An International Marine-Atmospheric 222Rn Measurement Intercomparison in Bermuda Part I: NIST Calibration and Methodology for Standardized Sample Additions

As part of an international ²²²Rn measurement intercomparison conducted at Bermuda in October 1991, NIST provided standardized sample additions of known, but undisclosed (“blind”) ²²²Rn concentrations that could be related to U.S. national standards. The standardized sample additions were obtained with a calibrated ²²⁶Ra source and a specially-designed manifold used to obtain well-known dilution factors from simultaneous flow-rate measurements. The additions were introduced over sampling periods of several hours (typically 4 h) into a common streamline on a sampling tower used by the participating laboratories for their measurements. The standardized ²²²Rn activity concentrations for the intercomparison ranged from approximately 2.5 Bq · m⁻³ to 35 Bq · m⁻³ (of which the lower end of this range approached concentration levels for ambient Bermudian air) and had overall uncertainties, approximating a 3 standard deviation uncertainty interval, of about 6 % to 13 %. This paper describes the calibration and methodology for the standardized sample additions.     

Thermal-Conductivity Apparatus for Steady-State,Comparative Measurement of Ceramic Coatings

An apparatus has been developed to measure the thermal conductivity of ceramic coatings. Since the method uses an infrared microscope for temperature measurement, coatings as thin as 20 μm can, in principle, be measured using this technique. This steady-state, comparative measurement method uses the known thermal conductivity of the substrate material as the reference material for heat-flow measurement. The experimental method is validated by measuring a plasma-sprayed coating that has been previously measured using an absolute, steady-state measurement method. The new measurement method has a relative standard uncertainty of about 10 %. The measurement of the plasma-sprayed coating gives 0.58 W·m⁻¹·K^−l which compares well with the 0.62 W·m⁻¹·K^−l measured using the absolute method.     

Results of a CIE Detector Response Intercomparison

A total of fifteen laboratories participated in the CIE detector response intercomparison which was designed to assess the level of agreement among participating laboratories in the absolute measurement (with respect to SI) of photodetector response in the visible spectral region. Most participants were either commercial laboratories or university laboratories with the National Institute of Standards and Technology (NIST) serving as the host laboratory. Each laboratory determined the absolute response of each of two silicon photodiode radiometers which were designed for the intercomparison by NIST. Approximately two-thirds of the laboratories reported response values which agreed with the NIST values to within ±1.0% at the two wavelengths of 488 and 633 nm.³     

Interlaboratory Comparison of Magnetic Thin Film Measurements

A potential low magnetic moment standard reference material (SRM) was studied in an interlaboratory comparison. The mean and the standard deviation of the saturation moment m_s, the remanent moment m_r, and the intrinsic coercivity H_c of nine samples were extracted from hysteresis-loop measurements. Samples were measured by thirteen laboratories using inductive-field loopers, vibrating-sample magnetometers, alternating-gradient force magnetometers, and superconducting quantum-interference-device magnetometers. NiFe films on Si substrates had saturation moment measurements reproduced within 5 % variation among the laboratories. The results show that a good candidate for an SRM must have a highly square hysteresis loop (m_r/m_s > 90 %), H_c ≈ 400 A·m⁻¹ (5 Oe), and m_s ≈ 2 × 10⁻⁷ A·m² (2 × 10⁻⁴ emu).     

Radiochemical evaluation of groundwater around Mika uranium mineralization and environs

Seventeen groundwater samples around Mika uranium mineralization were collected, and the ²²²Rn concentrations were measured using a DURRIDGE RAD7 electronic radon detector. The ²²²Rn concentrations in the groundwater ranged from 2350 to 46200 Bq m^–3 with an average of 29 400 Bq m^–3. The results show that 76.5% of the groundwater samples collected have ²²²Rn concentrations far above the US EPA maximum contaminant level (MCL) of 11.1 Bq L^–1 (for states without radon monitoring policy and enhanced indoor air programs), and only 23.5% have lower values. On the other hand, all the ²²²Rn levels were below the MCL of 100 Bq L^–1, recommended by EU as the level that warrants consideration of possible remedial actions. Borehole samples show relatively higher ²²²Rn concentrations than samples collected from open wells. The annual effective dose due to ingestion (H _ing) of ²²²Rn in the groundwater ranged from 0.05 to 0.92 mSv, with an average of 0.59 mSv. These values are within the ICRP recommended reference level of 1 mSv year^–1 for the intake of the radionuclide in water by the general public for a prolonged exposure.     

