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At least 37 records · Page 2

Data analysis for lidar and quartz crystal microbalance systems

Results are presented of the analysis of data taken on the stratospheric aerosol, using lidar, Quartz Crystal Microbalance (QCM), and the SAGE and SAM II satellite systems. The main objective of the work reported has been to use the data, taken with the NASA-LaRC instruments to study the stratospheric effects of volcanic eruptions during the period between the launch of the SAGE and SAM II satellite systems and October 1980. Four significant volcanic eruptions, for which data are available, occurred during this period--Soufriere, Sierra Negra, Mt. St. Helens, and Ulawun. Data on these have been analyzed to determine the changes in stratospheric mass loading produced by the eruptions, and to study the dispersion of the newly injected material.

Kent, G. S.↗

The Response of a Quartz Crystal Microbalance to a Liquid Deposit

A theory was developed for predicting the loss of response of a QCM (Quartz Crystal Microbalance) to a liquid deposit due to viscous effects in the deposit. The loss of response is expressed by a response factor, equal to the response of the QCM to a liquid film divided by its response to a solid film of the same mass per unit area. The theory assumes a droplet-type deposit morphology, and considers the influence of droplet distribution parameters. Experiments were conducted to examine the validity of the theory, using DC 704 silicone oil as the subject deposit material. Experiments were made in two series: one with constant deposit mass and variable temperature, the other with variable deposit mass and constant temperature. Interpretation of the data using the theory has enabled information on droplet area coverage and number density to be deduced.

Glassford, A. P. M.↗

The V-3 contamination test of the chamber A facility and a subsequent cryogenic/vacuum study of the V-3 test quartz crystal microbalance

The areas of orbital and ground contamination of flight experiment hardware have been well established. This report relates directly to results of vacuum chamber testing for the ground evaluation of flight experiment hardware performance. First, the data obtained during the V-3 contamination testing in the Johnson Space Center's Chamber A space simulation test facility are presented. Second, during the V-3 contamination tests, the MSFC Space Sciences Laboratory's quartz crystal microbalance exhibited two periods of anomalous readings. Therefore, a subsequent small chamber tests was conducted in a controlled cryogenic/vacuum environment. The objective was to reproduce with known parameters the anomalous behavior patterns of the V-3 test data. Analyses of the anomalous readings are made on the basis of these tests. Additionally, as a by-product of the small chamber tests, calibration curves then existing for the quartz crystal microbalance were empirically extended, and certain data-formatting aids were documented.

Moore, W. W., Jr.↗

Use of the quartz crystal microbalance to determine the monomeric friction coefficient of polyimides

When a thin film of polymer is coated on to a quartz crystal microbalance (QCM), the QCM can be used to detect the rate of increase in weight of the polymer film as the volatile penetrant diffuses into the polymer. From this rate information the diffusion coefficient of the penetrant into the polymer can be computed. Calculations requiring this diffusion coefficient lead to values which approximate the monomeric friction coefficient of the polymer. This project has been concerned with the trial of crystal oscillating circuits suitable for driving polymer coated crystals in an atmosphere of penetrant. For these studies done at room temperature, natural rubber was used as an easily applied polymer that is readily penetrated by toluene vapors, qualities anticipated with polyimides when they are tested at T(g) in the presence of toluene. Three quartz crystal oscillator circuits were tested. The simplest circuit used +/- 5 volt dc and had a transistor to transistor logic (TTL) inverter chip that provides a 180 deg phase shift via a feed back loop. This oscillator circuit was stable but would not drive the crystal when the crystal was coated with polymer and subjected to toluene vapors. Removal of a variable resistor from this circuit increased stability but did not otherwise increase performance. Another driver circuit tested contained a two stage differential input, differential output, wide band video amplifier and also contain a feed back loop. The circuit voltage could not be varied and operated at +/- 5 volts dc; this circuit was also stable but failed to oscillate the polymer coated crystal in an atmosphere saturated with toluene vapors. The third oscillator circuit was of similar construction and relied on the same video amplifier but allowed operation with variable voltage. This circuit would drive the crystal when the crystal was submerged in liquid toluene and when the crystal was coated with polymer and immersed in toluene vapors. The frequency readings obtained when using this oscillating circuit are highly variable. This circuit requires further modification to stabilize frequency readings before its use in studies to determine the diffusion coefficient of penetrant molecules into a polymer film coated on a QCM.

