Guest Editorial by Dr. Sabatino Nacson, CTO, Teknoscan Systems Inc.
Customs and Border protection agencies worldwide are charged with protecting the public against terrorist attacks, and one widely recognized vulnerability for entry of threat substances is through seaports.
Millions of containers arrive at a country’s seaports each year, and managing this large volume of maritime cargo requires a large manpower force, advanced intelligence, and effective inspection capabilities.
An effective inspection process includes screening shipping documentation and origin information, nonintrusive inspections, and physical examinations of cargo.
The most widely used nonintrusive inspection is X-ray imaging of containers, which looks for anomalies in the cargo and unusual object images in various areas in the container.
This process is time-consuming, as images are frequently not clear enough to identify hidden objects which can be easily concealed in organic-based materials.
Additionally, as geopolitical tensions rise globally, customs and border protection agencies must be alert for the potential transport of chemical warfare agents (CWAs), as their threats of use by individual terrorist groups have not diminished.
Chemical terrorism events, war conflicts, or other emergencies connected with misuse of leakage of CWAs could cause large-scale contamination in both soil and air – and affect millions of people.
(Learn more about the continually evolving and advancing Teknoscan solutions for screening containers, ULD3 air cargo, vehicles, boxes, bags, mail delivery items, people, and more. Courtesy of TeknoScan and YouTube.)
Any ship arriving at a seaport could potentially be transporting a container with enclosed chemical agents that could easily be released by remote detonation upon arrival or during the unloading of the container.
Many technologies have been applied to the rapid detection of CWAs but have not been used in the inspection process of marine containers.
This piece advocates for the capability of direct detection of CWA simulants in marine containers (also called sea containers), which is also applicable in screening air cargo containers.
Ion mobility spectrometer (Courtesy of TeknoScan Systems Inc.)
The technology is based on TeknoScan’s Ion mobility spectrometer with a fast-polarity switch for detecting positive and negative ions.
Ion mobility spectrometer units perform fast analysis (in 20 seconds) and internal secondary validation (ISV) GC analysis.
Gas chromatograph-dual polarity ion mobility spectrometry is widely used to detect explosive materials, illicit drugs, and human trafficking in maritime cargo containers.
Detection
To demonstrate the approach, Teknoscan Systems Inc. analyzed ten CWA simulants and studied the results of vapor sampling and the analysis of two examples, dipropylene glycol methyl ether (DPGME) and diethyl methyl phosphate (DEMP).
Measurements were carried out at various soak times at temperatures varying from 10-15oC inside the container.
The detector unit is based on a fast ion mobility spectrometer with an internal GC separator for dealing with complex samples acquired when screening air cargo and marine containers.
The analysis was executed using a chemically treated sample card to collect and concentrate both vapors and particulates of threat substances.
A handheld sampler unit containing a Lithium battery and bottom air jets was used to assist in dislodging particulates adhering to surfaces and agitating the air inside an enclosure to induce airborne particulates.
The front opening accommodates the sample card, all types of particulate filters 30mm and 45mm diameters can also be accommodated.
The sample card was next inserted into a desorption module, where the sample was evaporated into a primary short column.
The column is resistively heated to vaporize the concentrated sample into the analytical GC column, or part of the sample is directed into the ionization source of the IMS detector, this is schematically shown in Figure 1.
Detection limits for threat substances like explosives and narcotics vary from sub-nanogram to 5ng deposited on the sample card from a neat standard solution. The sensitivity is maintained on actual samples due to the instrument’s front-end GC separation and built-in sample processing methodology.
Most simulants (including real CW agents) form the monomer and dimer peaks in chemical ionization ion mobility spectrometry for a single GC peak. And this was used to identify the substance based on both GC peak and reduced mobility constants.
Sample preparation of the simulant involved diluting pure simulant with methanol to make a solution of 60% simulant in methanol. A 1ml volume of the diluted solution was deposited on a coffee filter of roughly 10cm diameter.
The filter was placed halfway into the 20 ft container on a cardboard box. The container walls and floor were covered with Kraft paper to reduce contamination (it also acted as an absorber of evaporating simulant into the air space of the container.
