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Determination of Water Contents of Granite Melt Inclusions by Confocal Laser Raman Microprobe Spectroscopy

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Determination of Water Contents of Granite Melt Inclusions by Confocal Laser Raman Microprobe Spectroscopy American Mineralogist, Volume 85, pages 868–872, 2000 Determination of water contents of granite melt inclusions by confocal laser Raman microprobe spectroscopy R. THOMAS GeoForschungsZentrum Potsdam, Telegrafenberg B120, D-14473 Potsdam, Germany ABSTRACT A new method of determining the water content of melt inclusions using confocal laser Raman microprobe spectroscopy is described. The water content of melt inclusions can be determined in the concentration range of 0 to 20 wt% with a high spatial resolution (~2 µm). Because the method works in reflection, minimal sample preparation is necessary. The method is fast, has good accuracy and precision (±0.25 wt%), and has the potential to become a useful, high resolution spectroscopic tool for melt inclusion studies. INTRODUCTION and Hofmeister 1988). Chabiron et al. (1999) developed a quan- Water is the most important magmatic volatile. Therefore, titative application of confocal micro-Raman spetrometry in knowledge about the evolution of water contents of melt dur- order to determine the water contents of individual melt inclu- ing magma fractionation processes is key to understanding the sions in a rapid and non-destructive way. This paper shows behavior of volatiles in silicate melts. Melt inclusions provide that water concentrations in quenched melt inclusions can be the best available samples of volatiles in silicate melts. Hence, accurately determined even in very small inclusions having µ valid determinations of volatile constituents is possibly the most diameters as small as 3 m over the entire concentration range significant and useful information obtainable from silicate-melt of interest (0 to 20 wt% H2O). inclusions (Roedder 1984; p. 484). For this, a simple and pre- EXPERIMENTAL AND ANALYTICAL DETAILS cise analytical method is desired. Several analytical techniques A Dilor XY Laser Raman Triple 800 mm spectrometer have been proposed for the determination of H2O in silicate melt inclusions: vacuum extraction, electron microprobe analy- equipped with an Olympus optical microscope and a long dis- × sis (EMPA), ion microprobe analysis (SIMS), and vibrational tance 80 objective was used. Spectra were collected with a spectroscopy including Fourier transform infrared (FTIR) and Peltier cooled CCD detector. The 514 nm line of a Coherent + Raman spectroscopy. A concise description of each technique Ar Laser Model Innova 70-3 and a power of 150 mW of the along with a discussion of their advantages and disadvantages argon laser were used for sample excitation. The confocal tech- are given by Ihinger et al. (1994). Most of these methods are nique provides an efficient way to obtain interference-free easily applied to large melt inclusions in minerals such as quartz, Raman spectra of small specimens embedded in a transparent feldspar, and topaz from extrusive rocks with low to moderate matrix. The derived empirical calibration curves for determin- water contents. However, for analysis of melt inclusions in ing water concentrations are only applicable to the instrument minerals from intrusive rocks there are some limitations: in- used in this study. A similar calibration procedure is necessary clusions are often smaller than 30 µm in diameter and there- for each particular instrument. fore difficult to analyze by SIMS methods. Furthermore, melt Figure 1 shows the Raman spectrum of a H2O-rich pegma- inclusions from intrusive rocks often crystallize daughter crys- tite glass collected at room temperature. The low-frequency tals during cooling, so the inclusions must be rehomogenized region is characterized by an asymmetric broad band in the –1 and quenched to a homogeneous glass before analysis. FTIR spec- 490 cm region which predominantly results from oxygen troscopy has the disadvantage that during the rehomogenization motions in the T-O-T symmetric stretching mode, where T rep- procedure the mineral host of the inclusions becomes brittle and resents tetrahedrally coordinated Si or Al (see Matson et al. it is difficult or impossible to prepare doubly polished thin sec- 1986; Sharma et al. 1997). Additional bands in the low-fre- –1 tions for FTIR measurements. The SIMS method may fail at quency region include symmetric bands near 800 and 920 cm , –1 high water concentrations above about 10 wt% in glasses of and a broad asymmetric band at 1100 cm with a shoulder to- –1 granitic to pegmatitic composition because of the dominance ward lower frequency at about 1020 cm . According to Mysen et al. (1997), appearance of the strong band near 900 cm–1 re- of mobile molecular H2O (see also Ihinger et al. 1994). In con- trast, micro-Raman spectroscopy has proved extremely useful sults from increasing amounts of H2O in the