DON26TZ01-NV004 TITLE: Non-Proximate Chemical Analysis by Field Portable Mass Spectrometry and Robotics

COMPONENT TECHNOLOGY PRIORITY AREA(S): Integrated Sensing and Cyber

PROJECTED CMMC LEVEL REQUIREMENT: Level 2 (Self)

OBJECTIVE: Design, build, and operate a portable mass spectrometer outfitted for proximal detection with a flexible inlet on a land-based robot, to collect real time mass spectra and chemical data at the source.

DESCRIPTION: Mass spectrometers provide unparalleled chemical detection and identification, specifically by use of high-resolution system or tandem mass spectrometry (MS/MS). Field portable mass spectrometers have been commercialized for decades and have led to the ability to detect chemicals of concern at the source. Unlike traditional mass spectrometry where sample preparation is required to get analytes into a form factor amenable for analysis, ambient ionization mass spectrometry has demonstrated proximate detection, with no sample preparation, if the test subject can be placed in front of the mass spectrometer inlet. A plethora of ambient ionization sources for drug, chemical warfare, explosive, and environmental detections of bulk objects in their original form factors with no sample preparation.

Not every test subject however will fit in front of the mass spectrometer’s inlet, nor can the ionization source be positioned in such a way to accommodate the test subject. Other ionization sources such as swabs and contact transfer touch sprays have been developed to sample an area and bring the sample to the mass spectrometer. This requires a trained user and sampling error can often be the largest challenge in these samplings.

Non-proximate methods, essentially changing the inlet of the mass spectrometer, have been developed and demonstrated. For example, sampling explosives and chemical warfare agents from ambient surfaces at distances of up to 3 meters from the mass spectrometer has been demonstrated [Ref 9]. However, this method was performed with a rigid inlet and while non-proximate distances were achieved, the flexibility of the sampling was limited, and it would be difficult to adapt to a robotic arm on a rover such as those used by Explosive Ordnance Disposal (EOD).

The objective of this STTR topic is to demonstrate a portable mass spectrometer that has a flexible inlet that could be brought to the test subject and manipulated by a robotic arm platform to collect chemical data at the source. The inlet and the subsequent ionization source combination must be ruggedized and manipulated by a robotic arm to move both to position for sampling. The mass spectrometer must provide remote red light / green light results to the operator from a standoff distance. It must be operational in varying levels of humidity, temperature, and ability to detect a wide array of chemicals.

PHASE I: Design a detailed model and parts inventory for a non-proximate mass spectrometry inlet or ion transport device that is flexible and positionable by a robotic arm. Detail ionization source that will be selected to interface with mass spectrometry inlet and demonstrate that it can be moved by a robotic arm. Design a detailed model and parts inventory for a field portable mass spectrometer (MS) that will couple to the flexible non-proximate inlet, taking into consideration Size, Weight and Power (SWaP) requirements and how it will interface and operate on a robotic arm on a rover. Adaptation of commercial field portable mass spectrometer to interface with a flexible inlet is also appropriate.

Provide a parts list with material type and weight for each component (required). The battery for the MS should last at least 3 hours before needing to be recharged. The casing of the flexible inlet, ionization source, and MS should be ruggedized, water resistant, and ensure that the instrument is not damaged upon movement. The MS must be operational during and after movement. Additionally, the MS must be operational at a temperature range of -25 °F to 120 °F (Threshold (T)), -35°F to 135°F (Objective (O)). Consult MIL-STD-810 Test Methods: 501.6 High Temperature, 502.6 Low Temperature, 507.6 Humidity, and 510.6 Sand and Dust when designing and selecting the material and layout of the system.

The overall layout of these components for the final system should be sketched and the overall size should be as compact as possible. The communication of the MS to the control system at the operator should be detailed. The MS should have an operating mass range at least from m/z 50 to m/z 500 to detect a wide range of chemical threats. Detection limits for chemical threats must be less than 100 ppb (T), in the ppt range (O).

The Phase I Option, if exercised, should be used to further develop and improve the design and, possibly, to demonstrate key components.

The Phase I effort will include prototype plans to be developed under Phase II.

PHASE II: Construct the non-proximate inlet and interface with field portable MS with the aforementioned operational specifications from Phase . Interface the non-proximate inlet and ionization source with a commercial off-the-shelf (COTS) robotic arm that could be mounted to a rover for sampling remote and hard to reach locations. The MS should be able to be operated remotely and have a database capability of providing red light / green light results to the operator based upon both mass spectra and tandem mass spectra. The system must provide remote results and be fully operational while the robotic arm is in motion. Demonstrate the detection of three target chemical threat simulants from surfaces that cannot be moved to a traditional stationary inlet. Guidance will be provided to threat simulants at the start of Phase II, but they will be within the required mass range. Deliver one operational unit to the Navy.

