Determination of Phenol in Hypersaline Groundwater by Continuous Flow Analysis Method
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摘要: 应用连续流动分析法测定氯化物或硝酸盐含量高于0.4g/L的地下水样品中的挥发酚，存在较为严重的基质干扰，在线蒸馏过程中生成了大量的氯化氢和二氧化氮气体，导致冷凝后的馏出液酸性强，造成缓冲溶液失效。另外，当水中含盐量超过0.15%时，蒸馏器管路易堵塞，使该方法无法得到广泛的应用。本文采用3%磷酸二氢钾和3%柠檬酸作为蒸馏试剂，可消除20g/L氯化物和1g/L硝酸盐的干扰。同时采用50%甘油水溶液作为蒸馏试剂溶剂，能够缓解蒸馏器系统管路堵塞的问题，可以测定含盐量低于40g/L的地下水。该方法测定地下水中的挥发酚在0.002~0.100mg/L浓度范围内线性关系良好，相关系数达到0.9999，实际样品的加标回收率为95.2%~104.6%，相对标准偏差（RSD，n=6） < 5%，方法检出限为0.001mg/L，适用于批量测定地下水样中的挥发酚。Abstract:
BACKGROUNDDetermination of phenol by the continuous flow analysis method is seriously compromised if the contents of chlorides or nitrates are greater than 0.4g/L in groundwater. Large amounts of HCl and NO2 during in situ distillation increase the acidity of product after condensation and cause the failure of buffer solution. In addition, distiller pipes can be easily blocked when the salt content is greater than 0.15% in groundwater. Current methods cannot be widely used because of these limitations. OBJECTIVESTo establish an easy and convenient way to detect phenol, especially in groundwater samples with high salt content. METHODSUsing 3% KH2PO4 and 3% citric acid solution as distillation solvents eliminated the interferences caused by chlorides (≤ 20g/L) and nitrates (≤ 1g/L). 50% glycerol used as the solvent of distillation reagent alleviated the pipeline blockage in the distiller. This method can be applied to determine groundwater samples with a salinity content of less than 40g/L. RESULTSThe calibration curve showed good linearity with the correlation coefficient higher than 0.9999 in the range of 0.002-0.100mg/L. The recoveries obtained by adding phenol standards to samples ranged from 95.2% to 104.6%. The relative standard deviation (n=6) was less than 5%. The method detection limit was 0.001mg/L. CONCLUSIONSThe method is suitable for the determination of phenol in high salt groundwater samples. -
Key words:
- groundwater /
- phenol /
- continuous flow analysis /
- sality /
- nitrate /
- acity
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表 1 连续流动分析仪工作参数
Table 1. Parameters of continuous flow analyzer
工作参数 设定值 测量波长 505nm 在线蒸馏器温度 155℃ 取样时间 90s 样品进样速度 1.73mL/min 反应剂进样速度 0.21mL/min 空气间隔时间 2s 分析速率 30样/h 清洗时间 30s 寻峰时段 45~90s 蒸馏试剂进样速度 0.29mL/min 显色剂进样速度 0.21mL/min 流通池 5cm 
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表 2 方法精密度及加标回收实验结果
Table 2. Precision and spiked recovery tests of the method
样品编号 氯离子含量(mg/L) 挥发酚含量(mg/L) RSD(%) 回收率(%) 本底值 加标量 6次测定值 W1 253 0.003 0.010 0.013
0.014
0.0130.012
0.013
00134.88 95.2~104.6 W2 1014 0.006 0.020 0.026
0.027
0.0270.027
0.026
00271.76 100.8~102.7 W3 12248 < 0.002 0.020 0.021
0.020
0.0210.019
0.021
0.0203.59 97.0~101.5
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