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At least 847 records · Page 47

Self-Supplied Liquid Injection Field Desorption/Ionization Ion Source for an Orthogonal Time-of-Flight Instrument

A new implementation of a dedicated ion source for field ionization (FI), field desorption (FD), and liquid injection field desorption/ionization (LIFDI) for the JEOL AccuTOF GC series of orthogonal-acceleration time-of-flight instruments is presented. In contrast to existing implementations, this third-party LIFDI probe and source combination does not require the exchange of the entire ion source comprising ion source block and lens stack to switch from electron ionization (EI) to LIFDI. Rather, the methods may be swapped conveniently by only exchanging the ion source block for a mechanical probe guide and inserting the LIFDI probe in place of the standard direct insertion probe (DIP) via the vacuum lock. Further, this LIFDI setup does not require any changes of the electronics or software of the AccuTOF mass spectrometer because it is self-supplied in terms of power supply, observation optics, and computer control. The setup offers advanced FI/FD/LIFDI control features such as emission-controlled emitter heating current and emitter flash baking during elongated runs as required for gas chromatography-FI-mass spectrometry (MS). The LIFDI source and probe and its operation are reported in detail. FI spectra of the volatile analytes toluene, heptane, and pentafluoroiodobenzene are presented. LIFDI operation is demonstrated for the analysis of the saturated hydrocarbon dotriacontane and the low-mass hydrocarbon polymers polystyrene 484 and polystyrene 1050. Further, the air-sensitive 2nd-generation Hoveyda–Grubbs catalyst is analyzed by LIFDI-MS. For comparison with long-established LIFDI instrumentation, some of the spectra obtained with the new setup are also compared with those from a double-focusing magnetic sector instrument. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Hedonic Price Estimates of Lake Water Quality: Valued Attribute, Instrumental Variables, and Ecological-Economic Benefits

We estimate the effect of lake water quality on residential housing prices using cross-sectional data on water clarity from 113 lakes across the United States. An instrumental-variables approach is developed to address potential endogeneity bias in the water-clarity variable. Three lake-based physical variables serve as instrumental variables: total nitrogen concentration in lake water, total phosphorus concentration in lake water, and water temperature near the lake surface. The econometric results include three methodological findings: the instruments are valid and strong; the ordinary-least-squares estimate of the coefficient on the water-clarity variable is unbiased; and water clarity is the attribute of water quality valued in the housing market. The estimated water-clarity effect shows that a one-tenth of a meter change in water clarity leads to a one-percent change in housing price, or an elasticity of 0.20 at mean clarity. Coupling this effect with estimates of an ecological production function, a lake-specific benefit index is developed that shows the effect on housing values of bringing lakes into compliance with the US Environmental Protection Agency's regional recommendations for phosphorous concentration in lake waters.

54 ENVIRONMENTAL SCIENCES↗

A proposal for assessing study quality: Biomonitoring, Environmental Epidemiology, and Short-lived Chemicals (BEES-C) instrument

The quality of exposure assessment is a major determinant of the overall quality of any environmental epidemiology study. The use of biomonitoring as a tool for assessing exposure to ubiquitous chemicals with short physiologic half-lives began relatively recently. These chemicals present several challenges, including their presence in analytical laboratories and sampling equipment, difficulty in establishing temporal order in cross-sectional studies, short- and longterm variability in exposures and biomarker concentrations, and a paucity of information on the number of measurements required for proper exposure classification. To date, the scientific community has not developed a set of systematic guidelines for designing, implementing and interpreting studies of short-lived chemicals that use biomonitoring as the exposure metric or for evaluating the quality of this type of research for WOE assessments or for peer review of grants or publications. We describe key issues that affect epidemiology studies using biomonitoring data on short-lived chemicals and propose a systematic instrument – the Biomonitoring, Environmental Epidemiology, and Short-lived Chemicals (BEES-C) instrument – for evaluating the quality of research proposals and studies that incorporate biomonitoring data on short-lived chemicals. Quality criteria for three areas considered fundamental to the evaluation of epidemiology studies that include biological measurements of short-lived chemicals are described: 1) biomarker selection and measurement, 2) study design and execution, and 3) general epidemiological study design considerations. We recognize that the development of an evaluative tool such as BEES-C is neither simple nor non-controversial. We hope and anticipate that the instrument will initiate further discussion/debate on this topic.

