Development of a portable high-energy neutron spectrometer

The design of a portable high-energy (20-800 MeV) neutron spectrometer based on CsI or BaF2 is described. The particle discrimination properties of these scintillators allow the light-ion spallation products (p, d, t and alpha) from neutron interactions to be identified uniquely. One or more of the resulting pulse-height spectra can be unfolded to reveal the incident neutron spectrum. Dosimetric quantities can then be calculated based on the unfolded spectrum. Due to the high stopping power of these scintillators, modest-sized crystals are suitable for this application. Combined with advances in electronics, a lightweight instrument capable of on-line particle discrimination with a real-time display of neutron-induced count rate is feasible. Preliminary experimental data are presented, and the importance of validating MCNPX-generated response functions is discussed. A brief discussion on future work follows.     

Development of a method for the determination of human skin moisture using a portable near-infrared system.

In this study, a portable near-infrared (NIR) system was newly integrated with a photodiode array detector that has no moving parts, and this system has been successfully applied for the evaluation of human skin moisture. The good correlation between NIR absorbance and the absolute water content of separated hairless mouse skin, in vitro, was showed, depending on the water content (7.4-84.9%) using this portable NIR system. Partial least squares (PLS) regression was used for calibration with the 1150-1650-nm wavelength range. For practical use for the evaluation of human skin moisture, the PLS model for human skin moisture was developed in vivo using the portable NIR system on the basis of the relative water content values of stratum corneum from the conventional capacitance method. The PLS model showed a good correlation. This study indicated that the portable NIR system, as compared to conventional methods, could be a powerful tool for human skin moisture, which may be much more stable to environmental conditions, such as temperature and humidity. Furthermore, to confirm the performance of the newly integrated portable NIR system, a scanning-type conventional NIR spectrometer was used in the same experiments, and the results were compared.     

Regional difference of water content in human skin studied by diffuse-reflectance near-infrared spectroscopy: consideration of measurement depth

Diffuse reflectance (DF) spectra in the 1250-2500 nm region were measured in vivo for the skin of the forehead, cheek, jaw, elbow, volar forearm, palm, knee, and heel of seven healthy volunteers, using a Fourier transform near-infrared (FT-NIR) spectrophotometer with a fiber-optic probe. Apparent regional differences of water content in the skin, as estimated from the diffuse reflectance NIR spectra, are discussed in relation to the influence of measurement depth. The NIR spectra were collected with or without a 300 microm gap between the fiber-optic probe and the skin surface. For comparison, in vitro NIR spectra of stratum corneum sheets equilibrated at 41, 50, 63, and 81% relative humidity, at 25 degrees C, were also obtained. There was a difference in the ratio of the two water bands centered near 1450 nm and 1900 nm between the contact and non-contact measurements. In addition, regional differences of water content calculated from the peak height of the 1900 nm water band, which was normalized to the peak height of the 2175 nm amide band, were compared. The results of Monte Carlo simulation indicated that the apparent regional differences arise at least in part from differences in the measurement depth due to differences in specular reflection at the skin surface and in the thickness of the stratum corneum.     

Fourier transform near-infrared spectrometer using a corner-cube integrated prism scanning interferometer

This paper describes a Fourier transform (FT) near-infrared spectrometer that uses an integrated prism scanning interferometer whose optical paths are stabilized by corner cubes. A combination of corner cubes and a retroreflection mirror, which is sometimes used in the conventional interferometer for FT spectrometers, is adopted and adapted to the integrated prism scanning interferometer through a special design. Without any degradation of spectroscopic properties, the optical path in the interferometer is highly stabilized and the moving distance of the stage is halved. These advantages provide a robust and portable FT spectrometer for field use.     

Development of a near-infrared/mid-infrared dual-region spectrometer for online process analysis

