应用全自动间断分析仪测定炼油化工废水中挥发酚的含量

Determination of Volatile Phenol in Waste Water of Petro-refinery by the Automatic-Intermittent Analyzer

废水样品250mL,加入100g·L-1硫酸铜溶液5mL,在pH 4.0的条件下进行蒸馏,接收馏上液250mL供测定其中挥发酚的含量,用Clever-chem 200全自动间断分析仪进行测定。测定的原理为分取部分蒸出液与pH 10.3的铁氰化钾及4-氨基-安替比林反应生成红色化合物,在波长510nm处测量其吸光度。测定中试样的进样量为200μL,试剂1及试剂2的加入量依次为90μL和135μL。挥发酚的质量浓度在0.05~2.00mg·L-1范围内与吸光度呈线性关系。方法的检出限(3s/k)为0.005mg·L-1。标准加入法测得方法的回收率在94.7%~108%之间。另在3个含量水平上做精密度试验,测定值的相对标准偏差(n=6)在2.6%~6.3%之间。用此分析仪所得测定值与国标法测定值基本相符。

Waste water sample(250mL)was distilled at pH 4.0in the presence of CuSO4(0.5g),and volatile phenol in an aliquot of the distillate(250 mL)was determined by the Clever-chem 200 analyzer automatically.The color reaction of phenol with alkaline solution of K3Fe(CN)6at pH 10.3(R1)and solution of 4-amino-antipyrine(R2)to form red colored compound withλmaxat 510 nm adopted by the analyzer.An aliquot of200μL of sample solution and 90μL of R1 as well as 135μL of R2 were used in the analyzer.Linearity range for phenol was kept between 0.05 to 2.00mg·L-1,with detection limit(3s/k)of 0.005mg·L-1.Tests for recovery and precision were made by standard addition method,giving values of recovery in the range of 94.7%-108%and RSD′s(n=6)ranged from 2.6%to 6.3%.Analytical results found by the analyzer were in consistency with those found by the GB standard method.