建立了甘露醇选择性析出硼酸中与B(Ⅲ)等量的H+和pH-NaOH滴定B(Ⅲ)的新方法.系统地研究了难溶解贵金属-硼焊料中B的酸分解及其含量测定的条件.简述了H2SO4 用量与Na盐量的关系及其对滴定的影响.比较了pH电极与指示剂对指示滴定终点的影响.讨论了提高测定B(Ⅲ)的准确度和精密度的条件.结果表明:采用自制简易回流装置,HNO3-H2SO4能完全分解样品中的B,并可避免B(Ⅲ)的挥发损失.于≤2.0mL H2SO4的滴定介质中,近终点NaOH微滴定和pH电极指示终点的方法,提高了滴定终点的敏锐度、分析结果的准确度和精密度.方法特点:分解完全,选择性好,准确度(测定2.00～12.00mg B,相对误差≤±0.50%)和精密度(测定4% B,相对平均误差-0.74%～+0.99%、相对标准偏差0.64%)高,操作简便,适用性强.已应用于B质量分数为1%～12%的难溶贵金属-硼焊料等样品中B的测定,结果满意.
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