Bechtold, Mary M.↗

A Comparison of Quartz Crystal Microbalance Measurements with Mass Spectrometer Determinations

An experimental program was undertaken in which mass accretion rates, as determined by a liquid nitrogen cooled quartz crystal microbalance, were compared with the mass flux rates, as determined by both a cycloidal type and a quadrupole type residual gas analyzer for five simple materials. The data indicate a high degree of correlation between these instruments insofar as the shape of the curves. There are large variations however among the absolute values.

Kruger, R.↗

Gas Dynamics, Characterization, and Calibration of Fast Flow Flight Cascade Impactor Quartz Crystal Microbalances (QCM) for Aerosol Measurements

During recent high altitude flights, we have tested the aerosol section of the fast flow flight cascade impactor quartz crystal microbalance (QCM) on loan to Howard University from NASA. The aerosol mass collected during these flights was disappointingly small. Increasing the flow through the QCM did not correct the problem. It was clear that the instrument was not being operated under proper conditions for aerosol collect ion primarily because the gas dynamics is not well understood. A laboratory study was therefore undertaken using two different fast flow QCM's in an attempt to establish the gas flow characteristics of the aerosol sections and its effect on particle collection, Some tests were made at low temperatures but most of the work reported here was carried out at room temperature. The QCM is a cascade type impactor originally designed by May (1945) and later modified by Anderson (1966) and Mercer et al (1970) for chemical gas analysis. The QCM has been used extensively for collecting and sizing stratospheric aerosol particles. In this paper all flow rates are given or corrected and referred to in terms of air at STP. All of the flow meters were kept at STP. Although there have been several calibration and evaluation studies of moderate flow cascade impactors of less than or equal to 1 L/rein., there is little experimental information on the gas flow characteristics for fast flow rates greater than 1 L/rein.

Grant, J.R.↗

Examining polymer‐protein biophysical interactions with small‐angle x‐ray scattering and quartz crystal microbalance with dissipation

Abstract Polymer‐protein hybrids can be deployed to improve protein solubility and stability in denaturing environments. While previous work used robotics and active machine learning to inform new designs, further biophysical information is required to ascertain structure–function behavior. Here, we show the value of tandem small‐angle x‐ray scattering (SAXS) and quartz crystal microbalance with dissipation (QCMD) experiments to reveal detailed polymer‐protein interactions with horseradish peroxidase (HRP) as a test case. Of particular interest was the process of polymer‐protein complex formation under thermal stress whereby SAXS monitors formation in solution while QCMD follows these dynamics at an interface. The radius of gyration ( R g ) of the protein as measured by SAXS does not change significantly in the presence of polymer under denaturing conditions, but thickness and dissipation changes were observed in QCMD data. SAXS data with and without thermal stress were utilized to create bead models of the potential complexes and denatured enzyme, and each model fit provided insight into the degree of interactions. Additionally, QCMD data demonstrated that HRP deforms by spreading upon surface adsorption at low concentration as shown by longer adsorption times and smaller frequency shifts. In contrast, thermally stressed and highly inactive HRP had faster adsorption kinetics. The combination of SAXS and QCMD serves as a framework for biophysical characterization of interactions between proteins and polymers which could be useful in designing polymer‐protein hybrids.

60 APPLIED LIFE SCIENCES↗

Flow Injection Electrochemical Quartz Crystal Microbalance with ICP-OES Detection: Electroprecipitation and Stripping of Lanthanum and Neodymium in a Flow Cell

We used an improved version of our hyphenated analysis technique, flow injection electrochemical quartz crystal microbalance (EQCM) with inductively coupled optical emission spectroscopy, to investigate the electroprecipitation of lanthanum and neodymium from flowing solutions. The improved version has two independent flow injection circuits, allowing different conditions for electrochemical precipitation (pH=4.3 or 2.6) and quick stripping (2% HNO3) with EQCM mass detection and ICP-OES elemental analysis. Lanthanum or neodymium ions in a 500 uL sample were injected into a carrier stream and deposited onto an EQCM housed in a micro flow cell, owing to a localized high-pH layer. The deposits are subsequently stripped from the electrode using HNO3 and analyzed downstream using an ICP-OES. We found that using acidic solutions without supporting electrolyte leads to an increase of the amount of lanthanum detected by 4-fold. The enhanced deposition can be attributed to enhanced mass transfer by migration. Furthermore, we showed that by applying chronopotentiometry, we can detect a change in the hydrogen evolution reaction mechanism that enables the precipitation of lanthanides on the surface of the electrode. Understanding and enhancing the deposition of lanthanides is relevant for elemental or isotopic detection in nuclear forensics.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Plume backscatter measurements using quartz crystal microbalances in JPL Molsink (molecular sink)

