Evaluation of the coprecipitation of incompatible trace elements with fluoride during silicate rock dissolution by acid digestion

Yokoyama, T.; Makishima, Akio; Nakamura, Eizo

doi:10.1016/s0009-2541(98)00206-x

Cited by 258 publications

(243 citation statements)

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“…This can cause erroneous determinations of Sm and Nd and subsequent erroneous dating of geological samples. Yokoyama et al (1999) examined three methods for acid digestion of basic rocks and concluded that step heating of digested samples in HClO 4 from 120°C to 190°C is effective in preventing fluoride precipitation. However, granitic and sedimentary rocks have a possibility containing insoluble minerals such as zircon highly resistant to mineral acids (Potts, 1987).…”

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Precise determination of REE for sedimentary reference rocks issued by the Geological Survey of Japan

2005

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In order to obtain precise rare earth element (REE) compositions of sedimentary reference rocks issued by the Geological Survey of Japan (JSd-1, -2, JSl-1, -2, JLk-1), we analyzed their REEs by inductively-coupled plasma mass spectrometry (ICP-MS) using methods employing both acid digestion (HF-HClO 4 ) and carbonate fusion (Na 2 CO 3 -H 3 BO 3 ). Analytical precision of these methods was estimated by analyzing JB-1a and BCR-1 with the same procedure. Analyses of these two reference rocks show good reproducibility and close agreement with compilation values, except for Ho in JB-1a and Tm in BCR-1. CI-normalized REE patterns of JB-1a and BCR-1 compilation values show deviations for Ho and Tm, respectively, from the smooth patterns. Therefore, the compilation values of those elements may be somewhat in error.After acid digestion of JSd-1, -2, JSl-1, -2 and JLk-1, 2-40% of total REEs were remained in the residues, i.e., secondary fluorides and/or undigested minerals. However, subsequent carbonate fusion effectively recovered the remained REEs. Analytical results by this study show relatively good agreement with compilation values, except for Pr, Ho, Er and Tm, and smooth REE patterns normalized to CI-chondrite. The REE patterns of compilation values show anomalous deviations of Pr, Ho Er, and Tm, suggesting that compilation values of these elements may be in errorneous. This study emphasizes that combined method of acid digestion and alkali fusion is an effective method for recovering REEs in sedimentary rocks for bulk REE determination.

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“…However, granitic and sedimentary rocks have a possibility containing insoluble minerals such as zircon highly resistant to mineral acids (Potts, 1987). For these rocks, therefore, the HF-HClO 4 method proposed by Yokoyama et al (1999) is not sufficient for bulk REE determinations.…”

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Precise determination of REE for sedimentary reference rocks issued by the Geological Survey of Japan

2005

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“…However, it does not explain the complex trace element patterns (Fig. 5d), which depend on several parameters including the initial composition of gas condensate, the ability of host-rock elements to dissolve into acidic fluids, and the selective co-precipitation of elements with fluorides (Yokoyama et al, 1999). The depletion of most volatile elements including Pb is not consistent with a simple dilution process, as evidenced by the enrichment in Pd and Tl, but rather suggests that samples formed from an evolved gas, which had lost most of its moderately volatile elements during early stages of condensation.…”

Section: The Low-temperature Fluoride Depositsmentioning

confidence: 97%

Lead isotopes behavior in the fumarolic environment of the Piton de la Fournaise volcano (Réunion Island)

Vlastelić

Staudacher

Deniel

et al. 2013

Geochimica et Cosmochimica Acta

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The recent activity of the Piton de la Fournaise volcano offers a rare opportunity to address the issue of Pb isotope behavior in volcanic fumaroles, as the composition of the degassing source is accurately and precisely known. Gas sublimates formed between 2007 and 2011 at temperature ranging from 400 to ca. 100°C include Na-K sulfate (aphthitalite), Ca-Cu sulfate (e.g., gypsum), Na sulfate (thenardite), Ca-Mg-Al-Fe fluoride (e.g., ralstonite) and native sulfur. The high-temperature deposits show trace element patterns typical of volcanic gas (with Pb concentration up to 836 ppm) while the lowtemperature deposits are depleted in most volatile elements (Pb <1 ppm) with the exception of Pd and Tl (in fluorides) and Se (in native sulfur).Only for low-temperature fluoride samples do Pb isotope compositions plot significantly outside the field of lavas. The isotopic shift is ascribed to leaching ubiquitous unradiogenic phases (e.g., sulfides) by acidic gas condensates. The similarity in Pb isotope signature between lavas and sublimate samples more representative of the gas phase (sulfates) indicates that the net fractionation of Pb isotopes resulting from volatilization and condensation processes is smaller than the precision of Pb isotope measurements (better than 60 ppm/a.m.u.). The absence of net fractionation could result from negligible isotope fractionation during Pb volatilization followed by extensive condensation of gaseous Pb, with possibly significant isotopic fractionation at this stage. Although this scenario has to be refined by more direct measurement of the gas phase, and its general applicability tested, it suggests that a small fraction (<10%) of initially volatilized Pb ultimately escapes to the atmosphere, while the remaining dominant fraction is trapped in sublimates. As sublimates are rapidly dissolved and entrained by runoff, the fumarolic environment appears as a factory efficiently transferring isotopically unfractionated Pb from magmas towards the hydrological system and seawater.Resolving very small isotopic differences between magmas and their gaseous products remains an analytical challenge. High-precision Pb isotope measurements rest not only on instrumental performance but also on high-yield chemistry, as Pb isotopes drastically fractionate (800 ppm/a.m.u.) upon elution on anionic resin. For 50% Pb recovery, the estimated isotopic bias is plus or minus 60-80 ppm/a.m.u., depending on which of the early (isotopically light) or late (isotopically heavy) Pb fraction is lost.

