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Geochemical Journal, Vol. 55 (No. 4), Pp. 209-222, 2021

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Geochemical Journal, Vol. 55 (No. 4), Pp. 209-222, 2021 Geochemical Journal, Vol. 55, pp. 209 to 222, 2021 doi:10.2343/geochemj.2.0630 10Be/9Be ratios of phenakite and beryl measured via direct Cs sputtering: Implications for selecting suitable Be carrier minerals for the measurement of low-level 10Be ATSUNORI NAKAMURA,1* ATSUYUKI OHTA,1 HIROYUKI MATSUZAKI2 and TAKASHI OKAI1 1Geological Survey of Japan, National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba Central 7, 1-1-1 Higashi, Tsukuba, Ibaraki 305-8567, Japan 2Micro Analysis Laboratory, Tandem Accelerator (MALT), The University Museum, The University of Tokyo, 2-11-16, Yayoi, Bunkyo-ku, Tokyo 113-0032, Japan (Received December 23, 2020; Accepted April 29, 2021) Preparing Be carrier solutions with low 10Be/9Be ratios is essential for the applications of in-situ-produced cosmogenic 10Be in geochronology. This is because commercially available Be carriers are non-negligibly contaminated by 10Be. Recently, in-house Be carriers have been successfully applied to samples that contain small amounts of in-situ-produced 10Be. The first step in preparing in-house Be carriers is selecting suitable Be-bearing minerals that contain less 10Be. Here, we present a simple method for selecting appropriate raw minerals for in-house Be carriers. That is, measuring the 10Be/ 9 10 9 Be ratios of Be-bearing minerals by direct Cs sputtering. Analyses of the Be/ Be ratios of phenakite (Be2SiO4) and beryl (Be3Al2Si6O18) obtained from a mineral collection at the Geological Survey of Japan indicate that phenakite gener- ally contains more 10B, interfering isobar of 10Be, than beryl. In addition to the necessity of finding raw materials that contain low 10Be, our results indicate that it is preferable to select a starting material with a low B concentration. Frag- ments of Be-bearing minerals from target samples were directly packed, and showed effective beam currents. Therefore, we anticipate that the direct packing method can also potentially be used to measure 10Be in Be-bearing minerals for geological applications. The measurement background of accelerator mass spectrometry was evaluated using a B-re- moved Be carrier solution. While B is partly adhered to hydroxide gel, we demonstrate that the hydroxide gel wash reduces B in a Be carrier solution. To highlight the 10Be/9Be ratios of Be-bearing minerals against commercially available Be solutions, we also investigated the 10Be/9Be ratios of commercially available Be solutions. Keywords: 10Be, cosmogenic nuclide, phenakite, beryl, beryllium carrier solution measurement of 10Be/9Be ratios using accelerator mass INTRODUCTION spectrometry (AMS). The 10Be concentrations are calcu- Lowering the measurement background of 10Be allows lated from the measured 10Be/9Be ratios and the amount us to broaden its applications in geochronology, and is of added 9Be. If a large amount of 10Be exists in the car- crucial for measuring in-situ-produced 10Be at geologi- rier, this overwrites the 10Be concentrations of the sam- cal settings with small amounts of nuclide accumulation. ples. This phenomenon cannot be corrected accurately by Although several challenges are associated with lower blank subtractions. The propagated uncertainties for 10Be background measures, preparation of in-house Be carrier concentrations in the samples are much smaller when the solutions from Be-bearing minerals has significantly im- 10Be/9Be ratios of the blanks are well below those of the proved the detection limit of measurements (Balco, 2011). samples. Therefore, Be carriers with low 10Be/9Be ratios Commercially available Be (9Be) carriers typically con- are required to measure low-level 10Be concentrations. tain a non-negligible amount of 10Be contamination, and Fortunately, the 10Be component of Be carriers was are, thus, less ideal for analysis (Middleton et al., 1984; recognized early in the development of 10Be analysis us- Bierman et al., 2002; Merchel et al., 2008; Balco, 2011; ing AMS (Middleton et al., 1984). However, in the 1980s Corbett et al., 2016). In laboratory procedures, a known and 1990s, a commercially variable Be carrier was the amount of Be carrier is added to samples to facilitate the only available solution for Be analysis (Balco, 2011). Subsequently, scientists developed a fusion method to prepare an in-house Be carrier from deep-mined beryl *Corresponding author (e-mail: [email protected]) (Stone, 1998) and an HF dissolving method for an in- Copyright © 2021 by The Geochemical Society of Japan. house Be carrier from phenakite (Merchel et al., 2008, 209 2013). For slightly more than a decade, in-house Be car- STUDY DESIGN riers have been successfully applied to samples that con- tain small amounts of in-situ-produced 10Be. These carri- Before presenting the 10Be/9Be ratios of the minerals, ers are used to date rocks with exposure ages of only a we first evaluated