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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.

One of the long-standing concerns in space exploration is the presence of trace organic contaminants in recycled spacecraft water supplies. At present, water samples on the International Space Station (ISS) are collected at regular intervals, stored in Teflon™-lined containers, and returned to Earth for characterization. This approach, while effective in defining water quality, has several notable problems. First, this method of archiving removes a significant volume of the ISS water supply. Second, the archived water consumes valuable cargo space in returning Shuttle and Soyuz vehicles. Third, the organic contaminants present in the collected samples may degrade upon extended storage. The latter problem clearly compromises sample integrity. Upon return to Earth, sample degradation is minimized by refrigeration. Due to present resource constraints, however, refrigeration is not a viable option in space.

A sorption-spectrophotometric platform for the concentration and subsequent quantification of biocides in spacecraft drinking water is described. This methodology, termed Colorimetric Solid Phase Extraction (C-SPE), is based on the extraction of analytes onto a membrane impregnated with a colorimetric reagent. Quantification of the extracted analytes is accomplished by interrogating the surface of the membrane with a commercially available diffuse reflectance spectrophotometer. Ground-based experiments have shown that C-SPE is a viable means to determine biocide concentrations in the range commonly found in water samples from the Space Shuttle and the International Space Station (ISS). This paper details efforts to advance C-SPE closer to space flight qualification and ISS implementation, starting with the modification of the ground based biocide detection platform to simplify operation in a microgravity environment.

Preliminary results on the development of quick, simple analytical method for the low level of lead(II) in water samples are described. The method concentrates lead(II) on a small solid-phase extraction disk, which is then quantified directly on the disk by diffuse reflectance spectroscopy (DRS). This method, termed colorimetric solid-phase extraction (C-SPE), requires only 1–2 min for complete workup and is suitable for use in a wide range of applications, including the microgravity environment on the International Space Station. The procedure first adds an excess of potassium iodide to a 10.0 mL sample at a pH of 3.0–3.5 to produce the anionic PbI42− colored complex, which is exhaustively extracted by the disk that was previously impregnated with cetylpyridinium chloride (CPC). The amount of complex extracted is then determined at 420 nm by a hand-held DRS instrument.

Contamination of spacecraft water by heavy metals, such as cadmium and lead, is of growing concern. As a consequence, there is need for a rapid, on-board, easy-to-use method for the determination of cadmium(II) at low ppb levels in spacecraft drinking water supplies. This paper describes the preliminary development of a method for the selective, low level determination of cadmium(II) based on colorimetric-solid phase extraction (C-SPE) [1, 2]. In C-SPE, an analyte is extracted from a water sample onto a membrane that has been previously impregnated with a colorimetric reagent, and then quantified as its colorimetric complex directly on the membrane surface using diffuse reflectance spectroscopy. Results from preliminary tests that screened the performance of 1-(4-nitrophenyl)-3-(4-phenyl-azophenyl)triazene (cadion), and organic dyes, rhodamine B, brilliant green, and methyl violet as colorimetric reagents for potential use in a C-SPE analysis of cadmium(II) are described.

The need to preserve crew health during space missions, combined with the level of demand on both crew time and cargo space, dictates the development of fast, facile methods capable of monitoring trace quantities of several analytes in spacecraft water. This presentation describes our efforts to address this need by using Multiplexed Colorimetric Solid Phase Extraction (MC-SPE). MC-SPE is a sorption-spectrophotometric platform based upon the extraction of analytes onto membranes impregnated with selective colorimetric agents. Quantification is accomplished using Kubelka-Munk values calculated from the diffuse reflectance spectrum of the complex on the surface of the membrane and calibration curves. In traditional C-SPE, concentration factors of up to 1000 can be realized for a single analysis, yielding low detection limits (ppb – ppm range) with a total analysis time of 75–90 s. Herein, we describe the performance and continued refinement of the MC-SPE platform.

We are developing a spacecraft water quality monitoring system based on measuring the change in diffuse reflectance of indicator disks following exposure to a water sample. The most widely used approach for deriving quantitative information from a diffuse reflectance spectrum involves an initial Kubelka-Munk transformation of the reflectance data. Provided the assumptions underlying the transformation are satisfied, the magnitude of the resulting function varies linearly with analyte concentration. We measure diffuse reflectance spectra using a commercial-off-the-shelf handheld spectrophotometer designed for color matching applications. Spectra are currently downloaded and transformed to obtain the value of the Kubelka-Munk function at a detection wavelength diagnostic of the analyte. This value is then used to quantify the analyte via a standard response curve.

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 [1, 2], 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 analyzed 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).

We are developing a drinking water test kit based on colorimetric-solid phase extraction (C-SPE) for use onboard the International Space Station (ISS) and on future Lunar and/or Mars missions. C-SPE involves measuring the change in diffuse reflectance of indicator disks following their exposure to a water sample. We previously demonstrated the effectiveness of C-SPE in measuring iodine in microgravity. This analytical method has now been extended to encompass the measurement of total I (i.e., iodine, iodide, and triiodide). This objective was accomplished by introducing an oxidizing agent to convert iodide and triiodide to iodine, which is then measured using the indicator disks previously developed for iodine. We report here the results of a recent series of C-9 microgravity tests of this method. The results demonstrate that C-SPE technology is poised to meet the total I monitoring requirements of the international space program.

Aqueous silver(I) is added at trace levels (0.1 – 1.0 mg/L) to spacecraft potable water as a biocide. Development of a method that can be deployed on orbit and in future Lunar and Mars missions is therefore central to maintenance of safe drinking water and crew health. To address this need, our laboratory has created an analytical technique that couples a selective sorption process based on solid phase extraction (SPE) with the quantitative measurement of the extract by a hand-held diffuse reflection spectrophotometer. This technique, referred to as colorimetric-solid phase extraction (C-SPE), enables the low level detection (limit of detection ∼5 ppb) of silver(I) by metering 1.0 mL of a water sample through a reagent-impregnated (i.e., 5-(p-dimethyl-aminobenzylidene)rhodanine, DMABR) SPE membrane. The total workup time for the analysis is only 60-90 s.