反相高效液相色谱法测定工业高盐废水中含氟有机酸含量

Determination of content of fluorine-containing organic acids in high salt industrial wastewater by reversed-phase high performance liquid chromatography

提出了反相高效液相色谱法同时测定高盐水体中三氟乙酸、五氟丙酸、七氟丁酸含量的方法,确定部分全氟有机酸很难被重铬酸钾氧化。样品以水作溶剂进行稀释或溶解,色谱柱为SHIM-PACK VP-ODS C18(4.6 mm×150 mm,5μm),以乙腈和40 mmol/L KH_2PO_4(pH=3.0)为流动相进行梯度洗脱,流速为0.6 m L/min,柱温为50℃,检测波长为195 nm。各种含氟有机酸的线性相关系数R≥0.999 2,线性范围为2~1 000μmol/L,方法检出限在0.002~0.01μmol/L之间,回收率在96.2%~109.4%之间。

A reversed-phase high performance liquid chromatography(RP-HPLC） method is developed to determine simultaneously trifluoroacetic acid,pentafluoropropionic acid and heptafluorobutyric acid in high salt wastewater.It is confirmed that some perfluoro organic acids are difficult to get oxidized by potassium dichromate. The sample is diluted or dissolved with water.The test is carried out on a SHIM-PACK VP-ODS C（18） column(4. 6 mm× 150 mm,5 μm） with a column temperature at 50℃. Gradient elution is performed by using a mixture of acetonitrile and 40 mmol·L（-1） KH2PO4(pH= 3. 0） as the mobile phase with a flowing rate of 0. 6 mL·min（-1）.The detection wavelength is set at 195 nm.The linear correlation coefficients for various fluorine-containing organic acids are no less than 0. 999 2. The linear ranges are in 2-1 000 μmol·L（-1） and the detection limit is between 0. 002 and 0. 01 μmol·L（-1）.The recovery rate is in the range of 96. 2%-109. 4%.