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超声浸提-离心分离-钼锑抗分光光度法测定中性及碱性土壤有效磷

Determination of available phosphorus in neutral and alkaline soils by molybdenum-antimony-ascorbic acid spectrophotometry with ultrasonic extraction and centrifugal separation

  • 摘要: 针对中性及碱性土壤有效磷的高通量检测需求,实验建立了超声浸提-离心分离-钼锑抗分光光度联用检测体系。通过优化浸提剂浓度、超声浸提温度和时间、离心分离时间等关键参数,确定了最佳浸提条件。基于钼锑抗显色原理在880 nm波长处建立了校准曲线,校准曲线的线性相关系数为0.999 8,表观摩尔吸光系数为1.75×104 L·mol-1·cm-1。方法检出限为0.34 mg/kg、定量限为1.36 mg/kg。实验方法用于测定4种土壤有效态成分分析标准物质有效磷,测定结果的相对标准偏差(RSD,n=6)为2.5%~8.5%;测定平均值均位于认定值的不确定度范围内,相对误差(RE)为-4.61%~1.33%。按照实验方法测定2个第三次全国土壤普查的典型土壤样品有效磷,回收率为92%~105%;分别采用本法与农业行业标准NY/T 1121.7—2014(样品前处理采用振荡浸提)测定第三次全国土壤普查的典型土壤样品有效磷,两种方法测定结果相一致。相较于标准方法,本体系浸提效率显著提升,为土壤普查等大规模检测任务提供了高效技术支撑。

     

    Abstract: To meet the high-throughput detection demand for available phosphorus in neutral and alkaline soils,a combined detection system integrating ultrasonic extraction,centrifugal separation and molybdenum-antimony-ascorbic acid spectrophotometry was established in this study.The key parameters including extractant concentration,ultrasonic extraction temperature,ultrasonic extraction duration and centrifugal separation time were optimized to determine the optimal extraction conditions.Based on the molybdenum-antimony-ascorbic acid chromogenic principle,the calibration curve was established at a wavelength of 880 nm.The linear correlation coefficient of the calibration curve was 0.999 8,and the apparent molar absorptivity was 1.75×104 L·mol-1·cm-1.The limit of detection(LOD) and limit of quantification(LOQ) of the method were 0.34 mg/kg and 1.36 mg/kg,respectively.The proposed method was applied for the determination of 4 certified reference materials(CRMs) for available nutrient analysis of soil available phosphorus.The relative standard deviations(RSD,n=6) of determination results ranged from 2.5% to 8.5%.The average values all fell within the uncertainty ranges of certified values,with relative errors(RE) of -4.61%-1.33%.The contents of available phosphorus in two typical soil samples from the Third National Soil Survey were determined according to the experimental method,and the recoveries were between 92% and 105%.Moreover,the available phosphorus contents in typical soil samples from the Third National Soil Survey were determined by the proposed method and the agricultural industry standard NY/T 1121.7-2014(the oscillation extraction is adopted for sample pretreatment),and the results of two methods were consistent.Compared with the standard method,this system presented significantly improved extraction efficiency,which provided efficient technical support for large-scale testing tasks such as national soil surveys.

     

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