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Porter, Marc D.

Publications and source records attributed to Porter, Marc D..

In-Flight Water Quality Monitoring on the International Space Station (ISS): Measuring Biocide Concentrations with Colorimetric Solid Phase Extraction (CSPE)

The colorimetric water quality monitoring kit (CWQMK) was delivered to the International Space Station (ISS) on STS-128/17A and was initially deployed in September 2009. The kit was flown as a station development test objective (SDTO) experiment to evaluate the acceptability of colorimetric solid phase extraction (CSPE) technology for routine water quality monitoring on the ISS. During the SDTO experiment, water samples from the U.S. water processor assembly (WPA), the U.S. potable water dispenser (PWD), and the Russian system for dispensing ground-supplied water (SVO-ZV) were collected and analyzed with the CWQMK. Samples from the U.S. segment of the ISS were analyzed for molecular iodine, which is the biocide added to water in the WPA. Samples from the SVOZV system were analyzed for ionic silver, the biocide used on the Russian segment of the ISS. In all, thirteen in-flight analysis sessions were completed as part of the SDTO experiment. This paper provides an overview of the experiment and reports the results obtained with the CWQMK. The forward plan for certifying the CWQMK as operational hardware and expanding the capabilities of the kit are also discussed.

Gazda, Daniel B.

Design, Certification, and Deployment of the Colorimetric Water Quality Monitoring Kit (CWQMK)

In August 2009, an experimental water quality monitoring kit based on Colorimetric Solid Phase Extraction (CSPE) technology was delivered to the International Space Station (ISS) aboard STS-128/17A. The kit, called the Colorimetric Water Quality Monitoring Kit (CWQMK), was flown and deployed as a Station Development Test Objective (SDTO) experiment on the ISS. The goal of the SDTO experiment is to evaluate the acceptability of CSPE technology for routine water quality monitoring on the ISS. This paper provides an overview of the SDTO experiment, as well as a detailed description of the CWQMK hardware and a summary of the testing and analysis conducted to certify the CWQMK for use on the ISS. The initial results obtained from the SDTO experiment are also reported and discussed in detail

Gazda, Daniel B.

Colorimetric Solid Phase Extraction (CSPE): Using Color to Monitor Spacecraft Water Quality

In August 2009, an experimental water quality monitoring kit based on Colorimetric Solid Phase Extraction (CSPE) technology was delivered to the International Space Station (ISS). The kit, called the Colorimetric Water Quality Monitoring Kit (CWQMK), was launched as a Station Development Test Objective (SDTO) experiment to evaluate the suitability of CSPE technology for routine use monitoring water quality on the ISS. CSPE is a sorption-spectrophotometric technique that combines colorimetric reagents, solid-phase extraction, and diffuse reflectance spectroscopy to quantify trace analytes in water samples. In CSPE, a known volume of sample is metered through a membrane disk that has been impregnated with an analyte-specific colorimetric reagent and any additives required to optimize the formation of the analyte-reagent complex. As the sample flows through the membrane disk, the target analyte is selectively extracted, concentrated, and complexed. Formation of the analyte-reagent complex causes a detectable change in the color of the membrane disk that is proportional to the amount of analyte present in the sample. The analyte is then quantified by measuring the color of the membrane disk surface using a hand-held diffuse reflectance spectrophotometer (DRS). The CWQMK provides the capability to measure the ionic silver (Ag +) and molecular iodine (I2) in water samples on-orbit. These analytes were selected for the evaluation of CSPE technology because they are the biocides used in the potable water storage and distribution systems on the ISS. Biocides are added to the potable water systems on spacecraft to inhibit microbial growth. On the United States (US) segment of the ISS molecular iodine serves as the biocide, while the Russian space agency utilizes silver as a biocide in their systems. In both cases, the biocides must be maintained at a level sufficient to control bacterial growth, but low enough to avoid any negative effects on crew health. For example, the presence of high levels of iodine in water can cause taste and odor issues that result in decreased water consumption by the crew. There are also concerns about potential impacts on thyroid function following exposure to high levels of iodine. With silver, there is a risk of developing argyria, an irreversible blue-gray discoloration of the skin, associated with long term consumption of water containing high concentrations of silver. The need to ensure that safe, effective levels of biocide are maintained in the potable water systems on the ISS provides a perfect platform for evaluating the suitability of CSPE technology for in-flight water quality monitoring. This paper provides an overview of CSPE technology and details on the silver and iodine methods used in the CWQMK. It also reports results obtained during in-flight analyses performed with the CWQMK and briefly discusses other potential applications for CSPE technology in both the spacecraft and terrestrial environments.

