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NASA NTRS2017

Method for the Collection, Gravimetric and Chemical Analysis of Nonvolatile Residue (NVR) on Surfaces

Nonvolatile residue (NVR), sometimes referred to as molecular contamination is the term used for the total composition of the inorganic and high boiling point organic components in particulates and molecular films deposited on critical surfaces surrounding space structures, with the particulate and NVR contamination originating primarily from pre-launch operations. The "nonvolatile" suggestion from the terminology NVR implies that the collected residue will not experience much loss under ambient conditions. NVR has been shown to have a dramatic impact on the ability to perform optical measurements from platforms based in space. Such contaminants can be detected early by the controlled application of various detection techniques and contamination analyses. Contamination analyses are the techniques used to determine if materials, components, and subsystems can be expected to meet the performance requirements of a system. Of particular concern is the quantity of NVR contaminants that might be deposited on critical payload surfaces from these sources. Subsequent chemical analysis of the contaminant samples by infrared spectroscopy and gas chromatography mass spectrometry identifies the components, gives semi-quantitative estimates of contaminant thickness, indicates possible sources of the NVR, and provides guidance for effective cleanup procedures. In this report, a method for the collection and determination of the mass of NVR was generated by the authors at NASA Langley Research Center. This report describes the method developed and implemented for collecting NVR contaminants, and procedures for gravimetric and chemical analysis of the residue obtained. The result of this NVR analysis collaboration will help pave the way for Langley's ability to certify flight hardware outgassing requirements in support of flight projects such as Stratospheric Aerosol and Gas Experiment III (SAGE III), Clouds and the Earth's Radiant Energy System (CERES), Materials International Space Station Experiment - X (MISSE-X), and Doppler Aerosol Wind Lidar (DAWN).

Gordon, Keith↗

NASA NTRS2009

Non-Volatile Residue (NVR) Contamination from Dry Handling and Solvent Cleaning

This slide presentation reviews the testing for Non-Volatile Residue contamination transferred to surfaces from handling and solvent cleaning. Included in the presentation is a list of the items tested, formal work instructions dealing with NVR. There is an explanation of the Gravimetric determination method used to test the NVR in a variety of items, i.e., Gloves, Swabs, Garments, Bagging material, film and Wipes. Another method to test for contamination from NVR is the contact transfer method. The use of this method for testing gloves, garments, bagging material and film is explained. Certain equations use in NVR analysis and the use of a database for testing of NVR in consumables are reviewed.

Sovinski, Marjorie F.↗

NASA NTRS1992

A high sensitivity real-time NVR monitor

The use of a temperature-controlled 200-MHz SAW resonator piezoelectric mass microbalance to monitor the mass of nonvolatile residue (NVR) deposited on its surface in real time is reported. The fundamental frequency of this device is mainly dependent on the configuration of the transducers and not on the thickness of the substrate. Therefore, higher operating frequencies can be achieved without reducing the thickness of the crystal. The real-time instrument was integrated onto a conventional stainless steel NVR plate and operated flawlessly over a 14-d period at Kennedy Space Center and successfully measured less than 1 ng/sq cm d NVR contamination. Contamination episodes detected by the instrument were correlated with scheduled activities on the test stand. Under the assumption of a baseline noise level of +/- 2 Hz, the absolute mass lower limit of detection would be 0.065 ng/sq cm. This would enable the detection of a daily NVR deposition rate of less than 0.1 ng/sq cm d.