All simulant solutions were purchased from Sigma-Aldrich with high purity (98-99%), with the exemption of diisopropyl methylphosphonate which was purchased from Cerilliant. Methanol was HPLC grade purchased from Caledon Chemicals, Ontario.
Table 1 shows the list of CWA simulants programmed in the detection system.
TABLE 1 CWA Simulants Detection Parameters |
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| Simulant | GC retention time (seconds) | Detection Mode | Drift Time | Reduced Mobility cm2/V.sec |
| m.sec | ||||
| DE2MP | 44 | Positive | 7.896 | 1.022 |
| Diethyl 2-methylallylphosphonate | ||||
| DE2MP | 44 | Positive | 5.654 | 1.428 |
| DE2MP | 44 | Negative | 5.044 | 1.606 |
| DE2PEP | 86 | Positive | 9.3 | 0.868 |
| Diethyl 2-phenylethylphosphonate | ||||
| DE2PEP | 86 | Positive | 6.27 | 1.288 |
| DE2PEP | 86 | Negative | 5.916 | 1.369 |
| DE2OBP | 58 | Positive | 5.869 | 1.376 |
| Diethyl 2-oxobutylphosphonate | ||||
| DE2OBP | 58 | Positive | 8.16 | 0.989 |
| DE2OBP | 58 | Negative | 5.62 | 1.441 |
| Methyl Salicylate | 78 | Negative | 5.632 | 1.438 |
| Methyl Salicylate | 78 | Positive | 5.796 | 1.393 |
| DIMP | 32 | Positive | 7.747 | 1.042 |
| Diso-propyl phosphonate | ||||
| DIMP | 32 | Positive | 5.5 | 1.468 |
| DEEP | 35 | Positive | 7.214 | 1.119 |
| Diethyl ethyl phosphonate | ||||
| DEEP | 35 | Positive | 5.29 | 1.526 |
| DEMP | 27 | Positive | 5.17 | 1.562 |
| Diethyl methyl phosphonate | ||||
| DEMP | 27 | Positive | 6.858 | 1.177 |
| DEDFMP | 34 | Positive | 7.216 | 1.119 |
| Diethyl difluoro-methyl phosphonate | ||||
| DEDFMP | 34 | Positive | 5.295 | 1.525 |
| Ammonium Nitrate (Explosive) | 30 | Negative | 3.9 | 2.079 |
| TNT (Explosive) | 81 | Negative | 5.259 | 1.54 |
| Triethyl Phosphate | 38 | Positive | 7.484 | 1.079 |
| Triethyl Phosphate | 38 | Positive | 5.532 | 1.459 |
| Trimethyl Phosphate | 21 | Positive | 6.101 | 1.323 |
| Trimethyl Phosphate | 21 | Positive | 4.84 | 1.668 |
| DPGME | 107 | Positive | 7.189 | 1.122 |
| Dipropylene glycol methyl ether | ||||
| DPGME | 23 | Positive | 5.202 | 1.552 |
*Assignment Positive Mode: Monomer MH+ ion and Dimer ion M2H+
*Assignment Negative Mode: M– ion and clustering with dopant reagent. Ammonium nitrate is ionized by dissociative electron capture to form NO3– peak and its hydrated ions.
2.4 Container Sampling
A probe attached to the hand-held sampler is inserted through a gap between the gasket and the door. A clean sample card is inserted in the sampler, and 1 minute of sampling is executed by pressing the button on the handle of the sampler to activate the aspiration of the sample.
The aspirated sample is concentrated on the solid-phase extraction film coating on the sample card.
The sample card is removed and inserted into the analyzer desorber module as shown in Figure 2.
The sampling flow rate is typically 100L/min, with collection efficiency ranging from 10-50% depending on the type of substance being sampled.
Another method of nonintrusive sampling of the container is to connect a magnetic latch to the air vent and sample the air at a flow rate of 1000L/min. Each container typically has two air vents, one on the side of the door and one at the back.
3. Soak Time in the Container
After placing the wet filter in the container, air samples were withdrawn with the hand-held sampler at various intervals. The outside temperature in North of Toronto was relatively cool, varying from the morning at 10oC to 15oC in the late afternoon.
