[1]刘晓铮,许成君.全自动消解-ICP-OES法测定含油污水中9种金属[J].中国给水排水,2021,37(10):164.
LIU Xiao-zheng,XU Cheng-jun.Determination of Nine Metal Elements in Oily Wastewater by ICP-OES with Automatic Digestion[J].China Water & Wastewater,2021,37(10):164.
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LIU Xiao-zheng,XU Cheng-jun.Determination of Nine Metal Elements in Oily Wastewater by ICP-OES with Automatic Digestion[J].China Water & Wastewater,2021,37(10):164.
全自动消解-ICP-OES法测定含油污水中9种金属
中国给水排水[ISSN:1000-4062/CN:12-1073/TU]
卷:
第37卷
期数:
2021年第10期
页码:
164
栏目:
出版日期:
2021-05-17
- Title:
- Determination of Nine Metal Elements in Oily Wastewater by ICP-OES with Automatic Digestion
- 摘要:
- 针对采油厂排放的污水中有时含油,造成前处理和检测都较为困难的情况,设计出一套样品前处理程序和检测方法。含油污水经全自动消解仪处理,升温程序为:25 mL水样,加入3 mL纯HNO3,120 ℃加热30 min;提升消解管,冷却10 min;加入3 mL纯HClO4,升温到150 ℃加热30 min;提升消解管,冷却10 min;升温到160 ℃加热至近干;冷却后采用1%HNO3定容至25 mL。经处理后的水样进行电感耦合等离子体发射光谱法(ICP-OES)分析,检测波长206.2~357.9 nm,观测方式:总钡为径向,其余元素为轴向,发射功率为1 500 W。结果表明,铜、锌、铅、镉、镍、铁、锰、铬、钡9种金属元素在0.00~1.00 mg/L范围内线性关系较好,所有元素r>0.995,该方法检出限范围是0.003~0.062 mg/L,实际含油污水样品的加标回收率为84.2%~113.2%,相对标准偏差(RSD)为0.49%~2.86%。该方法对人体伤害小,操作简单,准确度和精密度都较高,可用于含油污水中的9种金属元素浓度的测定。
- Abstract:
- Wastewater discharged from oil production plant sometimes contains oil, which makes it difficult to be pre-treated and detected. A set of sample pretreatment procedures and detection method were thus designed. The oil-containing wastewater was treated by an automatic digester. The temperature rising procedure was as follows: collecting 25 mL water sample, adding 3 mL pure HNO3 and heating the sample at 120 ℃ for 30 min; lifting the digestion tube and cooling it for 10 min; adding 3 mL pure HClO4 at 150 ℃ and heating it for 30 min; lifting the digestion tube and cooling it for 10 min; heating the sample to 160 ℃ near completely dry; after cooling, using 1% HNO3 to fix the volume to 25 mL. The treated water samples were analyzed by inductively coupled plasma emission spectrometry (ICP-OES) with detection wavelength between 206.2-357.9 nm. The observation method was as follows: radial of total barium, axial of other elements and the emission power of 1 500 W. The results showed that the linear relationship of 9 metal elements (copper, zinc, lead, cadmium, nickel, iron, manganese, chromium and barium) was good in the range of 0.00-1.00 mg/L. The value of r was larger than 0.995, detection limit was 0.003-0.062 mg/L, the recovery rate of oilcontaining wastewater sample was 84.2%-113.2% and relative standard deviation (RSD) was 0.49%-2.86%. The method has the advantages of little harm to human body, simple operation, high accuracy and precision, which can be used for the determination of 9 metal elements in oily wastewater.
更新日期/Last Update:
2021-05-17