Gazda, Daniel B.

Multiplexed Colorimetric Solid-Phase Extraction

Multiplexed colorimetric solid-phase extraction (MC-SPE) is an extension of colorimetric solid-phase extraction (C-SPE) an analytical platform that combines colorimetric reagents, solid phase extraction, and diffuse reflectance spectroscopy to quantify trace analytes in water. In CSPE, analytes are extracted and complexed on the surface of an extraction membrane impregnated with a colorimetric reagent. The analytes are then quantified directly on the membrane surface using a handheld diffuse reflectance spectrophotometer. Importantly, the use of solid-phase extraction membranes as the matrix for impregnation of the colorimetric reagents creates a concentration factor that enables the detection of low concentrations of analytes in small sample volumes. In extending C-SPE to a multiplexed format, a filter holder that incorporates discrete analysis channels and a jig that facilitates the concurrent operation of multiple sample syringes have been designed, enabling the simultaneous determination of multiple analytes. Separate, single analyte membranes, placed in a readout cartridge create unique, analyte-specific addresses at the exit of each channel. Following sample exposure, the diffuse reflectance spectrum of each address is collected serially and the Kubelka-Munk function is used to quantify each water quality parameter via calibration curves. In a demonstration, MC-SPE was used to measure the pH of a sample and quantitate Ag(I) and Ni(II).

Gazda, Daniel B.

Design, Certification, and Deployment of the Colorimetric Water Quality Monitoring Kit (CWQMK)

In August 2009, an experimental water quality monitoring kit based on Colorimetric Solid Phase Extraction (CSPE) technology was delivered to the International Space Station (ISS) aboard STS-128/17A. The kit, called the Colorimetric Water Quality Monitoring Kit (CWQMK), was developed by a team of scientists and engineers from NASA s Habitability and Environmental Factors Division in the Space Life Sciences Directorate at Johnson Space Center, the Wyle Integrated Science and Engineering Group in Houston, Texas, the University of Utah, and Iowa State University. The CWQMK was flown and deployed as a Station Development Test Objective (SDTO) experiment on ISS. The goal of the SDTO experiment was to evaluate the acceptability of CSPE technology for routine water quality monitoring on ISS. This paper provides an overview of the SDTO experiment, as well as a detailed description of the CWQMK hardware and a summary of the testing and analysis conducted to certify the CWQMK for use on ISS. The results obtained from the SDTO experiment are also reported and discussed in detail.

Gazda, Daniel B.

Colorimetric Solid Phase Extraction for the Measurement of Total I (Iodine, Iodide, and Triiodide) in Spacecraft Drinking Water

An experimental drinking water monitoring kit for the measurement of iodine and silver(I) was recently delivered to the International Space Station (ISS). The kit is based on Colorimetric Solid Phase Extraction (CSPE) technology, which measures the change in diffuse reflectance of indicator disks following exposure to a water sample. To satisfy additional spacecraft water monitoring requirements, CSPE has now been extended to encompass the measurement of total I (iodine, iodide, and triiodide) through the introduction of an oxidizing agent, which converts iodide and triiodide to iodine, for measurement using the same indicator disks currently being tested on ISS. These disks detect iodine, but are insensitive to iodide and triiodide. We report here the operational considerations, design, and ground-based performance of the CSPE method for total I. The results demonstrate that CSPE technology is poised to meet NASA's total I monitoring requirements.

Lipert, Robert J.