54 ENVIRONMENTAL SCIENCES↗

An ice lithography instrument

We describe the design of an instrument that can fully implement a new nanopatterning method called ice lithography, where ice is used as the resist. Water vapor is introduced into a scanning electron microscope (SEM) vacuum chamber above a sample cooled down to 110 K. The vapor condenses, covering the sample with an amorphous layer of ice. To form a lift-off mask, ice is removed by the SEM electron beam (e-beam) guided by an e-beam lithography system. Without breaking vacuum, the sample with the ice mask is then transferred into a metal deposition chamber where metals are deposited by sputtering. The cold sample is then unloaded from the vacuum system and immersed in isopropanol at room temperature. As the ice melts, metal deposited on the ice disperses while the metals deposited on the sample where the ice had been removed by the e-beam remains. The instrument combines a high beam-current thermal field emission SEM fitted with an e-beam lithography system, cryogenic systems, and a high vacuum metal deposition system in a design that optimizes ice lithography for high throughput nanodevice fabrication. The nanoscale capability of the instrument is demonstrated with the fabrication of nanoscale metal lines.

36 MATERIALS SCIENCE↗

Robotic reconnaissance platform. I. Spectroscopic instruments with rangefinders

In this paper, basic principles of the design and implementation of a portable, multi-functional scientific instrument, operating from a robotic reconnaissance mobile platform are discussed. The current version of the instrument includes a multi-gas laser sensor, multi-functional spectrometer, isotopes identifier, cameras, and rangefinder. An additional set of sensors monitors temperature, pressure, humidity, and background radiation. All components are installed on a mini-robotic platform, which provides data acquisition, processing, and transmittance. The design focuses on the development of calibration-free, reliable, low power-consumption devices. To create a highly survivable, accurate, and reliable instrument, a concept of an inhomogeneous sensory network has been developed. Such a network combines non-identical sensors and provides cross-use of information received from different sensors to describe environmental conditions, to choose appropriate algorithms of data processing, and to achieve high accuracy gas-concentration measurements. The system uses the same lasers to operate different optical devices such as sensors, rangefinders, spectrometers, and isotopes identifiers. Among the innovative elements described in this paper, are a calibration-free, laser multi-gas sensor with range-finding option; a high signal/noise ratio transmittance spectrometer; a single-frequency laser with nano-selector; and low repetition-rate femtosecond fiber lasers operating in near- and middle- infrared spectral ranges. New detailed analyses of absorption spectroscopy theoretical approximations made it possible to achieve high-accuracy gas-concentration measurements with miniature optical sensors.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

An instrument for 3D x-ray nano-imaging

We present an instrument dedicated to 3D scanning x-ray microscopy, allowing a sample to be precisely scanned through a beam while the angle of x-ray incidence can be changed. The position of the sample is controlled with respect to the beam-defining optics by laser interferometry. The instrument achieves a position stability better than 10 nm standard deviation. The instrument performance is assessed using scanning x-ray diffraction microscopy and we demonstrate a resolution of 18 nm in 2D imaging of a lithographic test pattern while the beam was defined by a pinhole of 3 {mu}m in diameter. In 3D on a test object of copper interconnects of a microprocessor, a resolution of 53 nm is achieved.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

A high precision instrument to measure angular and binocular deviation introduced by aircraft windscreens by using a shadow casting technique

Objects viewed through transparent sheets with residual non-parallelism and irregularity appear shifted and distorted. This distortion is measured in terms of angular and binocular deviation of an object viewed through the transparent sheet. The angular and binocular deviations introduced are particularly important in the context of aircraft windscreens and canopies as they can interfere with decision making of pilots especially while landing, leading to accidents. In this work, we have developed an instrument to measure both the angular and binocular deviations introduced by transparent sheets. This instrument is especially useful in the qualification of aircraft windscreens and canopies. It measures the deviation in the geometrical shadow cast by a periodic dot pattern trans-illuminated by the distorted light beam from the transparent test specimen compared to the reference pattern. Accurate quantification of the shift in the pattern is obtained by cross-correlating the reference shadow pattern with the specimen shadow pattern and measuring the location of the correlation peak. The developed instrument is handy to use and computes both angular and binocular deviation with an accuracy of less than {+-}0.1 mrad ( Almost-Equal-To 0.036 mrad) and has an excellent repeatability with an error of less than 2%.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Broadband wide-angle dispersion measurements: Instrumental setup, alignment, and pitfalls

