Draft_SOW_Lab_Support.doc

MS Department, Code MS33 Laboratory Support for Chemometric Method Development

PR: TBD

1. INTRODUCTION

The Naval Surface Warfare Center Corona (NSWCCO) Division, Measurement Science and Engineering Department, requires laboratory-based research support to complete the development of a chemical solvent analysis method that is based on multivariate analysis of Fourier-Transform Infrared (FTIR) spectroscopic data and to conduct testing and evaluation required for the Navy Metrology Research and Development (R&D) Program to adapt the methodology for use in Navy calibration laboratories.

2. BACKGROUND

Navy calibration laboratories use the solvent CFC-113 to clean oxygen system components that they calibrate. After cleaning the components, these laboratories are required to measure the level of contaminants that remain. They use this measurement to verify compliance with NAVAIR and NAVSEA requirements (established cleanliness levels). This process is a critical fire-prevention component of the Navy’s oxygen safety program. The cleanliness-verification method used by the calibration laboratories does not work with the non-ozone-depleting solvents that the Navy has approved for this application, nor is there an available substitute method. To meet that condition, the Navy Metrology Calibration (METCAL) Program must develop and field a method to enable affected laboratories to use approved non-ozone-depleting cleaning solvents. The R&D Program tasked MS Department to develop a quantitative cleanliness verification method to support the use of approved non-ozone-depleting solvents. MS Department has developed an initial method that uses a mathematical model to analyze infrared spectral data.

Since February 25, 2016, the MS Chemical Metrology Laboratory (CML) at NSWCCO has been under a complete work stoppage due to persisting facility problems. To mitigate additional risk and to recover the project schedule, MS is seeking to continue collaborating with researchers at University of California, Riverside, Bourns College of Engineering (UCR BCoE) that are known to possess the expertise required to carry out the remaining laboratory-based elements of this project. To meet the deadline imposed by the Chief of Naval Operations (CNO), MS Department must complete the work sought through this contract by 31 December 2019. An additional four-year extension of the waiver is being sought to give NAVAIR and NAVSEA METCAL Program Managers the lead-time they require to procure required hardware and to plan and implement logistics and program integration,

3. SCOPE

The scope of the effort is comprised of the laboratory work required to complete the development of a quantitative method to be used by Navy calibration laboratories to verify the cleanliness of oxygen system components and of the construction of three (3) Navy-designed prototype systems which can automatically and repeat ably clean FTIR transmission cells with solvent and ready them for sample measurement.

4. APPLICABLE DOCUMENTS

5. REQUIREMENTS

The required tasking is in part open-ended, in that it requires an iterative process to obtain spectral data, feed the data into the developing model, and then assess progress through single-blind trials. This process is repeated, applying knowledge gained to additional (revised) spectral data collection, etc., to obtain the required performance of the model. It thus requires the Offeror not only to be expert in making infrared spectral measurements, but also to be skilled in producing results on research-oriented projects. To ensure data file compatibility with all work done to date, only Bruker Optics model ALPHA FTIR spectrometers and Bruker Optics OPUS Spectroscopy Software with OPUS/QUANT quantitative analysis package can be used for this work.

5.1 The Offeror shall investigate multiple hydrocarbon contaminants and test multiple FTIR spectrometers for instrument bias. Investigation is to include:

5.1.1 Expand spectral database to further refine the multivariate analysis model by analyzing quantitatively-prepared solutions of mineral oil and a minimum of five (5) additional hydrocarbon analytes. Analytes will be selected by NSWCCO from hydrocarbon-based fluids common in Navy use. Each analyte is to be prepared in solutions with solvent NovecTM 71DE in concentrations from 0 to 10 ppm (weight) in 1 ppm increments, sequentially analyzing each sample on (3) ALPHA FTIRs.

5.1.2 Prepare and analyze batteries of hydrocarbon analytes to periodically assess the predictive ability of the model. Sample concentrations will be primarily between 0 & 10 ppm with outliers up to 100 ppm. The size of each battery of samples shall be at least 15 per analyte, but no fewer than 25 per battery. Spectral data files will be submitted to NSWCCO. NSWCCO will re-label data files and use them for a single-blind test of the performance of the model.

5.1.3 After data from five (5) different hydrocarbon analytes has been incorporated into model database with mineral oil sample data, the Offeror is to run at least one (1) battery of single hydrocarbon analytes and mixtures of multiple analytes to assess model performance. Sample concentrations will be primarily between 0 & 10 ppm, but with outliers up to 100 ppm. Battery to include spectral data files from samples prepared and analyzed by at least two (2) different researchers. The size of the battery is to be determined, but is anticipated to be composed of approximately 75 to 100 separate data files. Spectral data files shall be submitted to NSWCCO. (CDRL A001/ A003) 5.1.4 If required, the Offeror to analyze multiple mixtures of hydrocarbon analytes and additional single hydrocarbon analytes from 0 to 10 ppm in 1 ppm increments to further develop the database.

5.2 The Offeror shall conduct a long-term cell leak test. Since the original Navy-supplied FTIR liquid transmission cells had to be redesigned, NSWCCO requires UCR to purchase additional liquid transmission cells for these tests. All redesigned transmission cells will be returned to NSWCCO at the conclusion of the project for redeployment to the Navy’s Schoolhouse. The investigation is to include the following:

5.2.1 The Offeror shall fill multiple Navy liquid transmission cells with either pure NovecTM 71DE solvent or with known concentrations of mineral oil in NovecTM 71DE between 0 and 7 ppm. A total of at least six cells will be used for this test.

