SOW - ID Novec 71DE Residues Draft PDF.pdf

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STATEMENT OF WORK

IDENTIFICATION OF NOVEC 71DE RESIDUES

1. INTRODUCTION

Naval Surface Warfare Center (NSWC), Corona Division, Measurement Science Department, U.S. Navy Metrology Research and Development Program Code requires research, testing and additional chemical analysis tests on the residue and solvent of NOVEC 71 DE and investigation into non-volatile residue (NVR) methodology comparable to that which NASA originally used to test solvent cleaning performance.

2. BACKGROUND

The METCAL R&D program is developing a quantitative cleanliness verification method based upon Fourier-transform-infrared (FT-IR) analysis of Novec 71DE cleaning solvent samples.

This method relies on partial least squares (PLS) analysis of FT-IR data sets. We have recently become aware that Novec 71DE will leave a residue if the solvent is allowed to evaporate at room temperature. We noticed that a solid waxy like residue compound remained after a sample of Novec 71DE evaporated at room temperature. A solid residue was also observed inside the liquid transmission cell that METCAL R&D is using to make final cleaning measurements. The residue has presented itself as a waxy clear liquid, a thick brown honey like liquid, a white flaky solid, and as clear thick liquid droplets. We are now concerned that the process we have been preparing to transition could likely leave an unknown amount of residue in a “cleaned” oxygen gauge, potentially creating a fire hazard when a gauge is returned to service in its parent oxygen system. The residue is currently suspect and is likely 4-methoxyphenol, but cannot be confirmed until the residue has undergone analytical testing. There is a secondary concern with having this residue present in oxygen gauges that are used in breathing systems because of the inhalation hazards associated with 4-methoxyphenol. These residue materials need to be chemically identified prior to finalizing a cleanliness method so that there is assurance that all potential residue-forming materials have been removed. Chemical analysis of the residue material and examination of an alternate NVR method will assist in this effort.

3. SCOPE

Conduct chemical analysis tests on the residue and solvent, evaluate the membrane-based FT-IR method performed by OSS and investigate the non-volatile residue (NVR) methodology that NASA originally used to test solvent cleaning performance.

4. APPLICABLE DOCUMENTS

(a) OPNAV M-5090.1, 10 Jan 2014

(b) MIL-STD-1330, 28 June 2007

(c) MIL-STD-1622, 15 Nov 2006

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(d) NASA WSTF # 97-31189, CFC 113 Replacement Study with 3M HFE-71DE, 19 Nov 1997

(e) NASA WSTF # 96-29930, Chlorofluorocarbon (CFC) 113 Replacement Study with 3M L-13532, 28 May 1996

(f) NASA WSTF # 97-31554, Autogenous Ignition Temperature Determination in High-Pressure Oxygen (HFE-7100), 17 Feb 1998

(g) NASA WSTF # 97-30281, Autogenous Ignition Temperature Determination High-Pressure Oxygen (HFE-71DE), 21 Mar 1997

ATTACHMENTS

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

5. REQUIREMENTS

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.)

5. REQUIREMENTS CON’T

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 dissolving the residue and removing it from glassware. (One reference shows 4-methoxyphenol is soluble in ethanol at 25 mg/mL.)

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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 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 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.

5. REQUIREMENTS CON’T

v. Record the weight of the container + residue.

g. 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)

iv. Identify solid samples

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

v. Determine the optimal size and number of subsequent samples

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

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

j. Write a progress report

4. Examine hydrocarbon residue formation in pressure gauges.

d. (Navy to furnish a KIng Nutronics Model 3646-1-104 Instrument Cleaning System at University of Notre Dame)

e. 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 cleaning process with Novec 71DE using a King Nutronics Model 3646 instrument Cleaning System (Navy-supplied).

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

vi. Seal the tube at one end

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

viii. Affix an adapter on the open end to connect to 1/4 in PTFE tubing from the KN 3646.)

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

71DE to mimic cleaning a gauge.

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

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

v. Photograph it as evidence.

vi. 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.

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

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

g. Write a progress report.

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6. GOVERNMENT FURNISHED PROPERTY

6.1 Government Furnished Material

N/A

6.2 Government Furnished Equipment

Bruker FT-IR Spectrometer Alpha II KNC 3646 Portable Instrument Cleaning System

6.3 Government Furnished Information

SOW Attachment 1: Contaminants for Gauge Cleaning Tests.

SOW Attachment 2: Preparation of Standard Solutions of Hydrocarbon Oils in Novec 71DE

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

7. DELIVERABLES

NUMBER NAME

A001 Test/Inspection Report

8. ACRONYM LIST

ACRONYM DENOTATION

FT-IR Fourier-transform infrared GC-MS Gas Chromatography-Mass Spectrometry KN King Nutronics KNC King Nutronics Corporation LC-MS Liquid Chromatography-Mass Spectrometry NSWC Naval Surface Warfare Center OSS Orono Spectral Solutions PLS Partial Least Squares PTFE Polytetrafluoroethylene UV-VIS Ultraviolet-Visible VAC Volts, Alternating Current XRD X-Ray Diffraction

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ADDITIONAL INFORMATION

A. PERIOD OF PERFORMANCE / REQUIRED DELIVERY DATES

B. PLACE OF PERFORMANCE

C. SHIPPING ADDRESS

D. INSPECTION AND ACCEPTANCE

E. TECHNICAL POINT OF CONTACT

Upon contract award, service and delivery is required no later than 180 days after contract award

TBD

TBD

TBD

TBD