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 ∼60 s with a RSD of ∼6%

Rapid, Low Level Determination of Silver(I) in Drinking Water by Colorimetric–solid-phase Extraction

A rapid, highly sensitive two-step procedure for the trace analysis of silver(I) is described. The method is based on: (1) the solid-phase extraction (SPE) of silver(I) from a water sample onto a disk impregnated with a silver-selective colorimetric reagent, and (2) the determination of the amount of complexed analyte extracted by the disk by diffuse reflectance spectroscopy (DRS). This method, called colorimetric–solid-phase extraction (C–SPE), was recently shown effective in determining low concentrations (0.1–5.0 mg/ml) of iodine and iodide in drinking water. This report extends C–SPE to the trace (∼4 μg/l) level monitoring of silver(I) which is a biocide used on the International Space Station (ISS). The determination relies on the manually driven passage of a water sample through a polystyrene–divinylbenzene disk that has been impregnated with the colorimetric reagent 5-(p-dimethylaminobenzylidene) rhodanine (DMABR) and with an additive such as a semi-volatile alcohol (1,2-decanediol) or nonionic surfactant (Brij 30). The amount of concentrated silver(I) is then determined in a few seconds by using a hand-held diffuse reflectance spectrometer, with a total sample workup and readout time of ∼60 s. Importantly, the additive induces the uptake of water by the disk, which creates a local environment conducive to silver(I) complexation at an extremely high concentration factor (∼800). There is no detectable reaction between silver(I) and impregnated DMABR in the absence of the additive. This strategy represents an intriguing new dimension for C–SPE in which additives, directly loaded in the disk material, provide a means to manipulate the reactivity of the impregnated reagent

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

Chemical sensor and coating for same

An acoustic wave based-chemical sensor utilizing a crystal substrate and a coating of at least two blended materials is disclosed. The blended materials comprise a combination of (a) a high glass transition temperature polymer or a material of high melting point, and (b) a low glass transition temperature polymer or a material having a low melting point. Transducers are connected to the crystal substrate to generate an alternating potential across the crystal substrate, which in turn causes the crystal to resonate due to the converse piezoelectric effect. The blended coating absorbs the analyte, thus changing the mass of the chemical sensor, and accordingly changing its resonant frequency. The transducers detect this change in resonant frequency to indicate that the analyte is present. The use of blended materials results in a thicker coating combining the preferred properties of the blend constituents, such as improved detection sensitivities, faster response times, less acoustic wave damping, and higher operational temperature ranges

Dual-wavelength photometer and fiber optic sensor probe

A dual wavelength optical sensor for measuring chemical properties of a particular quantity, the optical sensor including a sensor probe having a thin sensing film whose optical characteristics are responsive to the chemical properties of the measured quantity The United States Government has certain rights in this invention pursuant to Contract No. ITA87-02 between the U.S. Department of Commerce and Iowa State University

Fluid pumping system based on electrochemically-induced surface tension changes

A pump for exerting a pumping force on a fluid in an attached conduit, the pump being actuated by a voltage from a power supply, the pump comprising a liquid metal pool, a containment vessel for confining the pool, an inner tubular member in hydraulic contact with the attached conduit and with an open end disposed in the pool to divide a free upper surface of the pool into an actuation surface and a working surface, an electrolyte in contact with the actuation surface, an electrode in contact with the electrolyte, and an electrode in contact with the pool, such that application of a voltage to the electrodes causes a surface tension change in the actuation surface and a resulting height change in the working surface, whereby a pumping action is transferred to the fluid in the attached conduit

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)

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

System and method for detecting cells or components thereof

A system and method for detecting a detectably labeled cell or componentthereof in a sample comprising one or more cells or components thereof, at least one cell or component thereof of which is detectably labeled with at least two detectable labels. In one embodiment, the method comprises: (i) introducing the sample into one or more flow cells of a flow cytometer, (ii) irradiating the sample with one or more light sources that are absorbed by the at least two detectable labels, the absorption of which is to be detected, and (iii) detectingsimultaneously the absorption of light by the at least two detectable labels on the detectably labeled cell or component thereof with an array of photomultiplier tubes, which are operably linked to two or more filters that selectively transmit detectable emissions from the at least two detectable labels