the background of AMS at the Micro few hundred years (e.g., Schaefer et al., 2009), to obtain Analysis Laboratory, Tandem accelerator (MALT), the remarkably fast denudation rates on steep landscapes (e.g., University of Tokyo, using an in-house Be carrier pre- Derrieux et al., 2014), to measure muon-produced 10Be pared at Purdue Rare Isotope Measurement (PRIME) labo- at deep depths (e.g., Braucher et al., 2011, 2013), and to ratory, Purdue University. Since preliminary measure- determine burial ages (e.g., Granger et al., 2015). Fur- ments indicated that the carrier contained a considerable thermore, in-house Be carriers have been successfully amount of 10B for measurements at MALT, we repeated used to measure in-situ-produced 10Be at unique settings the hydroxide wash to remove B from the carrier solu- such as the Greenland Ice Sheet Project Two (GISP2) tion. A hydroxide gel wash is a commonly used method bedrock core (Schaefer et al., 2016) and marine sediment to reduce B and other soluble elements from solution (von cores proximal to ice sheets (Bierman et al., 2016; Shakun Blanckenburg et al., 1996; Ochs and Ivy-Ochs, 1997; et al., 2018). Gosse and Phillips, 2001; Simon et al., 2013). However, Before conducting chemical procedures to prepare an to the best of our knowledge, the B reduction rate has not in-house Be carrier, suitable Be-bearing minerals that been reported with actual experimental data. This study contain only trace amounts of 10Be are required as the documents the sequential removal of B and reports the raw material. However, whether the occurrence of such efficiency of the hydroxide gel wash method. We then minerals is rare or common among available Be-bearing analyze the 10Be/9Be ratios of the Be-bearing minerals, minerals remains uncertain. Once the appropriate Be-bear- demonstrating the implications of selecting the appropri- ing minerals are located, Be is extracted from the min- ate minerals for an in-house Be carrier. Finally, we show eral following one of the well-documented procedures the 10Be/9Be ratios of commercial Be carrier solutions and (Stone, 1998; Merchel et al., 2008, 2013). Preliminary discuss possible origins of 10Be in the solutions. measurements of 10Be/9Be from the selected Be-bearing minerals prevents processing whole minerals that yield MATERIALS AND METHODS high 10Be/9Be ratios. In addition to the expense and time- consumption of processing a Be-bearing mineral with high Preparation of in-house Be carrier 10Be/9Be ratios, researchers are spared the difficulty of The ‘low-level Be carrier’ (2017.11.17-Be, bottle extracting from minerals that do not dissolve easily such number 20) was provided by PRIME lab, Purdue Univer- as beryl and phenakite (Langmyhr and Sveen, 1965). Here, sity, and is referred to hereafter as the original carrier. we present the details of 10Be/9Be measurements from Be- The carrier solution was made from phenakite. The con- bearing minerals without chemical treatment as a simple centration of Be was 1074 ± 8 µg/g (e.g., Lesnek et al., pioneer method for selecting appropriate Be-bearing min- 2020) and the recommended value of 10Be/9Be was 5 ± 1 erals. This study is motivated by the research of Merchel × 10–16. We prepared four targets with minimal treatments et al. (2013), who briefly reported a test measurement of to avoid possible contamination. In small quartz vials, untreated phenakite fragments before preparing an in- 300 µg of Be aliquots were evaporated, converted to BeO, house Be carrier solution. Our research revisits the method mixed with Nb at an approximately 1:1 molar ratio, and and provides details of pressing mineral fragments into pressed into Cu cathodes. cathodes and analyzing the resultant beam currents over sputtering time. We selected samples of phenakite and Boron removal from the in-house Be carrier beryl stored in the mineral collection at the Geological The direct evaporation procedure revealed high 10Be/ Museum, Geological Survey of Japan (GSJ), National 9Be ratios of 6–10 × 10–15 due to 7Be tails from the reac- Institute of Advanced Industrial Science and Technology tion of 10B(p,α)7Be (see results sections below). There- (AIST), to demonstrate an appropriate and cautious man- fore, we conducted hydroxide washes to remove B from ner for selecting minerals for in-house Be carrier prepa- the carrier solution. Thirty grams of the original carrier ration. Phenakite (Be2SiO4) is a rare mineral compared (2017.11.17-Be, bottle number 20) was transferred to a to beryl (Be3Al2Si6O18) and is difficult to obtain. How- 50 mL polypropylene tube. The hydroxide precipitate ever, phenakite has the advantage of not containing Al. washing procedure consisted of two stages (Fig. 1). The 26 2+ Given that in-situ-produced Al is often measured along- first wash precipitated Be(OH)2 from the Be solution at 10 side in-situ-produced Be, Al needs to be removed when a pH of 8 after adding 30% NH4OH. This was followed preparing an in-house Be carrier from beryl (Stone, 1998).
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