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    离子色谱法测定工业甲酸中4种痕量阴离子

    IC Determination of 4 Trace Anions in Industrial Formic Acid

    • 摘要: 用离子色谱法(IC)测定了工业甲酸中4种痕量阴离子F-、Cl-、NO3-和SO42-。取样品(20.000 g)加入100 g·L-1碳酸钠溶液0.4 mL于水浴上蒸发至干,残渣溶于水中并定容至100 mL作为试液供IC测定。将样品蒸干处理可消除甲酸的基体干扰,加入碳酸钠可避免F-及Cl-以氢氟酸及盐酸形式挥发损失。色谱分离时用IonPacTM AG23保护柱和IonPac AS23分离柱,并用4.5 mmol·L-1碳酸钠-0.8 mmol·L-1碳酸氢钠缓冲溶液作为淋洗液。在所选分析条件下,上述4种阴离子的质量浓度分别在一定范围内与相应峰面积呈线性关系,其检出限(3S/N)依次为0.01,0.02,0.03,0.03 mg·L-1。以实样为基体,用标准加入法进行回收试验,测得回收率在96.2%~106%之间。

       

      Abstract: IC was applied to the determination of 4 trace anions, i.e., F-, Cl-, NO3- and SO42-. The sample (20.000 g) was evaporated to dryness with addition of 0.4 mL of 100 g·L-1 Na2CO3 solution on a water bath, to eliminate matrix interference of HCOOH and to prevent loss of F- and Cl- by volatilization as HF and HCl during evaporation. The residue was taken up with water and its volume was made up to 100 mL for use in IC analysis. The columns of IonPacTM AG23 and IonPac AS23 were used as guarding column and analytical column respectively, and buffer solution of 4.5 mmol·L-1 Na2CO3-0.8 mmol·L-1 NaHCO3 solution was used as eluant in IC separation. Under the optimized condition, linear relationships between values of peak area and mass concentration of the 4 anions in definite ranges were kept, with detection limits (3S/N) of 0.01, 0.02, 0.03, 0.03 mg·L-1 respectively. Using substantial samples as matrixes, recovery was tested by standard addition method, giving results in the range of 96.2% to 106%.

       

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