Bowers, William D.↗

NASA NTRS1997

High sensitivity real-time NVR monitor

A real time non-volatile residue (NVR) monitor, which utilizes surface acoustic wave (SAW) resonators to detect molecular contamination in a given environment. The SAW resonators operate at a resonant frequency of approximately 200 MHz-2,000 MHz which enables the NVR monitor to detect molecular contamination on the order of 10.sup.-11 g-cm.sup.-2 to 10.sup.-13 g-cm.sup.2. The NVR monitor utilizes active temperature control of (SAW) resonators to achieve a stable resonant frequency. The temperature control system of the NVR monitor is able to directly heat and cool the SAW resonators utilizing a thermoelectric element to maintain the resonators at a present temperature independent of the environmental conditions. In order to enable the direct heating and cooling of the SAW resonators, the SAW resonators are operatively mounted to a heat sink. In one embodiment, the heat sink is located in between the SAW resonators and an electronic circuit board which contains at least a portion of the SAW control electronics. The electrical leads of the SAW resonators are connected through the heat sink to the circuit board via an electronic path which prevents inaccurate frequency measurement.

Bowers, William D.↗

NASA NTRS2004

Contamination of Critical Surfaces from NVR Glove Residues Via Dry Handling and Solvent Cleaning

Gloves are often used to prevent the contamination of critical surfaces during handling. The type of glove chosen for use should be the glove that produces the least amount of non-volatile residue (NVR). This paper covers the analysis of polyethylene, nitrile, latex, vinyl, and polyurethane gloves using the contact transfer and gravimetric determination methods covered in the NASA GSFC work instruction Gravimetric Determination and Contact Transfer of Non-volatile Residue (NVR) in Cleanroom Glove Samples, 541-WI-5330.1.21 and in the ASTM Standard E-1731M-95, Standard Test Method for Gravimetric Determination of Non-Volatile Residue from Cleanroom Gloves. The tests performed focus on contamination of critical surfaces at the molecular level. The study found that for the most part, all of the gloves performed equally well in the contact transfer testing. However, the polyethylene gloves performed the best in the gravimetric determination testing, and therefore should be used whenever solvent contact is a possibility. The nitrile gloves may be used as a substitute for latex gloves when latex sensitivity is an issue. The use of vinyl gloves should be avoided, especially if solvent contact is a possibility. A glove database will be established by Goddard Space Flight Center (GSFC) Code 541 to compile the results from future testing of new gloves and different glove lots.

Sovinski, Marjorie F.↗

NASA NTRS1985

Analysis of Nonvolatile Residue (NVR) from Spacecraft Systems

Organic contamination on critical spacecraft surfaces can cause electronic problems, serious attenuation of various optical signals, thermal control changes, and adhesion problems. Such contaminants can be detected early by the controlled use of witness mirrors, witness plates, wipe sampling, or direct solvent extraction. Each method requires careful control of variables of technique and materials to attain the ultimate sensitivities inherent to that procedure. Subsequent chemical analysis of the contaminant sample by infrared and mass spectrometry identifies the components, gives semiquantitative estimates of contaminant thickness, indicates possible sources of the nonvolatile residue (NVR), and provides guidance for effective cleanup procedures.

Colony, J. A.↗

NASA NTRS1995

A Real-Time Nonvolatile Residue (NVR) Monitor

New development and application of device described in "Surface-Acoustic-Wave Piezoelectric Microbalance," (LAR-14476). Active sensing element of Real-Time NVR Monitor comprises pair of piezoelectric surface-acoustic-wave resonators resonating at frequency of 200 MHz. Bare, uncoated resonator exposed to atmosphere and directly in contact with airborne volatile and nonvolatile materials leaving residues on surface. Resonant frequency of exposed resonator decreases with increasing mass of adsorbed residue; resulting beat frequency between two resonators increases with mass and serves as sensitive real-time indication of airborne contaminants or non-volatile residue.

Bowers, William D.↗

NASA NTRS1992

Sources and transport of silicone NVR

The retrieved LDEF had varying amounts of visible contamination films (brown stains) at many locations. FTIR spectra of heavy film deposits at vents and of optical windows from tray E5 indicated methyl silicone and silica in the contaminant films. Two possible sources of the methyl silicone are DC-710 phenyl methyl silicone in the shuttle-bay-liner beta cloth, and the shuttle tile waterproofing silane. It is concluded that much of the silicon and silica contamination came from ground operations and the orbiter.

