Improvements in the preparation of phosphate for oxygen isotope analysis from soils and sediments.
Improvements in the preparation of phosphate for oxygen isotope analysis from soils and sediments.
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用于土壤和沉积物氧同位素分析的磷酸盐制备方法的改进
DOI：
10.1371/journal.pone.0204203
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发表时间：
2018
期刊：
影响因子：
3.7
通讯作者：
Yin X
中科院分区：
文献类型：
--
作者：
Xu Z;Huang T;Yin X
相对于从水样中成功制备磷酸盐用于氧同位素分析，从土壤和沉积物中进行类似分析仍存在一系列问题。本文对土壤和沉积物氧同位素分析中磷酸银的制备方法进行了改进和优化。在制备过程中，采用次氯酸钠和XAD-2树脂去除有机物，采用快速微沉淀法和磷酸铵、磷酸镁铵去除单质银及其氧化物杂质。所制备的银磷酸盐对土壤和沉积物中的总有机碳和总氮的去除率分别为0.226±0.033%和0.030±0.0059%（n = 7），0.217±0.053%和0.034±0.0120%（n = 9），对有机物有较高的去除率。我们证实了在快速微沉淀过程中加入柠檬酸会引入元素银杂质，可以通过氨重结晶去除。快速微沉淀的溶液的pH范围被优化为7.0 〜 7.5。X射线衍射和稳定氧同位素分析结果表明，改进后的方法可以从土壤和沉积物样品中获得高纯度的磷酸银，而不需要氧同位素分馏。该方法的改进为利用磷氧同位素研究土壤和湖泊环境中磷的地球化学提供了基础。
In contrast to the successful preparation of phosphate for oxygen isotope analysis from water samples, there are still a series of problems for similar analyses from soils and sediments. Here, we improved and optimized the methods of silver phosphate preparation for oxygen isotope analysis from soils and sediments. During our preparations, organic matter was removed by sodium hypochlorite and XAD-2 resin, while the impurities of elemental silver and its oxide were removed by rapid microprecipitation and ammonium phospho-molybdate and magnesium ammonium phosphate. The total organic carbon and total nitrogen in the prepared silver phosphates from soils and sediments were 0.226±0.033% and 0.030±0.0059% (n = 7), 0.217±0.053% and 0.034±0.0120% (n = 9), respectively, indicating a high removal efficiency of organic matter. We confirmed that adding citric acid during rapid microprecipitation would introduce the impurity of elemental silver, which could be removed by ammonia recrystallization. The pH range of solutions for rapid microprecipitation was optimized at 7.0‒7.5. Results of X-ray Diffraction and stable oxygen isotope analyses showed that the improved method could obtain high pure silver phosphate from soil and sediment samples without oxygen isotope fractionation. This improved procedure provides a foundation for biogeochemical studies on phosphorus in soil and lacustrine environments by using phosphate oxygen isotopes.
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