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中国无机分析化学:2024,14(11):1544-1553
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不同消解方式测定土壤中的全硼含量对比
占国艳, 陈淑贤, 梁耀辉, 刘丽丽, 潘晓威
(中国热带农业科学院农产品加工研究所/农业农村部农产品加工质量安全风险评估实验室湛江)
Comparison of different digestion methods for the total boron determination in soil
ZHAN Guo-yan, CHEN Shu-xian, LIANG Yao-hui, LIU Li-li, PAN Xiao-wei
(Agricultural Product Processing Research Institute,Chinese Academy of Tropical Agricultural Sciences / Laboratory of Agricultural Products Processing Quality and Safety Risk Evaluation,Ministry of Agriculture and Rural Affairs,Zhanjiang)
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本文已被:浏览 140次   下载 79
投稿时间:2024-01-20    修订日期:2024-01-31
中文摘要: 针对土壤中全硼测定存在难消解、干扰大、易挥发损失等问题,本工作利用碱熔法、微波消解法以及微敞开石墨消解法对土壤全硼进行了测定分析,优化了消解条件,并对三种消解方式进行了验证对比。结果表明,碱熔剂种类以及用量会对碱熔法的准确性造成较大影响,选择KOH作为碱熔剂,并且KOH添加量为3.0g时,可以获得更准确的结果。加酸种类以及赶酸温度的选择对微波消解法测定结果影响较大,选择加酸体系(5 mLHNO3+1 mLHCl+3 mLHF+1.5 mLH3PO4),赶酸时温度选择170℃,测试效果较好。不同的加酸体系以及消解温度同样会引起微敞开石墨消解法测定结果出现较大误差,选择加酸体系(5 mLHNO3+1 mLHClO4+3 mLHF+1.5 mLH3PO4),消解温度设为170℃,测定结果更可靠。方法验证对比结果表明碱熔法检出限为0.7 mg/kg,微波消解法检出限为0. 9 mg/kg,微敞开石墨消解法检出限为1.0 mg/kg,均满足分析测定的要求。三种消解方式测定的准确度和精密度均符合要求,均可用于土壤全硼的测定,并且实际样品测定结果无显著性差异。三种消解方式优缺点和适用范围不同,实际测试时可以根据样品数量及样品中全硼大致含量等选择具体的消解方式。本工作可以为第三次全国土壤普查内业检测提供参考和借鉴。
Abstract:In view of the problems of difficult digestion, large interference and volatile loss in the determination of total boron in soil, the alkaline melting method, microwave digestion method and micro-open graphite digestion method were used to detect and analyze the total boron in soil. The digestion conditions were optimized, and the three digestion methods were verified and compared. The results show that the types of alkali fusion agent and the amount of alkali fusion have a great impact on the accuracy of the alkali fusion method. When KOH is selected as the alkali fusion agent and the addition amount of KOH added is 3.0g, more accurate results can be obtained. The types of acid addition and the temperature of acid removal process have a major effect on the determination results of microwave digestion method. The optimal test results were obtained with acid addition system (5 mL HNO3 + 1 mL HCI + 3 mL HF + 1.5 mL H3PO4) and removal temperature of 170.Different acid addition systems and digestion temperature also cause large errors in the determination results of micro-open graphite digestion method. When the acid addition system (5 mL HNO3 + 1 mL HClO4 + 3 mL HF + 1.5 mLH3PO4) is selected, and the digestion temperature is set as 170 °C. The determination results are more reliable. The verification and comparison results display that the limit of detection of alkali fusion method is 0.7 mg/kg, the limit of detection of microwave digestion method is 0.9 mg/kg, and the limit of detection of micro-open graphite digestion method is 1.0 mg/kg, which all meet the requirements of determination and analysis. Addition, the results of the three digestion methods exhibit satisfactory accuracy and precision, which can be used for the determination of total boron in soil, and there is no significant difference in the results of actual samples.The advantages and deficiency of the three digestion methods and the scope of application are different. In the actual test, the specific digestion method can be selected according to the number of samples and the approximate content of total boron in the sample. This work can provide reference for The 3rd National Soil Survey.
文章编号:     中图分类号:    文献标志码:
基金项目:海南省自然科学基金(323QN289,321QN0927)
引用文本:
占国艳,陈淑贤,梁耀辉,刘丽丽,潘晓威.不同消解方式测定土壤中的全硼含量对比[J].中国无机分析化学,2024,14(11):1544-1553.
ZHAN Guo-yan,CHEN Shu-xian,LIANG Yao-hui,LIU Li-li,PAN Xiao-wei.Comparison of different digestion methods for the total boron determination in soil[J].Chinese Journal of Inorganic Analytical Chemistry,2024,14(11):1544-1553.

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