed in environmental chambers having controllable and
adjustable temperature and relative humidity, most likely at Finnish Meteorological Institute. The tests
for environmental performance will be performed adopting IEC 62706 (2012) [9].
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3.5 Requirements for mechanical performance
The microphonic requirements for devices like a mobile spectrometer are defined in IEC 62706 [7].
These include the stability of the spectrometer against low-intensity impact from sharp contact with
hard surfaces and stability against functional and mechanical changes caused by vibration. These
properties will be tested and observed in practise during field tests.
3.6 Tests in field
Provided that the previous tests in laboratory described in 2.3 are accepted, the functionality of the
spectrometer can be verified in outdoors field testing. Environmental conditions during the field test
should fill the requirements listed in Table 6.
Environmental factor Value
Temperature 10 - 35 °C
Atmospheric pressure 70-106.6 kPa (525-800 mm of mercury at 0 °C)
Humidity 65 - 85% RH
Wind speed 0 – 10 m/s
Gamma background including cosmic
radiation
≤ 250 nSv/h
Electromagnetic field of external origin Natural conditions without man-made generators
Magnetic induction of external origin Natural conditions without man-made generators
Table 6. Probable environmental conditions during field testing.
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3.6.1 Preliminary test plan for field
A spectroscopic detector (NaI, HPGe, etc.) is used to ensure that only NORM and cosmogenic
radionuclides (40K, 232Th series, 238U series) are present forming the background activity in the testing
area.
One or two radiation sources of artificial radionuclides, containing enough radioactivity to be detected
from tens of meters distance, are selected. Most probably these will be 60Co and 131I sources. Necessary
formalities and precautions will be taken care of for transferring the sources from laboratory to field
in good time.
The varying parameters in field testing are (Table 7):
a) source-detector distance (three different distances),
b) radiation sources (two different sources),
c) background radioactivity (two different: normal background and NORM-rich background,
simulated with a NORM-source having adequate activity)
Increasing distance between the radiation source and detector, i.e. the altitude of the RPAS from the
ground, changes the incoming angle of gamma radiation to the detector. In other words, a greater part
of the gamma photons pass by the detector, with a longer source-detector distance. For this reason,
the response from gamma radiation source, expressed as count rate, decreases with increasing source-
detector distance. On the other hand, the energy resolution of the detector increases with increasing
source-detector distance, since the incoming angle of gamma radiation is smaller when the distance is
larger between the source and the detector.
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Radioactive source Distance source –
detector/altitude
Background
activity (NORM)
The shape of flying
track/course
60Co small Low
medium Low
large Low
small High
medium High
large High
131I small Low
medium Low
large Low
small High
medium High
large High
Table 7. Parameter combinations to be tested in the first field exercise (November 2017).
The detector is mounted to a drone/RPAS and the drone system is started. The first radiation source
is positioned to an open area. The drone is adjusted to fly on the closest source-detector distance, and
the detector is switched on. A dynamic measurement is performed while the drone is flying over the
radiation source/circulating around the radiation source. Dose rate/count rate/activity is stored. The
identification results and confidence indicators (if applicable) are stored and the alarm is reset. The
dynamic measurement is repeated 9 more times. Then the drone is lifted to the medium altitude, and
similar measurements are performed, and then the 10 parallel measurements are performed with the
largest altitude.
A similar series of ten parallel measurements are performed for the second radiation source with three
different altitudes. After that, a NORM-source having adequate activity concentration to produce a
clear gamma peak of 1460 keV, is positioned close to the first radiation source, to simulate NORM-rich
environment. Drone is sent flying on the closest source-detector distance. Again dynamic
measurement is performed while the drone is flying over the radiation source/circulating around the
radiation source. Dose rate/count rate/activity is stored. The identification results and confidence
indicators (if applicable) are stored and the alarm is reset. The dynamic measurement is repeated 9
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more times. Then the drone is lifted to the medium altitude, and similar measurements are performed,
and then the measurements are performed with the largest altitude. Similar measurements are
performed with both radiation sources (sources separately, not combined) having NORM source in
proximity, with three different altitudes.
The previous planned field test order and amount of repeats may be changed during the tests when it
is seen in practice, what is possible and what is not.
Each measurement listed in Table 7 – having a certain combination of detector distance and
background level - will be repeated 10 times, producing a total of 120 results. At least one spectrum
of 10 parallel measurements is stored. From the recorded results, mean value, standard deviation, and
coefficient of variation (COV) will be calculated for dose rate and/or count rate. COV should be ≤ 12%
for gamma dose rate and count rate and in the case of COV exceeding 12%, the distance between
radiation source and detector should be decreased for improving the counting statistics. The
acceptable range of dose rate and count rate is ±15% of the calculated mean value.
3. Conclusions
Performance of the CZT detector was evaluated based on the laboratory tests at UH and field tests in
Helsinki. The test plan was modified before and during the first tests in 2017 keeping in mind
maintaining the reliability of the validation results. In the next tests in May 2018 the focus was mainly
on correct identification of radionuclides. All tests gave valuable preliminary information about the
capacity of the RN detector and the planned program might be used later as modified for testing the
ready product “RanidFly” of EOY.
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References
[1] ANSI N42.34 American National Standard Performance Criteria for Hand-Held Instruments for the Detection and Identification of Radionuclides. IEEE Standard Association (2006).
[2] ANSI N42.43-2016 (Revision of ANSI N42.43-2006). IEEE Standard Association. American National Standard Performance Criteria for Mobile and Transportable Radiation Monitors Used for Homeland Security. Accredited by the American National Standards Institute, sponsored by the National Committee on Radiation Instrumentation, N42.
[3] IEC 62327. Radiation protection instrumentation – Hand-held instruments for the detection and identification of radionuclides and for the indication of ambient dose equivalent rate from proton radiation. International Electrotechnical Commission, Geneva, Switzerland (2006).
[4] IEC 62618. Radiation protection instrumentation – Spectroscopy-based alarming Personal Radiation Detectors (SPRD) for the detection of illicit trafficking of radioactive material. International Electrotechnical Commission, Geneva, Switzerland (2013).
[5] ANSI N42.42-2012 - American National Standard Data Format for Radiation Detectors Used for Homeland Security. Accredited by the American National Standards Institute.
[6] Categorization of Radioactive Sources. IAEA Safety Standard Series No. RS-G-1.9, International Atomic Energy Agency, Vienna 2005.
[7] G.Lutter, I. Vandael Schreurs, T. Croymans, W. Schroeyers, S. Schreurs, M. Hult, G. Marissens, H. Stroh, F. Tzika. A low-energy set-up for gamma-ray spectrometry of NORM tailored to the needs of a secondary smelting facility. Applied Radiation and Isotopes 126, August 2017, 296-299.
[8] Environics Oy. Nuclide identification in RanidPro200. Description 21.11.2011.
[9] Radiation protection instrumentation - Environmental, electromagnetic and mechanical performance requirements. IEC 62706 (2012).
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