Examination of the reliability of X‐ray powder diffraction analysis to determine mineral composition of soils

X‐ray powder diffraction (XRPD) is an effective technique for identifying and quantifying mineral types in soil. However, few studies have compared quantitative values based on XRPD with those from conventional wet chemical methods (WCMs). Here, we determined the primary mineral content in artificia...

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Veröffentlicht in:Soil Science Society of America journal 2024-11, Vol.88 (6), p.1942-1958
Hauptverfasser: Kurokawa, Kohei, Azuma, Kazuki, Nakao, Atsushi, Suzuki, Atsuhito, Wakabayashi, Shokichi, Fujimura, Shigeto, Shinano, Takuro, Yanai, Junta
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container_end_page 1958
container_issue 6
container_start_page 1942
container_title Soil Science Society of America journal
container_volume 88
creator Kurokawa, Kohei
Azuma, Kazuki
Nakao, Atsushi
Suzuki, Atsuhito
Wakabayashi, Shokichi
Fujimura, Shigeto
Shinano, Takuro
Yanai, Junta
description X‐ray powder diffraction (XRPD) is an effective technique for identifying and quantifying mineral types in soil. However, few studies have compared quantitative values based on XRPD with those from conventional wet chemical methods (WCMs). Here, we determined the primary mineral content in artificial mineral mixtures and 79 agricultural soils from across Japan using WCMs and two XRPD‐based quantitative methods: the mineral intensity factor (MIF) and the full‐pattern summation (FPS) methods performed with the powdR package for R. For artificial mixtures, the accuracy of mineral content determination (i.e., micas, quartz, K‐feldspar, and plagioclase) followed the order: WCMs > FPS > MIF. For Japanese agricultural soils, the contents of each mineral were highly similar between WCMs and FPS, based on mean absolute differences and correlation coefficients. Alternatively, MIF displayed lower similarities with WCMs, likely due to preferred orientation and peak shift or overlap issues. Using the FPS method, the mica and amorphous phase contents were positively and significantly correlated with nonexchangeable K content and cation exchange capacity, respectively. Additionally, the plagioclase content was negatively and significantly correlated with clay content. Thus, the powdR‐based FPS method is recommended for determining the mineral composition of soils, as it allows for a clearer and more quantitative demonstration of the relationship between individual minerals and soil properties. Core Ideas Mineral contents were quantified using wet chemical methods (WCMs) and two X‐ray powder diffraction (XRPD)‐based methods. XRPD‐based methods included full‐pattern summation (FPS) and mineral intensity factor (MIF) methods. The accuracy of determining mineral content in artificial mineral mixtures followed the order: WCMs > FPS > MIF. WCMs and FPS yielded highly similar contents of micas, quartz, K‐feldspar, and plagioclase in soils. Precise quantification of individual minerals can reveal close relationships to soil properties. Plain Language Summary X‐ray powder diffraction analysis is the most common method to identify mineralogical variation in soil. However, without proper pretreatment and analysis, only qualitative or at best semi‐quantitative information can be obtained. Therefore, mineralogical variation in soils has often been placed last in the priority order of analytical items. This study aimed to accurately determine mineral contents in agricultural soils by
doi_str_mv 10.1002/saj2.20757
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However, few studies have compared quantitative values based on XRPD with those from conventional wet chemical methods (WCMs). Here, we determined the primary mineral content in artificial mineral mixtures and 79 agricultural soils from across Japan using WCMs and two XRPD‐based quantitative methods: the mineral intensity factor (MIF) and the full‐pattern summation (FPS) methods performed with the powdR package for R. For artificial mixtures, the accuracy of mineral content determination (i.e., micas, quartz, K‐feldspar, and plagioclase) followed the order: WCMs &gt; FPS &gt; MIF. For Japanese agricultural soils, the contents of each mineral were highly similar between WCMs and FPS, based on mean absolute differences and correlation coefficients. Alternatively, MIF displayed lower similarities with WCMs, likely due to preferred orientation and peak shift or overlap issues. Using the FPS method, the mica and amorphous phase contents were positively and significantly correlated with nonexchangeable K content and cation exchange capacity, respectively. Additionally, the plagioclase content was negatively and significantly correlated with clay content. Thus, the powdR‐based FPS method is recommended for determining the mineral composition of soils, as it allows for a clearer and more quantitative demonstration of the relationship between individual minerals and soil properties. Core Ideas Mineral contents were quantified using wet chemical methods (WCMs) and two X‐ray powder diffraction (XRPD)‐based methods. XRPD‐based methods included full‐pattern summation (FPS) and mineral intensity factor (MIF) methods. The accuracy of determining mineral content in artificial mineral mixtures followed the order: WCMs &gt; FPS &gt; MIF. WCMs and FPS yielded highly similar contents of micas, quartz, K‐feldspar, and plagioclase in soils. Precise quantification of individual minerals can reveal close relationships to soil properties. Plain Language Summary X‐ray powder diffraction analysis is the most common method to identify mineralogical variation in soil. However, without proper pretreatment and analysis, only qualitative or at best semi‐quantitative information can be obtained. Therefore, mineralogical variation in soils has often been placed last in the priority order of analytical items. This study aimed to accurately determine mineral contents in agricultural soils by using X‐ray powder diffraction analysis. Full‐pattern fitting method using R package, powdR, was confirmed to be highly useful for this purpose, if we prepared our own mineral library for fitting standards. 