The construction, alignment, and performance of a setup for broadband wide-angle dispersion measurements, with emphasis on surface plasmon resonance (SPR) measurements, are presented in comprehensive detail. In contrast with most SPR instruments working with a monochromatic source, this setup takes advantage of a broadband/white light source and has full capability for automated angle vs. wavelength dispersion measurements for any arbitrary nanostructure array. A cylindrical prism is used rather than a triangular one in order to mitigate refraction induced effects and allow for such measurements. Although seemingly simple, this instrument requires use of many non-trivial methods in order to achieve proper alignment over all angles of incidence. Here we describe the alignment procedure for such a setup, the pitfalls introduced from the finite beam width incident onto the cylindrical prism, and deviations in the reflected/transmitted beam resulting from the finite thickness of the sample substrate. We address every one of these issues and provide experimental evidences on the success of this instrument and the alignment procedure used.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Ultrasonic wave-based structural health monitoring embedded instrument

Piezoelectric sensors and actuators are the bridge between electronic and mechanical systems in structures. This type of sensor is a key element in the integrity monitoring of aeronautic structures, bridges, pressure vessels, wind turbine blades, and gas pipelines. In this paper, an all-in-one system for Structural Health Monitoring (SHM) based on ultrasonic waves is presented, called Phased Array Monitoring for Enhanced Life Assessment. This integrated instrument is able to generate excitation signals that are sent through piezoelectric actuators, acquire the received signals in the piezoelectric sensors, and carry out signal processing to check the health of structures. To accomplish this task, the instrument uses a piezoelectric phased-array transducer that performs the actuation and sensing of the signals. The flexibility and strength of the instrument allow the user to develop and implement a substantial part of the SHM technique using Lamb waves. The entire system is controlled using configuration software and has been validated through functional, electrical loading, mechanical loading, and thermal loading resistance tests.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Angular scattering of 1–50 keV ions through graphene and thin carbon foils: Potential applications for space plasma instrumentation

We present experimental results for the angular scattering of ∼1–50 keV H, He, C, O, N, Ne, and Ar ions transiting through graphene foils and compare them with scattering through nominal ∼0.5 μg cm{sup −2} carbon foils. Thin carbon foils play a critical role in time-of-flight ion mass spectrometers and energetic neutral atom sensors in space. These instruments take advantage of the charge exchange and secondary electron emission produced as ions or neutral atoms transit these foils. This interaction also produces angular scattering and energy straggling for the incident ion or neutral atom that acts to decrease the performance of a given instrument. Our results show that the angular scattering of ions through graphene is less pronounced than through the state-of-the-art 0.5 μg cm{sup −2} carbon foils used in space-based particle detectors. At energies less than 50 keV, the scattering angle half width at half maximum, ψ{sub 1/2}, for ∼3–5 atoms thick graphene is up to a factor of 3.5 smaller than for 0.5 μg cm{sup −2} (∼20 atoms thick) carbon foils. Thus, graphene foils have the potential to improve the performance of space-based plasma instruments for energies below ∼50 keV.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

The development and deployment of a ground-based, laser-induced fluorescence instrument for the in situ detection of iodine monoxide radicals

High abundances of iodine monoxide (IO) are known to exist and to participate in local photochemistry of the marine boundary layer. Of particular interest are the roles IO plays in the formation of new particles in coastal marine environments and in depletion episodes of ozone and mercury in the Arctic polar spring. This paper describes a ground-based instrument that measures IO at mixing ratios less than one part in 10{sup 12}. The IO radical is measured by detecting laser-induced fluorescence at wavelengths longer that 500 nm. Tunable visible light is used to pump the A{sup 2}Π{sub 3/2} (v{sup ′} = 2) ← X{sup 2}Π{sub 3/2} (v{sup ″} = 0) transition of IO near 445 nm. The laser light is produced by a solid-state, Nd:YAG-pumped Ti:Sapphire laser at 5 kHz repetition rate. The laser-induced fluorescence instrument performs reliably with very high signal-to-noise ratios (>10) achieved in short integration times (<1 min). The observations from a validation deployment to the Shoals Marine Lab on Appledore Island, ME are presented and are broadly consistent with in situ observations from European Coastal Sites. Mixing ratios ranged from the instrumental detection limit (<1 pptv) to 10 pptv. These data represent the first in situ point measurements of IO in North America.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

