电感耦合等离子体发射光谱法测定油田水中的硼
Determination of Boron in Oil Field Water by Inductively Coupled Plasma-Atomic Emission Spectrometry
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摘要: 样品经硝酸酸化、滤膜过滤处理后,用电感耦合等离子体发射光谱法直接测定其中硼的含量。通过正交实验优选仪器参数和分析谱线,在选定的波长208.959 nm下,对样品稀释倍数和介质酸种类进行选择,结果表明,硼含量低于10 mg/L的样品不用稀释,高于10 mg/L的样品一般稀释20倍,介质选用硝酸可使测定结果更加准确。对油田水中共存的7种主要金属元素进行了干扰试验,样品中存在20 mg/L的Sr、Ba、Fe,50 mg/L的Mg、Ca,100 mg/L的K,200 mg/L的Na对待测元素的测定没有影响。选取油田水样品进行加标回收试验,方法平均回收率为95.3%~102.0%,精密度(RSD,n=11)为0.43%~0.92%,检出限为0.0020 mg/L。方法简便、快速,结果令人满意,与姜黄素分光光度法比较,克服了分析流程长、使用试剂较多且不易操作的不足。Abstract: Boron in oil field water has been directly determined by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) after sample were treated with nitric acid and filtrated. This method overcomes the problems of spectrophotometry such as long analysis flow, more reagent and difficulty in controlling the chemical procedure. The working parameters and the spectral line were optimized by orthogonal tests. The dilute multiple and acid medium were analyzed using the selected 208.959 nm frequency. The results show that it is not necessary to dilute the sample when the content of B is less than 10 mg/L, and the dilution factor is 20 when B is greater than 10 mg/L. The selected HNO3 as the acid medium, improved the accuracy of the results. The interference tests were carried out for 7 major metals in oil field water. 20 mg/L Sr, Ba and Fe, 50 mg/L Mg and Ca, 100 mg/L K and 200 mg/L Na have no interference for the measurements of the target element. The detection limit of boron was 0.0020 mg/L and the recoveries ranged from 95.3% to 102.0% with a precision in the range of 0.43%~0.92% (RSD, n=11). Compared to the method of curcumin spectrophotometry, this method is simpler and faster and the results are more accurate.