Harvey, Gale A.↗

NASA NTRS2011

Failure Analysis of Nonvolatile Residue (NVR) Analyzer Model SP-1000

National Aeronautics and Space Administration (NASA) subcontractor Wiltech contacted the NASA Electrical Lab (NE-L) and requested a failure analysis of a Solvent Purity Meter; model SP-IOOO produced by the VerTis Instrument Company. The meter, used to measure the contaminate in a solvent to determine the relative contamination on spacecraft flight hardware and ground servicing equipment, had been inoperable and in storage for an unknown amount of time. NE-L was asked to troubleshoot the unit and make a determination on what may be required to make the unit operational. Through the use of general troubleshooting processes and the review of a unit in service at the time of analysis, the unit was found to be repairable but would need the replacement of multiple components.

Potter, Joseph C.↗

NASA NTRS1996

The Development of Methodologies and Solvent Systems to Replace CFC-113 in the Validation of Large-Scale Spacecraft Hardware

Liquid oxygen is used as the oxidizer for the liquid fueled main engines during the launch of the space shuttle. Any hardware that comes into contact with pure oxygen either during servicing of the shuttle or in the operation of the shuttle must be validated as being free of nonvolatile residue (NVR). This is a safety requirement to prevent spontaneous combustion of carbonaceous NVR if it was to come into contact with pure oxygen. Previous NVR validation testing of space hardware used Freon (CFC-113) as the test solvent. Because CFC-113 no longer can be used, a program was conducted to develop a NVR test procedure that uses a safe environmentally friendly solvent. The solvent that has been used in the new NVR test procedure is water. Work that has been conducted over the past three years has served to demonstrate that when small parts are subjected to ultrasound in a water bath and NVR is present a sufficient quantity is dispersed into the water to analyze for its concentration by the TOC method. The work that is described in this report extends the water wash NVR validation test to large-scale parts; that is, parts too large to be subjected to ultrasound. The method consists of concentrating the NVR in the water wash onto a bed of silica gel. The total adsorbent bed is then analyzed for TOC content by using a solid sample probe. Work that has been completed thus far has demonstrated that hydrocarbon based NVR's can be detected at levels of less than 0.1 mg per square foot of part's surface area by using a simple water wash.

Clausen, Christian A., III↗

NASA NTRS2009

Characterization of Monomethyihydrazine (MMH) Non-Volatile Residue

The Space Shuttle program has a unique propellant purity requirement for determination of nonvolatile residue (NVR) in monomethylhydrazine (MMH). TIis requirement differs from the Military Specification procurement specification by requiring a NVR analysis with a limit of less than or equal to 10 milligrams per liter. In June 2008, a routine MMH replenishment delivery was transferred into a NASA KSC owned tanker for future delivery to the Space Shuffle pad MMH storage tank. Per Shuffle standard operating procedure, the receiving tanker was sampled and analyzed for purity and surprisingly it failed the Shuttle use NVR specification limit. Detailed examination of the NVR revealed that it was fundamentally different than the typical MMH NVR. This paper will examine various aspects of NVR determination in MMH and the analytical characterization processes used to identify the NVR.

Davis, Chuck↗

NASA NTRS1995

Precision Cleaning Verification of Fluid Components by Air/Water Impingement and Total Carbon Analysis