Thermal Conductivity of Magnesium Oxide From Absolute,Steady-State Measurements

The thermal conductivity of polycrystalline magnesium oxide has been measured over the temperature range from 400 K to 1300 K using a modified guarded-hot-plate design. Three different thicknesses of specimens having 93 % of theoretical density were tested to verify the operation, accuracy, and reproducibility of our apparatus. The measured thermal conductivity ranges from 30 W · m⁻¹ · K⁻¹ down to 8 W · m⁻¹ · K⁻¹ and has an inverse-temperature functionality. The results agree well with literature values for this material.     

Preparation and Calibration of Carrier-Free 209Po Solution Standards

Carrier-free ²⁰⁹Po solution standards have been prepared and calibrated. The standards, which will be disseminated by the National Institute of Standards and Technology as Standard Reference Material SRM 4326, consist of (5.1597 ±0.0024) g of a solution of polonium in nominal 2 mol · L⁻¹ hydrochloric acid (having a solution density of (1.031±0.004) g · mL⁻¹ at 22 °C) that is contained in 5 mL flame-sealed borosilicate glass ampoules, and are certified to contain a ²⁰⁹Po alpha-particle emission rate concentration of (85.42±0.29) s⁻¹ · g⁻¹ (corresponding to a ²⁰⁹Po activity concentration of (85.83 ±0.30) Bq · g⁻¹) as of the reference time of 1200 EST 15 March 1994. The calibration was based on 4πα liquid scintillation (LS) measurements with two different LS counting systems and under wide variations in measurement and sample conditions. Confirmatory measurements by 2πα gas-flow proportional counting were also performed. The only known radionuclidic impurity, based on α- and photon-emission spectrometry, is a trace quantity of ²⁰⁸Po. The ²⁰⁸Po to ²⁰⁹Po impurity ratio as of the reference time was 0.00124 ±0.00020. All of the above cited uncertainty intervals correspond to a combined standard uncertainty multiplied by a coverage factor of k = 2. Although ²⁰⁹Po is nearly a pure α emitter with only a weak electron capture branch to ²⁰⁹Bi, LS measurements of the ²⁰⁹Po a decay are confounded by an a transition to a 2.3 keV (J^π= 1/2⁻) level in ²⁰⁵Pb which was previously unknown to be a delayed isomeric state.     

36Cl/Cl Accelerator-Mass-Spectrometry Standards: Verification of Their Serial-Dilution-Solution Preparations by Radioactivity Measurements

A consortium of accclerator-mass-spectrometry (AMS) laboratories recently prepared a series of ³⁶Cl/Cl isotopic ratio AMS standards by an eight-step serial gravimetric dilution scheme. Of the resulting nine solutions, only the latter six could be assayed by AMS to confirm the gravimetric dilution factors. This paper provides the results of relative radioactivity measurements on the first four solutions to verify the first three dilution factors. The fourth solution was the only dilution capable of being directly measured by both AMS and radionuclidic metrology of ³⁶Cl, and therefore its assay by radioactivity counting was deemed of considerable importance. Assays were performed by 4πβ⁻ liquid scintillation (LS) counting of gravimetric aliquots of the solutions, with confirmatory measurements by 2πβ⁻ gas-flow proportional counting of gravimetrically-prepared solid sources. The radioactivity measurements on the fourth solution were complex and difficult because of the conflicting combination of a low activity concentration (0.036 Bq · g⁻¹) and high salt content (146 mg NaCl per g of solution). These conditions necessitated independent studies of the ³⁶Cl LS efficiency as a function of NaCl loading in the LS cocktails and of the feasibility of LS counting of precipitated samples, both of which are also reported here. The results of the radioactivity measurements confirmed the dilution factors for the first three solutions to absolute differences of about 1%, and that for the fourth solution to about 1% to 2%. The overall uncertainties for these verification measurements, at a relative three standard deviation uncertainty interval, were of comparable magnitude, i.e., in the range of ±1% to ±2% for the first three solutions and roughly ±3% for the fourth solution.     