LabVIEW-based control software for para-hydrogen induced polarization instrumentation

The elucidation of cell metabolic mechanisms is the modern underpinning of the diagnosis, treatment, and in some cases the prevention of disease. Para-Hydrogen induced polarization (PHIP) enhances magnetic resonance imaging (MRI) signals over 10 000 fold, allowing for the MRI of cell metabolic mechanisms. This signal enhancement is the result of hyperpolarizing endogenous substances used as contrast agents during imaging. PHIP instrumentation hyperpolarizes Carbon-13 ({sup 13}C) based substances using a process requiring control of a number of factors: chemical reaction timing, gas flow, monitoring of a static magnetic field (B{sub o}), radio frequency (RF) irradiation timing, reaction temperature, and gas pressures. Current PHIP instruments manually control the hyperpolarization process resulting in the lack of the precise control of factors listed above, resulting in non-reproducible results. We discuss the design and implementation of a LabVIEW based computer program that automatically and precisely controls the delivery and manipulation of gases and samples, monitoring gas pressures, environmental temperature, and RF sample irradiation. We show that the automated control over the hyperpolarization process results in the hyperpolarization of hydroxyethylpropionate. The implementation of this software provides the fast prototyping of PHIP instrumentation for the evaluation of a myriad of {sup 13}C based endogenous contrast agents used in molecular imaging.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

A fluorescence XAFS measurement instrument in the soft x-ray region toward observation under operando conditions

X-ray absorption fine structure (XAFS) measurements are widely used for the analysis of electronic structure. Generally, XAFS in the soft X-ray region is measured under vacuum, but chemical structures under vacuum are typically different from those under operando conditions, where chemical species exhibit their function. Here, we developed an XAFS measurement instrument, as a step toward operando fluorescent, which yields XAFS measurement using synchrotron radiation in the soft X-ray region. We applied this method to analyze the local electronic structure of the sulfur atoms in L-cysteine in different pH solutions. In water at pH 7, the hydrogen atom does not dissociate from the thiol (-SH) group in L-cysteine, which forms a structure surrounded by and interacting with water molecules. The XAFS spectrum of L-cysteine in solution was altered by changing the pH. At pH 9, the hydrogen atom dissociated and a thiolate anion was formed. Although the -SH group was oxidized to SO{sub 4}{sup 2−} when L-cysteine was adsorbed on a metal surface and dried, no oxidation was observed in solution. This may be because the water molecules were densely packed and protected the -SH group from oxidation. Our results show that this instrument aimed toward operando fluorescence XAFS measurements in the soft X-ray region is useful for structural analysis of sulfur atoms in organic molecules in air and in solution. The instrument will be applied to the structural analysis of materials containing elements that have absorption edges in soft X-ray region, such as phosphorus and alkali metals (potassium and cesium). It will be also particularly useful for the analysis of samples that are difficult to handle under vacuum and materials that have specific functions in solution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High precision tilt stage as a key element to a universal test mirror for characterization and calibration of slope measuring instruments

The ultimate performance of surface slope metrology instrumentation, such as long trace profilers and auto-collimator based deflectometers, is limited by systematic errors that are increased when the entire angular range is used for metrology of significantly curved optics. At the ALS X-Ray Optics Laboratory, in collaboration with the HZB/BESSY-II and PTB (Germany) metrology teams, we are working on a calibration method for deflectometers, based on a concept of a universal test mirror (UTM) [V. V. Yashchuk et al., Proc. SPIE 6704, 67040A (2007)]. Potentially, the UTM method provides high performance calibration and accounts for peculiarities of the optics under test (e.g., slope distribution) and the experimental arrangement (e.g., the distance between the sensor and the optic under test). At the same time, the UTM calibration method is inherently universal, applicable to a variety of optics and experimental arrangements. In this work, we present the results of tests with a key component of the UTM system, a custom high precision tilt stage, which has been recently developed in collaboration with Physik Instrumente, GmbH. The tests have demonstrated high performance of the stage and its capability (after additional calibration) to provide angular calibration of surface slope measuring profilers over the entire instrumental dynamic range with absolute accuracy better than 30 nrad. The details of the stage design and tests are presented. We also discuss the foundation of the UTM method and calibration algorithm, as well as the possible design of a full scale UTM system.