NASA personnel at Kennedy Space Center's Material Science Laboratory have developed new environmentally sound precision cleaning and verification techniques for systems and components found at the center. This technology is required to replace existing methods traditionally employing CFC-113. The new patent-pending technique of precision cleaning verification is for large components of cryogenic fluid systems. These are stainless steel, sand cast valve bodies with internal surface areas ranging from 0.2 to 0.9 m(exp 2). Extrapolation of this technique to components of even larger sizes (by orders of magnitude) is planned. Currently, the verification process is completely manual. In the new technique, a high velocity, low volume water stream impacts the part to be verified. This process is referred to as Breathing Air/Water Impingement and forms the basis for the Impingement Verification System (IVS). The system is unique in that a gas stream is used to accelerate the water droplets to high speeds. Water is injected into the gas stream in a small, continuous amount. The air/water mixture is then passed through a converging-diverging nozzle where the gas is accelerated to supersonic velocities. These droplets impart sufficient energy to the precision cleaned surface to place non-volatile residue (NVR) contaminants into suspension in the water. The sample water is collected and its NVR level is determined by total organic carbon (TOC) analysis at 880 C. The TOC, in ppm carbon, is used to establish the NVR level. A correlation between the present gravimetric CFC-113 NVR and the IVS NVR is found from experimental sensitivity factors measured for various contaminants. The sensitivity has the units of ppm of carbon per mg-ft(exp 2) of contaminant. In this paper, the equipment is described and data are presented showing the development of the sensitivity factors from a test set including four NVR's impinged from witness plates of 0.05 to 0.75 m(exp 2).

Barile, Ronald G.↗

NASA NTRS1994

Precision cleaning verification of fluid components by air/water impingement and total carbon analysis

NASA personnel at Kennedy Space Center's Material Science Laboratory have developed new environmentally sound precision cleaning and verification techniques for systems and components found at the center. This technology is required to replace existing methods traditionally employing CFC-113. The new patent-pending technique of precision cleaning verification is for large components of cryogenic fluid systems. These are stainless steel, sand cast valve bodies with internal surface areas ranging from 0.2 to 0.9 sq m. Extrapolation of this technique to components of even larger sizes (by orders of magnitude) is planned. Currently, the verification process is completely manual. In the new technique, a high velocity, low volume water stream impacts the part to be verified. This process is referred to as Breathing Air/Water Impingement and forms the basis for the Impingement Verification System (IVS). The system is unique in that a gas stream is used to accelerate the water droplets to high speeds. Water is injected into the gas stream in a small, continuous amount. The air/water mixture is then passed through a converging/diverging nozzle where the gas is accelerated to supersonic velocities. These droplets impart sufficient energy to the precision cleaned surface to place non-volatile residue (NVR) contaminants into suspension in the water. The sample water is collected and its NVR level is determined by total organic carbon (TOC) analysis at 880 C. The TOC, in ppm carbon, is used to establish the NVR level. A correlation between the present gravimetric CFC113 NVR and the IVS NVR is found from experimental sensitivity factors measured for various contaminants. The sensitivity has the units of ppm of carbon per mg/sq ft of contaminant. In this paper, the equipment is described and data are presented showing the development of the sensitivity factors from a test set including four NVRs impinged from witness plates of 0.05 to 0.75 sq m.

Barile, Ronald G.↗

NASA NTRS2003

Changes in the Optical Properties of Simulated Shuttle Waste Water Deposits: Urine Darkening

Manned spacecraft have historically dumped the crew generated waste water overboard, into the environment in which the spacecraft operates, sometimes depositing the waste water on the external spacecraft surfaces. The change in optical properties of wastewater deposited on spacecraft external surfaces, from exposure to space environmental effects, is not well understood. This study used nonvolatile residue (NVR) from Human Urine to simulate wastewater deposits and documents the changes in the optical properties of the NVR deposits after exposure to ultra violet(UV)radiation. Twenty four NVR samples of, 0-angstromes/sq cm to 1000-angstromes/sq cm, and one sample contaminated with 1 to 2-mg/sq cm were exposed to UV radiation over the course of approximately 6151 equivalent sun hours (ESH). Random changes in sample mass, NVR, solar absorbance, and infrared emission were observed during the study. Significant changes in the UV transmittance were observed for one sample contaminated at the mg/sq cm level.

