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高频红外碳硫仪测定土壤和水系沉积物中的硫实验条件改进

Improvement of Experimental Conditions for the Determination of Sulfur in Soil and Stream Sediments by High-frequency Infrared Carbon and Sulfur Analyzer

  • 摘要: 硫是多目标区域地球化学调查项目中的必测元素。应用高频红外碳硫仪测定样品过程中,由于坩埚空白、管路中水蒸汽、样品称样量、样品和助熔剂叠放顺序、助熔剂添加量等因素影响,导致硫测试值的重复性和准确度差,甚至为负数。本文研究了以上因素对硫测试值重复性和准确度的具体影响以及解决措施,着重对样品称样量、样品和助熔剂叠放顺序、助熔剂添加量进行对比实验,优化出适合分析土壤和水系沉积物中硫含量的最佳条件。结果表明:在降低坩埚空白,严格控制仪器气管中湿度的情况下,采用0.08g样品、0.5g铁和1.0g钨三者混合燃烧的方式分析样品后,其校准曲线线性良好(r ≥ 0.9990)。对不同分析结果采用分段做校准曲线校准,结果对数差△lg为-0.036~0.062,RSD为7.13%~9.93%,两者均符合《多目标区域地球化学调查规范(1:2500000)》(DZ/T 0258-2014)中要求,说明本方法分析结果准确度高、重复性良好。

     

    Abstract:
    BACKGROUNDIn the multi-target regional geochemi-cal survey project, sulfur is one of the analyzed elements. During measurement of samples with a high-frequency infrared carbon-sulfur analyzer, different factors include the blank of the crucible, water vapor in the pipeline, different sample weights, sample and flux stacking order, and different flux additions, which would result in poor reproducibility of sulfur and even a negative value.
    OBJECTIVESTo eliminate factors that affect the repeatability of sulfur analysis and improve the accuracy of sulfur analysis.
    METHODSThe conditions for determination of sulfur in soil-stream sediments were optimized by comparing the sample weight, sample and flux stacking order, and flux amount.
    RESULTSIn the case of reducing the blank value of the crucible and strictly controlling the humidity in the trachea of the instrument, the calibration curve shows a good relationship (r ≥ 0.9990) after the sample was analyzed by mixing 0.08g sample, 0.5g iron and 1.0g tungsten. After analyzing the different results using a calibration curve of the appropriate concentration, the logarithmic differences of the sulfur analysis results are -0.036-0.062 and the relative standard deviations (RSDs) are 7.13%-9.93%.
    CONCLUSIONSBoth the logarithmic difference and the standard deviation meet the requirement of multi-target regional geochemical survey (1:2500000), indicating that the analytical results of this method are accurate and reproducible.

     

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