Tetsuya Yokoyama & Eizo Nakamura (2002) Precise determination of ferrous iron in silicate rocks, Geochimica et Cosmochimica Acta, 66, 1085-1093, doi: 10.1016/S0016-7037(01)00809-2. < 20181025122944-742474 > pub

Map on Earth or stone. Places and analyses are shown.

  • abstract:

    We have developed a highly precise method for the determination of ferrous iron (Fe2+) in silicate rocks. Our new method is based on Wilson’s procedure (1955) in which surplus V5+ is used to oxidize Fe2+ into Fe3+ while equivalently reducing V5+ into V4+. Because V4+ is more resistant to atmospheric oxidation than Fe2+, Fe2+ in the sample can be determined by measuring unreacted V5+ by adding excess Fe2+ after sample decomposition and then titrating the unreacted Fe2+ with Cr6+. With our method, which involves conditioning the sample solution with 5 M H2SO4 in a relatively small beaker (7 mL), the oxidation of Fe2+ or V4+ that leads to erroneous results can be completely avoided, even in 100-h sample decompositions at 100°C. We have measured the concentration of FeO in 15 standard silicate rock powders provided by the Geological Survey of Japan (GSJ). Analytical reproducibility was better than 0.5% (1σ) for all but those samples that had small amounts of Fe2+ ( < 1.5 wt.% of FeO). Fourteen of these samples gave FeO contents significantly higher than the GSJ reference values. This likely indicates that the GSJ reference values, obtained by compiling previously published data, contain a large number of poor-quality data obtained by methods with lower recovery of Fe2+ caused by oxidation or insufficient sample decomposition during analyses. To achieve accurate determinations of Fe2+ in our method, several factors besides the oxidation must be considered, including: (1) long-term variations in the concentration of Fe2+ solution must be corrected; (2) excess use of the indicator must be avoided; and (3) the formation of inert FeF+ complex must be avoided during titration when using boric acid as a masking agent.

  • doi: 10.1016/S0016-7037(01)00809-2
  • modified at 17 h ago


(a) Titration_procedures of Yokoyama and Nakamura (2002)
Tixhr 1512897544 thumb JB-1b < 20160921102320-366434 >pub
  • classification: volcanic:basaltic
  • physical-form: powder
  • status: (unknown)
  • description: Geological Survey of Japan silicate reference material - basalt; split 2, position 244
  • modified at 2020-04-24
Img 8252@58452bedef311c2498f872f thumb JB-2 < 20130416090250-887738 >pub
  • classification: volcanic:basaltic
  • physical-form: powder
  • status: (unknown)
  • description: Geological Survey of Japan silicate reference material - tholeiitic basalt from Izu-Oshima, Japan (erupted in 1950 AD); split 7, position 19
  • modified at 2020-05-11
Tixhr1947484362 thumb JB-3 powder < 20170620122529-773001 >pub
  • classification: volcanic:basaltic
  • physical-form: aliquot
  • quantity (g): 1.56
  • description: Geological Survey of Japan silicate reference material - basaltic rock from Mt.Fuji
  • modified at 2020-05-12
Tixhr 173820514 thumb JR-1 powder < 20170620122635-904078 >pub
  • classification: volcanic:rhyolitic
  • physical-form: aliquot
  • quantity (g): 2.61
  • description: Geological Survey of Japan silicate reference material; rhyolite
  • modified at 2020-04-23
Tixhr887022129 thumb JA-2 < 20160921101920-406882 >pub
  • classification: volcanic:andesitic
  • physical-form: powder
  • status: (unknown)
  • description: Geological Survey of Japan silicate reference material; andesite; split 9, position 56
  • modified at 2020-04-24
Tixhr 971257100 thumb JA-3 < 20160921102120-558345 >pub
  • classification: volcanic:andesitic
  • physical-form: powder
  • status: (unknown)
  • description: Geological Survey of Japan silicate reference material; andesite
  • modified at 2020-04-23
Tixhr 854746915 thumb JP-1 < 20190301111946-454924 >pub
  • classification: plutonic:ultramafic
  • physical-form: powder
  • quantity (g): 12.8
  • description: Harzburgite, GSJ; split 10, position 84
  • modified at 2020-04-24
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JA-3_S (Max, 2012) pub ICPMS Thermo-Fisher Neptune 1 20191223153531-773978
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ref-gl-ja3 pub Q-ICPMS Agilent 7500cs 51 20170302124518-005148
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JA-3 powder_TE_Max2006 pub Q-ICPMS Agilent 7500cs 42 20191018155015-993443
JA-3 powder_Li pub ICPMS Yokogawa PMS2000 1 20191015113423-430051
name spots global-id
caption ID assembly stone
Table 2. FeO (wt.%) of GSJ standard rocks pub 20191009135142-150123 FeO (Yokoyama et al., 2002) 7
manual
  • name
  • Tetsuya Yokoyama
  • Eizo Nakamura