气相色谱-质谱法分析固井水泥浆添加剂中磷酸三丁酯

Determination of TBP in cementing slurry additives by GC-MS

采用气相色谱-质谱法测定固井水泥浆添加剂中磷酸三丁酯(TBP)的含量。选择m/z=99、155和211的麦氏重排离子为特征离子。TBP在0.20g/L^5.13g/L含量范围内,其特征离子丰度与含量呈线性关系,线性方程为:Y=1.05×107 X+1.75×105,相关系数γ2=0.999,方法检出限(S/N=3)0.000073g/L,定量限(S/N=10)0.00024g/L,平均回收率为106.2%~109.2,相对标准偏差为0.36%~1.70%(n=6)。实际应用表明:该方法适用于油田固井水泥浆添加剂中磷酸三丁酯的质控分析。

A method was established for the determination of tributyl phosphate （TBP） in cementing slurry additives by GC-MS. The characteristic ions were chosen at the m/z of 99 ,155 ,and 211 by McLaf-ferty rearrangement. The TBP content range was 0.20-5.13 g/L which had linear relation with the abun-dance of characteristic ions. Thelinear equation of TBP content was Y =1.05 × 107 X＋1.75 × 105 with the correlation coefficient ：γ2 = 0.999. The detection limit and quantification limit were 0.000073 g/L and 0.00024 g/L for TBP ,respectively. The average recovery rate was 106.2 % -109.2 with the relative standard deviation （n=6） of 0.36% -1.70%. The practical application shows the method is suitable for the qualitative control of TBP in cementing slurry additives.