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However, few studies have compared quantitative values based on XRPD with those from conventional wet chemical methods (WCMs). Here, we determined the primary mineral content in artificial mineral mixtures and 79 agricultural soils from across Japan using WCMs and two XRPD‐based quantitative methods: the mineral intensity factor (MIF) and the full‐pattern summation (FPS) methods performed with the powdR package for R. For artificial mixtures, the accuracy of mineral content determination (i.e., micas, quartz, K‐feldspar, and plagioclase) followed the order: WCMs &gt; FPS &gt; MIF. For Japanese agricultural soils, the contents of each mineral were highly similar between WCMs and FPS, based on mean absolute differences and correlation coefficients. Alternatively, MIF displayed lower similarities with WCMs, likely due to preferred orientation and peak shift or overlap issues. Using the FPS method, the mica and amorphous phase contents were positively and significantly correlated with nonexchangeable K content and cation exchange capacity, respectively. Additionally, the plagioclase content was negatively and significantly correlated with clay content. Thus, the powdR‐based FPS method is recommended for determining the mineral composition of soils, as it allows for a clearer and more quantitative demonstration of the relationship between individual minerals and soil properties. Core Ideas Mineral contents were quantified using wet chemical methods (WCMs) and two X‐ray powder diffraction (XRPD)‐based methods. XRPD‐based methods included full‐pattern summation (FPS) and mineral intensity factor (MIF) methods. The accuracy of determining mineral content in artificial mineral mixtures followed the order: WCMs &gt; FPS &gt; MIF. WCMs and FPS yielded highly similar contents of micas, quartz, K‐feldspar, and plagioclase in soils. Precise quantification of individual minerals can reveal close relationships to soil properties. Plain Language Summary X‐ray powder diffraction analysis is the most common method to identify mineralogical variation in soil. However, without proper pretreatment and analysis, only qualitative or at best semi‐quantitative information can be obtained. Therefore, mineralogical variation in soils has often been placed last in the priority order of analytical items. This study aimed to accurately determine mineral contents in agricultural soils by using X‐ray powder diffraction analysis. Full‐pattern fitting method using R package, powdR, was confirmed to be highly useful for this purpose, if we prepared our own mineral library for fitting standards. 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However, few studies have compared quantitative values based on XRPD with those from conventional wet chemical methods (WCMs). Here, we determined the primary mineral content in artificial mineral mixtures and 79 agricultural soils from across Japan using WCMs and two XRPD‐based quantitative methods: the mineral intensity factor (MIF) and the full‐pattern summation (FPS) methods performed with the powdR package for R. For artificial mixtures, the accuracy of mineral content determination (i.e., micas, quartz, K‐feldspar, and plagioclase) followed the order: WCMs &gt; FPS &gt; MIF. For Japanese agricultural soils, the contents of each mineral were highly similar between WCMs and FPS, based on mean absolute differences and correlation coefficients. Alternatively, MIF displayed lower similarities with WCMs, likely due to preferred orientation and peak shift or overlap issues. Using the FPS method, the mica and amorphous phase contents were positively and significantly correlated with nonexchangeable K content and cation exchange capacity, respectively. Additionally, the plagioclase content was negatively and significantly correlated with clay content. Thus, the powdR‐based FPS method is recommended for determining the mineral composition of soils, as it allows for a clearer and more quantitative demonstration of the relationship between individual minerals and soil properties. Core Ideas Mineral contents were quantified using wet chemical methods (WCMs) and two X‐ray powder diffraction (XRPD)‐based methods. XRPD‐based methods included full‐pattern summation (FPS) and mineral intensity factor (MIF) methods. The accuracy of determining mineral content in artificial mineral mixtures followed the order: WCMs &gt; FPS &gt; MIF. WCMs and FPS yielded highly similar contents of micas, quartz, K‐feldspar, and plagioclase in soils. Precise quantification of individual minerals can reveal close relationships to soil properties. Plain Language Summary X‐ray powder diffraction analysis is the most common method to identify mineralogical variation in soil. However, without proper pretreatment and analysis, only qualitative or at best semi‐quantitative information can be obtained. Therefore, mineralogical variation in soils has often been placed last in the priority order of analytical items. This study aimed to accurately determine mineral contents in agricultural soils by using X‐ray powder diffraction analysis. Full‐pattern fitting method using R package, powdR, was confirmed to be highly useful for this purpose, if we prepared our own mineral library for fitting standards. 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title Examination of the reliability of X‐ray powder diffraction analysis to determine mineral composition of soils
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