Calibration of Electret-Based Integral Radon Monitors Using NIST Polyethylene-Encapsulated 226Ra/222Rn Emanation (PERE) Standards

The recently developed ²²²Rn emanation standards that are based on polyethylene-encapsulated ²²⁶Ra solutions were employed for a first field-measurement application test to demonstrate their efficacy in calibrating passive integral radon monitors. The performance of the capsules was evaluated with respect to the calibration needs of electret ionization chambers (E-PERM^®, Rad Elec Inc.). The encapsulated standards emanate well-characterized and known quantities of ²²²Rn, and were used in two different-sized, relatively-small, accumulation vessels (about 3.6 L and 10 L) which also contained the deployed electret monitors under test. Calculated integral ²²²Rn activities from the capsules over various accumulation times were compared to the averaged electret responses. Evaluations were made with four encapsulated standards ranging in ²²⁶Ra activity from approximately 15 Bq to 540 Bq (with ²²²Rn emanation fractions of 0.888); over accumulation times from 1 d to 33 d; and with four different types of E-PERM detectors that were independently calibrated. The ratio of the electret chamber response E_Rn to the integral ²²²Rn activity I_Rn was constant (within statistical variations) over the variables of the specific capsule used, the accumulation volume, accumulation time, and detector type. The results clearly demonstrated the practicality and suitability of the encapsulated standards for providing a simple and readily-available calibration for those measurement applications. However, the mean ratio E_Rn/I_Rn was approximately 0.91, suggesting a possible systematic bias in the extant E-PERM calibrations. This 9 % systematic difference was verified by an independent test of the E-PERM calibration based on measurements with the NIST radon-in-water standard generator.     

A Compendium on the NIST Radionuclidic Assays of the Massic Activity of 63Ni and 55Fe Solutions Used for an International Intercomparison of Liquid Scintillation Spectrometry Techniques

The National Institute of Standards and Technology recently participated in an international measurement intercomparison for ⁶³Ni and ⁵⁵Fe, which was conducted amongst principal national radionuclidic metrology laboratories. The intercomparison was sponsored by EUROMET, and was primarily intended to evaluate the capabilities of liquid scintillation (LS) spectrometry techniques for standardizing nuclides that decay by low-energy β-emission (like ⁶³Ni) and by low-Z (atomic number) electron capture (like ⁵⁵Fe). The intercomparison findings exhibit a very good agreement for ⁶³Ni amongst the various participating laboratories, including that for NIST, which suggests that the presently invoked LS methodologies are very capable of providing internationally-compatible standardizations for low-energy β-emitters. The results for ⁵⁵Fe are in considerably poorer agreement, and demonstrated the existence of several unresolved problems. It has thus become apparent that there is a need for the various international laboratories to conduct rigorous, systematic evaluations of their LS capabilities in assaying radionuclides that decay by low-Z electron capture.     

Electronic conduction in La-based perovskite-type oxides

A systematic study of La-based perovskite-type oxides from the viewpoint of their electronic conduction properties was performed. LaCo_0.5Ni_0.5O_3±δ was found to be a promising candidate as a replacement for standard metals used in oxide electrodes and wiring that are operated at temperatures up to 1173 K in air because of its high electrical conductivity and stability at high temperatures. LaCo_0.5Ni_0.5O_3±δ exhibits a high conductivity of 1.9 × 10³ S cm⁻¹ at room temperature (R.T.) because of a high carrier concentration n of 2.2 × 10²² cm⁻³ and a small effective mass m∗ of 0.10 m_e. Notably, LaCo_0.5Ni_0.5O_3±δ exhibits this high electrical conductivity from R.T. to 1173 K, and little change in the oxygen content occurs under these conditions. LaCo_0.5Ni_0.5O_3±δ is the most suitable for the fabrication of oxide electrodes and wiring, though La_1−xSr_xCoO_3±δ and La_1−xSr_xMnO_3±δ also exhibit high electronic conductivity at R.T., with maximum electrical conductivities of 4.4 × 10³ S cm⁻¹ for La_0.5Sr_0.5CoO_3±δ and 1.5 × 10³ S cm⁻¹ for La_0.6Sr_0.4MnO_3±δ because oxygen release occurs in La_1−xSr_xCoO_3±δ as elevating temperature and the electrical conductivity of La_0.6Sr_0.4MnO_3±δ slightly decreases at temperatures above 400 K.     