Colorimetric-Solid Phase Extraction Technology for Water Quality Monitoring: Evaluation of C-SPE and Debubbling Methods in Microgravity

Colorimetric-solid phase extraction (C-SPE) is being developed as a method for in-flight monitoring of spacecraft water quality. C-SPE is based on measuring the change in the diffuse reflectance spectrum of indicator disks following exposure to a water sample. Previous microgravity testing has shown that air bubbles suspended in water samples can cause uncertainty in the volume of liquid passed through the disks, leading to errors in the determination of water quality parameter concentrations. We report here the results of a recent series of C-9 microgravity experiments designed to evaluate manual manipulation as a means to collect bubble-free water samples of specified volumes from water sample bags containing up to 47% air. The effectiveness of manual manipulation was verified by comparing the results from C-SPE analyses of silver(I) and iodine performed in-flight using samples collected and debubbled in microgravity to those performed on-ground using bubble-free samples. The ground and flight results showed excellent agreement, demonstrating that manual manipulation is an effective means for collecting bubble-free water samples in microgravity.

Hazen-Bosveld, April

Application of Colorimetric Solid Phase Extraction (C-SPE) to Monitoring Nickel(II) and Lead(II) in Spacecraft Water Supplies

Archived water samples collected on the International Space Station (ISS) and returned to Earth for analysis have, in a few instances, contained trace levels of heavy metals. Building on our previous advances using Colorimetric Solid Phase Extraction (C-SPE) as a biocide monitoring technique, we are devising methods for the low level monitoring of nickel(II), lead(II) and other heavy metals. C-SPE is a sorption-spectrophotometric platform based on the extraction of analytes onto a membrane impregnated with a colorimetric reagent that are then quantified on the surface of the membrane using a diffuse reflectance spectrophotometer. Along these lines, we have determined nickel(II) via complexation with dimethylglyoxime (DMG) and begun to examine the analysis of lead(II) by its reaction with 2,5- dimercapto-1,3,4-thiadiazole (DMTD) and 4-(2- pyridylazo)-resorcinol (PAR). These developments are also extending a new variant of C-SPE in which immobilized reagents are being incorporated into this methodology in order to optimize sample reaction conditions and to introduce the colorimetric reagent. This paper describes the status of our development of these two new methods.

Diaz, Neil C.

Rapid determination of ions by combined solid-phase extraction--diffuse reflectance spectroscopy

We introduce colorimetric solid-phase extraction (C-SPE) for the rapid determination of selected ions. This new technique links the exhaustive concentration of an analyte by SPE onto a membrane disk surface for quantitative measurement with a hand-held diffuse reflectance spectrometer. The concentration/measurement procedure is complete in approximately 1 min and can be performed almost anywhere. This method has been used to monitor iodine and iodide in spacecraft water in the 0.1-5.0 ppm range and silver(I) in the range of 5.0-1000 microg/l. Applications to the trace analysis of copper(II), nickel(II), iron(III) and chromium(VI) are described. Studies on the mechanism of extraction showed that impregnation of the disk with a surfactant as well as a complexing reagent results in uptake of additional water, which markedly improves the extraction efficiency.

NASA Program Advanced Human Support Technology

Rapid, specific determination of iodine and iodide by combined solid-phase extraction/diffuse reflectance spectroscopy

A new, rapid methodology for trace analysis using solid-phase extraction is described. The two-step methodology is based on the concentration of an analyte onto a membrane disk and on the determination by diffuse reflectance spectroscopy of the amount of analyte extracted on the disk surface. This method, which is adaptable to a wide range of analytes, has been used for monitoring ppm levels of iodine and iodide in spacecraft water. Iodine is used as a biocide in spacecraft water. For these determinations, a water sample is passed through a membrane disk by means of a 10-mL syringe that is attached to a disk holder assembly. The disk, which is a polystyrene-divinylbenzene composite, is impregnated with poly(vinylpyrrolidone) (PVP), which exhaustively concentrates iodine as a yellow iodine-PVP complex. The amount of concentrated iodine is then determined in only 2 s by using a hand-held diffuse reflectance spectrometer by comparing the result with a calibration curve based on the Kubelka-Munk function. The same general procedure can be used to determine iodide levels after its facile and exhaustive oxidation to iodine by peroxymonosulfate (i.e., Oxone reagent). For samples containing both analytes, a two-step procedure can be used in which the iodide concentration is calculated from the difference in iodine levels before and after treatment of the sample with peroxymonosulfate. With this methodology, iodine and iodide levels in the 0.1-5.0 ppm range can be determined with a total workup time of approximately 60 s with a RSD of approximately 6%.