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“…Although minor components, these minerals strongly affect bulk rock chemical composition because of the high abundance of Zr, Hf, and heavy rare earth elements (HREEs). The most widely accepted method for dissolving bulk rock powders is acid digestion (AD) with HF, HNO 3 , and HClO 4 (e.g., Yokoyama et al, 1999). However, acidresistant minerals are insoluble even with the use of Teflon bombs in microwave digestion technique (e.g., Jarvis and Jarvis, 1992;Yu et al, 2001) and fusion of rock powders with alkali flux up to 900°C is often used (e.g., Jarvis and Jarvis, 1992;Yu et al, 2001).…”

Section: Introductionmentioning

confidence: 99%

“…The AD step reduces the amount of the silica fraction, by releasing SiF 4 , so that less Na 2 CO 3 is required for the following fusion step. Fusion of the sample residue ensures decomposition of acid-resistant minerals or minerals that precipitate during AD, such as fluorides (e.g., Yokoyama et al, 1999).…”

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Evaluation of a rapid, effective sample digestion method for trace element analysis of granitoid samples containing acid-resistant minerals: Alkali fusion after acid digestion

2014

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Alkali fusion after acid digestion method (AFAD) was used for determination by ICP-MS of twenty-five trace elements (Rb, Sr, Y, Zr, Nb, Cs, Ba, Hf, Pb, Th, U, and rare earth elements) in four silicate reference materials (JG-1a, JG-2, and JG-3 granitoids and JB-2 basalt) from the Geological Survey of Japan (GSJ). Results were compared with those obtained by acid digestion (AD) method. Our results are in excellent agreement with previously reported data obtained by fusion methods. The reproducibility of replicate analyses is better than 5% (1σ) for all the elements, except Rb, Cs, and Pb in JG-2.Keywords: silicate digestion method, trace element abundance, silicate reference material, alkali fusion INTRODUCTIONAcid-resistant minerals, such as zircon, fluorides and chromite make rocks difficult to dissolve completely, leading to poor bulk rock trace element analysis. Although minor components, these minerals strongly affect bulk rock chemical composition because of the high abundance of Zr, Hf, and heavy rare earth elements (HREEs). The most widely accepted method for dissolving bulk rock powders is acid digestion (AD) with HF, HNO 3 , and HClO 4 (e.g., Yokoyama et al., 1999). However, acidresistant minerals are insoluble even with the use of Teflon bombs in microwave digestion technique (e.g., Jarvis and Jarvis, 1992;Yu et al., 2001) and fusion of rock powders with alkali flux up to 900°C is often used (e.g., Jarvis and Jarvis, 1992;Yu et al., 2001). Fusion methods are subject to matrix-induced instability during analyses owing to increased matrix elements from the flux (e.g., Li, B, C and Na). Pt or zirconium crucibles used for hightemperature fusion are another source of contamination. All these factors must be accounted for a correct application of fusion methods. Roser et al. (2000) proposed a method, referred to as Alkali Fusion after Acid Digestion (AFAD). This method consists of AD with HF-HClO 4 in a Pt-crucible, followed 100 R. Senda et al.ing at progressively increasing temperature up to 160°C (Fig. 1). The total time required to prepare 12 samples by AFAD was ~6 h, including preparations for ICP-QMS analyses. ICP-QMS analysisICP-QMS analysis was performed on an Agilent 7500ce at IFREE/JAMSTEC (Supplementary Table S2) following Nakamura and Chang (2007). Calibration solutions (1, 10, 100, and 1000 pg/g) were prepared by gravimetric serial dilution (Table S1). For AD, the sample solutions were diluted 5,000-30,000 fold with a mixed solution of 2% HNO 3 and 0.1% HF by weight containing 1 ng/mL internal standard 115 In and 209 Bi. To reduce the effects of high C and Na concentrations in the matrix, we used >20,000 fold dilution for AFAD. Calibration solutions for AFAD were prepared by addition of standard solutions to the procedural blank solution prepared with the samples to match the matrix.Although the instrumental conditions were adjusted to maintain the best balance between high sensitivity and low oxide formation, we had to correct for overlaps between the spectra of oxides and hydroxides for some ...

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Evaluation of the coprecipitation of incompatible trace elements with fluoride during silicate rock dissolution by acid digestion

Cited by 258 publications

References 28 publications

Precise determination of REE for sedimentary reference rocks issued by the Geological Survey of Japan

Precise determination of REE for sedimentary reference rocks issued by the Geological Survey of Japan

Lead isotopes behavior in the fumarolic environment of the Piton de la Fournaise volcano (Réunion Island)

Evaluation of a rapid, effective sample digestion method for trace element analysis of granitoid samples containing acid-resistant minerals: Alkali fusion after acid digestion

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