Quantitative evidence of gas flows in the far upstream region of small nozzles with large boundary layer flow are discussed. Gas mass fluxes were measured using quartz crystal microbalances. Both nitrogen and carbon dioxide gases were used as test gases. Gas deposition rates on the order of 100 monolayers per minute were detected 13 inches upstream of the nozzle exit plane. It is significant to note that the crystals detected gases considerably beyond the Prandtl-Meyer turning angle. The data from these tests will be essential in the formulation of scaling laws and analytical prediction methods for viscous plume behavior.

Simon, W.↗

From bulk to interface: electrochemical phenomena and mechanism studies in batteries via electrochemical quartz crystal microbalance

Understanding the bulk and interfacial behaviors during the operation of batteries (e.g., Li-ion, Na-ion, Li–O 2 batteries, etc.) is of great significance for the continuing improvement of the performance. Electrochemical quartz crystal microbalance (EQCM) is a powerful tool to this end, as it enables in situ investigation into various phenomena, including ion insertion/deinsertion within electrodes, solid nucleation from the electrolyte, interphasial formation/evolution and solid–liquid coordination. As such, EQCM analysis helps to decipher the underlying mechanisms both in the bulk and at the interface. This tutorial review will present the recent progress in mechanistic studies of batteries achieved by the EQCM technology. Here, the fundamentals and unique capability of EQCM are first discussed and compared with other techniques, and then the combination of EQCM with other in situ techniques is also covered. In addition, the recent studies utilizing EQCM technologies in revealing phenomena and mechanisms of various batteries are reviewed. Perspectives regarding the future application of EQCM in battery studies are given at the end.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Flight evidence of spacecraft surface contamination rate enhancement by spacecraft charging obtained with a quartz crystal microbalance

The significance of the fraction of the mass outgassed by a negatively charged space vehicle which is ionized within the vehicle plasma sheath and electrostatically reattracted to the space vehicle was determined. The ML-12 retarding potential analyzer/temperature controlled quartz crystal microbalances (RPA/TQCMs) distinguishes between charged and neutral molecules and investigates contamination mass transport mechanism. Two long term, quick look flight data sets indicate that on the average a significant fraction of mass arriving at one RPA/TQCM is ionized. It is assumed that vehicle frame charging during these periods was approximately uniformly distributed in degree and frequency. It is shown that electrostatic reattraction of ionized molecules is an important contamination mechanism at and near geosynchronous altitudes.

Clark, D. M.↗

Feasibility demonstration for hydrogen chloride detection using a chemisorption technique and a quartz crystal microbalance

A method of measuring concentrations of hydrogen chloride between 1 part per billion and 10 parts per million at standard temperature and pressure is presented. The feasibility of a low-cost device incorporating a chemisorption technique coupled with a quartz crystal microbalance was demonstrated in the field at the Viking B launch using a Titan-Centaur vehicle from Kennedy Space Center on August 20, 1975. Hydrogen chloride is a product of solid rocket combustion. The concentration level of hydrogen chloride for this particular launch was measured as approximately 0.2 parts per million at 4 km from the launch site.

Jex, D. W.↗

Using a temperature-controlled quartz crystal microbalance in a space equipment cleanroom to monitor molecular contamination

There is a need for continuous monitoring for molecular contamination in clean rooms where spaceflight equipment is assembled, integrated, and tested to insure that contamination budgets are met. The TQCM (temperature-controlled quartz crystal microbalance) can be used to provide both a real time warning and a cumulative measurement of molecular contamination. It has advantages over the other measurement methods such as witness mirrors, NVR (non-volatile residue) plates, and gas analyzers. A comparison of the TQCM sensitivity and ease of operations is made with the other methods. The surface acoustic wave microbalance (SAW), a newly developed instrument similar to TQCM, is considered in the comparison. An example is provided of TQCM use at Goddard Space Flight Center when the Wide Field Planetary Camera 2(WFPC-2) and the Corrective Optics Space Telescope Axial Replacement (COSTAR) were undergoing integrated testing prior to their installation in the Hubble Space Telescope on its first servicing mission. Areas for further investigation are presented.

