Published March 2020 | Version v1
Journal article

Quantification of montmorillonite in clay mineral and soil by powder X-ray diffraction/Rietveld refinement

  • 1. Rigaku Corporation, X-ray Instrument Division, Akishima, Tokyo (Japan)
  • 2. Meiji University, Graduate School of Science and Technology, Applied Chemistry Course, Kawasaki, Kanagawa (Japan)
  • 3. Meiji University, School of Science and Technology, Department of Applied Chemistry, Kawasaki, Kanagawa (Japan)

Description

Quantitativity of Rietveld refinement has been evaluated using montmorillonite without the existence a pure material. For Rietveld refinement, the JCSS-3101 clay reference material with the known concentration of montmorillonite and the corundum powder as an internal standard material were added to the waste earthenware and akadama soil as matrix mixed by the V-type mixing machine for 60 min. Quantification values of montmorillonite in the two samples were shown in good agreement with the preparation values. Existence of montmorillonite in the bentonite has been confirmed by preparing the orientated specimens using the ethylene glycol. The fraction of montmorillonite quantified by Rietveld refinement was compared with the result estimated by the calibration curve which was prepared from the integrated intensity of montmorillonite (001) divided by the integrated intensity of corundum (104). The relative error of quantification values between Rietveld refinement and calibration curve method was 1.2%, and their values were shown in good agreement. Quantitativity of Rietveld refinement can be evaluated by using the JCSS-3101 clay reference material with the known concentration of montmorillonite. (author)

Abstract (Japanese)

純物質が存在しないモンモリロナイトを解析対象結晶相として,Rietveld解析による定量性を評価した.マトリックスとしての廃陶器,赤玉土にモンモリロナイト量既知のJCSS-3101参考粘土試料と,内部標準物質としてコランダムを一定量添加した試料に対してRietveld解析を行ったところ,解析値と調製値は良く一致した.なお解析用の試料は,V形混合器で60分間混合して均一な試料とした.ベントナイト中のモンモリロナイトは,エチレングリコールを用いた定方位試料を作製することで含有の有無を確認した.ベントナイト中のモンモリロナイトのRietveld定量値は,モンモリロナイト(001)反射の回折強度を,内部標準物質あるコランダム(104)反射の回折強度で除することで検量線を作成して検証した.Rietveld解析法によるベントナイト中のモンモリロナイト定量値と検量線法による定量値相対誤差は1.2%であり,両者の値はほぼ一致した.モンモリロナイト既知量のJCSS-3101参考粘土試料を用いることで,Rietveld解析の定量性を評価することが可能あった.(著者)

Additional details

Additional titles

Original title (Japanese)
粉末X線回折/Rietveld解析による粘土鉱物・土壌中のモンモリロナイトの定量

Publishing Information

Journal Title
X-sen Bunseki No Shinpo
Journal Volume
51
Series
雑誌名:X線分析の進歩
Journal Page Range
p. 107-117
ISSN
0911-7806

Optional Information

Notes
22 refs., 5 figs., 2 tabs.