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Volume 172, 1 January 2016, Pages 159–176 Speleothem inclusion-water isotope compositions are a promising new climatic proxy, but their applicability is limited by their low content in water and by analytical challenges. We have developed a precise and accurate isotopic technique that is based on cavity ring-down spectroscopy (CRDS). This method features a newly developed crushing apparatus, a refined sample extraction line, careful evaluation of the water/carbonate adsorption effect. After crushing chipped speleothem in a newly-developed crushing device, released inclusion water is purified and mixed with a limited amount of nitrogen gas in the extraction line for CRDS measurement. We have measured 50–260 nL of inclusion water from 77 to 286 mg of stalagmite deposits sampled from Gyokusen Cave, Okinawa Island, Japan. The small sample size requirement demonstrates that our analytical technique can offer high-resolution inclusion water-based paleoclimate reconstructions. The 1σ reproducibility for different stalagmites ranges from ±0.05 to 0.61‰ for δ18O and ±0.0 to 2.9‰ for δD.

The δD vs. δ18O plot for inclusion water from modern stalagmites is consistent with the local meteoric water line. The 1000 ln α values based on calcite and fluid inclusion measurements from decades-old stalagmites are in agreement with the data from present-day farmed calcite experiment. Combination of coeval carbonate and fluid inclusion data suggests that past temperatures at 9–10 thousand years ago (ka) and 26 ka were 3.4 ± 0.7 °C and 8.2 ± 2.4 °C colder than at present, respectively.Owing to their abundant tracer composition, as well as their absolute chronology and applicability from the Anthropocene to the Pleistocene, speleothems are considered one of the most important natural archives of past climate (Fairchild et al., 2006 and Fairchild and Baker, 2012). The speleothem carbonate oxygen isotope ratio (δ18O) has been used as a proxy for precipitation (e.g., Wang et al., 2001, Wang et al., 2006, Wang et al., 2008, Bar-Matthews et al., 2003, Partin et al., 2007, Cheng et al., 2012, Ayliffe et al., 2013 and Liu et al., 2014) or temperature (e.g., Gascoyne, 1992, Talma and Vogel, 1992, Dorale et al.

, 1998, Lauritzen and Lundberg, 1999, Mangini et al., 2005 and Sundqvist et al., 2013). However, the complex oxygen fractionation processes from the moisture source to the formation of speleothem hinder the quantitative reconstruction of past thermal and hydrological conditions (e.g., McDermott, 2004, Fairchild et al., 2006 and Lachniet, 2009). The oxygen and hydrogen isotopic signatures of speleothem inclusion water in sealed cavities can offer a possibility of paleo temperature estimates and provide direct evidence of past hydrological cycles (e.g., McDermott, 2004).Drip water can be trapped as fluid inclusions in defect intercrystalline spaces during crystallization, and these fluid inclusions constitute 0.01–0.5% of speleothem by weight (Schwarcz et al., 1976 and McDermott et al., 2005). Recent studies have indicated that the isotopic compositions of inclusion water can match those of cave drip water (Dennis et al., 2001, Genty et al., 2002, Fleitmann et al., 2003, Demeny and Siklosy, 2008, van Breukelen et al., 2008, Zhang et al., 2008, Dublyansky and Spotl, 2009, Griffiths et al., 2010, Griffiths et al., 2013 and Labuhn et al., 2015), suggesting that inclusion water may preserve the original isotopic features of paleo-rainwater.

The first attempt at hydroclimatic application was conducted by Schwarcz et al. (1976). Related subsequent studies have been summarized by McDermott (2004) and McDermott et al. (2005). For example, Matthews et al. (2000) used the inclusion water hydrogen stable isotope ratio (δD) to reveal climate-driven changes in the Mediterranean meteoric water cycle over the past 120 thousand years (ka). Fleitmann et al. (2003) used inclusion water δD to clarify different glacial-interglacial moisture sources in Oman. Griffiths et al. (2010) used speleothem inclusion water δ18O and coeval carbonate δ18O data to reconstruct cave temperature and rainfall sequences over the past 12.64 ka in southern Indonesia.Although the importance of speleothem fluid inclusion was recognized in the 1970s (Schwarcz et al., 1976), limitations in the volume of water and the analytical difficulties associated with isotopic measurements hindered subsequent studies. For example, in early labor-intensive studies, water was extracted using a vacuum line and converted to H2 and/or equilibrated with CO2 (Schwarcz et al., 1976, Harmon et al., 1979 and Dennis et al., 2001) for isotope ratio mass spectrometric (IRMS) measurements.

Continuous-flow mass spectrometry combined with pyrolysis at 1400 °C reduced the sample requirement to 0.1–0.2 μL of inclusion water and the measurement time (Vonhof et al., 2006 and Dublyansky and Spotl, 2009). However, water still needs be converted to measurable gases, such as H2 and CO.The molecular conversion step can be avoided by using cavity ring-down spectroscopy (CRDS), a recently developed technique with low instrumental and running costs compared with IRMS methods (e.g., Brand et al., 2009 and Gupta et al., 2009). In CRDS, an infrared laser is used to detect the isotopologues of water molecules, enabling the direct measurement of water δ18O and δD. Newly developed CRDS techniques (Arienzo et al., 2013 and Affolter et al., 2014) or other laser-based spectroscopy techniques (Czuppon et al., 2014) offer a 1σ reproducibility of ±0.4–0.5‰ for δ18O and ±1.5–2.0‰ for δD for 0.4–1.2 μL of inclusion water. However, the requirement for a relatively large volume of inclusion water has hindered the development of a high-temporal-resolution speleothem hydroclimatic record.

In this study, we developed techniques for measuring the δ18O and δD values of speleothem fluid inclusions with a water requirement of only hundreds of nanoliters (nL) by using CRDS methods. This paper describes the new analytical system and techniques in Section 2, their performance evaluation in Section 3.1, and the application of the results to paleoclimate reconstruction in Section 3.2.Our experimental apparatus for water inclusion isotope measurements incorporates a crushing device made of glass and is illustrated schematically in Fig. 1. The apparatus is composed of the following: (1) a device to extract water from carbonate, (2) a dilution apparatus for on-line isotopic measurement, and (3) a CRDS unit. Carbonate was mechanically crushed in a vacuum, and the released water was cryogenically trapped using processes modified from Dennis et al. (2001). The dilution component is an adaptation of a commercially available liquid water evaporator (Picarro Inc. Santa Clara, California, USA) (Gupta et al., 2009).