5.2.2 The Offeror shall ensure to seal the cells by tightening the caps to Swagelok-supplied specifications.

5.2.3 The Offeror shall pressurize the cells to no more than 15 psig. (Actual pressure used will be determined jointly between NSWCCO, UCR, and Spectral Systems (the cell manufacturer).

5.2.4 The Offeror shall inspect the cells for leaks at least monthly over a 12-month period by a suitable method (e.g., observance of air bubble formation inside the cells, by mass change, or by monitoring internal pressure). The duration of the test may be shortened if conducted at elevated pressure. The test duration will be determined jointly between NSWCCO, UCR, and Spectral Systems.

5.2.5 The Offeror shall note and report the total elapsed time to any observed cell leakage, and the cause, if it is apparent. Duration of leak test surveillance for each cell is to be either 12-month if the cells are unpressurized or until the first confirmed observance of cell leakage. (The duration of the test may vary by cell.)

5.3 The Offeror shall conduct a long-term test (12 months, minimum) to determine if cell construction materials leach into the solvent and to determine if there is any change in the mineral oil concentration of the sealed sample over time. The investigation is to include, the following:

5.3.1 The Offeror shall use the filled, sealed cells from 05.2.1. The Offeror shall perform an initial analysis using the FTIR hydrocarbon measurement method and document the initial spectral measurement data files and the version of the model used to make these baseline measurements.

5.3.2 The Offeror shall analyze each of the cells at regular intervals (at least monthly) for hydrocarbon concentration using the same version of the spectral analysis model that was used to produce the initial baseline measurements. The Offeror shall document (report) the FTIR data file for each measurement of each cell.

5.3.3 The Offeror shall continue to make and record these measurements on all cells for the full 12-month duration of the test, including cells that may have leaked, unless leakage is severe.

5.4 The Offeror shall conduct laboratory work required to help assess a solvent filtration process for use by Navy calibration technicians. NSWCCO has determined that Navy laboratories must filter virgin solvent for this application. Laboratories currently filter solvent by gravity using an open-top filter. Disparate evaporation characteristics of the replacement solvent’s constituents create a compelling need for a closed filtering process for NovecTM 71DE to avoid changing the solvent’s composition. NSWCCO has identified a bottle-top hand pump and closed filter that comprise the major hardware components.

5.4.1 The Offeror shall conduct laboratory work necessary to help NSWCCO finalize a hardware configuration suitable for deployment to Navy laboratories. This effort will entail determining, selecting, and configuring required ancillary hardware and testing the apparatus.

5.4.2 The Offeror shall conduct a test to determine if the construction materials of the pump and filter assembly will leach interfering contaminants into the solvent over time. The duration of the test will be a minimum of three (3) months. Fresh solvent samples straight from the manufacturer’s bottle will be compared with filtered samples at regular intervals. FTIR measurements of both solvent samples will be made using the one (1) mm sealed liquid cells and the spectral analysis model. The investigation is to include, the following:

5.4.2.1 To start the leaching test, a hand pump will be affixed to a bottle of solvent, fitted with the filtration device, and filled with solvent by normal pumping action. After collecting samples for analysis, the pressure will be released using the pump pressure relief valve, but the pump and filter assembly will remain attached to the solvent bottle for the duration of the test.

5.4.2.2 At regular intervals (at least once every two weeks), the Offeror shall collect solvent samples from the pump/filter assembly for FTIR analysis. The Offeror shall collect FTIR data for the filtered solvent and for an unfiltered solvent sample at each interval. All FTIR data files from the tests will be recorded and reported to NSWCCO.

5.5 The Offeror shall conduct laboratory work required to assist NSWCCO in developing a robust system to fill and empty Navy FTIR transmission cells. The goal is to modify the standard cell filling, emptying, and flushing process by eliminating glass syringes that may be prone to breakage in a Navy calibration laboratory. The envisioned solution will make use of readily available Commercial off the Shelf (COTS) hardware to provide a robust apparatus suitable for deployment to Navy calibration laboratories. The primary components of the apparatus are multiple electrically-operated valves, a variable-speed reversible peristaltic pump, and a Programmable Logic Controller (PLC) with assorted interconnecting hardware. The Offeror will help to determine, select, and configure required ancillary hardware, and help to program the PLC and test the apparatus. If determined to be needed by the Navy, UCR will work with NSWCCO to build two packaged cell flushing and filling systems suitable for deployment at the Navy’s Schoolhouse. These systems will be returned to NSWCCO at the conclusion of this project.

5.6 When the performance of the model is acceptable, NSWCCO will need to determine the optimum number of different sealed mineral oil reference cells required to field the method and to determine the optimal reference concentrations to field. This effort will require the Offeror to conduct “proof of concept” trials to verify the approach.

6. GOVERNMENT FURNISHED PROPERTY

N/A

6.1 Government Furnished Material

N/A

6.2 Government Furnished Equipment

NSWC Corona will provide three (3) Bruker Optics model ALPHA FTIR spectrometers and nine (9) Spectral Systems “Navy design” 1-mm sealed cells with Calcium fluoride windows for use in testing. All three ALPHA spectrometers and sealed cells are to be returned to NSWC Corona at the conclusion of testing. Additional ancillary hardware may be provided with the provision that it be returned to NSWCCO as well.

6.3 Government Furnished Information

NSWC Corona will provide/make available spectral data, FTIR setup parameters and other information necessary to ensure compatibility between vendor and NSWC Corona-generated measurements.

7. DELIVERABLES

8. ACRONYM LIST

N/A

PERIOD OF PERFORMANCE / REQUIRED DELIVERY DATES

One (1) Base Year from Date of Award (DOA)