PHASE III DUAL USE APPLICATIONS: Final testing and demonstration / evaluation would be conducted in theater and on forward operating bases. Scenarios could be standoff detection of unknown objects and suspected hazardous threats, gathering chemical information from object difficult to sample that may have moved through a hazardous environment (under side wing of an aircraft), or when human / physical interaction with a sample is not ideal.

Ample forensic applications for this technology exist in drug, chemical warfare agent, and explosives detection. There are also potential dual use applications in the pharmaceutical and industrial processes such as inspecting the inside of a chemical reactor / checking the cleanliness after a process or within quality control areas. There are also environmental dual use applications for traversing hard to sample locations and instead being able to send the rover and sampling apparatus into the space.

REFERENCES:

1. Snyder, Dalton T.; Pulliam, Christopher J.; Ouyang, Zheng and Cooks, R. Graham. "Miniature and Fieldable Mass Spectrometers: Recent Advances." Analytical Chemistry 2016, 88 (1), pp. 2-29. DOI: 10.1021/acs.analchem.5b03070
2. Fedick, Patrick W.; Fatigante, William L.; Lawton, Zachary E.; O’Leary, Adam E.; Hall, Seth E.; Bain, Ryan M.; Ayrton, Stehen T.; Ludwig, Joseph A. and Mullian, Christopher C. "A Low-Cost, Simplified Platform of Interchangeable, Ambient Ionization Sources for Rapid, Forensic Evidence Screening on Portable Mass Spectrometric Instrumentation." Instruments 2018, 2 (2), 5. DOI: 10.3390/instruments2020005
3. Peacock, Patricia M.; Zhang, Wen-Jing and Trimpin, Sarah. "Advances in Ionization for Mass Spectrometry." Analytical Chemistry 2017, 89 (1), pp. 372-388. DOI: 10.1021/acs.analchem.6b04348
4. Lawton, Zachary E.; Traub, Angelica; Fatigante, William L.; Mancias, Jose; O’Leary, Adam E.; Hall, Seth E.; Wieland, Jamie R.; Oberacher, Herbert; Gizzi, Michael C. and Mulligan, Christopher C. "Analytical Validation of a Portable Mass Spectrometer Featuring Interchangeable, Ambient Ionization Sources for High Throughput Forensic Evidence Screening." Journal of the American Society for Mass Spectrometry 2016, 28 (6), pp. 1048-1059. DOI: 10.1007/s13361-016-1562-2
5. Giannoukos, Stamatios; Brkic, Boris; Taylor, Stephen; Marshall, Alan and Verbeck, Guido F. "Chemical Sniffing Instrumentation for Security Applications." Chemical Reviews 2016, 116 (14), pp. 8146-8172. DOI: 10.1021/acs.chemrev.6b00065
6. Hendricks, Paul I.; Dalgleish, Jon K.; Shelley, Jacob T.; Kirleis, Matthew A.; McNicholas, Matthew T.; Li, Linfan; Chen, Tsung-Chi; Chen, Chien-Hsun; Duncan, Jason S.; Boudreau, Frank; Noll, Robert J.; Denton, John P.; Roach, Timothy A.; Ouyang, Zheng and Cooks, R. Graham. "Autonomous in Situ Analysis and Real-Time Chemical Detection Using a Backpack Miniature Mass Spectrometer: Concept, Instrumentation Development, and Performance." Analytical Chemistry 2014, 86 (6), pp. 2900-2908. https://pubs.acs.org/doi/10.1021/ac403765x
7. Usmanov, Dilshadbek T.; Hiraoka, Kenzo; Wada, Hiroshi; Matsumura, Masaya; Sanada-Morimura, Sachiyo; Nonami, Hiroshi and Yamabe, Shinichi. "Non-proximate mass spectrometry using a heated 1-m long PTFE tube and an air-tight APCI ion source." Analytica Chimica Acta, 2017, 973 (22), pp. 59-67. https://www.sciencedirect.com/science/article/abs/pii/S0003267017303987
8. Cotte-Rodriguez, Ismael; Mulligan, Christopher C. and Cooks, R. Graham. "Non-Proximate Detection of Small and Large Molecules by Desorption Electrospray Ionization and Desorption Atmospheric Pressure Chemical Ionization Mass Spectrometry: Instrumentation and Applications in Forensics, Chemistry, and Biology." Analytical Chemistry, 2007, 79 (18), pp. 7069-7077. https://pubs.acs.org/doi/10.1021/ac0707939
9. Cotte-Rodriguez, Ismael and Cooks, R. Graham. "Non-Proximate Detection of Explosives and Chemical Warfare Agent Simulants by Desorption Electrospray Ionization Mass Spectrometry." Chemical Communications, 2006, 28, pp. 2968-2970. https://pubs.rsc.org/en/content/articlelanding/2006/cc/b606020j

KEYWORDS: Mass spectrometry; Non-proximate detection; Rover; Field portable; Automation; Chemical analysis

TPOC 1
Patrick Fedick
(760) 608-6917
patrick.w.fedick.civ@us.navy.mil

TPOC 2
Elise Tseng
elise.e.tseng.civ@us.navy.mil