Non-NASA Center

Electrochemical method of controlling thiolate coverage on a conductive substrate such as gold

An electrochemical method for forming a partial monomolecular layer of a predetermined extent of coverage of a thiolate of the formula, XRS--, therein R can be a linear or branched chain hydrocarbon or an aromatic or the like and X can be any compatible end group, e.g., OH, COOH, CH.sub.3 or the like, upon a substrate such as gold, which involves applying in an electrochemical system a constant voltage preselected to yield the desired predetermined extent of coverage.

Porter, Marc D.

Electrochemical Deposition Of Thiolate Monolayers On Metals

Electrochemical method devised for coating metal (usually, gold) surfaces with adherent thiolate monolayers. Affords greater control over location and amount of material deposited and makes it easier to control chemical composition of deposits. One important potential use for this method lies in fabrication of chemically selective thin-film resonators for microwave oscillators used to detect pollutants: monolayer formulated to bind selectively pollutant chemical species of interest, causing increase in mass of monolayer and corresponding decrease in frequency of resonance. Another important potential use lies in selective chemical derivatization for purposes of improving adhesion, lubrication, protection against corrosion, electrocatalysis, and electroanalysis.

Porter, Marc D.

Novel approaches to the construction of miniaturized analytical instrumentation

This paper focuses on the design, construction, preliminary testing, and potential applications of three forms of miniaturized analytical instrumentation. The first is an optical fiber instrument for monitoring pH and other cations in aqueous solutions. The instrument couples chemically selective indicators that were immobilized at porous polymeric films with a hardware package that provides the excitation light source, required optical components, and detection and data processing hardware. The second is a new form of a piezoelectric mass sensor. The sensor was fabricated by the deposition of a thin (5.5 micron) film of piezoelectric aluminum nitride (AIN). The completed deposition process yields a thin film resonator (TFR) that is shaped as a 400 micron square and supports a standing bulk acoustic wave in a longitudinal mode at frequencies of approx. 1 GHz. Various deposition and vapor sorption studies indicate that the mass sensitivity of the TFR's rival those of the most sensitive mass sensors currently available, though offering such performance in a markedly smaller device. The third couples a novel form of liquid chromatography with microlithographic miniaturization techniques. The status of the miniaturization effort, the goal of which is to achieve chip-scale separations, is briefly discussed.

Porter, Marc D.

Novel approaches to the construction of miniaturized analytical instrumentation

This paper focuses on the design, construction, preliminary testing, and potential applications of three forms of miniaturized analytical instrumentation. The first is an optical fiber instrument for monitoring pH and other cations in aqueous solutions. The instrument couples chemically selective indicators that were immobilized at porous polymeric films with a hardware package that provides the excitation light source, required optical components, and detection and data processing hardware. The second is a new form of a piezoelectric mass sensor. The sensor was fabricated by the deposition of a thin (5.5 micron) film of piezoelectric aluminum nitride (AIN). The completed deposition process yields a thin film resonator (TFR) that is shaped as a 400 micron square and supports a standing bulk acoustic wave in a longitudinal mode at frequencies of approx. 1 GHz. Various deposition and vapor sorption studies indicate that the mass sensitivity of the TFR's rival those of the most sensitive mass sensors currently available, though offering such performance in a markedly smaller device. The third couples a novel form of liquid chromatography with microlithographic miniaturization techniques. The status of the miniaturization effort, the goal of which is to achieve chip-scale separations, is briefly discussed.

Porter, Marc D.