Christopher B. Winstead

Optical-fiber sensor using tailored porous sol-gel fiber core

A new concept in optical-fiber chemical sensors, the active fiber core optical sensor (AFCOS), is presented. In this sensor, the fiber core acts as a transducer. The sensitivity of an AFCOS sensor is compared with that of an active coating [evanescent wave (EW)] based optical-fiber sensor. Requirements for a fiber core to act as a chemical sensor are discussed. Novel techniques for making a porous sol-gel silica fiber, doping chemical reagents into the fiber, and constructing a chemical sensor using the porous fiber as a transducer have been developed. The microstructure of the fabricated sol-gel silica fiber and the effect of the fibers microstructure on the capability of the porous sol-gel silica fiber for guiding light are discussed. A humidity sensor employing a CoCl/sub 2/-doped porous sol-gel fiber as a transducer has been constructed as an example. The test results for the humidity sensor verified a theoretical analysis indicating that an optical-fiber chemical sensor using an active fiber core as a transducer has a much higher sensitivity than that of an EW-based sensor.

Cavity Ringdown Spectroscopy for Diagnostic and Analytical Measurements in an Inductively Coupled Plasma

The use of cavity ringdown spectroscopy (CRDS) for atomic absorption measurements in a 27-MHz low-power argon inductively coupled plasma (ICP) is described. These results are used to demonstrate the utility of CRDS for both plasma diagnostic and analytical measurements. In these experiments, an aqueous solution of lead was introduced into a modified torch designed to enhance the ICP conditions for atomic absorption measurements. Absorption intensity characteristics of the lead 283.3-nm absorption line as a function of observation height and lateral position in the plasma were recorded for three different ICP powers (700, 500, and 200 W). The radial distribution of the ground-state lead atom density was derived from Abel inversion of the lateral measurements. At the novel 200 W operating condition, spectral line shapes vs. height and lateral position were fitted to Voigt profiles. Line-of-sight values of the gas kinetic temperature and electron density at different plasma locations were estimated from Gaussian and Lorentzian broadening components, respectively. The results are discussed and compared with those from other methods. The unique flexibility of CRDS for atomic and ionic absorption measurements in an ICP and the potential application of the ICP-CRDS technique for analytical measurements are demonstrated. Analytical results are compared with theoretical estimates of the lead detection limit.

Optical fiber sensor using tailored porous sol-gel fiber core

Novel techniques for fabricating a porous sol-gel fiber, doping chemical reagent into the fiber, and constructing an optical fiber chemical sensor using the porous fiber as a transducer, have been invented. A moisture sensor employing a CoCl/sub 2/ doped porous sol-gel fiber as a transducer has been constructed as an example. The test result of the moisture sensor verified a conclusion from theoretical analysis. That is an optical fiber chemical sensor using an active fiber core as a transducer should have a much higher sensitivity than that of active coating based sensor.

Diode Laser Microwave Induced Plasma Cavity Ringdown Spectrometer: Performance and Perspective

Recent studies combining an atmospheric-pressure plasma source (inductively coupled plasma or microwave induced plasma) with cavity ringdown spectroscopy (plasma-CRDS) have indicated significant promise for ultra-sensitive elemental measurements. Initial plasma-CRDS efforts employed an inductively coupled plasma as the atomization source and a pulsed laser system as the light source. In an effort to improve the portability and reduce the cost of the system for application purposes, we have modified our approach to include a compact microwave induced plasma and a continuous wave diode laser. A technique for controlling the coupling of the continuous wave laser to the ringdown cavity has been implemented using a standard power combiner. No acouto-optic modulator or cavity modulation is required. To test the system performance, diluted standard solutions of strontium (Sr) were introduced into the plasma by an in-house fabricated sampling device combined with an ultrasonic nebulizer. SrOH radicals were genera...

Measurements of OH Radicals in a Low-Power Atmospheric Inductively Coupled Plasma by Cavity Ringdown Spectroscopy

Cavity ringdown spectroscopy is applied to line-of-sight measurements of OH radicals in an atmospheric-pressure argon inductively coupled plasma, operating at low power (200 W) and low gas flows (∼18 liters/min). Density populations of the single S21(1) rotational line in the OH A2Σ+–X2Π (0–0) band are extracted from the measured line-of-sight absorbance. Plasma gas kinetic temperatures, derived from the recorded line shapes of the S21(1) line, ranged from 1858 to 2000 K with an average uncertainty of 10%. Assuming local thermodynamic equilibrium, an assumption supported by the comparison of the experimental and simulated spectra, the spatially averaged total OH number density at different observation heights was determined to be in the range of 1.7 × 1020–8.5 × 1020 (m−3) with the highest OH density in the plasma tail. This work demonstrates that ringdown spectra of the OH radical may be used both as a thermometer for high-temperature environments and as a diagnostic tool to probe the thermodynamic properties of plasmas.