Albyn, Keith↗

NASA NTRS2004

Changes in the Optical Properties of Simulated Shuttle Waste Water Deposits- Urine Darkening

Manned spacecraft have historically dumped the crew generated waste waster overboard, into the environment in which the spacecraft operates, sometimes depositing the waste water on the external spacecraft surfaces. The change in optical properties of wastewater deposited on spacecraft external surfaces, from exposure to space environmental effects, is not well understood. This study used nonvolatile residue (NVR) from Human Urine to simulate wastewater deposits and documents the changes in the optical properties of the NVR deposits after exposure to ultra violet (UV) radiation. Twenty NVR samples of, 0-angstromes/sq cm to 1000-angstromes/sq cm, and one sample contaminated with 1 to 2-mg/sq cm were exposed to UV radiation over the course of approximately 6151 equivalent sun hours (ESH). Random changes in sample mass, NVR, solar absorbance, and infrared emission were observed during the study. Significant changes in the UV transmittance were observed for one sample contaminated at the mg/sq cm level.

Albyn, Keith↗

NASA NTRS2012

The Search for Nonflammable Solvent Alternatives for Cleaning Aerospace Oxygen Systems

Oxygen systems are susceptible to fires caused by particle and nonvolatile residue (NVR) contaminants, therefore cleaning and verification is essential for system safety. . Cleaning solvents used on oxygen system components must be either nonflammable in pure oxygen or complete removal must be assured for system safety. . CFC -113 was the solvent of choice before 1996 because it was effective, least toxic, compatible with most materials of construction, and non ]reactive with oxygen. When CFC -113 was phased out in 1996, HCFC -225 was selected as an interim replacement for cleaning propulsion oxygen systems at NASA. HCFC-225 production phase-out date is 01/01/2015. HCFC ]225 (AK ]225G) is used extensively at Marshall Space Flight Center and Stennis Space Center for cleaning and NVR verification on large propulsion oxygen systems, and propulsion test stands and ground support equipment. . Many components are too large for ultrasonic agitation - necessary for effective aqueous cleaning and NVR sampling. . Test stand equipment must be cleaned prior to installation of test hardware. Many items must be cleaned by wipe or flush in situ where complete removal of a flammable solvent cannot be assured. The search for a replacement solvent for these applications is ongoing.

Mitchell, Mark↗

NASA NTRS1983

Induced environment contamination monitor (IECM) cascade impactor

The Cascade Impactor on the IECM is an aerosol sampling instrument which employs three cascade impaction-type nozzles of progressively smaller diameter. The considered approach makes it possible to achieve particle size discrimination involving three ranges (5 microns and larger, 1 to 5 microns, and 0.3 to 1 micron). In addition to the particulate measuring cascade stages, a fourth quartz crystal microbalance measures the cumulative airborne molecular nonvolatile residue (NVR) at ambient temperature. The cascade measurements provide a temporal record of the payload bay's particulate environment during ascent, descent, and immediate postlanding periods. The NVR stage functions throughout the mission. Particulates of a size greater than five microns in diameter were below 10 micrograms per cu m throughout the mission.

Duncan, B. J.↗

NASA NTRS1995

Investigation of cleanliness verification techniques for rocket engine hardware

Oxidizer propellant systems for liquid-fueled rocket engines must meet stringent cleanliness requirements for particulate and nonvolatile residue. These requirements were established to limit residual contaminants which could block small orifices or ignite in the oxidizer system during engine operation. Limiting organic residues in high pressure oxygen systems is particularly important. The current method of cleanliness verification used by Rocketdyne requires an organic solvent flush of the critical hardware surfaces. The solvent is filtered and analyzed for particulate matter, followed by gravimetric determination of the nonvolatile residue (NVR) content of the filtered solvent. The organic solvents currently specified for use (1,1,1-trichloroethane and CFC-113) are ozone-depleting chemicals slated for elimination by December 1995. A test program is in progress to evaluate alternative methods for cleanliness verification that do not require the use of ozone-depleting chemicals and that minimize or eliminate the use of solvents regulated as hazardous air pollutants or smog precursors. Initial results from the laboratory test program to evaluate aqueous-based methods and organic solvent flush methods for NVR verification are provided and compared with results obtained using the current method. Evaluation of the alternative methods was conducted using a range of contaminants encountered in the manufacture of rocket engine hardware.

Fritzemeier, Marilyn L.↗