Recipient Organization
TDA RESEARCH, INC.
12345 WEST 52ND AVENUE
WHEAT RIDGE,CO 80033
Performing Department
(N/A)
Non Technical Summary
Protecting the quality of water in the nation's streams, rivers, lakes, and estuaries is a critical need and important for human and ecosystem health.Efficient protection requires knowledge gained from real-time or near real time information on nutrient concentrations and loads. Thisinformation feeds into predictive models and informs policy decisions. In this project, we are creating a new tool to add to the arsenal of those protecting the nations water assets based on low-magnetic field nuclear magnetic resonance (NMR) spectroscopy.
Animal Health Component
40%
Research Effort Categories
Basic
20%
Applied
40%
Developmental
40%
Goals / Objectives
Phosphorous (P) is one of the primary nutrients that plants require, but it can disrupt aquatic systems when its concentrations are too high. Excess P can cause eutrophication, resulting in fish kills, toxic algae, and degraded drinking water quality, especially in rural, agricultural areas. Careful monitoring of P levels is required to effectively manage human interactions with water sources, and to manage P runoff. Currently measuring P in water sources requires sample send out to a lab. The results turn around (3-4 weeks) is much longer than the timescale of P cycling in the ecosystem. Information to guide management related to fast occurring events (like storms) that can release more P from high runoff areas (like farms) is often missing. There is an immediate need for lab-quality data to be generated at the water source, at higher temporal resolution (i.e. faster times), to drive effective water management decisions, and inform agricultural best management practices. TDA proposes a novel method to monitor phosphorous (P) concentrations in surface waters, such as lakes and rivers, that is fast, inexpensive, and remotely deployable. This is in direct response to Topic 8.4: Conservation of Natural Resources, specifically the "water quality and quantity" research priority. This proposal also has a connection to "agriculturally related technology", a broader USDA SBIR program priority. USDA Strategic Objective 2.3 is to foster agricultural innovation. Monitoring is crucial for making data-informed decisions regarding farm-level practices to manage phosphorus, and continuous, remote monitoring is a major innovation.Technical ObjectivesWe will develop the 31P-NMR measurement for phosphorus in surface waters in a form factor which can be deployed for long term remote monitoring. We will demonstrate measurement success through controlled measurements of lake water samples, comparing with laboratory measurements of standard P solutions. We aim to prove that the 31P-NMR approach can detect the median urban water P concentration of 0.25 mg/L, or lower, and within 2 hours of averaging by the end of the Phase II. To accomplish these goals, we have laid out the following goals and objectives for our Phase I work:(Goal 1) Design & construct permanent magnet (B0) with sufficient magnetic field homogeneity.Obj. 1 - Simulate permanent magnetic design in COMSOL to achieve very high magnetic field homogeneityObj. 2 - Build permanent magnet prototpyeObj.3 - Measure homogeneity with high sensitivity magnetometers and compare to simulation. Iterate between simulation and design, if needed, to achieve mangetic field homogeneityObj. 4 - Demonstrate 1H-NMR and 31P-NMR using permanent magnet design as final test of sufficient field homogeneity(Goal 2) Upgrade our FPGA board for RF handling to execute hyperpolarization experiment.Obj. 1 - Start with currnet FPGA design for NMR only experiment, and plan out addiiton of RF excitation chainObj. 2 - Build and Test FPGA NMR + RF chain on test benchObj. 3 - Demonstrate FPGA ability to complete hyperpolarization experiment3. Perform head-to-head comparison between the 31P-NMR sonde and atomic emission analysis to show the in-situ technique provides comparable analysis to the laboratory method.Obj. 1 - Make up stock solutions of 31P containingsolutions at low and high concentrationsObj. 2 - Analyze stock solutions with in-house microwave-power atomic emission spectrometer (MP-AES) to quantitfy stock solution concentrationsObj. 3 - Measure stock solutions with 31P-NMR. Sub-objectives are measureing with NMR only and long averaging, or with NMR+Hyperpolarization to decrease measurement timeObj. 4 - Compare "gold standard" MP-AES data with 31P-NMR and assess LOD capabilities of 31P-NMR4. Demonstrate 31P-NMR function on lake water samplesObj. 1 - Collect lake water from nearby Evergreen Lake and analyze for 31P-NMR content in "natural" stateObj. 2 - Spike lake water with known concentrations of 31P-compounds and measure with 31P-NMR without any other sample prepObj. 3 - Take lake water samples and execute extensive preparation done for high-magnetic field 31P-NMR, including removing Fe and Mn ions, and bringing up to pH 12. Run samples and compare to literature examples of 31P-NMR at high magnetic field.