Mitchell, William J.↗

Orientation matters: Measuring the correct surface of polyamide membranes with quartz crystal microbalance

The surface of polyamide reverse osmosis (RO) membranes which regulates interface-dominated phenomena, such as partitioning and fouling, is the one facing the feed during operation. However, the opposite surface of the polyamide selective layer, the one facing the permeate and in contact with the polysulfone porous support, is commonly analyzed in quartz crystal microbalance (QCM) measurements due to limitations of state-of-the-art transfer methodologies. Such measurements on the back surface cannot be generalized because the polyamide layer is chemically and morphologically asymmetric. Herein, we introduce a simple method to coat QCM sensors with polyamide active layers in the correct orientation (i.e., exposing their front surface) and show that interface-dominated phenomena differ significantly between orientations. We start by describing a transfer protocol to coat any surface with a polyamide layer on its front surface orientation. We then systematically analyze the chemical and morphological differences between the two surfaces of the polyamide layer of a commercial RO membrane. Finally, we demonstrate that interface-dominated phenomena depend on the orientation by showing that NaCl partitioning at pH 6 was 1.3 to 2.3-fold higher on the front surface and that organic fouling with humic acid occurred at a lower rate on this surface. The new method presented herein enables measurements on the front surface of polyamide RO membranes, which should be the standard in any future QCM studies.

Fouling behavior↗

Rocket effluent size distributions made with a cascade quartz crystal microbalance

Airborne particulate size distribution measurements were made in the stabilized ground cloud from a Titan III C rocket just after launch from the Kennedy Space Center on May 12, 1977. The measurements were made from aboard a small twin engine aircraft instrumented with particle and gas sensors. The plume was followed for about 1 hour while making multiple passes through the cloud at varying altitudes. The results obtained with a ten-stage cascade quartz crystal microbalance impactor show that the mass concentration as a function of particle diameter is bimodal with the first maximum between 0.05 micrometers and 0.1 micrometers and the second maximum between 0.8 and 1.0 micrometer. Scanning electron microscope analysis were performed on the material collected and show distinctly different kinds of particles in the two modes.

Woods, D. C.↗

A Method for Incorporating Quartz Crystal Microbalance Thermo-Gravimetric Assessment Data in Contamination Modeling

The science objectives of increasingly ambitious space missions require meeting stringent contamination requirements. Contamination transport models are based on established principles such as Fick’s law for contamination diffusion within the source material, Arrhenius factors to account for temperature variations and free molecular transport for spacecraft operating in vacuum. In addition to the science principles, empirical data obtained from ASTM E1559 testing is used for engineering contamination modeling. The ASTM E1559 test provides outgassing rate data for materials at expected spacecraft temperatures during a mission. Multiple quartz crystal microbalances (QCMs) can be operated at different temperatures to measure the amount of contamination condensation that can occur on various spacecraft surfaces. At the conclusion of the ASTM E1559 test a thermo-gravimetric assessment (TGA) can be performed by heating the QCMs at a linear rate to obtain contamination desorption data. This TGA data provides a wealth of information that can be incorporated into contamination models. A method for applying this data is presented.

Anderson, John R↗

Flow Injection Electrochemical Quartz Crystal Microbalance with ICP-OES Detection: Recovery of Silver by Electrodeposition with Redox Replacement in a Flow Cell

We developed a new on-line hyphenated flow injection analysis technique (FI-EQCM-ICP-OES) that allows electrochemical deposition and stripping with mass detection and elemental analysis. This technique was used to study a new system for electrochemical recovery of silver from a 0.5 mM Ag + /5 mM Cu 2+ /0.5 M H 2 SO 4 solution by pulsed electrodeposition with redox replacement (EDRR) in a small flow cell. The metal ions in a 500 μ l sample are injected into the sulfuric acid carrier stream and deposited onto an electrochemical quartz crystal microbalance (EQCM) electrode housed in a 50 μ l flow cell. The deposits are subsequently stripped off electrochemically in the same cell and analyzed downstream in an ICP-OES. The stripped metal layer was found to be composed of Ag with no detectable Cu for a redox replacement time of 10 s, and 91 wt.% Ag–9 wt.% Cu for a redox replacement time of 5 s. Microscopy measurements demonstrated that the electrode was covered with silver particles, some of which contain Cu in the case of the 5 s replacement time. This technique allowed the study of mass changes on the electrode during electrodeposition and open circuit times in each EDRR cycle in flowing solutions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