47 OTHER INSTRUMENTATION↗

Calibration of space instruments at the Metrology Light Source

PTB has more than 20 years of experience in the calibration of space-based instruments using synchrotron radiation to cover the UV, VUV and X-ray spectral range. New instrumentation at the electron storage ring Metrology Light Source (MLS) opens up extended calibration possibilities within this framework. In particular, the set-up of a large vacuum vessel that can accommodate entire space instruments opens up new prospects. Moreover, a new facility for the calibration of radiation transfer source standards with a considerably extended spectral range has been put into operation. Besides, characterization and calibration of single components like e.g. mirrors, filters, gratings, and detectors is continued.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

A high-precision instrument for analyzing nonlinear dynamic behavior of bearing cage

The high-precision ball bearing is fundamental to the performance of complex mechanical systems. As the speed increases, the cage behavior becomes a key factor in influencing the bearing performance, especially life and reliability. This paper develops a high-precision instrument for analyzing nonlinear dynamic behavior of the bearing cage. The trajectory of the rotational center and non-repetitive run-out (NRRO) of the cage are used to evaluate the instability of cage motion. This instrument applied an aerostatic spindle to support and spin test the bearing to decrease the influence of system error. Then, a high-speed camera is used to capture images when the bearing works at high speeds. A 3D trajectory tracking software TEMA Motion is used to track the spot which marked the cage surface. Finally, by developing the MATLAB program, a Lissajous’ figure was used to evaluate the nonlinear dynamic behavior of the cage with different speeds. The trajectory of rotational center and NRRO of the cage with various speeds are analyzed. The results can be used to predict the initial failure and optimize cage structural parameters. In addition, the repeatability precision of instrument is also validated. In the future, the motorized spindle will be applied to increase testing speed and image processing algorithms will be developed to analyze the trajectory of the cage.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

The phase-contrast imaging instrument at the matter in extreme conditions endstation at LCLS

Here, we describe the phase-contrast imaging instrument at the Matter in Extreme Conditions (MEC) endstation of the Linac Coherent Light Source. The instrument can image phenomena with a spatial resolution of a few hundreds of nanometers and at the same time reveal the atomic structure through X-ray diffraction, with a temporal resolution better than 100 fs. It was specifically designed for studies relevant to high-energy-density science and can monitor, e.g., shock fronts, phase transitions, or void collapses. This versatile instrument was commissioned last year and is now available to the MEC user community.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

The LAMP instrument at the Linac Coherent Light Source free-electron laser

The Laser Applications in Materials Processing (LAMP) instrument is a new end-station for soft X-ray imaging, high-field physics, and ultrafast X-ray science experiments that is available to users at the Linac Coherent Light Source (LCLS) free-electron laser. While the instrument resides in the Atomic, Molecular and Optical science hutch, its components can be used at any LCLS beamline. The end-station has a modular design that provides high flexibility in order to meet user-defined experimental requirements and specifications. The ultra-high-vacuum environment supports different sample delivery systems, including pulsed and continuous atomic, molecular, and cluster jets; liquid and aerosols jets; and effusive metal vapor beams. It also houses movable, large-format, high-speed pnCCD X-ray detectors for detecting scattered and fluorescent photons. Multiple charged-particle spectrometer options are compatible with the LAMP chamber, including a double-sided spectrometer for simultaneous and even coincident measurements of electrons, ions, and photons produced by the interaction of the high-intensity X-ray beam with the various samples. Here in this paper we describe the design and capabilities of the spectrometers along with some general aspects of the LAMP chamber and show some results from the initial instrument commissioning.

47 OTHER INSTRUMENTATION↗