Light Scattering by Commercial Sugar Solutions

Using a direct measure of scattered light, it was found that commercial sugar solutions scatter light predominantly in a forward direction. The scattering at angles less than 30° was as much as one hundred times that at right angles to the incident beam.It was found that the light scattering by commercial sugar solutions is inversely dependent on wavelength to a power of between 2 and 3, and that severe multiple scattering occurs when the turbidity of the solution is larger than 2×10⁻¹cm⁻¹ at 436 mµ. The scattering of commercial sugar solutions is compared with that of highly purified sucrose.A method is discussed that will enable a good approximation of the turbidity of commercial sugar solutions to be made from a single forward scattering measurement at an angle of about 20° with respect to the incident light beam. A correction for scattered light in transmission measurements of these solutions is also introduced.     

Low-cost and fast synthesis of nanoporous silica cryogels for thermal insulation applications

Nanoporous silica cryogels with a high specific surface area of 1095 m² g⁻¹ were fabricated using tert-butyl alcohol as a reaction solvent, via a cost-effective sol–gel process followed by vacuum freeze drying. The total time of cryogel production was reduced markedly to one day. The molar ratio of solvent/precursor, which was varied from 5 to 13, significantly affected the porous structure and thermal insulating properties of the cryogels. The silica cryogels with low densities in the range of 0.08–0.18 g cm⁻³ and thermal conductivities as low as 6.7 mW (m·K)⁻¹ at 100 Pa and 28.3 mW (m·K)⁻¹ at 10⁵ Pa were obtained using this new technique.     

Light alters nociceptive effects of magnetic field shielding in mice: intensity and wavelength considerations

Previous experiments with mice have shown that repeated 1 hour daily exposure to an ambient magnetic field-shielded environment induces analgesia (antinociception). The exposures were carried out in the dark (less than 2.0×10¹⁶ photons s⁻¹ m⁻²) during the mid-light phase of the diurnal cycle. However, if the mice were exposed in the presence of visible light (2.0×10¹⁸ photons s⁻¹ m⁻², 400–750 nm), then the analgesic effects of shielding were eliminated. Here, we show that this effect of light is intensity and wavelength dependent. Introduction of red light (peak at 635 nm) had little or no effect, presumably because mice do not have photoreceptors sensitive to red light above 600 nm in their eyes. By contrast, introduction of ultraviolet light (peak at 405 nm) abolished the effect, presumably because mice do have ultraviolet A receptors. Blue light exposures (peak at 465 nm) of different intensities demonstrate that the effect has an intensity threshold of approximately 12% of the blue light in the housing facility, corresponding to 5×10¹⁶ photons s⁻¹ m⁻² (integral). This intensity is similar to that associated with photoreceptor-based magnetoreception in birds and in mice stimulates photopic/cone vision. Could the detection mechanism that senses ambient magnetic fields in mice be similar to that in bird navigation?     

<Superscript>220</Superscript>Rn as an additional factor of radiation hazard in the Shelter

In 2003–2007, the content of ²¹²Pb (²²⁰Rn daughter product) inside the Shelter was, as a rule, in the range 0.5–5 Bq m⁻³. No seasonal and time dynamics of the ²¹²Pb concentration and no relationship with the technical activity were revealed. At simultaneous sampling of aerosols, the volume activities of ²¹²Pb in the bypass were higher by 1–2 orders of magnitude than in the surrounding medium (local zone). Hence, the sources of ²²⁰Rn emanation, in particular, ²³²U are inside the Shelter. Among 220 samples taken in the bypass, 94% had the activity median aerodynamic diameter of aerosol particles bearing ²²²Rn and ²²⁰Rn daughter products in the range from 0.05 to 0.4 μm. For the Shelter staff members, ²²²Rn and ²²⁰Rn daughter products, and also submicron size of their carriers are negative factors which were not taken into account previously when determining ionizing irradiation doses. The additional inhalation doses can reach tens of percents of the permissible annual dose.     

