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曾美云, 王迪民, 陈燕波, 杨梅, 宋松. 二苯碳酰二肼光度法测定超基性岩石中三氧化二铬的改进[J]. 岩矿测试, 2011, 30(4): 501-504.
引用本文: 曾美云, 王迪民, 陈燕波, 杨梅, 宋松. 二苯碳酰二肼光度法测定超基性岩石中三氧化二铬的改进[J]. 岩矿测试, 2011, 30(4): 501-504.
ZENG Mei-yun, WANG Di-min, CHEN Yan-bo, YANG Mei, SONG Song. Improvement in the Determination of Chromic Oxide in Ultramafic Rocks by Diphenylcarbazide Spectrophotometry[J]. Rock and Mineral Analysis, 2011, 30(4): 501-504.
Citation: ZENG Mei-yun, WANG Di-min, CHEN Yan-bo, YANG Mei, SONG Song. Improvement in the Determination of Chromic Oxide in Ultramafic Rocks by Diphenylcarbazide Spectrophotometry[J]. Rock and Mineral Analysis, 2011, 30(4): 501-504.

二苯碳酰二肼光度法测定超基性岩石中三氧化二铬的改进

Improvement in the Determination of Chromic Oxide in Ultramafic Rocks by Diphenylcarbazide Spectrophotometry

  • 摘要: 二苯碳酰二肼光度法是测定微量Cr(Ⅵ)的行业标准方法,以硫酸作为显色介质,酸度要求严格,显色稳定时间短,体系显色后需在10 min~1 h测定完毕,灵敏度较差。本文对标准方法进行改进,将显色介质由硫酸改为磷酸。结果表明,在H3PO4介质中显色剂与Cr(Ⅵ)反应生成的络合物可稳定3 h,方法相对标准偏差(RSD)≤5.25%,加标回收率为99.2%~102.0%,检出限由标准方法的13.6 μg/g降至3.8 μg/g。建立的方法用于超基性岩标准物质分析,相比于标准方法,稳定性、精密度和准确性均有提高。

     

    Abstract: Diphenylcarbazide Spectrophotometry is a standard method to measure trace Cr (Ⅵ). However, using H2SO4 as the chromogenic medium has limitations such as a strict sulfuric acid concentration, short stability time of 10-60 min and poor sensitivity. An improvement was made to the diphenylcarbazide spectrophotometric method by replacing sulfuric acid with phosphoric acid as the chromogenic medium. Results indicate that the reaction is stable for 3 h in the phosphoric medium, and the detection limit is reduced from 13.6 μg/g to 3.8 μg/g with a recovery factor of 99.2%-102.0% and RSD≤5.25%. Compared with the routine method, the improved method, when applied to ultramafic rock standard materials demonstrates higher stabilization, precision and accuracy.

     

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