Project Methods
Mobile, low-magnetic field-NMR is built around the idea of the "on-site" sensor or probe. In traditional NMR, a very small amount of sample is brought to the laboratory spectrometer. In mobile-NMR, the sensor comes to the sample. As such the sample size which is interrogated can be greatly increased. The analysis of much larger sample sizes in mobile-NMR applications offsets the loss in signal intensity from operating at lower magnetic fields. For existing high-magnetic field analysis, sample sizes used are 1 cm x 4 cm (V ~ 3 mL). The limiting factor is the difficulty in maintaining a high magnetic field homogeneity over a large space. The signal amplitude which can be observed is directly related to the concentration of spins (magnetically active nuclei), the volume of spins, and the applied magnetic field. If the volume of spins is limited by small sample size, the easiest way to increase signal amplitude is to increase the magnetic field strength. Thishas been the default approach for NMR for the past 70 years. However, when performing NMR in low-magnetic fields, one is not limited by sample volume, and some of the decreased signal amplitude lost by decreasing magnetic field strength can be regained by using a larger sample.The project will be accomplished through use of a well synchronized highly skilled team. The team leader, Dr.Biller, has 14 years of experience in designing, buidling, and validating low-magnetic field paramagnetic and nuclear magnetic resoannce hardware. Dr. Kevin Finch is an Analytical Chemist with a background in elemental analysis and will help set the "gold-standard" 31P measurements used to validate the new 31P-NMR technology. Mr. David Long holds dual degrees in Electrical and Mechancial Engineering, an associates degree in Precision Machining, and is currently completing his MS in Electrical Engineering on top of a full work week. In additon, Mr. Long has prior experience deisgning and building permanent magnets. Mr. Cory Van Beek is an electrical engineer who logged more than 42,000 lines of FPGA code at GE Healthcare prior to coming to TDA Research. Dr. Adrienne Delluva is a skilled materials scientist with a background in thin polymer films which will suppor the hyperpolarization film for signal amplification. Finally, Mr. Bradley Spatafore is a Sr. Mechanical Engineer who specializes in porting in-lab scientific measurements into the "real-world". Mr. Spatafore has worked with Dr. Biller in other projects to produce a consumer ready portable technology.Progress meetings are held weekly to identify problems early so we keep the project moving forward. Every new design is tested with stepwise measurement and components are validated independently from one another. For instance, we do not simply build a permanent magnet we "think" will work and attempt to measure NMR. We will model a design in COMSOL software which produces a field amplitude and homogeneity over a working volume we can confirm by using our exisitng library of high-sensitivity magnetometer devices. Once we've indpendently measured sufficient field homogenetiy, we will validate it can produce NMR using our well characterized existing benchtop NMR system (built by Dr. Biller). At the same time, the FPGA-NMR and RF-signal amplification chain can be independently validated by an existing benchtop electromagnet to ensure all experiment parameters are executed correctly. After the in-field permanent magnet and the in-field electronics are separately validated, they are combined to form the heart of an in-field NMR spectrometer.From here we can quickly bench mark the limit of detection of our new in-field NMR technique by comparison with gold-standard elemental analysis with MP-AES. We do this comparison not just with laboratory grade water samples spiked with phosphorus, but with lake water samples spiked with phosphorus and with lake water samples prepared for phosphorus analysis under high magnetic field NMR conditions.The three main metrics of success in the Phase I will be 1.) a compact permanent magnetic field design for in-situ large volume sample analysis 2.) A robust set of miniaturized electronics to run the experiment with high fidelity and acquire and process raw data into a NMR spectrum and 3.) the brand new knowledge of the trade offs between sample size, magnetic field strength and signal amplication for 31P-NMR in clean (lab water) and dirty (lake water) matrixes.Completion of the 3 main metrics set the state for aPhase II programto transition the Phase I work into a new commercial tool by the end of the two year Phase II time frame.