摘要
目的建立连续流动分析仪同时测定生活饮用水中挥发酚、氰化物、阴离子合成洗涤剂和硫化物的方法。方法采用在线蒸馏,馏出物在碱性铁氰化钾存在下与4-氨基安替比林反应,利用分光光度法测定挥发酚的含量,采用在线蒸馏,馏出物与氯胺-T反应,再与异烟酸-吡唑酮反应生成蓝色化合物,利用分光光度法测定氰化物的含量,在线萃取,利用亚甲蓝分光光度法测定阴离子合成洗涤剂的含量,利用硫离子与N,N-二甲基对苯二胺二盐酸盐反应生成蓝色化合物进行测定硫化物含量。结果挥发酚与氰化物在质量浓度为2~100μg/L时,线性相关系数r≥0.9999,检出限分别为0.2和0.4μg/L,相对标准偏差分别为0.75%~2.80%和0.36%~2.26%,加标回收率为98.0%~103.6%和101.0%~102.0%。阴离子合成洗涤剂与硫化物在质量浓度为20~1000μg/L时,线性相关系数为0.9995和0.9999,检出限分别为4.4和1.6μg/L,相对标准偏差为0.55%~1.08%和0.33%~1.97%,加标回收率为93.6%~95.8%和99.0%~101.9%。与国家标准方法相比,差异无统计学意义(P>0.05)。结论所建立的方法比国标法省时省力、检出限更低、精密度与准确度更好、污染更小,更适于大批量样品的分析测定。
Objective To establish a method for simultaneous determination of volatile phenol,cyanide,anionic synthetic detergent and sulfide in drinking water by continuous flow analyzer.Methods Using on-line distillation,the distillate reacted with 4-aminoantipyrine in the presence of basic potassium ferricyanide,and the content of volatile phenol was determined by spectrophotometry.Using on-line distllation,the distillate reacted with chloramine-T,and then reacted with isonicotinic acid pyrazolone to form blue compounds,the content of cyanide was determined by spectrophotometry.Usingon-line extraction,the content of anionic synthetic detergent was determined by methylene blue spectrophotometry,and sulfide was determined by the reaction of sulfur ion with N,N-dimethyl-p-phenylenediamine dihydrochloride.Results When the mass concentration of volatile phenol and cyanide was 2-100μg/L,the linear correlation coefficients(r)were≥0.9999,and the detection limits were 0.2 and 0.4μg/L respectively,the relative standard deviations were 0.75%-2.80%and 0.36%-2.26%respectively,and the recoveries were 98.0%-103.6%and 101.0%-102.0%respectively.When the mass concentration of anionic synthetic detergent and sulfide was 20-1000μg/L,the linear correlation coefficients were 0.9995 and 0.9999 respectively,and the detection limits were 4.4 and 1.6μg/L respectively,the relative standard deviations were 0.55%-1.08%and 0.33%-1.97%respectively,and the recoveries were 93.6%-95.8%and 99%-101.9%respectively.Compared with the national standard method,the difference was not statistically significant.Conclusion Compared with the national standard method,this method saves time and labor,has lower detection limit,better precision and accuracy,less pollution,and is more suitable for the analysis and determination of large quantitiesof samples.
作者
邹柯婷
巩胜利
赵桂鹏
何丰瑞
程训强
秦国富
ZOU Ke-ting;GONG Sheng-li;ZHAO Gui-peng;HE Feng-rui;CHENG Xun-qiang;QIN Guo-fu(Physical and Chemical Laboratory,Xi'an Center for Disease Control and Prevention,Xi'an Shaanxi,710054,China;Medical Imaging Department,Gansu Provincial Armed Police Corps Hospital,Gansu Lanzhou,730000,China;Shanghai Baozhongying Instrument Co.,Ltd,Shanghai,201108,China)
出处
《职业与健康》
CAS
2023年第6期760-763,768,共5页
Occupation and Health
基金
陕西省重点研发计划项目(2021SF-468)
西安市卫生健康委一般研究项目(2020yb45)。