A near-infrared (NIR) and mid-infrared (mid-IR) dual-region spectrometer having two immersion probes, a transmission probe for NIR, and an attenuated total reflection (ATR) probe for mid-IR has been developed for highly reliable process monitoring and deep process understanding. This spectrometer facilitates sequential acquisition of both NIR (10,000-4000 cm(-1)) and mid-IR (5000-1200 cm(-1)) spectra by switching the light path leading to the probes without the need for probe replacement. The use of a single light source and a single beam splitter enables achievement of a permanent alignment of the optical system and sequential data acquisition. The transmission NIR and ATR mid-IR probes designed and developed in the present study facilitate the acquisition of NIR/mid-IR spectra with optimized absorption intensities in both regions by simply placing the probes into a sample solution. The performance of the developed spectrometer was demonstrated in monitoring the ethanol fermentation process. NIR/mid-IR spectra of the fermentation solution with multiplicative scatter correction (MSC) represent the relative changes in the concentrations of glucose and ethanol in both regions. Principal component analysis (PCA) was performed on the MSC-treated spectra in the regions 6300-5650 cm(-1), 4850-4300 cm(-1), and 3500-2880 cm(-1) to detect the end-point of the fermentation as an example of process monitoring. For all the regions, the score plot of the first principal component (PC) indicates that the fermentation progresses with the fermentation time and stops after 210 minutes and thus the end-point of the fermentation exists at around 210 minutes. The loading plot indicates that all of the first PCs are the relative changes in the concentrations of glucose and ethanol. This result reveals that the same chemical changes are observed in both transmission NIR and ATR mid-IR spectra. Multiple and simultaneous analysis was also performed, and intensity change in light scattering relating the growth of yeasts was monitored by the NIR spectra.     

Ettringite and calcium sulfoaluminate cement: investigation of water content by near-infrared spectroscopy

Calcium sulfoaluminate (CSA) cement is a sulfate-based binder whose high-performance hydraulic behavior depends on the rapid formation of ettringite, when grinded clinker is hydrated in presence of gypsum. Ettringite is a calcium aluminum sulfate mineral characterized by high water content, estimated as 32 water molecules per formula unit. Three examples of utilization of near-infrared (NIR) spectroscopy are here shown. First of all, information on water distribution in pure ettringite was deduced and compared with infrared analyses. Then its thermal behavior has been followed up to 400 °C, allowing to improve the knowledge about water loss and thermal decomposition of this hydrated phase. Finally, the obtained results have been employed in order to follow hydration of CSA cement sample, demonstrating thus that NIR spectroscopy, being highly sensitive to water amount and distribution, can be an extremely useful tool for hydration studies.     

CHELSI: a portable neutron spectrometer for the 20-800 MeV region

CHELSI is a CsI-based portable spectrometer being developed at Los Alamos National Laboratory for use in high-energy neutron fields. Based on the inherent pulse shape discrimination properties of CsI(Tl), the instrument flags charged particle events produced via neutron-induced spallation events. Scintillation events are processed in real time using digital signal processing and a conservative estimate of neutron dose rate is made based on the charged particle energy distribution. A more accurate dose estimate can be made by unfolding the 2D charged particle versus pulse height distribution to reveal the incident neutron spectrum from which dose is readily obtained. A prototype probe has been assembled and data collected in quasi-monoenergetic fields at The Svedberg Laboratory (TSL) in Uppsala as well as at the Los Alamos Neutron Science Center (LANSCE). Preliminary efforts at deconvoluting the shape/energy data using empirical response functions derived from time-of-flight measurements are described.     

A least squares procedure for calculating the calibration constants of a portable gamma-ray spectrometer

In this study, a least squares procedure for calculating the calibration constants of a portable gamma-ray spectrometer using the general inverse matrix method is presented. The procedure weights the model equations fitting to the calibration data, taking into account the variances in the counting rates and in the radioactive standard concentrations. The application of the described procedure is illustrated by calibrating twice the same gamma-ray spectrometer, with two independent data sets collected approximately 18 months apart in the same calibration facility.     

On-line near-infrared spectrometer to monitor urea removal in real time during hemodialysis

The ex vivo removal of urea during hemodialysis treatments is monitored in real time with a noninvasive near-infrared spectrometer. The spectrometer uses a temperature-controlled acousto optical tunable filter (AOFT) in conjunction with a thermoelectrically cooled extended wavelength InGaAs detector to provide spectra with a 20 cm(-1) resolution over the combination region (4000-5000 cm(-1)) of the near-infrared spectrum. Spectra are signal averaged over 15 seconds to provide root mean square noise levels of 24 micro-absorbance units for 100% lines generated over the 4600-4500 cm(-1) spectral range. Combination spectra of the spent dialysate stream are collected in real-time as a portion of this stream passes through a sample holder constructed from a 1.1 mm inner diameter tube of Teflon. Real-time spectra are collected during 17 individual dialysis sessions over a period of 10 days. Reference samples were extracted periodically during each session to generate 87 unique samples with corresponding reference concentrations for urea, glucose, lactate, and creatinine. A series of calibration models are generated for urea by using the partial least squares (PLS) algorithm and each model is optimized in terms of number of factors and spectral range. The best calibration model gives a standard error of prediction (SEP) of 0.30 mM based on a random splitting of spectra generated from all 87 reference samples collected across the 17 dialysis sessions. PLS models were also developed by using spectra collected in early sessions to predict urea concentrations from spectra collected in subsequent sessions. SEP values for these prospective models range from 0.37 mM to 0.52 mM. Although higher than when spectra are pooled from all 17 sessions, these prospective SEP values are acceptable for monitoring the hemodialysis process. Selectivity for urea is demonstrated and the selectivity properties of the PLS calibration models are characterized with a pure component selectivity analysis.     

