为实现水中挥发酚和氰化物的同步检测,建立了基于双通道流路设计的连续流动-分光光度分析方法(以下简称为连续流动分析法),通过优化标准曲线稀释溶液,考察纯水、NaOH(0.01 mol/L)、NaOH(0.02 mol/L)3种介质对检验体系的影响,确定最优稀释溶液参数是NaOH(0.01 mol/L),可实现标准曲线与待测试样的基体匹配,有效校正基体效应干扰,同时对移液管选用、进样与冲洗时间、蠕动泵泵速等条件进行考察优化,结果表明,在最佳实验条件下,采用连续流动分析法同时测定水中挥发酚和氰化物的标准曲线线性关系良好,在0~0.1 mg/L质量浓度范围内线性相关系数均在0.999以上;挥发酚和氰化物方法检出限分别为0.000 46 mg/L和0.000 23 mg/L,最低检测质量浓度分别为0.001 84 mg/L和0.000 92 mg/L,加标回收率介于90.17%~107.09%,经有证水质标准样品验证,相对误差≤0.4%,相对标准偏差≤1.33%,验证了方法具有较好的准确度和精密度,与GB/T 5750系列国标方法相比,本方法氰化物检测较国标方法中最低检测质量浓度下降42.5%,灵敏度显著提升,且具备操作简便、自动化程度高的优势,适用于大批量水样同步检测。

To achieve simultaneous determination of volatile phenols and cyanides in water,a continuous flow spectrophotometric method (hereinafter referred to as continuous flow analysis,CFA) based on a dual-channel flow path design was established.By optimizing the standard curve dilution solution,the effects of three media—pure water,NaOH (0.01 mol/L),and NaOH (0.02 mol/L)—on the detection system were investigated,and the optimal dilution solution was determined to be NaOH (0.01 mol/L),which achieves matrix matching between the standard curve and test samples,effectively correcting matrix interference.Meanwhile,conditions such as pipette selection,sampling and rinsing time,and peristaltic pump speed were optimized.Under optimal experimental conditions,the CFA method showed good linearity for simultaneous determination of volatile phenols and cyanides in water,with correlation coefficients (R²) above 0.999 in the mass concentration range of 0-0.1 mg/L.The method detection limits (MDLs) for volatile phenols and cyanides were 0.000 46 mg/L and 0.000 23 mg/L,respectively,and the minimum detectable mass concentrations were 0.001 84 mg/L and 0.000 92 mg/L,respectively.The spiked recoveries ranged from 90.17% to 107.09%.Validation using certified water quality reference materials showed relative errors ≤0.4% and relative standard deviations (RSD)≤1.33%,confirming the good accuracy and precision of the method.Compared with the GB/T 5750 series of national standard methods,the minimum detectable mass concentration for cyanide was reduced by 42.5%,with significantly improved sensitivity.The proposed method offers the advantages of simple operation and high automation,making it suitable for simultaneous batch analysis of large numbers of water samples.