glasses. for samples of only a few micrometers in size (see McMillan The H-O-H bending vibration of molecular H2O dissolved in the glass is indicated by the presence of a weak peak near 1630 cm–1 (see McMillan 1994). However, a relationship be- tween the total water content in glass, the intensity of this peak, *E-mail: [email protected] and the observed shift of the peak position (∆ ~ 30 cm–1) could 0003-004X/00/0506–868$05.00 868 THOMAS: DETERMINATION OF WATER CONTENTS BY RAMAN SPECTROSCOPY 869 FIGURE 1. Raman spectrum of a melt inclusion in pegmatite quartz from Ehrenfriedersdorf- Erzgebirge. The inclusion was rehomogenized at a temperature of 650 °C and a pressure of 1 kbar using the conventional hydrothermal rapid-quench technique. The run duration was 96 hours. The water content of the glass is 10 wt%. The partial spectrum on the right side shows the changed intensity and the new formed band near 3650 cm–1 after heat treatment of an identical inclusion. not be positively established. According to Stolper (1982) this because a larger scattering of the integral intensity with H2O- discrepancy is most probably due to the relative insensitivity concentration was observed during the calibration procedure. of Raman spectroscopy for detection of molecular water. The This may be a result of the strong asymmetry of the 3550 cm–1 high-frequency region (3000–4000 cm–1) of the unpolarized band (see Fig. 1) caused by contributions from a number of Raman spectrum is characterized by an asymmetric OH stretch species (e.g., OH, Si-OH, Al-OH, H2O, etc.). These species band centered at 3550 cm–1 with a tail to lower frequencies, an may have different cross-sections which could lead to more obvious broad shoulder maximized near 3290 cm–1, and typi- scatter in the integral intensity of the fundamental OH-stretch- cally a shoulder or sharp band at 3630 cm–1 (Fig. 1). The breadth ing peak at ~3550 cm–1 (see Pandya et al. 1992). Before and and asymmetry of the band at 3550 cm–1 reflects contributions after each measurement, the optical configuration was verified from both molecular water and other OH-containing species using a large, totally homogenized melt inclusion of known (Pandya et al. 1992). Gaussian deconvolution (e.g., Mysen et H2O content (10 wt%) as a standard. Verifying the intensities al. 1997) reveals that this peak may be the result of three main is important, because it is necessary to use exactly the same –1 bands at 3350, 3500, and 3575 cm , and an additional weak experimental conditions for all H2O determinations. A varia- band around 3640 cm–1. The presence of a weak 3640 cm–1 tion of the intensity of 2.3% (1σ) as the relative standard de- band was confirmed in spectra collected from silica glasses viation was obtained from 25 measurements at different focal having high water contents (i.e., > 10 wt%). At very high bulk depths in the standard melt inclusion. water contents (> 20 wt%) molecular H2O becomes the most dominant species as shown by a shift of the very strong main band in the direction of the molecular water position ν1 (see Ihinger et al. 1994) now centered at 3450 cm–1. This is shown in the spectra in Figure 2 obtained from a 4-phase melt inclu- sion containing two silicate melts, a fluid phase and a vapor bubble (see Thomas et al. 2000). The composition of such an extremely H2O-rich silicate melt is given below. In this case the Raman spectrum is also characterized by a strong peak cen- tered at 1642 cm–1. There are two methods for water determination in glass with the micro-Raman spectrometry. Both methods work in reflec- tion and can be applied to very small sample volumes depend- ing on the optical characteristics of the spectrometer. In the first method, the linear relationship between the H2O content of silicate glass and the intensity of the asymmetric OH stretch band centered at 3550 cm–1 is utilized (see also Stolper 1982). The intensity at the 3550 cm–1 position was ana- lyzed with a single spectral window. The acquisition time was 200 s, and 3 accumulations were used in each case. The baseline FIGURE 2. Three Raman spectra from a silicate melt inclusion in correction was performed with a first-degree polynomal. With pegmatite quartz: melt 1 (silicate-rich, water-poor melt), melt 2 (water- this method, the peak height was used instead of the peak area, rich silicate melt), and an aqueous solution. 870 THOMAS: DETERMINATION OF WATER CONTENTS BY RAMAN SPECTROSCOPY In the second method, the ratio of the 3550 cm–1 band inten- The highest quality spectra are obtained from an excitation sity and the intensity at 490 cm–1 attributed to a delocalized volume that is near the polished surface of the melt inclusion. vibrational mode involving the symmetric stretching of bridg- The Raman signal from depths >10 µm beneath the surface is ing O atoms in T-O-T linkages (Matson at al. 1986) is used. significantly reduced and a correction procedure must be ap- Applying the ratio method eliminates sampling problems and plied.
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