Determining water in ammonium nitrate with Fischer's reagent

Translated from Izmeritel'naya Tekhnika, No. 3, pp. 59–60, March, 1988.     

水中汞的电感耦合等离子体-质谱法测定

为解决水中汞不稳定以及易吸附而引起记忆效应的问题,建立分析水中汞的电感耦合等离子体质谱新方法,汞标准溶液中加金形成金汞齐,采用200μg/LAu2+-5%HNO3溶液作为清洗液,选取Rh103作为内标元素。结果标明:在79d内,汞溶液的标准曲线稳定,其相关系数在0.9993⁰.9998之间,仪器检出限在1.15×10-30.9998之间,仪器检出限在1.15×10-3³.11×10-2μg/L范围内。该方法分析水中痕量汞具有检出限低、数据准确性高、再现性好的特点,所用试剂种类少且毒性小。     

Analysis of captan on nitrile glove surfaces using a portable attenuated total reflection fourier transform infrared spectrometer

This study developed a method to produce uniform captan surface films on a disposable nitrile glove for quantitation with a portable attenuated total reflection Fourier transform infrared (ATR-FTIR) spectrometer. A permeation test was performed using aqueous captan formulation. Uniform captan surface films were produced using solvent casting with 2-propanol and a 25 mm filter holder connected to a vacuum manifold to control solvent evaporation. The coefficient of variation of the reflectance at 1735 +/- 5 cm(-1) was minimized by selection of the optimum solvent volume, airflow rate, and evaporation time. At room temperature, the lower to upper quantifiable limits were 0.31-20.7 microg/cm2 (r = 0.9967; p < or = 0.05) for the outer glove surface and 0.55-17.5 microg/cm2 (r = 0.9409; p < or = 0.05) for the inner surface. Relative humidity and temperature did not affect the uncoated gloves at the wavelength of captan analysis. Glove screening using ATR-FTIR was necessary as a control for between-glove variation. Captan permeation, after 8 hours exposure to an aqueous concentration of 217 mg/mL of Captan 50-WP, was detected at 0.8 +/- 0.3 microg/cm2 on the inner glove surface. ATR-FTIR can detect captan permeation and can determine the protectiveness of this glove in the field.     

水中汞的电感耦合等离子体-质谱法测定

为解决水中汞不稳定以及易吸附而引起记忆效应的问题,建立分析水中汞的电感耦合等离子体质谱新方法,汞标准溶液中加金形成金汞齐,采用200μg/LAu2＋-5%HNO3溶液作为清洗液,选取Rh103作为内标元素。结果标明：在79d内,汞溶液的标准曲线稳定,其相关系数在0.9993~0.9998之间,仪器检出限在1.15×10-3~3.11×10-2μg/L范围内。该方法分析水中痕量汞具有检出限低、数据准确性高、再现性好的特点,所用试剂种类少且毒性小。     

Explosives detection with a frequency modulation spectrometer

An explosives detection instrument was designed and tested at SRI International. The instrument uses frequency modulation spectroscopy with midinfrared lead-salt diode lasers to perform high-sensitivity detection of characteristic nitrogen-containing decomposition products of explosives. Ultimately, the instrument should be capable of detecting and identifying subpicogram levels of plastic explosives, which would be suitable for screening passengers at airports. Using the laboratory breadboard instrument and two different explosive vapor generators, we demonstrated a lower limit of detection of 5-10 pg for cyclotrimethylene trinitramine and linearity of the signal over an order of magnitude.     

Hyperboloid mass spectrometer with a truncated trap

A hyperboloid mass spectrometer is proposed in which the analyzer is a three-dimensional ion trap truncated by the plane z=0. The mass peaks for different operating regimes of the mass analyzer are constructed from the results of a numerical modeling of the electric field and a simulation of the process of sorting the charged particles. The results serve as a basis for the construction of a hyperboloid mass spectrometer with a simple electrode system and a high resolving power. Pis’ma Zh. Tekh. Fiz. 25, 51–56 (May 26, 1999)     

石墨炉原子吸收法测定废水中铅的不确定度分析

对石墨炉原子吸收法测定废水中铅的不确定度进行评定,系统分析不确定度的来源,计算出该方法的不确定度,为评价方法的可靠性和分析的准确性提供参考。