Utilizing smear mounts for X-ray diffraction as a fully quantitative approach in rapidly characterizing the mineralogy of shale gas reservoirs

Erik O. Munson , Gareth R.L. Chalmers , R. Marc Bustin , Kristal Li
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引用次数: 8

Abstract

X-ray diffraction (XRD) sample preparation methods were compared for fine grained reservoir rocks. The viability of using a hand ground, smear mount method was investigated compared to the widely used micronized, cavity mount method of sample preparation for quantitative phase analysis. Micronizing a sample before analyzing by XRD has been used successfully to reduce the average crystallite size to 10 μm. However, because of the fine grained nature of shale gas reservoirs, the average crystallite size is already below 10 μm. Therefore, the sample only requires disaggregation of larger particles which is easily accomplished by hand grinding. Samples were prepared using smear and cavity mount methods to compare the differences in quantitative phase abundances determined by Rietveld refinement. In addition, samples of known composition were prepared to assess the accuracy and precision of the methods. Quantitative analysis on whole rock samples shows excellent precision between the methods of sample preparation with an absolute error of ±2.25 wt.% at the 95% confidence level per individual phase. Quantitative analysis on artificially prepared samples using the smear mount method shows both excellent precision and accuracy with an absolute error of ±0.9 wt.% at the 95% confidence level per individual phase. A hand ground, smear mount method is therefore a quantitative and viable method for quickly assessing the mineralogy of shale gas reservoirs and fine grained rocks.

利用x射线衍射涂片作为一种完全定量的方法来快速表征页岩气藏的矿物学特征
比较了细粒储层x射线衍射(XRD)样品制备方法。研究了手磨涂片法与广泛使用的微粉腔贴装法进行定量相分析的可行性。在XRD分析前对样品进行微粉化处理,成功地将样品的平均晶粒尺寸减小到10 μm。然而,由于页岩气储层的细粒性,平均晶粒尺寸已经小于10 μm。因此,样品只需要分解较大的颗粒,这很容易通过手工研磨完成。采用涂片法和空腔贴装法制备样品,比较Rietveld精化法测定的定量相丰度的差异。此外,还制备了已知成分的样品,以评估方法的准确性和精密度。对整个岩石样品的定量分析表明,在每个相95%的置信水平上,样品制备方法之间的绝对误差为±2.25 wt.%,具有极好的精度。使用涂片贴装法对人工制备的样品进行定量分析,显示出良好的精密度和准确度,在95%的置信水平下,每个相的绝对误差为±0.9 wt.%。因此,手工地面涂抹法是快速评估页岩气储层和细粒岩石矿物学的一种定量和可行的方法。
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