【作者】 陆建军；

【导师】 龚琦；

【作者基本信息】 广西大学 ， 应用化学， 2006， 硕士

【摘要】 本文在综述国内外测硼方法的应用和进展基础上，采用微波增压样品处理技术，快速处理土壤样品和柑桔样品，并选择原子吸收光谱法（AAS）直接或间接对硼进行测定。主要就AAS法测硼方法和有效硼提取方法的研究做了如下工作： 1 研究了新铜试剂（NCP）-Cu（Ⅰ）-BF₄^-离子缔合萃取-火焰原子吸收光谱法（FAAS）间接测定柑桔园土壤中的全硼。土壤样品经微波密闭酸消解后，被测元素B形成的BF₄^-与[Cu（NCP）]⁺生成[Cu（NCP）]⁺BF₄^-疏水性离子缔合物，用MIBK萃取，FAAS测定有机相中的铜，间接测定全硼的含量。测定标准样品、人工合成铝、铁、钙和镁样品，得到满意的结果。 2 研究了在微波供能的聚四氟乙烯密闭杯内浸提土壤中有效硼。当微波入射功率为1.36KW时，经0.1MPa／90s，0.2MPa／125s两步程序，浸出硼的量与回流浸提法有良好的相关性（R=0.991）。统计检验表明，置信度为95％时，两方法之间没有显著性差异。本法RSD=3.4％，精密度稍优于回流法，操作简便，节省时间。 3 研究了用涂钯全热解石墨管原子吸收法（GFAAS）测定柑桔中的硼。结果表明，用涂钯热解石墨管测硼，比用一般热解管有更高的分析灵敏度。若再使用1mg/mL氯化钙、2.5mg／mL抗坏血酸和2mg/mL硝酸铵的混合液作为复合化学改进剂，则可以进一步提高测定硼的灵敏度。测定了柑桔果肉、果汁、果皮和果树叶中硼的含量。该方法检出限为0.01μg/mL，回收率=95.8～99.5％，RSD％=3.6～8.1。 4 对平台GFAAS测定柑桔中硼作了探讨，重新优化了GFAAS测定硼更多还原

【Abstract】 On the basis of a review of the application and progress in the methods of determination of Boron in China and abroad, the microwave samples treatment technique under pressure was used for rapid samples treatment and the methods for direct or indirect determination of Boron by atomic absorption spectrometry （AAS） was selected. This research focused on the methods of determination Boron by AAS and extraction of available Boron. The following aspects were investigated in this thesis:The indirect determination of total Boron in the soil of orange plantation by flame atomic absorption spectrometry （FAAS） with Neocuproine- Cu（ Ⅰ ）-BF₄^-was investigated. After the sample was digested by HF, H₃PO₄, H₂SO₄ with microwave, BF₄^- had come into being. The BF₄^- and [Cu（NCP）]⁺ formed a hydrophobic grouping of association molecule, which can be extracted by 4-mothyl-2-pentanone. The amount of total Boron was measured by determination of Copper in the organic phase by FAAS. The results of determination of Boron in standard samples and artificial Aluminum, Iron ,Calcium, Magnesium samples were satisfactory.It was studied that the availible Boron in the soil can be extracted in a closed PTFE cup by microwave energy. The radiation power of microwave was 1.36KW. Both the pressure and the heating time were programmed from 0.10MPa for 90s, and then 0.2MPa for 125s, respectively. The test results of this method were in good agreement with refluxing extraction method. When the confident level was 95%, there was no significant difference between this更多还原