Statement of Work Phase 1.pdf

Identification of NOVEC 71DE Residues (Apr. 1, 2022 to Sept. 30, 2022)

The overarching objectives of the proposed work are to identify the NOVEC 71DE residue by conducting detailed chemical analysis and to determine if the Navy’s cleaning process is likely to cause Novec 71DE to deposit residue(s) on interior bourdon tube surfaces.

Attachments

Attachments 1 and 2, originally prepared to support testing for an associated project, are provided here for reference.

1. Contaminants for Gauge Cleaning Tests, Rev. 4, 7 March 2022

2. Preparation of Standard Solutions of Hydrocarbon Oils in Novec 71DE, Rev. 2, 9 Jun 2021

1. Conduct detailed analysis of NOVEC 71DE residue samples provided from NAVSEA Corona

a. Identify solid samples

b. Write a progress report

2. Analyze NOVEC 71 DE residues

a. Examine hydrocarbon residue formation from NOVEC 71DE by drop casting various amounts of NOVEC 71DE solvents on different substrates (e.g., glass and stainless-steel sheets)

i. Write a progress report

b. Use the following procedure to prepare an initial residue sample for analysis.

i. Use a glass syringe or pipette to transfer 500 mL of Novec 71DE directly from the original solvent bottle into a tared glass container. If the liquid sample or resulting residue will be transferred elsewhere for chemical analysis, the container should either be equipped with a ground glass stopper or have a tight-fitting lid that has a PTFE liner.

ii. Record the initial weight of the solvent sample + container.

iii. Allow the sample to evaporate to constant-weight dryness at room temperature. (Optional: A gentle stream of clean air or nitrogen may be directed at the liquid surface to speed evaporation.) The gas flow should not be more than what is required to make a slight deflection on the solvent surface.

iv. Record the weight of the container + residue.

c. Determine chemical composition of Novec 71DE residues using start-of-the art analytical instruments (e.g., FT-IR, RAMAN, Optical Microscopy, UV-VIS, XRD, GC-

MS, LC-MS)

i. Identify solid samples

d. Determine if additional residue analyses are required for confirmation of residue composition

ii. Determine the optimal size and number of subsequent samples

iii. Modify sample size and repeat steps b.i) – ii) as required per b.iii)

e. (Ref. step 3 below.) Test various solvents that may be suitable for disolving the residue and removing it from glassware. (One reference shows 4-methoxyphenol is soluble in ethanol at 25 mg/mL.)

f. Write a progress report

3. Examine hydrocarbon residue formation in pressure gauges.

a. (Navy to furnish a KIng Nutronics Model 3646-1-104 Instrument Cleaning System at

University of Notre Dame)

b. Work with Notre Dame Glass Shop to construct a test article of ~5/8 in ID glass tubing to simulate a closed-end Bourdon tube that can be put through a simulated cleaning process with Novec 71DE using a King Nutronics Model 3646 instrument Cleaning System (Navy-supplied).

i. Cut a length of 5/8 in diameter glass tubing ~12 in long

ii. Seal the tube at one end

iii. Bend the tube in a ~270 degree arc ~5” diameter 270 degree arc (~60 mL internal volume and ~152 cm2 internal wetted surface area).

iv. Affix an adapter on the open end to connect to 1/4 in PTFE tubing from the KN

3646.)

c. Connect the test article to the 3646 and perform five cleaning cycles with clean

NOVEC 71DE to mimic cleaning a gauge.

i. Record the total volume of solvent collected for five cleaning cycles.

d. If residue is formed on the walls of the tube:

i. photograph Photograph it as evidence.

ii. Rinse the test article with an appropriate clean solvent to dissolve and remove the residue. (ref. 2.d above)

a) The test article may be rinsed using a glass syringe.

iii. Determine the quantity and the chemical composition of the residue by suitable means (ref. 2 above).

iv. Repeat 3.c and d twice (three cleaning tests, total)

e. Write a progress report

4. Help assess a potential Navy oxygen cleanliness verification method developed by Orono Spectral Solutions and Bruker Optics. The scope of support needed is threefold:

a. Prepare standard solutions of known concentrations of hydrocarbon-based materials in Novec 71DE solvent prior to demonstration.

i. Prepare standard solutions of hydrocarbon material(s) in Novec 71DE.

a) Use one or more of the materials listed in Attachment 1 (Contaminants for Gauge Cleaning Tests, Rev. 34, 23 Feb7 Mar 2022).

b) Prepare solutions of five different concentrations from 1 through 6 ppm (by weight), plus two different concentrations from 7 through 10 ppm.

c) Prepare solutions using standard analytical techniques, such as in Attachment 2 (Preparation of Standard Solutions of Hydrocarbon Oils in Novec 71DE, Rev. 2, 9 Jun 2021).

ii. Prepare 24 test solutions labeled only with non-descriptive identifiers (e.g.

numbered 1-24 or similar) and record the solution identity and concentration for each for Notre Dame and Navy personnel. Samples are to be presented to OSS as unknowns for their demonstration.

a) Test solutions shall be comprised of three samples from each of the standard solutions prepared in 4.a.i above, plus three samples of unaltered Novec 71DE for blanks.

b. Host a demonstration by an OSS representative, to include:

i. Provide laboratory space with a fume hood and 120 VAC electrical connection.

Laboratory needs to be accessible for rolling equipment (i.e., by elevator if lab is not at ground level).

ii. Present 24 test solutions from 4.a.ii above to OSS personnel.

iii. Compare the OSS test results for each test solution against each solution’s known concentration.

iv. Reimburse OSS for time and travel costs ($4,500)

c. Write a report (assessing the method for Navy use in verifying the acceptance of solvent samples- Navy oxygen cleaning acceptance critereon is for samples to be less than 5 ppm hydrocarbon material)