电位滴定法测定丁基硼酸的含量

Determination of Butylboronic Acid by Potentiometric Titration

目的:建立一种丁基硼酸起始物料的含量测定检测方法。方法:采用电位滴定法,用氢氧化钠滴定液进行滴定。结果:本方法空白试验溶液消耗滴定液体积为0.000 mL,对供试品滴定终点的判断无干扰,供试品滴定过程中有明显、单一的滴定突跃,专属性良好;重复性试验和中间精密度试验RSD均小于1.0%;在供试品约0.12~0.48 g范围内线性关系良好,r=0.999 9;含量回收率应在98%~101%,6份含量测定结果的RSD小于1.0%,准确度良好;分别对水浴加热时间、水浴温度、双氧水用量、D-甘露醇用量和滴定杯溶液总体积等五个因素各三个水平进行了分析方法的耐用性考察,各组考察因素下三个不同水平含量测定结果的RSD均小于1.0%,耐用性良好。结论:该方法操作简便、准确度好、精密度高、耐用性优良,可用于本品的含量检测。

Purpose:A method for the determination of the content of butylboronic acid starting material was established.Methods:Potentiometric titration was used for titration with sodium hydroxide titration solution.Result:The blank test solution of this method consumes 0.000 mL of titrant,which does not interfere with the judgment of the titration end point of the test product.There is an obvious and single titration jump in the test product titration process,and the specificity is good;the repeatability test and intermediate The RSD of the precision test is less than 1.0%;the linear relationship is good in the range of about 0.12~0.48 g of the test sample,r=0.9999;the content recovery rate should be 98%~101%,and the RSD of 6 content determination results is less than 1.0%,the accuracy was good;the durability of the analytical method was investigated at three levels for five factors,including the heating time of the water bath,the temperature of the water bath,the amount of hydrogen peroxide,the amount of D-manni tol,and the total volume of the titration cup solution.The RSD of the three different levels of assay results are all less than 1.0%,and the durability is good.Conclusion:The method is easy to operate,has good accuracy,high precision and excellent durability,and can be used for the content detection of this product.