<p>A method has been developed for the trace level quantitation of sulphur as sulphate in silicate minerals using ion chromatography. The success of the method is based on the (i) drastic reduction (~900 times) of sulphate blank in HF used for the digestion of samples and (ii) release of sulphate from insoluble alkaline earth metal sulphates using potassium oxalate solution. Linear range of ion chromatography for the sulphate was established between 1.0 and 10.0&#xa0;mgL<sup>–1</sup> (<i>R</i><sup>2</sup>&#xa0;=&#xa0;0.9994) for the analysis of sulphur as sulphate in quartz and other silicate minerals. Limit of quantification at 10 σ was calculated to be 6&#xa0;mg kg<sup>–1</sup> (as sulphur). Analysis of Silicon 57A-CRM using the developed method resulted in 0.0031&#xa0;±&#xa0;0.0003% m/m of sulphur which is in close agreement with the certified value of 0.003&#xa0;±&#xa0;0.002% m/m, establishing the trueness of the developed method. The method has shown good repeatability (RSD&#xa0;=&#xa0;1.7%) and reproducibility (RSD&#xa0;=&#xa0;9.6%). The developed method was successfully applied for the analysis of sulphur in quartz powders where concentration of sulphur varied from 10 to 60&#xa0;mg kg<sup>–1</sup>. The method was further utilised to analyse sulphur in other geological silicate materials like basalt (BHVO-1, BIR-1) and granite (G2) where, the values of sulphur obtained by the developed method were found to be in close agreement with those published in the literature as suggested by Student’s <i>t</i>-test. The results obtained by the developed method were cross validated with C-S analyser.</p> Graphical abstract <p>The study reports a sensitive ion chromatography–based method for the trace-level quantification of sulphur as SO<sub>4</sub><sup>2–</sup> in silicate minerals. The method involves minimising sulphur blanks in HF and liberating sulphate from samplesusing K<sub>2</sub>C<sub>2</sub>O<sub>4</sub>. The limit of quantification (LOQ) is&#xa0;6&#xa0;mg kg<sup>–1</sup> (as sulphur). The developed method demonstrates high accuracy, repeatability and reproducibility.</p>

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Accurate determination of trace levels of sulphur in silicate minerals by ion-chromatography

  • Lori Rastogi,
  • A Durga Prasad,
  • K Dash

摘要

A method has been developed for the trace level quantitation of sulphur as sulphate in silicate minerals using ion chromatography. The success of the method is based on the (i) drastic reduction (~900 times) of sulphate blank in HF used for the digestion of samples and (ii) release of sulphate from insoluble alkaline earth metal sulphates using potassium oxalate solution. Linear range of ion chromatography for the sulphate was established between 1.0 and 10.0 mgL–1 (R2 = 0.9994) for the analysis of sulphur as sulphate in quartz and other silicate minerals. Limit of quantification at 10 σ was calculated to be 6 mg kg–1 (as sulphur). Analysis of Silicon 57A-CRM using the developed method resulted in 0.0031 ± 0.0003% m/m of sulphur which is in close agreement with the certified value of 0.003 ± 0.002% m/m, establishing the trueness of the developed method. The method has shown good repeatability (RSD = 1.7%) and reproducibility (RSD = 9.6%). The developed method was successfully applied for the analysis of sulphur in quartz powders where concentration of sulphur varied from 10 to 60 mg kg–1. The method was further utilised to analyse sulphur in other geological silicate materials like basalt (BHVO-1, BIR-1) and granite (G2) where, the values of sulphur obtained by the developed method were found to be in close agreement with those published in the literature as suggested by Student’s t-test. The results obtained by the developed method were cross validated with C-S analyser.

Graphical abstract

The study reports a sensitive ion chromatography–based method for the trace-level quantification of sulphur as SO42– in silicate minerals. The method involves minimising sulphur blanks in HF and liberating sulphate from samplesusing K2C2O4. The limit of quantification (LOQ) is 6 mg kg–1 (as sulphur). The developed method demonstrates high accuracy, repeatability and reproducibility.