Isotopic Measurements of Uranium Using Inductively Coupled Plasma Cavity Ringdown Spectroscopy

Inductively coupled plasma cavity ringdown spectroscopy (ICP-CRDS) is applied to isotopic measurements of uranium. We have successfully obtained the isotopic-resolved spectra of uranium at three different atomic/ionic transition lines, 286.57, 358.49, and 409.01 nm. Of the three lines, the largest isotope shift of approximately 9 pm was measured at the 286.57 ionic line. Isotopic-resolved spectra were recorded in ratio of 1:1 (235U/238U, 2.5 μg/mL) and at the natural abundance ratio of 0.714% (235U/238U, 1.25 μg/mL 235U). The smallest measurable isotope shift of approximately 3 pm was determined for the 409.01 nm ion spectral line. Detection limits (DL) were obtained under optimized ICP operating conditions to be in the range of 70∼150 ng/mL, except for the 238U component of the 286.57 nm line (300 ng/mL). This latter result was determined to be due to a strong, previously unreported, absorption interference from the argon plasma. The 235U isotope component (DL 70 ng/mL) was found to be unaffected. This work demonstrates the applicability of ICP-CRDS for uranium isotopic measurements. The potential of development of a field-deployable, on-line uranium isotope monitor using plasma-CRDS is discussed.

Porous solgel fiber as a transducer for highly sensitive chemical sensing.

A novel solgel process for making porous silica fiber and doping the fiber core with sensing material is described. A CoCl(2) -doped solgel fiber was fabricated and was used to construct an active-core optical fiber moisture sensor. Test results show that the sensitivity of the active-core optical fiber sensor is much higher than that of an evanescent-wave-based optical fiber sensor.

Determination of elemental mercury by cavity ringdown spectrometry

Cold vapor cavity ringdown spectroscopy has been successfully applied to the detection of elemental mercury. Using an absorption cell 0.18 m in length, detection limits of 0.027 and 0.12 ng were obtained using peak area and peak height measurements, respectively. For the peak area measurement, this corresponds to a gas phase concentration of less than 25 ng m−3. For comparison, using a similar absorption cell, standard AAS yielded a Hg detection limit (peak height) of 9 ng, (gas phase concentration of ≡ 8.3 μg m−3).

Cavity ringdown measurements of mercury and its hyperfine structures at 254 nm in an atmospheric microwave plasma: spectral interference and analytical performance

The plasma-cavity ringdown spectroscopic (Plasma-CRDS) technique has been demonstrated as a powerful tool for elemental and isotopic measurements in recent studies. This work reports the first application of plasma-CRDS to measurements of elemental mercury and its stable isotopes at the 254 nm transition under atmospheric conditions. A microwave-induced plasma (MIP) operating at 80–100 W is used to generate Hg atoms from standard HgCl2 solutions diluted by 2% nitric acid solvent. It is found that a background absorption, attributed to the overlap of two broadened rovibrational transitions R21(21) and P1(15) of the OH A-X (3-0) band located at 253.65 nm, generates significant spectral interference with the absorption peak of Hg at 254 nm. With an optimized operating condition, including plasma powers, gas flow rates, and laser beam positions in the plasma, the detection sensitivity of Hg is determined to be 9.1 ng ml−1 in aqueous solution, equivalently 221 pptv in the gas phase; this detection limit is approximately 2-fold higher than the theoretical detection limit, 126 pptv, which was estimated by using the parameters of the instrument system and the calculated absorption cross-section, 2.64 × 10−14 cm2 atom−1, of the transition under atmospheric plasma conditions. High-resolution spectral scans show a clear contour of the stable isotopes of the 254 nm transition. The technical challenges encountered and the potential for further development of the Hg analyzer using the MIP-CRDS technique are discussed.

A highly sensitive hexachromium monitor using water core optical fiber with UV LED

A simply structured, cheap hexachromium monitor was developed. The monitor is based on UV/VIS absorption technique. A 2-m long water core optical fiber was employed as a long path length sample cell and a UV light emitting diode (LED) was used as a light source. The emission profile of the UV LED fits very well with the absorption spectrum of chromate ions in water. Therefore, the light-dispersing element, which is usually used in an optical spectrometer, is not necessary in this monitor design. The water core fiber as a long path length makes the monitor highly sensitive for hexachromium detection. This monitor is specific for hexachromium detection without interference from tri-valence chromium ions. A detection limit of 0.1 ng Cr(VI) ml(-1) was obtained with this simple monitor.