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Developing a quantitative mudrock calibration for a handheld energy dispersive X-ray fluorescence spectrometer

机译：为手持式能量分散X射线荧光光谱仪开发定量的浑浊校准

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Handheld energy dispersive X-ray fluorescence (hhEDXRF) spectrometers enable rapid and non-destructive means of quantifying the elemental composition of rocks. Advances in hhEDXRF technology have resulted in their widespread usage in the geological sciences. Currently, most popular hhEDXRFs lack lithology-specific calibrations and in turn acquire datasets with high precision but in many cases with unknown or low accuracy. This study derives a methodology to create an internal regression-based mudrock calibration for a hhEDXRF analyzer, with the aim of increasing the analytical quality of elemental data collected from core and outcrop samples. For this study we utilize 64 compositionally diverse Middle Devonian mudrock samples from four cored locations within the central Appalachian basin. Samples were analyzed on both a hhEDXRI and a quantitatively superior bench-top wavelength-dispersive XRF (WDXRF) spectrometer. Utilizing linear regressions, hhEDXRF values were calibrated to the values of the WDXRF for individual elements. Measurements from the two XRF modes record the following coefficients of determination: Zn. Mo, and Ca (r(2) 0.99), Al, K, Ti, Fe, Ni, V, Cu, and Pb (r(2) 0.92), Zr and Si (r(2) 0.78). and Cr (r(2)= 0.56). To assess precision, relative standard deviations (RSD) were calculated for each element based on repeated measurements collected on internal reference samples. All elements recorded RSD values of 8.8%, excluding Cr, which recorded values of 14-25%. Magnesium (Mg), CI, and Ag were below the limit of detection by the hhEDXRF and thus RSD values could not be computed. To assess hhEDXRF accuracy, we propose a novel "iterative blind test" approach, which quantifies accuracy through deriving the percentage difference between the calibrated hhEDXRF value, derived from the blind test, and WDXRF values for each element. Si, Ti, Al, Fe, Ni, Cu. Zn, and Zr record percentage difference values of 10%. For Mn, Ca, Cr, V, Mo and Pb, a minority of samples (13% on average) record concentrations below their reliable detection limit (RDL). Excluding measurements below the RDL, the elements record percent difference values between 6 and 15%. Potassium yielded measurements outside of the RDL and was the only element that returned percentage difference values of 20%, outside of the acceptable limit. The internal mudrock calibration creates high analytical quality datasets for more robust analyses when compared to previous approaches. Published by Elsevier B.V.
机译：手持能量分散X射线荧光（HHEDXRF）光谱仪使得量化岩石元素组成的快速和非破坏性手段。 HHEDXRF技术的进展导致了地质科学的广泛使用。目前，最受欢迎的HHEDXRFS缺乏特定岩性的校准，并反过来获得高精度的数据集，但在许多情况下具有未知或低精度的情况。本研究源于为HHEDXRF分析仪创建基于内部回归的牡蛎校准的方法，目的是提高从核心和露出样本所收集的元素数据的分析质量。对于这项研究，我们利用来自阿巴拉契亚盆地中的四个核心位置的64个合成多样的中间侦探样品。在HHEDXRI和定量高位台压波长分散XRF（WDXRF）光谱仪上分析样品。利用线性回归，HHEDXRF值被校准到WDXRF的值为各个元素。来自两个XRF模式的测量记录了以下确定系数：Zn。 Mo，和Ca（R（2）> 0.99），Al，K，Ti，Fe，Ni，V，Cu和Pb（R（2）> 0.92），Zr和Si（R（2）> 0.78）。和Cr（r（2）= 0.56）。为了评估精确度，基于在内部参考样品上收集的重复测量计算每个元素的相对标准偏差（RSD）。所有元素记录了<8.8％的RSD值，不包括CR，录制值14-25％。镁（Mg），CI和Ag低于HHEDXRF检测限，因此无法计算RSD值。为了评估HHEDXRF精度，我们提出了一种新颖的“迭代盲试验”方法，通过导出校准的HHEDXRF值之间的百分比差异，从盲检测到每个元素的WDXRF值来定量精度。 Si，Ti，Al，Fe，Ni，Cu。 Zn，Zr记录百分比差值<10％。对于Mn，Ca，Cr，V，Mo和Pb，少数样品（平均值<13％）记录浓度低于其可靠检测限（RDL）。在RDL下方排除测量值，该元素在6到15％之间记录差值百分比。钾在RDL之外产生的测量，并且是唯一返回百分比差值> 20％的元素，以外的可接受限制。与以前的方法相比，内部混浊校准会产生高分析质量数据集以进行更强大的分析。由elsevier b.v出版。

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