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Register a new userA convenient approach to $10^{-12}~g/g$ ICP-MS limits for Th and U in Aurubis electrolytic NA-ESN brand copper
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D.S. Leonard
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Inductively coupled plasma mass spectroscopy is a powerful technique for measuring trace levels of radioactive contaminants, specifically Th and U, in materials for use in construction of low-background rare-event detectors such as double beta decay and dark matter detectors. I describe here a technique for measuring Th and U contamination in copper using direct acid digestion and dilution, without further chemical processing, achieving results comparable to previous work which utilized more complex chemical pre-concentration techniques. A convenient research-oriented analysis environment is described as well. Results are presented for measurements of three samples from the production line of electrolytically-purified, LME (London Metal Exchange) grade A, NA-ESN Aurubis copper. Purified samples showed levels consistent with zero contamination for both elements, while weak but inconclusive indications of contamination were present for the un-purified anode copper. The best limits achieved are near $1cdot 10^{-12}$~g/g (95% CL) for both Th and U measured for copper from the cathode of the purification process.
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Inductively coupled plasma mass (ICP-MS) spectroscopy is widely used for screening materials of low background detectors in dark matter and double beta decay searches due to its high sensitivity to trace $^{238}$U and $^{232}$Th. This work describes a novel co-precipitation approach to measure the amount of $^{238}$U in high-purity copper to sub-ppt level. Such an approach allows the pre-concentration of U and removal of the matrix, by selecting a proper precipitator to co-precipitate with $^{238}$U and using excess ammonia water to separate the uranium hydroxide from copper by forming water-soluble tetra-amminecopper (II). The isotope dilution method and standard addition method were both used to mitigate the matrix effect and cross-check each other. The latter was also used to measure the recovery efficiency of $^{238}$U by using $^{233}$U as the tracer. The method detection limit (MDL) reached $sim$0.1 pg $^{238}$U /g Cu for both methods while the recovery efficiency of uranium robustly remains 65%--85%. Various sources of interference in the ICP-MS analysis were thoroughly evaluated, and the contamination from reagents were found to be the dominant factor that affected the MDL. Further purification will allow significant improvements in the MDL. This co-precipitate approach can be easily extended to measure $^{232}$Th by using $^{229}$Th as the tracer.
New Experiments with Spheres-Gas (NEWS-G) is a dark matter direct detection experiment that will operate at SNOLAB (Canada). Similar to other rare-event searches, the materials used in the detector construction are subject to stringent radiopurity requirements. The detector features a 140-cm diameter proportional counter comprising two hemispheres made from commercially sourced 99.99% pure copper. Such copper is widely used in rare-event searches because it is readily available, there are no long-lived Cu radioisotopes, and levels of non-Cu radiocontaminants are generally low. However, measurements performed with a dedicated 210Po alpha counting method using an XIA detector confirmed a problematic concentration of 210Pb in bulk of the copper. To shield the proportional counters active volume, a low-background electroforming method was adapted to the hemispherical shape to grow a 500-$mu$m thick layer of ultra-radiopure copper to the detectors inner surface. In this paper the process is described, which was prototyped at Pacific Northwest National Laboratory (PNNL), USA, and then conducted at full scale in the Laboratoire Souterrain de Modane in France. The radiopurity of the electroplated copper was assessed through Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Measurements of samples from the first (second) hemisphere give 68% confidence upper limits of <0.58 $mu$Bq/kg (<0.24 $mu$Bq/kg) and <0.26 $mu$Bq/kg (<0.11 $mu$Bq/kg) on the 232Th and 238U contamination levels, respectively. These results are comparable to previously reported measurements of electroformed copper produced for other rare-event searches, which were also found to have low concentration of 210Pb consistent with the background goals of the NEWS-G experiment.
The Jiangmen Underground Neutrino Observatory will build the worlds largest liquid scintillator detector to study neutrinos from various sources. The 20 kt liquid scintillator will be stored in a $sim$600 t acrylic sphere with 35.4 m diameter due to the good light transparency, chemical compatibility and low radioactivity of acrylic. The concentration of U/Th in acrylic is required to be less than 1 ppt (10$^{-12}$ g/g) to achieve a low radioactive background in the fiducial volume of the JUNO detector. The mass production of acrylic has started, and the quality control requires a fast and reliable radioassay on U/Th in acrylic. We have developed a practical method of measuring U/Th in acrylic to sub-ppt level using the Inductively Coupled Plasma Mass Spectrometer (ICP-MS). The U/Th in acrylic can be concentrated by vaporizing acrylic in a class 100 environment, and the residue will be collected and sent to ICP-MS for measuring U/Th. All the other chemical operation is done in a class 100 clean room, and the ICP-MS measurement is done in a class 1000 clean room. The recovery efficiency is studied by adding the natural nonexistent nuclei $^{229}$Th and $^{233}$U as the tracers. The resulting method detection limit (MDL) with 99% confidence can reach 0.02/0.06 pg $^{238}$U/$^{232}$Th /g acrylic with $sim$75% recovery efficiency. This equipment and method can not only be used for the quality control of JUNO acrylic, but also be further optimized for the radioassay on other materials with extremely low radioactivity, such as ultra-pure water and liquid scintillator.
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A new experiment at Fermilab will measure the anomalous magnetic moment of the muon with a precision of 140 parts per billion (ppb). This measurement is motivated by the results of the Brookhaven E821 experiment that were first released more than a decade ago, which reached a precision of 540 ppb. As the corresponding Standard Model predictions have been refined, the experimental and theoretical values have persistently differed by about 3 standard deviations. If the Brookhaven result is confirmed at Fermilab with this improved precision, it will constitute definitive evidence for physics beyond the Standard Model. The experiment observes the muon spin precession frequency in flight in a well-calibrated magnetic field; the improvement in precision will require both 20 times as many recorded muon decay events as in E821 and a reduction by a factor of 3 in the systematic uncertainties. This paper describes the current experimental status as well as the plans for the upgraded magnet, detector and storage ring systems that are being prepared for the start of beam data collection in 2017.
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