Standardization of 63Ni by 4πβ Liquid Scintillation Spectrometry With 3H-Standard Efficiency Tracing

The low energy (E_βmax = 66.945 keV ± 0.004 keV) β-emitter ⁶³Ni has become increasingly important in the field of radionuclidic metrology. In addition to having a low β-endpoint energy, the relatively long half-life (101.1 a ± 1.4 a) makes it an appealing standard for such applications. This paper describes the recent preparation and calibration of a new solution Standard Reference Material of ⁶³Ni, SRM 4226C, released by the National Institute of Standards and Technology. The massic activity C_A for these standards was determined using 4πβ liquid scintillation (LS) spectrometry with ³H-standard efficiency tracing using the CIEMAT/NIST method, and is certified as 50.53 kBq ·g⁻¹ ± 0.46 Bq · g⁻¹ at the reference time of 1200 EST August 15, 1995. The uncertainty given is the expanded (coverage factor k = 2 and thus a 2 standard deviation estimate) uncertainty based on the evaluation of 28 different uncertainty components. These components were evaluated on the basis of an exhaustive number (976) of LS counting measurements investigating over 15 variables. Through the study of these variables it was found that LS cocktail water mass fraction and ion concentration play important roles in cocktail stability and consistency of counting results. The results of all of these experiments are discussed.     

Self-Broadening of Carbon Monoxide in the 2 v and 3 v Bands

The self-broadening of carbon monoxide has been measured for the 2 v and 3 v bands with pressures up to 3.5 atmospheres. A grating spectrometer of high resolving power was used for the measurements and the correction for finite slits was small. The corrections varied from 3 to 20 percent for the different conditions of measurement. The half-widths per atmosphere, γ°, decreased from 0.089 cm⁻¹ for |m| = 1 to 0.053 cm⁻¹ for |m| = 21. The half-widths are compared with those obtained by other investigators and it is shown that the results reported in this work fall in between the self-broadening values previously obtained.     

Preparation of macroporous zirconia monoliths from ionic precursors via an epoxide-mediated sol-gel process accompanied by phase separation

Monolithic macroporous zirconia (ZrO₂) derived from ionic precursors has been successfully fabricated via the epoxide-mediated sol-gel route accompanied by phase separation in the presence of propylene oxide (PO) and poly(ethylene oxide) (PEO). The addition of PO used as an acid scavenger mediates the gelation, whereas PEO enhances the polymerization-induced phase separation. The appropriate choice of the starting compositions allows the production of a macroporous zirconia monolith with a porosity of 52.9% and a Brunauer–Emmett–Teller (BET) surface area of 171.9 m² · g⁻¹. The resultant dried gel is amorphous, whereas tetragonal ZrO₂ and monoclinic ZrO₂ are precipitated at 400 and 600 °C, respectively, without spoiling the macroporous morphology. After solvothermal treatment with an ethanol solution of ammonia, tetragonal ZrO₂ monoliths with smooth skeletons and well-defined mesopores can be obtained, and the BET surface area is enhanced to 583.8 m² · g⁻¹.     

Surface force spectroscopic point load measurements and viscoelastic modelling of the micromechanical properties of air flow sensitive hairs of a spider (Cupiennius salei)

The micromechanical properties of spider air flow hair sensilla (trichobothria) were characterized with nanometre resolution using surface force spectroscopy (SFS) under conditions of different constant deflection angular velocities (rad s⁻¹) for hairs 900–950 μm long prior to shortening for measurement purposes. In the range of angular velocities examined (4×10⁻⁴−2.6×10⁻¹ rad s⁻¹), the torque T (Nm) resisting hair motion and its time rate of change (Nm s⁻¹) were found to vary with deflection velocity according to power functions. In this range of angular velocities, the motion of the hair is most accurately captured by a three-parameter solid model, which numerically describes the properties of the hair suspension. A fit of the three-parameter model (3p) to the experimental data yielded the two torsional restoring parameters, S _3p=2.91×10⁻¹¹ Nm rad⁻¹ and =2.77×10⁻¹¹ Nm rad⁻¹ and the damping parameter R _3p=1.46×10⁻¹² Nm s rad⁻¹. For angular velocities larger than 0.05 rad s⁻¹, which are common under natural conditions, a more accurate angular momentum equation was found to be given by a two-parameter Kelvin solid model. For this case, the multiple regression fit yielded S _2p=4.89×10⁻¹¹ Nm rad⁻¹ and R _2p=2.83×10⁻¹⁴ Nm s rad⁻¹ for the model parameters. While the two-parameter model has been used extensively in earlier work primarily at high hair angular velocities, to correctly capture the motion of the hair at both low and high angular velocities it is necessary to employ the three-parameter model. It is suggested that the viscoelastic mechanical properties of the hair suspension work to promote the phasic response behaviour of the sensilla.