The test continued the next day, and the measurements’ data as a function of soak time are plotted in Figure 3 for CWA simulants DPGME and diethyl methyl phosphonate (DEMP).
Vapor buildup was relatively quick in 100 minutes, and the next set of measurements was done later, showing a clear decrease in concentration inside the container. DPGME concentration continued to decrease over time, but still the vapor was detected even after approximately 26.7 hours.
DEMP concentration remained steady but decreased after roughly 20 hours of incubation or soak time.
Modeling the evaporation of DPGME based on its vapor pressure at inside container temperature produced roughly 2.4ng/sec evaporation rate into a container volume of 33m3 at different times.
For example, after 2 hours, concentration buildup inside the container would be roughly 0.5ng/L, assuming no losses to the walls and surrounding surfaces.
The signal obtained after 2 hours was 299dc or the equivalent of 10ng (see calibration curve). The sampling flow rate was at 100L/min, and sampling done in 1 minute with a collection efficiency of approximately 10% would mean the vapor concentration of DPGME at roughly 1ng/L, which is in close agreement with the predicted concentration from the model.
At these low concentration levels, there are no concerns with EPA regulations and exposure limits.
This work demonstrates the importance of sampling and detecting threat chemicals that could be transported in a marine container.
Furthermore, sample cards allow for rapid purging and heating of contaminated sample card and regeneration of active sites (utilizing TeknoScan SCC-1000 Sample Cleaner Unit), which cleans five sample cards in 3 minutes, so they require no consumables.
(See how TeknoScan’s Hand-Held Sampler allows users to collect air samples from marine, sea, air, or other containers, vehicles, areas, enclosures, skids, packages, or even hard-to-reach surfaces where swabbing is not a viable approach. Air samples from an object, vehicle, package, pallet, or person are drawn through a TeknoScan sample card for analysis. Courtesy of TeknoScan and YouTube.)
Conclusion
Present GC-IMS technology could better enable U.S. Customs and Border Protection (CBP) Agents with the ability to rapidly detect and identify explosives, illicit drugs, and chemical threats during cargo inspections.
Based on the mass volume of cargo containers entering the country annually, I believe that concealed CWP agents within maritime cargo shipments pose the highest risk of chemical weapons entering the United States.
Integrating intelligence information, X-ray imaging, and chemical detection as a primary or secondary inspection will provide the most benefit and needed security at a seaport.
About the Author
Dr. Sabatino Nacson, B.Sc., M.Eng., Ph.D., is a world leader in new product development for the trace detection industry and has more than 25 years of experience in analytical chemistry and instrument development, including explosives, drugs, chemicals, pharmaceuticals, chemical warfare, and biological agents.
As TeknoScan’s CTO, Dr. Nacson has demonstrated the leadership and experience in worldwide chemical trace detection required of a first-rank company.
Dr. Nacson has developed and introduced scanning and security products, having achieved $1 billion in international sales (all figures US).
His products have covered various applications from security, defense, and life sciences to environmental and industrial processes.
Law enforcement agencies such as the FBI, ATF and RCMP have routinely sought his expertise, along with several other governments.
TeknoScan Systems is currently focused on developing and deploying its advanced Trace Chemical Detection (TCD) solutions to quickly detect and identify explosives, drugs, and other contraband in cargo containers, which makes 100 percent cargo inspection requirements achievable.
TeknoScan Systems’ state-of-the-art award-winning patented technologies detect and identify banned or hazardous materials through its sampling and analysis of trace vapors and particles in the air or on surfaces.
TeknoScan’s advanced sampling and analyzing technologies rapidly and reliably detect and identify organic compounds such as explosives, drugs, and other target substances.
TeknoScan Systems Returns to Compete in 2023 ‘ASTORS’ Homeland Security Awards
American Security Today’s Annual ‘ASTORS’ Awards is the preeminent U.S. Homeland Security Awards Program, and now in its Eighth Year, continues to recognize industry leaders of Physical and Border Security, Cybersecurity, Emergency Preparedness – Management and Response, Law Enforcement, First Responders, as well as federal, state and municipal government agencies in the acknowledgment of their outstanding efforts to Keep our Nation Secure.
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